■<* Copy no. National Research Council of Canada WAR HISTORY OF DIVISION OF CHEMISTRY 2> . ^^3 OTTAWA C'dU^^^ Page PREFACE 1 Ao HISTORICAL INTRODUCTION 4 Bo INORGANIC CHEMISTRY AuOulXC ilineX^^^o oooocopeooooeoeoeoooaooooooooocoooeo A.\J X\OX X^cLC u OX^l 6 9 o oeooeooooooooeoooaooooeoboooooeaooeoo JLO rxQ CO Vdl^^ OX rrLEL^riO SlSlooOOOOOOoo<>cooo*«oegceoeoeoooo Ml ju£L§n6 SlUlUo ooooooccouocooaooooeoooooooaeooeoooooooo i,\f X\6CO VOl^jr OX AXVUlHrioL ooooeoooooooocoooQoooooeooooooo 'wO Drying Air for Blast Furnace Uaeo «. «.«o «.•<,.. o o o » o 24 Utilization of Open Hearth Slag^ .. , , o . o . » o o » « o . « o » • 25 VanaCLlUin lieCOVeryo eooaoeooooe90coeeooeoo*eoooooooo ^ I Nickel, Copper,, and Platinum Metals* o<,... c «»• o o o o o 28 AwUlOSpnenC X^OXJLUuXOno eocooeoooceoocioe*eooeooscuoo ti\f onarcoax. x or i* ixse r^owcier o oeoooo(>«oooooo«ooooeeooee <^x X/eXCXng anCl UeXrOSuXngo ooeooooeenoooooooooeoeeoooo 00 Rain Repellents for Aircraft VifindowSo » . . • » o o o o « » « . 37 Analytical Laboratoryo oooooe oo.e«oo.c*oooo.oo 40 •3i*X Vtt^vJ Oknoai/oeocccooeooeooosoocoaoAoeooaeoeoaaono 4x Miscellaneous Inorganic Investigations^ o o « . » » « o «, o « 41 Review of Foreign Research Organizations ooooo 44 nepOruS anCl * auenuS© ooooooeoo««o»oooeoaooeooeooeon 40 Co ORGANIC CHEMISTRY Experimental Explosives Ejstablishmento , . . o . « . » » . » » 54 £< wnyXene UXIUO oooec«eooee«*e«eo«noeoooeeeooo«ee*ee OO J-i \J llcl n O XcXulX no 9ooooooe'^ooeo«o**eo««ooe*oo«o*«o«rooo« OO Free Radical Reactions „ » . « » . o » 60 ^UDuer eoeoooooeeeoooe«ne«uo»«**»*««ae»b«»oooeeo«ee OVJ iiUDDer LrOOClSo ooenoo«oeooo**ooeo«e«eooonoocoooooooe OO *JLclOuXCOoC'Ooooc>oeeoooeooo«eoe«*e»o«oonooooooeoo««o Oi Lubricating Grease - Fundamental Studies, •» o . o ». o . 70 i% -i- M\.tx XC/XCLSoooenooonorooooo*a**ooeoooovooooor'uo*oooo l\J MXCrO V^rganXC ivnaxySlSo ooeooeooeeeooeeooo&oaoooeoo ( JL ^ w CX X^ V XI eooooocooooocoecoooooooaaooobooouoooeoeooooe iJL AWCXuooooftoof^^oooooootiooccocoooooooooooooevoooooooo f ^ Miscellaneous Organic Investigations. .. o» o » c • o . o « o 74 X\6pOr vS a nCl ^ a wenuSo oorooo«n«oei>oo*ooeouuobooeoooo If Page Do PROTECTION OP PERSONNEL AND EQUIPMENT Specifications, Testing and Test MethodSo o o o o o » o o 93 X \S J^ u.LJLO£>oooeoooooeooooooooeoooe«oooeooooooooooooo %P jt Leather and Allied Products. o o » » o » o o o o o o » o o o o c » o « 105 \J\)i X OOJ.OXI0 ooocoooooooouoooeocouoooooooooooooooeoo X,\J I "rOteCulVe OOaulngSa ooocoouocoooouoo«oooooonceooo 111 Treatment for "Trench Mouth" o « o « » o » » » « o 0 o o <> o o o . o « 115 Miscellaneous Investigationso o o o » « o . » o o ., o o c o o o o o o 117 X\v3pOX uSoounooeoocooaoooeooooooooooosoooov 00000000 X XO Eo CHEMICAL WAIiFARE Evolution of Organization within Chemistry Division^ National Research Councilo » 0 o . c o o 0 » c o 129 r\"3pXXcXuOA3oneoeoooooooo<'Ooooeooooeoooooooooooooo XOm Carbon Monoxide Container Development* o o .. o o 00 « o « 134 X U^X C OLmS>ueLXiCvOoooooneoooro«»*ooooei>o«oooooooooo ^O I Ventilation and Anti-Gas Protection in Armoured JL CXXiJ\0 ouoooooooooooootceoocouoooncooo^oooooouoou ^0«7 Combustion Products of Plame-ThrowerSo o » o » « » e o o » « 141 Analysis of Air for Toxic P\ime3„ « . o o o » o o o o o » » o » o « 142 Miniature Incendiary Bombs » c o o . « . 0 . o o o » » . o » » o o » c o 143 Anti-Gas Fabrics and Clothing* o « . c * o . . o « o o . 144 Protective Coatings* •o*o0««oooo«aoobebeo*oooeoooo 150 Po APPENDIX Miscellaneous Papers* ooooeoe«e**oooo*oooeoooeooDo 152 S9 •301 . .01 . ill 5X1 5^1 j3I <, .. Iioni/oO r^Gi PREFACE The scope and extent of the war-time activities of the Division of Chemistry were such that an all inclusive re- port would have been beyond the practical limits of this vol- ume. Details of extensive and valuable work of a more or less routine nature havep therefore, been omitted from this account, except for passing mention. Nor is it possible here to discuss the considerable contributions which members of the staff have made in administering the work of various Associate Committees of the National Research Council. Discussion of work done for the Associate Committees has been confined for the most part to actual experimental investigations carried out in the Di- visional laboratories. The tremendously valuable work of these various Associate Committees is to be treated extensively in another volume. It is perhaps well to warn the reader that the im- portance or value of any project is not to be inferred from the space devoted to it in this History© Work which has been adequately described by publication in the literature has been treated very briefly here; whereas work idiich has not been published is treated much more extensively© The primary purpose of this volume is to give the technical reader an informative summary of the contribution made by the Division of Chemistry during the period of the Second World War. It is also the purpose of this volur^e to guide those interested to more detailed sources of information. To this end a rather extensive bibliography of publications, internal reports, and patents has been included. It has been the policy to include references which describe work done dur- ing the period of the war, regardless of the actual date of publication or issue. It might here be mentioned, paren- thetically, that work done after VJ-day has sometimes been included when it served to complete an Investigation previously started, or to show the significance and value of previous worko The publications listed in the bibliography are be- lieved to be a complete record of all publications, descrip- tive of war-time work, published prior to June 15, 1946, ex- cept for a few minor articles of no particular scientific Interest which were published In some of the trade journals. The patent references are believed to include all patent ap- plications covering war-time inventions in the Division of Chemistry filed in Canada and the United States prior to June 15, 1946. The patent number and date of issue are given, when these are known, otherwise the application number and date of .;if-l4 ^.---j filing are giveno It should b© noted that the Council has no direct knowledge of issue of a patent when the patent • rights have been assigned before the patent issues© There- fore absence of a patent number is not to be considered as evidence that the patent has not yet issued^, for.o indeed^ many of these applications actually have issuedo This bib- liography is not intended as a record of the Research Council *s patent position, but rather as a record of the work done in the laboratories j as the Canadian and United States applications give adequate disclosures in this respect,, United Kingdom and foreign patent applications and patents have not been listed© More than ten thousand reports were issued by the Division of Chemistry during the war years,. Obviously^, it has been possible to include only a few of them in this bi- bliographyo An effort has been made to include the more important reports covering investigations not recorded else- where andj in general, to include enough reports to serve as examples of the work of the various laboratories o Some- times reports on typical investigations have been included in the bibliography even though that work is not specifically referred to in the textj and conversely work is sometimes referred to in the text for which no report references are giveno Anything like a completely consistent record with respect to reports would be a task of Impracticable magnitude, and such completeness has not been attemptedo In arranging the bibliographies an effort has been made„ in so far as possible., to list the references in the order in which their subject matter is discussed in the preceding texto A few miscellaneous publications which could not conveniently be classified have been grouped together as an appendixo A final work regarding the arrangement of this History may be in ordero No one method of classifying the material was entirely without faults,, but it was found most expedient to classify the work of the various laboratories according to the nature of the worko Thus there are chapters on Chemical Warfare (both offensive and defensive), and on Protection of Personnel and Equipment (including fields such as textiles, corrosion, and protective coatings)o These two chapters deal entirely with specific applications of chem- istry to the problems of waro Other work was classified either as Inorganic or as Organic Chemistry., depending on the composition of the principal substance involvedo While these two chapters also include direct applications of chem- istry to war problems, they tend somewhat more towards the "'^'■"^ B'fi i' r -r I I J - 2I10W c) j f p p_ r -iT •^•'v ,=> 7 "^c } rj ^-T ebf/" '>,-> ©rf yi'::' e js c. eOi ;/ot: «r-, •■ ■ t C:he President of the National Research Council as its chairman, "to receive and suggest research problems, to coordinate the available research f acilities, to assess the relative im- portance of the problems to be dealt with, and to allocate these problems to the various laboratories"* In view of the fact that these are specific functions of the National Re- search Council and that the Council already had facilities for effectively discharging these functions. It was decided not to appoint a committee with such executive powers, but to d evelop the services of the Council in every way that seemed appropriate, in receiving proposals for research^ and In ensuring that such work was undertaken in those labora- tories where it could be most effectively prosecuted j and, to this end, it was decided that the Assisted Researches Committee would be enlarged and reorganized. On October 17th, General McNaughton.o President of the National Research Councils assumed his duties as Officer Commanding the First Canadian Division^ and on the following day Dean C.J. Mackenzie came to Ottawa as Acting President of the Research Council. Two weeks later, on October Slst^ Dean Mackenzie met with a small group of key men in the field of industrial research^, all of whom had been present at the July Conference. The manner in vti ich the National Research Council iould a ct as the liaison and coordinating body for war research was discussedo with particular re- ference to the cheinical field. It was agreed that a chemical advisory committee should be set up to advise the Assisted Researches Committee of the National Research Council on problems relating to the war effort in the chemical field, and to cooperate through the Council with research organ- izations in Great Britain with a view to the correlation of ^ ,. ledrii. bn .G : a c ^.Bcio e?i an. OB't £)j8il Y-Dii^ JDllB --■ rw t? "1 p i"-' * r-^.-^rf: :o of! .oafal' chemical research work on war problemso At this point in the conference p it was announced that Dr© Maass had been appointed to the National Research Council, whereupon it was decided that he should act as Chairman of this advisory committee. At the next meeting of the Councilp on December i4.o 1939« such a co:nmittee was formally established under the name of the Advisory C'^mmittee of Industrial Chemist s^ with Dro Maass as its chairrr.anr, and its personnel consisting of those present at the October Conference^ namelys Dr, AoP. Go Cadenhead^ JoRo Donaldp Dr. RoTo Blworthy, Dr„ I.Ro I^cHaffie.o Dro Ho Bo Speakman„ DTo EoWoR. Steacie, Dro RcKo Stratford. So Jo Cook (Secretary) and Dro CoAo ^acConkey (Assto Secretary) « At this same Council meeting, five Subcommittees on War Researches of the Standing Committee on Assisted Researches were sot up on (i) Chemical Problems., (ii) Biological Problems, (iii) Physics Problems^, (Iv) Engineering Problems., and (v) Medical Problems, The Subcommittee on Chemical Problems con- sisted of Dr, 0« Maass (chairman). o Dr, EoW.Ro Steacie and Dro RqKo Stratford. During the late winter and spring of 1940, Dr* Maass, as chairman of the Advisory Commitfee of Industrial Chemists, called together advisory subcommittees in the fields of ex- plosives ana petroleum technology. These High Explosives and Petroleum Subcommittees were very active, and ably carried out the advisory functions assigned to them© Later^, It became desirable that these committees should administer the very extensive research activities which had been initiated^ their membership wqs then broadened, and they were formally con- stituted as Associate Committees of the National Research Council. Under Dr. Maass' direction., and with the advice of these various committees^, research work in the fields of chem- ical warfare, explosives., and petroleum were initiated, during 1940, in various laboratories^, particularly at McGill Univer- sity of Toronto. Thus an extra-mural research program of con- siderable extent was got under way, funds being supplied in- itially by the Assisted Researches Committee of the National Research Council. These Committees Inevitably were associated in many ways with the activities of the Division of Chemistry^ a detailed discussion of their work is reserved, however, for another volume. Until the time of Dunkirk;, the funds available for special war research were somewhat limited, a s the full ex- tent of the contribution which Canada could make to the war effort was not visualized until after Britain had lost her chief ally and stood alone.o facing a powerful e nemy across the narrow Channel. It was at about this time that a small , I. no eea?"* ^■tn^rfoo': a-mslc f-7l'; i-'i -— --xe to eb.' £>n jb e ^ V 1 a o I q > ..■. - ; _. 6rn.ao©cf -itl ,. : ^ia¥ e"^ '■■' '■ '■ - ■ ■ -noo lo. m'B'ig'. 10 1 G aLrtij'i. en *i^6ii J £ o 1 b b:1 cl 1 0 ;t 1 £ group of Canadian business men offered to donate a sum total= ling about one million dollars in aid of Canada's war effort o This offer was f£rst received by the Acting Deputy Minister for Air^ who called a meeting of ranking officials of various departments of Government concerned, to discuss with repre- sentatives of the donors the question as to how these funds could most effectively be appliedo At this meeting various proposals were presented,, but when the Acting President of the Research Council outlined what the Council was doing both during peace and during war^ it was unanimously agreed that these monleo could most effectively be expended on research projects proposed by the National Research Councilo A War Technical and Scientific Development Committee was therefore set up by PoCo 4260, August 27^ 1940, consisting of represen- tatives of the National Research Council, of the various government departments directly concerned in the prosecution of the war„ and of the donors. This committee was authorized to receive funds from private donors and to transfer to the National Research Council funds for the carrying out of pro- jects proposed by the National Research Council and approA^ed by the Committeeo The National Research Council represen- tatives on this Committee were Dean C*Jo Mackenzie^ Sir Frederick Banting and Dro Otto Maasso Latere in July 1941, after the tragic death of Sir Frederick Banting, the fund was renamed the Sir Frederick Banting Fund, and the committee, the Sir Frederick Banting Fund Committee, Dr. Jo Bo Collip was named to replace Sir Frederick on the Committeeo By February of 1943 the sum available to the National Research Council through the fund had reached $1,300, OOOo This money made possible the development of the early work in such fields as chemical warfare, explosives, ballistics, radar J, optics, aviation medicine, and aeronautics, up to the point of proven success where money from regular sources was readily available to carry the projects to completion. One other event of that summer was of significance in the field of chemistry© The rapid expansion of the act- ivities of the Research Council made necessary the appoint- ment of a Special Assistant to the Acting President. Dr© Maass, who was already a key figure In the organizing of chemical war research, was appointed to assume the respon^ sibilities of this position - a position which he filled with distinction throughout the war. These events were, then., the background against which we must consider the history of the wartime activities of the Division of Chemistry, to which we will now turn more speci- fically. ni ^ncr-N Y T'T 3 rJ :) t- on r eh a X J" . w . ■/id vin.-.aO i.>ic.li \'Wien Dr. E.WoRc Stsacie assumed the post Director of the Division of Chemistry in July 1939, projects were already under way ° thanks to the foresight of the President, General McNaughton - which were to be of significance in Canada's war effort 5 most notable of these were the investigation of methods of producing metallic magnesium, and the proofing of active charcoal and containers for respirators. With the incidence of war in Se orembep., the program of the Division was rapidly converted to a wartime basis 5 several projects were terminated as rapidly as practicable and new ones were initiated During the course of the war there was a tremendous increase in the activities of the Division of Chemistry, and the staff of the Division approximately tripled in size. Throughout the war, administrative duties in con- nection with the Associate Committees on Textiles, Explosives, Petroleum, and Rubber engaged almost the full attention of two s enior members of the staff. A number of noteworthy changes in the Division took place during the years of the wan- The respirator container proofing laboratory rapidly expanded, as interest in other aspects of chemical warfare developed, until it was taken over by the Department of National Defence early in 1941, becoming the Research Establishment (C.Wo) of the Directorate of Technical Research. Early in 1943, laboratory and pilot plant work on refractories was transferred to the new laboratories of Canadian Refractories Ltdo 5 at Kilmar, Que. A year later development work on met- allic magnesium was taken over directly by Dominion Magnesium Ltdo Each of these were projects which, launched under the aegis of the Division of Chemistry, had developed into self- reliant drganizations, able to carry on an Independent ex- istence. Early in 1941 an Explosive Testing Laboratory was established as joint activity of the Department of Mines and Resources and the National Research Councllo The laboratory was administered by the Division of Chemistry. In addition to functioning in its statutory capacity for the Inspection of explosives under the supervision of the Department of Mines and Resources^ the laboratory has conducted extensive researches under the direction of the Associate Committee on Explosive Testing and Research, which later, towards the end of 1942, became part of the newly formed Associate Committee on Ex- plosives. These investigations will be discussed in the volume h^:i'^ ;c-i;:i:v.lC iTi S'A' ^n 1 ecE ic; ail? 1-0 La-. . Aivy uoqu, r t r\ r p f >■■■ rH iT' ,>_ V i. -i J-i^iinojr . .1 . I J. IB bf'-f: C'^ :ec'iGx:'l m- ©fni/Xov rouii'i 8 of this History dealing with the work of the Associate Com- mitteeSo On January Ist, 1943., the staff and laboratory fac^ ilities of the Customs and Excise Laboratory were transferred from the Department of National Revenue to the Division of Chemistry of the National Research Coxincilo Under this new arrangement the laboratory is operated jointly by the Council and the Department of National Revenueo It has continued to function In its statutory capacity for the exantination of com- mercial products for customs and excise purposes. The need for a Chemical Engineering Section within the Division had been becoming increasingly apparent as activities of a pilot plant nature increased in importance « The r emoval of the refractories and magnesium pilot plants provided an opportunity for the consolidation of such engineering activ- ities, and, early in 1944p a Chemical Engineering Section was created, with the group working on sulphur recovery as its nucleus© This new Section was almost immediately asked to undertake heat transfer pilot plant studies in connection with the Chalk River atomic energy pile, llfhen^, at the end of that year 5 water treatment studies were commenced at Chalk River, the Chemical Engineering Section provided most of the staff and facilities. These projects so completely engaged the staff of the new section that,, when the Division of Chemistry was requested a few months later to undertake pilot plant studies of the chemical separation processes for the Chalk River plant, it was necessary to create what was, in effect, a new section^ but which was more generally known as the "Pilot Plant Group". The "Design Group" which converted these pilot plant studies into full scale plant designs, was a similar temporary section. Later, and after the close of hostilities^ when the plans for the chemical separation plant were largely complete, there was a considerable contraction in the size of the staff engaged in the work; the remnants were consolidated under the Chemical Engineering Section and formed the Chemical Engineering Labor- atory at Chalk River. In the meantime.., in May 1944^, DTo EoWoRo Steacie had been appointed Deputy Director of the Council *s Montreal Laboratories, which were the c entr© of the Atomic Energy Pro- ject, and responsibility for the direction of the activities of the Division of Chemistry was given to Dr. Ao Cambron, who becfiime Acting Director. mol) £• ^T'l:.: &cii nln J-B:!? :o jjH ».-l ;t .♦Gl:tod&- W€ iii £i0^-. iij,\.' .i. ». i .' «ov-' c 4-1 9 Following the close of hostilities a gradual re- organization of the Division of Chemistry took place ^ v/hich was complete by the end of June 1946, Plutonium pilot plant and engineering work had been t ransf erred to Chalk River as mentioned above, and the transition from war to post-war re- search programs had been completed. Because of the greatly increased size of the Division it had, in the spring of 1946,, been divided into two parts « a Fundamental Chemistry Branch under the Director, Dr« Steacie, and an Applied Chemistry Branch under the Assistant Director, Dro Cambron, The first of these will deal with such basic branches of chemistry as organic, inorganic, physical^ and colloid chemistry, while the latter will deal with engineering and pilot plant oper- ations, and with industrial chemistry related specifically to industries such a s the textile, rubber^ and protective coating industries. EJB -lev dor. li ■X.3V : lO-Ji X ~ rf .Lb :eeo ?. I V 'loqc JT.»A5lq :tC'Ixj f 10 Bo INORGANIC CHEMISTRY ATOMIC ENERGY Before the completion of the Chalk River Laboratories, Canadian research and development work on atomic energy was centered in the Montreal Laboratories of the National Research Council, which were established for this purpose. However, other divisions of the Research Council as well as some other government laboratories were called upon to contribute to the program, '■'•'he present account will be confined to the contribution of the Division of Chemistry of the Ottawa Lab- oratories of the National Research Council.. At first the full extent of the participation of the Division of Chemistry was not clear, and problems referred to the Ottawa Group multiplied more rapidly than laboratory space, equipment, and a staff could be assembled to handle them. In Ottawa, as elsewhere „ a great sense of urgency at- tended the work, laboratories were rapidly blacked out, and those fortunate enough to participate in this epoch-making achievement began to burn the midnight oil behind locked doorso The work done by the Division of Chemistry falls largely in that field of technology known a s chemical engineering. For purposes of description, the organization at Ottawa may be divided into four groups, although actually there was an almost continual e xchange of laboratory space, equipment, and staff. These groups were the Heat Transfer Group, the Water Treat- ment Group, the Pilot Plant Group, and the Design Group. The Heat Transfer and Water Treatment Groups The Canadian pile consists essentially of a large quantity of pure uranium ^and heavy water enclosed in a mass of concrete. The uranium Is a nat\iral mixture of the isotopes of mass 235 and 238. By fission of atoms of U235 enough neutrons are released to provide for absorption in the U238, for absorption in the other materials and impurities com- prising the pile, for loss through the shielding surrounding the pile, and for enough residual neutrons to initiate the fission of more U235 atoms., thereby maintaining the chain reaction. Neutrons absorbed by the U238 result in the form- ation of Plutonium according to the now well known reactions s- ax 3ni3lBm-rloC'. oE*IOC;iD beiiOoL tri\..l^'0 ^-,.:.'.. ' ■... ©.: ^, Bv/Bcr^C "iB j-aofrfjB HB et.w a^ierf ..liBTa i:)nB ,rjnor. -d-B©iT 'i©itsV/ 0 ■ nl beeolcne i© -^P 5?qocroBl 9rfct lo ^^jj^xi.Ti J -moo SQUXIUqail IHTj;; fix Brio ■ 'Eii o; 3ao.i J^oBei rrsRron?( .£Ie j • '^ 11 238 1 239 o U n Np e 92 +0 ^93 + -1 239 239 o Np Pu e 93 => 94 + -1 In these equations mass numbers are shown as superscripts and atomic numbers as subscripts; Np and Pu are the symbols wiiich have been adopted for the synthetic elements, neptunium and Plutonium; o^^ represents the neutron of mass unity and no charge; and -1©^ represents the electron of negligible mass and one negative charge o The sum of the masses of the fission fragments is measurably less than the auss of the original U235.„ and the mass which is lost reappears as energy according to the well known Einstein equation E = c^mi, where c is the velocity of lighto Expressed in common units^ this energy equivalent of mass is 3o87 x 10^^ BTUAbo This energy appears initially as kinetic energy of the fragments of the disrupted atoms and as electro-magnetic radiation, but all of It is ultimately converted into heat within the shleldlngo In brief, then^ a chain reacting pile may be des- cribed as a machine in which U235 is burned to convert U238 into plutoniumo Considered from this vlewpointo the heat associated with the process is a necessary evil and must be dissipated as efficiently as possibleo The heat of fission of U235 has been measured by Henderson*, who reported a value of 177 Mev per atom; this is lc74 x 10^0 cals„ per gram of U235 per day would be, therefore ;, about 380.. 000 KW. The removal of these tremendous quantities of heat becomes, then one of the major problems of pile design^ Since very large quantities of a cooling medium of relatively high specific heat are required, the choice naturally falls on watero And because a pile is a relatively compact machine compared with the amount of energy to be dissipatedp the heat transferred per unit area of cooling surface must be exceptionally hlgho Water has a relatively high heat transfer coefficient for clean surfaces; but^ in ordinary industrial practice, generous allowance must always be made for the scale which inevitably fouls the cooling sur- faceSi, and the equipment must be overhauled regularly to re- move the scaleo However, in a piler, fouling of the cooling surfaces is a serious matter because of the high heat transfer rates which must be maintained^ and because the surfaces are # PhySoRevo 58, 774, NoVo 1940o j'seri Sii-'t SSTJ 8Q Do '5 1 i'f^n "to r 12 not accessible for cleaning due to the intense radio-activity produced in the structiiral materials of the pile once it has been in operation© Because of the great volumes of cooling water usedp a water treatment olant is required large enoiigh to serve a city© It is perhaps not generally realized that no two natural watel»s require quite the same treatment ^ and that a year or two of development work is usually required before satisfactory treatment is achievedo It was„ thenj, the re^ sponsibility of the Water Treatment Group to produce a sup- ply of water for cooling which would produce neither scaling of the cooling sxirfaces nor corrosion of any part of the water systemo Considerations involving radioactivity phen- omena also imposed certain restrictions on the type of water treatment employedo It was the responsibility of the Heat Transfer Group to test the water produced in order to deter- mine that satisfactory heat transfer rates would be maintained under the conditions existing in the plleo They were also expected to keep a weather eye open for signs of corrosion and to investigate suitable inhibitors of scale and of corrosion for addition to the treated water o Because this investigation had to be carried out on the actual source of water to be employed in cooling the pilep most of the work had to be done at the plant site 5 and be- cause the program was necessarily a lengthy one, this work had to be started very early© Consequently^ the buildings to house this work were the first permanent buildings constructed and members of this group were the first National Research Council personnel to t ake up residence at the plant site. This little group spent the first winter in three "-finterlzed" summer cottages., which were on the property about a mile from the actual plant siteo It was November when they arrived^ and winter was upon them almost before they were able to obtain a supply of fuelo Soon the bush road to the cottages was Impassible to vehicles, and all provisions had to be hauled In on tobogganso I>uring this early stage of construe'- tionp conditions at the plant site were most unfavo\irable for research activitieso Water^ steam^ and electric power,, all of vital importance ;, were obtained f rom t emporary equipment whioh^ suitable enough for construction purposes^ was not sufficiently stable in output for the needs of a research laboratory and was subject to frequent,, irritating breakdownSo A whole chemical and engineering laboratory had to be equipped in the wildernessp starting from scratchy and many discouraging delays resulted from the lack of simple items^ unexpectedly required^ i*iich usually could not be obtained from Ottawa in r-' TOii ti* Eri^'r', f-iB^- 13 less than a weeko So the group not only lived under difficult conditions^ "but also worked under difficult conditionso Meanwhile p in Ottawa^, the other half of the group worked night and day to design and fabricate the special equipment required^, and to obtain the laboratory equipment and supplies so urgently needed at Chalk Rivero In those days even the highest priority was no guarantee of early de= livery^ and many of the items involved special or ^'critical" materials and unusual types of fabricationo By Springy short- ages of staffp laboratory space^ materials^ and equipment were largely overcome | more adequate supplies of steam.„ water,, and electric power were available | many of the earlier problems of existing and of working had been resolved •= and progress be- came much more rapldo Before the construction of the pile was complete, the Ottawa group were able to report that a suitable supply of water would be available and that the cooling provided would be satisfactory© The Pilot Plant Group The reactions by which U238 is converted into plutonium in a chain-reacting pile have already been describedo When the charge is removed from the pile, it contains not only plu= tonlum and unreadted uranium but also fission products in con- centrations similar to that of the plutonium itself o When it is realized that the fission products produced include selenium, bromine, krypton, rubidium, 3trontl\im,, yttrioim^ zirconium, columtiim, nolybdenum^ antimony, tellurium, iodine ^ xenon.o cesium, barium, lanthanum, cerium, and possibly other elements, the complexity of the separation and purification problem can be readily appreciatedo Furthermore, these fission products are present In the form of highly radioactive isotopes, so that processing must be carried out behind several feet of concrete shielding, or its equivalent thickness of leado This not only requires remote control of all operations^ but prevents ser- vicing of equipment^ for the equipment itself becomes so radio- active that it cannot be approachedo even when emptyo The problem was, therefore, one of evolving a process capable of separating a fifth of all the elements in the periodic table from an element which had not even been discovered a few short years ago - much less its chemical properties understood -- and of embodying this process in a plant which would be absolutley free of such normally tolerable Inconveniences as leaking valves and pumps, and free of mechanical parts requiring lubrlcatlono As only very limited information was available regarding the processes used in the United States, and entirely new process of separating fissile materials from the pile charge was de- veloped by the scientists and engineers of the Canadian projecto 14 It was th6 responsibility of the Division of Chemistry of the Montreal Laboratories to investigate the hundreds of possible operations and reagents for effecting these separations and to make a decision as to what process was to be usedo Once the Montreal Laboratories had' sketched in the outlines of the chemical process^ the task of filling in the details and of converting them into practicable plant opera^ tions was the responsibility of the Ottawa Oroupo Usually^ when engineers are designing a plant;, they are able to turn to standard handbooks for densities^, solubilities, specific heats^ and similar datao Because of the novelty of the mater= ials involved:, such basic data were not usually available in the literature^, and the first task of the Pilot Plant Group was to obtain such fundamental Informationo They also had to make a more thorough-, quantitative, laboratory study of the chemical reactions and systems encountered in the process^ than had been attempted in the original exploratory invest i= gations in the Montreal LaboratorieSo Two complete pilot plants were built and operatedi in additionp many smaller pilot plant Investigations were carried out to study specific items of equipment required to meet the unusual needs of such a processo Unfortunately, no details of this work are available for release at this time„ but the program may be summarized by saying that all the processes to be used in the Chalk River chemical processing plant were successfully operated on a pilot plant scale by the Ottawa Group, using non -radioactive materialo The Design Group The actual working drawings for the construction of the Chalk River plant were prepared by the Special Projects Department of Defence Industries Limitedo These drawings were made from detailed sketches and according to Instructions pre- pared by the engineering staff of the National Research Council^, and were at all stages subject to the approval of the National Research Councils In general^, these sketches and instructions were issued by the Engineering Division of the Montreal Labora- toriesp but in the case of the chemical processing plant s^ this responsibility was assumed by the Design Group at Ottawao In the normal course of process development;, labor- atory and pilot plant investigations are essentially complete before plant design Is seriously under taken© In the present casep because of the urgency of the work,, plant design was com-- menced before the pilot plant work was mol*e than well started© ' *■- iO e-ie^ ^;i-. 'f. X. a J ^ oi- ■" 15 Indeed^ it was not unusual for sections of the plant design to be tentatively completed on the basis of the preliminary investigations in Montreal, before reports were received on thorough laboratory investigation or on pilot plant operation© Changes had to be made in the designs as more information be^ came available , but in this way a development program that would normally have required ten years was compressed into twice that many months© AJ-thoughp for purposes of discussion^, the work of the various groups has been considered separately,, in practice^, much consultation and discussion was necessary between the Design and Pilot Plant Groups and the staff of the Montreal Laboratories p and between the Design Group and the Design and Operating Departments of Defence Industries Limitedo All of these groups were working simultaneously^ and problems arising in one group were continually being referred to an= other groups better able to cope with them© The final culmination of this effort is a unique chemical processing plant at Chalk Rlver^ irtiich represents a milestone in the industrial development of atomic energy© The plant has been designed so that additions can be made for the recovery of various by-products as this becomes desirable and construction will doubtless continue for some time© REFRACTORIES This Industrial investigation was begun in 1925 at the request of the Dominion Government and on behalf of a key industry© Basic refractories are essential in smelting opera- tions and it was considered in the country's Interests to develop such an industry In Canada© The raw material aval lab le^ a magnesltic dolomite;, was at first regarded as unsuitable for this purpose© Howeverp persistent research on the part of the group assigned to this project resulted in the development of a variety of useful products© Chief of thesep developed before and improved during the warp was a chemically bonded hearth refractory© During the war it came to be accepted as the best open hearth bed material, because it eliminated that lengthy burning-in-period and hence made a substantial contribution towards the rapid expansion of the steel industry, especially in the United States© Other products developed before World War II but continuously improved included spalling-resistant brlckj, refractory cements,, chemically bonded brick and a refractory highly resistant to hydration© '8X '^ -i ^•.■^fc. J -J i^e'i lo 3-nen; 16 One other major development was a refractory brick for use in rotary cement kilns. This has at least three times the life of any other competing product and is being sold all over the world. During the war the nature of the research carried out changed substantial ly* There became available for the first time calcined brucite granules produced in a plant near Ottawa by a method worked out by the Bureau of Mines and much research was required to utilize this material commerciallyo The major applications have been in the manufacture of burned brickp the production of unburned brick by means of new chem- ical bondSp and the development of rammedo chemically-bonded hearth refractories. All of these have been important com- mercially., and Canadian and foreign patents have been obtained on the special processes involved© Shortly after the outbreak of war it became doubtful whether the supply of high-grade magnesia available to the United Nations would be equal to the demando In order to pro- vide against eventualities, work was undertaken on the puri- fication of Canadian raw materialSp using a number of different methodSo Prom impure material it was found possible to leach lime economically and to divide the residue of magnesia into two portions,, one high in magnesia and low in silica^ and the other relatively high in silica but nevertheless suitable for many applications. Patents were obtained on the process^, but the necessity for its use has not yet ariseno Other methods novel in character have been developed through the initial experimental stage, and work will be continued as opportunity affords. In keeping with the policy adopted early in the in- vestigationp research has been actively continued in the im- provement of products previously developed and processes al- ready adoptedo This work has resulted in many improvements whichp although not of outstanding character i ndi vi dually f, together represent important developments and have made pos- sible the application of products in fields for which they were not previously considered suitableo As frequently happens, even small improvements in the properties of a material greatly enhance its commercial value and competitive position. One of the major problems arising out of the war has been that of finding suitable raw materials to replace those cut off by the shortage of shipping. Of these the most im- portant has been chrome ore, previously obtained by the Can^ adian refractories industry from India, South Africa,, and Turkey. To a degree, substitution was found possible if •uo ;?.^4 Z^si -[ ■ i- 17 certain precautions were observed; the proportion of chrome ore consuuned has also been reduced substantiallyo Certain chemicals previously used have been unavailable at reason^ able prices^ and satisfactory substitutes had to be foundo As a result of such conditions and the research work carried out^ the revision of manufacturing formulae has become almost a continuous processo In this jrefractories investigation^ as is usually the case^ progress in research has been by no means constant^ but may be said to have a wave formo When some important basic advance is made,, it starts a series of fruitful experiments intended to discover all possible commercial applications, and the attention of the research staff is accordingly transferred to a considerable degree from fundamental to practical lineso Without fundamental research, however , practical applications may soon be exhausted, and in recent years as much attention as possible Pms therefore been paid to theoretical consldera- tionSj such as are involved in phase equilibrium diagramso Recently some very promising new fields have thus been opened up, and these are now being explored in a practical wayo It is expected that full patent protection can be secured, since the approach is distinctly novele Early in 1943 the research work carried out on re- fractories was transferred from the laboratories of the Council to newly erected laboratories at Kilmar^) Quebec, near the mine and treatment plant of Canadian Refractories Limitedo Opera- tions are being conducted there on substantially the same scale as previously,n and contact with the Council has not been com- pletely broken© During the twenty-year period in TRrtiich this inves- tigation has been carried on,n well over .one hundred Canadian and foreign patents have been issued on more than thirty different processes and products© The principal patents arising from work carried out during the war are listed at the end of Section B, together with the title of a paper con- trasting the situation with respect to Canadian sources of basic refractory materials at the beginning of the first and second world warso The paten s listed are on different pro- cesses, with no duplication other than those noted© RECOVERY OP MAGNESIA When the war broke out it was obvious that the United Nations' requirements of magnesia would be greatly increased^ both for refractories, to be used in the metallurgical in- dustries, and for the production of metallic magnesium© n ef? "*' T S i ■■■nic .1;-^ ' K' «"v nr 'l'\ 3e#T 18 Fortunately the situation had already been given close study for some years^ in connection with the refractories inves- tigations carried out in the National Research LaboratorieSo In 1940^ at the request of the Metals Controller^ a survey was carried out of potential sources of magnesia in Canada for all purposes^ including refractories^ metallic magnesiuffly and magnesium sulphate o This survey covered not only Canadian mineral deposits and a study of their commercial possibilities^ but also an evaluation of many methods of re- covering pure magnesia that had been suggested to the Dominion Government as being worthy of support© Later p the survey was extended to include the probable requirements of magnesia in Canada and the United States for 1942 o It was evident that large new sources of magnesia must be developed© As a result of this siirvey the following potential sources of magnesia for refractories and metallic magnesium were recommended to the Metals Controller as being of nearly equal interests- lo Magnesitic dolomite occurring at Kilmar^ Quebec© Operations at this property were greatly enlarged during the warp and It was the country's major source of basic refrac- torieSo while exports were also made to many countries© 2o Bruclte rock near Wakefield, Quebec,, from which magnesia was recovered by a fliethod worked out by the Bureau of Mines© This was likewise developed and became an Important source of refractories© 3© Sea water treated with calcined dolomiteo In this process magnesia is recovered In equal quantities from the two raw materials used© Although no commercial developments took place in Canada, a careful survey in Nova Scotia by the provincial Department of Mines led to the discovery of a deposit suitably situated for commercial operation^, and exper- iments in the National Research Laboratories demonstrated that this raw material was entirely satisfactory for the purpose© Further., very large developments along this line took place in both Great Britain and the United States© As a source of magnesium sulphate, it was indicated that serpentine treated with acid by a method developed in the National Research Laboratories held greatest promise* No com°' mercial development has yet occurred© p f r:^ 0 .. i.l II B^ ••:■ ■-■ \r ii .1. ■-> er. .'"■•7 ja-'ii0 e. r:OC QJ^ 19 Dolomite was recommended as the most promising source of magnesiiam metal in Canadao A commercial plant was built at Haley^, OntariOp and was operated successfully until the end of the waro The evolution of the process employed in this plant is described in the following section© MAGUESIUM Although metallic magnesium was first isolated by Sir Humphrey Davy in 1808 and small amounts were produced com- mercially for photographic purposes as early as 1857^ the industrial production of magnesium dates only from 1896, when a plant for the electrolysis of fused magnesium chloride com^ menced operation at Bitterfeld.. Germanyo Progress was slow^ and even in 1937 world production was estimated to be only 27^000 tons per annum^ of which half was produced in Germanyo In that year an Associate Committee on Metallic Mag- nesium was formed in Canada*, consisting of representatives of the Departments of National Defence ;» Mines and Re source So and the National Research Council 5 and the Council was asked to conduct "literature and laboratory studies of the possible processes for the recovery of metallic magnesium^ with a view to being able to assess the technical difficulties vi^ich might be met in the use of Canadian raw materials"© At that time most commercial processes were based on the electro- lysis of fused magnesium chloride© The raw materials used were either carnallite (MgCl2oKClo6H20)p magnesium chloride from natural brines, sea water^ magnesite (MgCOj), or dolomite (MgCOs© CaCOj)! the process varied from placd to place chiefly in the method used to obtain anhydrous magnesium chloride from the raw material available© Since magnesia can be obtained in Canada from magnesite, dolomite^ or naturally occurring brucite gran- ules (Mg(0H)2), the method of preparation of chief interest in this country was that represented in its simplest form by the equations MgO •♦• C -»• CI2 — ^ MgCl2 + CO The early experimental work carried out followed pre- vious commercial practice in that fine magnesia was mixed with reducing agents, such as coal and either wood;> flour or sawdustp and was briquetted with magnesium chloride solution, with which the magnesia forms magnesium oxychloride© The main purposes of the wood flour or sawdust were to produce a pcrous briquette, into which the chlorine could penetrate ^ and at the same time provide sufficient pore space to accommodate the voluminous magnesiiam chloride formedo Such briquettes., calcined to drive ex "lo ^Vl'JX o 20 off all contained moisture^^ were found to chlorinate rapidly at f iratp but the rate of reaction decreased with the pro= gress of chlorination and became very slow by the time half the magnesia had been converted to magnesium chlorideo Experiments were then begun with granular magnesia of various degrees of density^ and it was soon found that,, if the granules were of a size sufficient to permit the chlorine gas to penetrate the mass and the magnesium chloride formed to run off in a molten condition^, and were themselves sufficiently porous^ chlorination took place with greatly improved rapidity and corapletenesSo Patents were obtained on the optimum ranges of particle size and densltyo Calcined brucite granules obtained from the deposit near Ottawa by the method worked out by the Bureau of Mines (see po B--16) were found to be particularly suitable In both of these respectSo The anhydrous magnesium chloride produced experimentally was used in small-scale tests designed to familiarize the oper-- ators with commercial practice in the production of magnesium by electrolysiSo Ty"- However^, as the commercial production of an anhydrous magnesium chloride suitable for electrolysis is usually a complicated processy attention was given to the direct re- duction "t)f magnesium oxide by means of carbon^ calcium carbide^ aluminum;^ and sllicono Of these various reducing agents., the first and last had received most attention^, and semi- commercial plants hadp in fact, been operated intermittently using carbon, in what is now known as the carbothermic processo This has the disadvantages (i) that reduction with carbon requires a very high temperature (above 2000**C)^ (ii) that the vapours must be cooled very rapidly through the region of unfavourable equilibrlump and (ill) that the product is obtained as magnesium dust which requires further treatment to produce a compact metalo The use of silicon, preferably In the form of ferro- silicon^, has the advantages that (1) compact metal is formed in one operation., (ii) the operating temperature is only about 1200**Co .0 and (ill) the much cheaper and more widely distri- buted dolomite may be used instead of magnesite^ Indeed^ in the ferrosllicon process.^ calcined dolomite is preferred© When straight magnesia is used, some of the silica first formed by the oxidation of silicon combines with magnesia i this not only reduces the utilization efficiency of the magnesia^ but may, at the temperature used, lead to the formation of liquid silicates in the reaction retort^ involving serious operating difficultieso With dolomite, on the other hand, the amount of lime present is theoretically just enough to combine with all Xitzq^^i '■ firrv et'.: a sv J Jbsnijetdn '^^t '3'./ ? f -1- benJolBt exij Y"^ > eT6W .-.eloeq SBW Xi -, , ^- •leqo 0^ £^ rajLfiao .-J-' ?>'j erid a I ■^J . 7 ICTIO ,J xiKe.B bnx r'VieoQ'i :'' aBEeootq Jir?^'^^-''- •.- ^- -f .bexilBcJ-cfo ex v. ^u: jBf.i:f (xii-j b/ti=« a; t' ' ^' • ""■■" /x »■ ..AM. • oboTiQleTq Qi Job ben' 3 iJCf ..^ B i 3 fc ■•- f .■) I i i 8 nr, X .1 .0 s 1 1 TO ejj-oi'ie^ 21 the silica formed^ thereby leaving the magnesia free to be reduced by silicon^ and the dicalclum silicate formed is so highly refractory that it can readily be removed from the retort ir. the solid condltiono Purther^o the heat generated by formation of dicalclum silicate is sufficient to promote the desired reducing reactions 2MgC + 2CaO + Si ^ (CaO)2Si02 ••' 2Mg Work on the development of a commercial process baaed on this reaction was begun by the Council even before the ex= periments with electrolysis were completed*, It was recognized that under Canadian conditions the advantages offered by it were substantial^ particularly with respect to the availability of cheap dolomite and the fact that Canada was already a large producer of ferrosillcon In electric furnaceso Although this reaction had long been considered else- where, and a number of patents on it had in fact been issued,, it had not been found possible to overcome the numerous tech- nical difficulties involved, and the process had consequently never been brought into commercial operation* Indeed,, one authority after an extensive investigation had published a report stating that the successful application of the ferro^ silicon process was impossibleo This^, then,, was the situ- ation when the Canadian group set to worko It was soon found that;, using calcined dolomite and 75% ferrosilicon.o the reaction could be made to proceed at a satisfactory rate if (1) the constituents of the charge were finely pulverized., mixed and brlquetted; in order to bring them into the most intimate contact possible, (ii) a temper- ature of about 1100®C. was used.- and (ill] the process was carried out under a sufficiently high vacuum to remove as vapour all magnesium metal as rapidly as it was formedp Under these conditions the magnesium was found to distill out of the reaction mixture and to condense in the cool end of the alloy steel retort usedo One difficulty encountered in previous work was that the small amount of sodium always present in dolomite, was reduced and condensed with the magnesium, thereby causing ignition of the condensed metal and consequent loss of the product when the retort was openedo Cooling the retort be- fore discharging was both uneconomical and inconveniento This problem was solved by fractional condensation of the sodium in the outermost part of the retort„ A method was developed for opening the retort^ removing the product and spent charge, and reloading^, without removing the retort f i: m 22 from the furnace o The perfection of this technique made it possible to suggest commercial operation in a manner some- what similar to that adopted in the established horizontal retort zinc processo By the autumn of 1940, a small furnace with a four- inch retort was in regular operation. This furnace was ex° amined by a group of industrialists from Toronto., who con- sidered the development sufficiently promising that they for- med a private company under the name Dominion Magnesium Limitedo Under an agreement with the National Research Council, the company took ever the work., and a pilot plant using larger retorts was constructed and placed in continuous production by July, 1941. In November of that year plans were made to build a commercial plant;, and in December authorization for the construction of a two-ton per day plant was received from the Department of Munitions and Supply. A month later the plans were expanded to provide for ten tons pet day. This plant was built at a cost of $3,300,000 at Haley, Onto, near the dolomite deposit from which raw material was obtained in the experimental worko Operations began in July^ 1942, and the plant was later operated at a capacity of 15.5 tons of magnesium per day. It is interesting to note that the pro- cess and plant are also well suited to the production of met- allic calcium, and calcium haS;, Indeed, been produced by Dominion Magnesium Limitedo Planning for the Canadian plant coincided with the attack at Pearl Harbor and the subsequent rapid expansion of the magnesium industry In the United State So In November, 1941, the National Research Council's pilot plant was visited by officials of the United States War Production Board. After a special committee on magnesium examined the pilot plant in January, 1942, it was decided to adopt the process in the United States for a total daily production of 135 tons. All available information was given to the American engineers and the fol- lowing plants were erectedo at an estimated cost of $35.o000j;000o Capacity New England Lime COo 15 tons/day Magnesium Reduction Co. (subsidiary of National Lead Co) 15 " " American Metals Co© 16 *• *• Permanente Metals (H. Kaiser) 30 " " Ford Motor Coo 60 *• " Throughout 1942 the pilot plant at the National Research Council operated day and night, testing dolomites from various United States locations^ and training men for plant operation. Since the process was new and had never "ifcl B ^"^rt.rw eoB; - -TO 1 hbIi ^BSit'l- IB en nt ben .. .- ■^-.. io :ti5'ieqO '• "on ^:'^ji .- .X-4- ..a '1 -*■ ,. ledmevoPl nl Iq- zfollq 3riJ elcffi.r ;: a^tlnU o oOOO Bm i:c ..r'<: ^: Jfe/t •,;l ; .a ■ LV.Oi arm 6*5 v., fj-^:.l 23 been operated commercially^, mapy problems arose o Until the spring of 1944p when Dominion Magnesium Limited terminated its agreement with the National Research Councllr, development work continued,, directed towards improving the processo REC0V}'31Y OP ALUMINA Because of the enormous demand for aluminum metal during the war, and the great expansion of this industry In Canada, this country's requirements for bauxite were corres- pondingly increasedo None is produced in Canadao and it be- came necessary to bring from the bauxite mines of South America 5000 tons per day, or morOo '-^he demands upon ship- ping were obviously very greats and thought was therefore given to other possible sources of alumina then bauxite o The most obvious of these sources is clay„ which^ although it contains only about half as much alumina as bau- xite, is available in any desired quantity at a cost little more than that of digging the material up with a steam shovelo Some alumina was^ in factp produced from clay in Germany prior to the war, and following tests in the laboratories of the Bureau of Mines in Ottawa a company was formed to undertake large-scale pilot^plant work in the United StateSo It was therefore known that recovery could be effected from clay^ but it had not yet been demonstrated that the production of alumina of sufficiently high purity to satisfy the require- ments of the industry could be obtained at a price competi- tive with that of baxixlteo Further work by the usual methods therefore seemed scarcely justlfiedo However, two new approaches to the pro- blem was investigatedo For some years The Consolidated Mining and Smelting Company of Canada at Trail.. BoCo.o have been producing ammonium sulphate for use as a fertilizer by combining sulphuric acid made from the sulphur dioxide in their waste gases with am- monia produced by synthesis* It was thought that this pro- cedure could to advantage be combined with the treatment of clay, the ultimate products being ammonium sulphate^, as pre™ vlously.. and aluminao The latter.n if not sufficiently pure for direct use in the production of aluminum^ would at least afford a high-grade raw material for purification by the standard Bayer procesSo 24 Clay was first calcined to dehydrate it^, to render the silica insoluble o and to convert the alumina to a more soluble formo The temperature range 550-900°Co was found satisfactoryo Leaching was effected by using a sulphuric acid solution containing 60^ of acid by welghto By this means it was possible to dissolve over 90^ of the alumina from kaolin containing 40o6% AI2O3 and loO% PegOj,, but some of the iron also dissolvedo When, after filtering off the silica^ ammonia was added to precipitate the alumina^, this dissolved iron also came down., thereby contaminating the aluminao Three possible methods of purification were proved applicable s- lu Magnesium powder was found to precipitate iron readily from the slightly acid solution resulting from leaching.; and it could then be separated by filtration^ 2o The addition of ammonium sulphate to the filtrate from the silica precipitated ammonium alum as crystals free from irono By dissolving these crystals in water and adding ammonia^ alumina was precipitated in a sLate cf satisfactory purity;; and, following filtration, the ammonium sulphate was recovered by evaporationo 3o The impure precipitate of alumina produced by the addition of ammonia to the original clear leach liquor was dissolved in caustic soda (the iron remaining insoluble) and the solution filteredo Alumina was then precipitated from this solution as in the usual Bayer processo These methods were worked out only on a small labor- atory scale;, but they appeared to give considerably promise of the cheap production of alumina of high purltyo There was no opportunity to continue the work on larger quantities In a cyclic procesSr such as would be necessary before a pilot- plant operation could be justifledo DRYING AIR FOR BLAST FURNACE USE The exceptional demand for steel during the war and the shortage of scrap led to greatly increased requirements for pig iron^ and consideration was therefore given by in- dustry to methods of increasing productiono Of these,, one of the most promising was the drying of the blast usedo The method had been introduced by Gayley in 1904s but owing to the high capital and operating costs involved in his refrig- eration system most of the dry blast plants were discontinued by 1916o In the early part of the recent war, several plants were built using modern methods of drying blasts and in some d3 Y/ o t. ^ 1 1 1 IB b1 *-'8 -'■:. ed^ 1} . ■■■ . em "em 25 cases excellent results were claimed, production being sub^- stantially increased and coke consumption decreased© Work carried out previously in the National Research Laboratories had indicated that one of the best and most economical drying agents was active silica, produced by the acid treatment of serpentine* Steps were therefore taken to investigate its possible application to the drying of blast furnace aire A search of the literature was made, and the subject was discussed with experts at steel plants at Sault Steo Marie, Ontario, at Sydney, NcSo, at Middletown^, Ohio, and at Baltimore, Mdo Experiments were carried out to determine (i) the resistance to flow of blast passing through active silica of various particle sizes^ (ii) the rate of adsorption of moisture, and (iii) the conditions necessary for the regeneration of the silicao Prom this data an adsorption system was designed in outline© The results of this work indicated that an adsor- ption system using active silica might be the cheapest in both capital and operating costs, and a paper describing the findings was published© Since that time, hov/ever, it ia believed that no new dry blast plants have been erected., and there has consequently been no opportunity to try the system on a commercial scale. UTILIZATION OP OPEN HEARTH SLAG Por nearly half a centxiry a large steel plant has been operated at Sydney, Nova Scotia,, and during the whole of this period the open hearth slag produced has been wastedu The magnitude of this waste will be realized from the fact that the phosphoric acid and lime contents of the slag have substantially exceeded the quantities of these materials used as fertilizer and soil amendment in all of the Maritime Provinces put together. The major reason for this continued waste was the fact thatp because of the use of fluorspar in the steel furnace operations, the phosphoric acid in the slag was of low availability to plants. Such growth experiments as were carried out with it indicated that its value as fertilizer was quite small, and its application to the soil was believed not to be justified by the results obtained. This problem was brought to the attention of the National Research Council late in 1938 in the form of a re- solution passed by the Maritime Board of Trade, then in session at Sydney, The Council shortly afterwards wrote Tv. "xio b'3x'ri^.^o bnE ....... - its esnEl. J V7C bciQ .bo:', - ^oiiiOK L£-f o'lOiWiOD Ai no f'Oft /v r £Bri- :tr. :^ 1!£ lo alorlw v!?f neacf ©vBcl mbIe er^ j-Biii ■,'X' ed:i ..'/oil • 'les sett :rBr[^ ' .riiBO tidvei.r ^0 3 ^n? c..' nolJiio.L lij p ebw D. -©1 ..03 26 the Dominion Steel and Coal Corporation^ suggesting that the availability of the phosphoric acid might be improved by rapid chilling of the molten slag, as by granulating it in watero Preliminary experiments carried out by the company shortly afterwards indicated that the idea might have merits but no further action was taken until the spring of 1941^, when the Nova Scotia Economic Council asked the National Re- search Council to make a complete investigationo This work was undertaken in co-operation with the Dominion Steel and Coal Corporation and a slag committee set up by the Premier of Nova Scotia under the chairmanship of Dro G^Ro Smithy Provincial Agricultural Chemist o Later, when granulated slag became available i, comprehensive greenhouse and field tests were carried out over a period of several years by the Dominion Department of Agriculture o through its Central Experimental Farm at Ottawa and its experimental and Illustration stations in Nova Scotia, and also by the Nova Scotia Department of Agriculture. In the early experiments the slag was not chilled with sufficient rapidity and the availability of the phos- phoric acid was, in fact., reduced during the succeeding dry- ing operation* Although growth tests showed some Increase in yield for the garden and field crops trled^, the results were not regarded as conclusive o A complicating factor was an unfavourable growing season in Nova Scotia, as a result of which the effects of drought in some cases completely masked the effect of the fertilizers applledo In the spring of 1944^, however., the Steel Company granulated several hundred tons of slag by a semi-coramerclal method, and this was tested on a large number of farms in various parts of Nova Scotlao Pair results were obtained in that season with grain^ in spite of exceptionally dry weather and in 1945 grass wasr.grown on the same areas with very striking re suits o On many farms the Increased yield of hay from the application of one ton of slag per acre amounted to 50-75/5 ando on the average for all farms., the application of slag gave a highly favourable result^, both as to increase in yield and Improvement in the quality of the hay cropo Higher applications of slag gave still greater yields but not sufficient to pay in one year for the extra expense involved© These results were regarded as extremely promising,, and steps were immediately taken to put in a commercial plant for slag granulation and grindingo It is expected that this plant will shortly be in operation, and that one of the major waste products of the Maritime Provinces will thereafter be converted into a valuable fertilizer materials rtemd'iBaeC p "./' ■,V-.' '^d &8Vo^• ::_ ■it linl: '^n^qmoo 9x1 ct ^I'teiif evBff T erfd' Y-^ ■■•B7e no Id- BITS J. "'^''■*-' ^ rf.-ti'A •* i t ffp ^T 6/^"* ■^- fi no X}9:teei • rjaie "Uj ^^"jlqe ill ■'^•■■"i no nwoig. ':* ■-. cf.f^T.-.fovsl >rj' -»i ■:-^:-::. Sao ilx "Vii<^ Oj jau^LJXlliU' iua J.'Jt r, ^'liJE cc , . .^.^.. .. . .-8fiW fiOf) 27 The Sydney steel plant is the only one m Canada burning out an open hearth slag containing much phosphoric acidu In Britain, however,, there are many sucho and inform- ation regarding progress in this investigation was there- fore sent currently to the British Ministry of Supply^ They expressed great interest in the project r^ duplicated the liter- ature review for distribution to all British steel producers^ and undertook extensive experimental work to determine the ap' plicability of the findings to British practicOo To date^, the final results have not been received in Ottawao VANADIUM RECOVERY In the spring of 1942 there developed a critical shortage of vanadium^ which finds one of its main applica- tions as a constituent of tool steelo About this time the Council learned that the ore of the Wabana Mlnen Newfound-- landi contains about OoOSjS vanadium, and that as a conse- quence the pig iron produced at Sydney Nova Scotia by the Dominion Steel and Coal Corpcratlon^ has a vanadium content of slightly over OolO%o Although this proportion is not large p the total quantity going to waste amounted to more than one ton per day whlch^ if recovered^ would go far toward meeting Canada's most urgent requirements of this Important alloying element o Because of this situation, a study of the literature on vanadium recovery was made to determine whether there was any reasonable chance of obtaining the vanadium from Sydney pig iron in marketable formo Some encouragement was obtained andi as a resultn an investigation was undertaken at the re- quest of the Metals Controller in the summer of 1942 , and continued for about six months,. During this period a large number of experiments were carried out at Sydney in co- operation with the staff of the Dominion Steel and Coal Cor- porationo The oxidation of the vanadium in the pig iron was brought about by the addition of iron oxide to the blas-c furnace ladles at the time of tapping and the slag so pro- duced was resmelted with substantially complete recovery of both vanadiiim and Irono The results were regarded as suf- ficiently encouraging that work was done on the design of a rotary reaction drum which might permit the partial desill- conization of the pig iron and,., at the same time.r substan- tially complete oxidation of the contained vanadiumo It was proposed to resmelt the slag produced and again concentrate the vanadium by treatment of the resulting pig iron with iron oxide in the same equipmento It was believed that steel production would be increased by the oxidation of silicon in i9"ti. j^j-Trgw -.■t t.e .fcen . -. raij .i. - ago-Bi ',-. fc ^ '•< i.'b TOO ••■'iq O'li 28 the reaction drum and the consequent shortening of the open hearth operation, and that vanadium could be produced in marketable form at a cost below the pre-war price of the metalo ,ine i- Early In 1943 these proposals were laid before the Metals G on tr oiler o By this time,, however o the vanadium situation had become much less critical, steps already had been t aken to increase the production of vanadium in the United States and that country had agreed to supply Canada with her complete requirements of the metalo Under these circumstances it was felt that the capital expenditure re« quired for the erection of a vanadium plant at Sydney by the Dominion Government could not be justifiedo NICKEL,, COPPER. AND PLATIHUM METALS Three projects were undertaken all arising out of practical experience in the Canadian nickel industry, as followsj- ( 1 ) The rec o very of platimum metals from Monel metal matte In the usual practice^ the nickel-copper matte chosen for the production of Monel metal is one relatively low in platinum metals and by the usual methods of treatment their recovery Is not profitableo It was suggested that at least part of these metals could be cheaply recovered by blowing a charge of regular matte to produce a small quantity of copper and ut llizing the selective solubility of this element for gold and the platinum metalSo Preliminary experiments in the labora- tory indicated that this method was promising,, but there was no opportunity to follow it up on a larger scale o (2) Selective separation of copper and nickel in the converting operationo Much of the copper reverberatory and Orford mattes produced by the International Nickel Company contains a little nickel^ which subsequently enters the anode metal and considerably increases the cost of the subsequent refining operationo It was hoped that, because of the easier reduclbillty of copper, most of this metal could be separated m the converting operation substantially free from nickelo Preliminary laboratory experiments proved that some c-oncen- tration took place under such conditions^ but it was not re- garded as commercially promislngo (3) Analytical separation of the platinum metalSo One of the most difficult analytical or assaying problems is the separation of the platinum metals from one another and from Oo» xiaqo t' ed^ to '^i"" erfd ^-nolod bti^l. ^^t: i3 jJ ^:S ^ - Cl.t r.: ae bj: oi ^ "TiU -^cf ^9n.. -■' *. "■ ■■!l\l ■> r>V fwri. , '■> to OjPilBdO £ ,>; . "^''- - :ij[/ £)*Tft Tec :: jbOfi Jblo;' i e ^if^it lo i.xXi: ed:t^^ nl le.- f'if_,^ -91 Jon z . ^ iU r'oo ■:*:t^n ■ _ f.;, < <■ '. ni ; e-T^I ,£>'i-i 29 gold and silver ^ with which^ in Canadian ores,, they are in- variably associatedo Inquiries had been received from time to time as to practical methods of separation and deter- minationo These eventually led to a review of the literature and to the preparation of a paper describing methods used by the writer in his own work;, for distribution to inquirerso ATMOSPHERIC POLLUTION Several requests were made during the war for in-- vestigations regarding atmospheric pollution by heavy in-- dustry and the proper disposal of waste products resulting from such operations to prevent serious damage to agricul° tural and ornamental plants and forest species s- The Trail Smelter (^estion At Trail, British Columbiao is locate.d the largest lead-zinc smelter in the world, and in its operation large qiiantltles of sulphur dioxide have been discharged into the atmosphere o In 1928 the United States Government officially entered claims against the Dominion Government for damages alleged to have been done by fumes from the Trail smelter to farms and forests in the northern part of the State of Washlngtono The Dominion Government thereupon asked the National Research Council to make a full investigation of the matter^, and work was subsequently carried on by the Council almost continuously for a period of about ten yearso Later.o and during the war;, work was mainly confined to periodical surveys of the area and assistance in connection with the prosecution of the case before the courtso In 1940 reports were submitted to the Department of External AffairS;, covering the atmospheric sulphur dioxide conditions over the period 1937 to 1940 from data obtained from the operation of a number of automatic recorders in the Columbia river valley., on both sides of the International Boundary p in the path of fumes emitted by the plant at Trailp Records of sulphur dioxide concentrations at three points in the Columbia River Valley^ south of Trail, are still being regularly scrutinized by the staffs However., remedial measures undertaken by the Consolidated Mining and Smelting Company of Canada have resulted in a reduction in the amount of sulphur dioxide evolved, and have eliminated all damage south of the International Boundary« ^'■i "■ •""' 3: . "cT&nrn.lii ©iij :■ n.uoO .■•iw .■+r TJencfj:^ ,T 9.-tx5i lo ,,., ;oy #i3 Tr ^.Lq ■ 'XO0 9H c yrfBqmoO 30 Air pollution by smelter smoke in Sudbury region The Sudbury area of Ontario has for many years pro- duced 75-90% of the world's nickel, and has been at the same time one of the major copper producers and the source of more than half of the world's supply of metals of the platinum groupo In conjunction with these operations great quantities of sulphur dioxide have been produced by the three large smelters in the Sudbury district o Unlike Trail,, which lies in a valley that serves as a natural channel for the gases^ Sudbury is in relatively flat country and by the use of high stacks the operating companies have been able to keep to a minimum the damage done by smelter fumeso The Ontario Department of Mines has long maintained an arbitrat.or in Sudbury, and he has adjudicated any claims for smoke damage o During the war a major increase took place In the scale of operations in the Sudbury district^, and the evolu- tion of sulphur dioxide to the atmosphere was correspondingly increasedo The Ontario Government became concerned lest the Important provincial forests should be seriously damaged and asked the National Research Council for assistance in studying the problemo Following consultation in the spring of 1944, plans were laid for surveys of the vegetation, for meteoro- logical s tudieSn and for the determination of the concen- tration of sulphur dioxide in the a tmosphere and of sulphur in th« needles of coniferSo In several localities trees were bordd, pencil*" of wood removed, and annual growth carefully measured,, in order to determine to what degree, if any the trees had been damaged by sulphur dioxide in prevlou? years « In 1945 automatic sulphur dioxide recorders were set up by the Council's staff in several districts, and general super- vision was given to the investigation^ During 1945 the following studies were carried out in the course of this investlgationji- lo Continuous measurements of sulphur dioxide concen-' tration, by means of automatic recorders^ at four stations situated at distances varying from 20 to 60 miles from the smelters^ 2o Measurements of the concentration at various alti- tudes in the path of the smoke stream by means of portable equipment on an airplane in flighty 3o The simultaneous determination of sulphur trioxide and sulphur dioxide by mobile portable equipment i, i.uo b' nt 31 4o The extent of penetration of smelter smoke by a study of the abnormal sulphur content of various species of plants within the smoke area in comparison with similar species in normal control zoneso Three additional automatic sulphiir dioxide recorders were constructed for use in 1946o The observations are being correlated with studies of meteorological conditions at ground level and at various altitudes^ and with biological investigations, in order to delimit the zones of smoke damage and arrive at a satis^ factory solution of this problemo This work is still under wayp although the decreased s cale of operations resulting from the cessation of hostilities has substantially reduced the sulphur dioxide hazard to vegetatioiio CHARCOAL FOR PITSS POWDER Production The Charcoal used in manufacturing certain slow- burning fuse powders according i;o British specifications is obtained by carbonizing wood from the species Rhamus frangula (alder) o In September. 1939. the National Research Council received from the British Mission an enquiry regarding the availability of this tree in Canadao A survey, conducted by the Division of Applied Biology^ resulted In the discovery of two stands in Eastern Canada^ one of which was in the vicinity of Ottawa^ and samples were sent to Britaino While this search was in progress, it was suggested that carbonization experiments be carried out in Canada,, and as no information was available regarding the special equip- ment used in this work or the qualities sought in the char^ coal produced,-, the Department of National Defence was asked to obtain this information from Englandu Some details of the plant and manufacturing methods were received in January^ 1940y but work from Britain Indicated thaii no further action was required at the timeo However.; British supplies of Rhamus frangula were cut off by the fall of Prance .0 and an urgent request was received in August for six tons of this charcoal^ to be de- livered during 1941« It was decided that this work should be carried out by the Chemistry Division of the National Research Councilo Equipment was ordered at once and factory space rented nearbyo .b ■illn 'X ew :'-J-!e, er- ertct ^0T<1 > 01/ .jiJDi'j r.t :ltucf , , : actcfo >vi©oei bet rr SB •3ae^r aj.-r;:3nB ■^"i £)ii£ eono .t.s :jp:i 32 In view of the urgent need for charcoal there was no thought of trying to follow the British plan of air drying the woodo A new method of debarking the wood was developed in which the wood was predried at llO^Co. making the bark hard and brittle o Crushing the wood then reduced the bark to a fine powder^ which was rejected as undersize by the pre- carbonization screeningo Pull scale, twenty -four -^ho\xr operation began late in May, and. despite minor difficulties, it was possible to keep the Beloeil explosives plant supplied with its needSo In all^ slightly over six tons of fuse powder charcoal were produced in Ottawa and shipped to Beioeilo Some of this charcoal was prepared from alder supplied by Defence In- dustries Llmitedo In the meantime, Defence Industries Limited had been instructed to take over the charcoal productlono Because of experience in assembling the carbonizing units, the Re- search Council was requested by Allied War Supplies to pur- chase and to assemble for Defence Industries Limited the car- bonizing units required© Engineers from Defence Industries Limited visited Ottawa to observe the plant in operation and were given all information based on experience in Ottawa to aid in designing their proposed plant at Beloeilo By mid- October r, 1941p the Beloeil plant was able to t ake over all productionp but the Research Council continued development work for a tlmeo Development and Research Prom the very start of fuse powder charcoal produc- tion,, the relative scarcity of Ro frangula had caused concerno It was not a native shrub, there was a definite limit to the supply available^ and plantation planting could not be ar- ranged in time to bring in a supply for the years 1943;, 1944 and 1945o The most promising approach seemed to lie in the use of alternative woodSo Accordingly sample batches of carbonized Ro purshianar^ Ro cathartica. Canadian alder.,, willow, sumac and chokecherry were made and sent to Defence Industries Limitedo Pinal reports on the use of these char« coals was quite effective, and that after some preliminary trials an acceptable powder was made from Ito Owing to the scarcity of wood, the losses due to sawdust and fines caused some worryo Some reduction in the sawdust loss was made by using a chopping device instead of a saw for cutting branches of smaller diameter^ Later It dJJ. rr^r..••■ i;":.:fQnl ) 1 ■ i lo Ef^: Jfi f-t 3Li :r ■J,.. 33 was thought that the loss of fines could be eliminated by not grinding the pieces till after carbonization^ it was also thought that debarking and carbonizing might be carried out in one operaticno In thifc treatment,, the short pieces of wood v/ith the bark still on were chopped into the car- bonizing drum and brought up to the desired temperature m.ore slowly thanWien the wood was pre dried and groundo When the run was completed the charge was emptied onto a coarse screen and the fines which were chiefly from the carbonized bark,,, were discardedo The charcoal remaining on the screen was crushed and used as usualo With this process, control was more difficult, but the product obtained was aliaost as uni- form as that produced by the stands.rd methodo As initial operating and control difficulties abated, there wa;s some interest in determining the properties of char- coal which made it suitable o or otherwise, for fuse powder pro- ductiono It was thought that if any such relationship could be found, it might be of value and save considerable time when alternative woods were being investigatedo The reactivities of charcoals were compared by passing a controlled flow of oxygen through a sample of charcoaln im- mersed in a bath where the temperature was being slowly raised*, and noting the bath temperature at which the temperature of the charcoal rose above that of the batho By microscopic ex- amination in polarized light some carbons were found to be com- pletely isotropic, while others were completely anisotropic^ some were a mixtureo The refractive indices also were measuredo There appeared to be some correlation between these optical properties of the charcoal and the performance of the fuse powdero This work was reported to Defence Industries Limited, but was not carried further at the Research Council because it had reached a point where any further progress depended on making and proving batches of powder,' at the time, production was much too urgent to permit following up experimental work, no matter how promlsingo Besides that it appeared^ from proof of powders already made^ that alder would prove in place of Ro frangula, and indeed., this work on optical pro~ perties received some degree of confirmation thereby^ DEICING AND DEPKOSTINQ The accumulation of ice on the propellers and aero- foils of aircraft in flight constitutes one of the greatest remaining hazards to aviationo Many efforts have been made to prevent or remove such accumulatlonSo As a corollaryc it is also necessary, before the plane t akes off ,> to remove frost vd f BBr:<3sa isda 1: , "iq 'i&bw'i bluoo : emit .: :;r li^q 1/. =ms C9^^ 'tri^so nofT f-avo'iqrai 35 except for (d) and (m) above? however^ one hour-s dry flight in mld-=winter entirely destroyed its effectiveness just where it matters most --- on the upper wing surface So This remarkable difference at the higher altitude is thought to be due„ not to the greater intensity of ultraviolet light there^,: but to the presence of shorter^ very destructive ^ wave lengths o which are not present at ground level due to atmospheric absorption© Work on this problem ia continuingo Carburettor Deicing Because of certain disadvantages in the use of ethanol blended with fuel for carburettor deicing, a study was under- taken of the properties of other substituteso The significant properties are ice-melting capacity^, freezing point., volatility, heat combustion, and general suitability as a fuel blending agent* Methanol la obviously by far the best and cheapest ice melter^ and in most chemical properties is superior ro ethanolo However^, it has a rather poor fuel value^ and haa the disadvantage of being rather insoluble in gasoline, es~ pecially if traces of water are alao present « A number of materials were investigated for blending with the methanol^, and their octane ratings were determined by the Gas and Oil Laboratory of the Division of Mechanical Engineering© N-propyl alcohol, with an octane rating of 138, proved quite outstanding in all respects. Propeller Deicing (a) Using Deicing Pastea?- Delcing pastes for wings were again shown by ground tests to be ineffective, but similar use on propellers ap- pears to have some value since centrifugal force then removes non'*adherent ice. A feeder was designed which feeds soft deicer paste to the blades continuously and produces very good blade coverage^ without appreciable expense or loss of powero A number of commercial pastes were tested and also a number of locally compounded pastes. This work has been continued since the close of hostilities and very promising results are now being obtained. (b) By Heating Electrically}^- In co-operation with the Division of Physics and the Deicing Laboratory of the Division of Mechanical Engineeringn a Neoprene heater shoe was developed to cover the leading edge wjn (d) .1. .' ' a 36 of the propeller blade* Incorporation of acetylene black in the Neoprene renders it electrically conducting^ the degree of conductivity being controlled by the type and quantity of the Acetylene black and by the method of incor" porationo In ccoporation with Shawinlgan Chemicals Ltd<, ^ studies were mad-w of Shawinigan acetylene black in natural and synthetic rubber. The difficulty that had to be over- come in this case was the non-uniformity of the electrical conductivity of compounds containing Shawinigan blacko \Tnen the black was incorporated into the rubber, in the ordinary way on the rubber mill, the structure of 'the particles v/as broken down considerably and in an unccrfcro liable manner, resulting in low and non-uniform conductiivity. By deter- mining beforehand the degree of structure of the black by an absorption test, and by adding the black to a solution of the rubber.« the structure was preserved and a predictable and unflrm conductivity obtained. This method was used in the manufacture of the electrically conducting Neoprene heater shoeso These heater shoes are effective in removing ice that has already formed, since the layer next to the pro- peller is melted, permitting the removal of the non-adherent ice by centrifugal force* Methods employing alcohol or similar fluids are ineffective against ice which has formed before the application of the deicing fluid. The electrical method has the additional advantage that it is not dependent on the consumption of material, the supply of which may be- come exhausted if the flight or icing conditions are unduly prolonged. Successful flight trials have been made with pro- pellers so-equipped, patents have been applied for^ and the problems encountered by the rubber manufacturers have been largely overcome. Rate of Icinfi Indicator An instrument has been developed to indicate rate of icing, thus permitting prediction of the plane's future condition. Previous instruments have only been capable of measuring the thickness of ice after it had accumulated^ The first model was flight tested by the Deicing Laboratory and gave satisfactory indications. Work is being continued to include a few desirable refinements. 9x1 a ,j>fi.t:t-ouij.:ioo . ^n£ eq^o saj vo - -•-• . TO Dill 1o £ o fi o QXi-T 0 d ■ ^n e-- j. -7 .■ ; ■ c> - iBlud-Bii n.i: ^G£ild er- . - . "T6V0 ed Go t/ifl :tB.:.;' vj^'i.' .Illli:^ eri ■lBoi'.ccroeXo ©rict " -iliu-. nerfV/ o:>io^Ici" aB^ii:.. ,, ''.r YiBrriijio erfrf ni .t&g>/ "\ v ^)e:t sio cxoo ^isnnsm oXd&Ij...;:.:-. .. ^ Xd jlOBlcf drier ""ic w'lj'r:^ -,.. s.:^ ; lo oe'T-^eb oau r enoiqoell g- ^ - - - . - - ' *^^^ d-neierfb.B-non srict lo " • ' • Irf-tJn:' f)8fniox BBri flolriw or r ;jbrnll" e;/oni .!.>'•- - .' ' e^tBisaoa ©lirlw ,, elcfixlv ■^iil^<:i luo'i'i c; -iiIj. :. ^nlv/ sricr eoriie .Jbnt --.'>t neav.'-'ocf a ex.. seonBcTBcfj/a ^-^^^ QJ^-"^ :tB:i^ i:)07/or^£ ^'oos s^'caer tIt:b'£ •ImeB iBloq~non 6ri:J otlb efeoqiLrc eir'..- to'1 e. ^v- ^ 8 b i: I o 8 i "X e ^ B -.7 L ^ rie :i- on o b b a or: ^^ ■'■ ' '■<' : ^ ^ ^ j 2 alrid" eeol nooa la-ii'l ctB in^I^ '-^ aiOilDB eoonBcJ'scfue isloc t^I lo ejrj 11 o.-. on i)nocf *iBloq-non b riox/e v'in.*B.tcfo ni eeoooiie :f£'ij:"i e/iT flj-lw 0eBl§ Qi[-j --ini^rjfii-iBeiiioo ' OifT ■ pjirlil xBv/ B DO Ln;roqnoo zh..^ , . ^ ^, ...,.„ „ — nilil XBv/ 9f[d- Lhb vnomj-drii- odzt votnjjo cf Ylmii'': si; r . ellxje jborI:t9in 8lri.i- ^-^^^leJ-Brfp^ i^j o ^ d^ TBnxb^:oBi^x9 I:'9'"ijj.^ - .. -. ., rrict o^i£jnB\.. ■ - • -,; --^-^^ no'i.'i ee':s'li/jc; a.iBig erid 3ninc©Io nl r^oolI-uB lYrfcfexnlb lo eeir orU bbw jribr-f-'V,') -r-n r ctxon odT oct £)0li:B'i hr^d s^io'no IIb Eiri-'-o , . " .-xq^ .^^^ Ijeqlf: d^Brfil bniso'l 3BW ■ '' ^^i'c gnIcf:::fj:/T: Y-ts'^'-itr i _ ..li'v B bnB tiice Oi;k-o''].o noicfBvictcB i. 3 e:f:t- n--. •/ivvelicT 38 strongly repellent film was readily produced which would not wet with water 5 and which was remarkably difficult to remove. It was then found that this is a very general pro- perty of organic silicon compounds; friction on glass with rouge breaks them, and the fragments attach themselves to the glasso All organic silicon compounds available acted simil- arly, producing varying degrees of attachment and repellency. Prom a general consideration of such compounds it was considered that if the friction could activate it, the finest result might be secured if the silicon compound had a chain of two or more silicon atoms, and all side chains were hydrocarbon. Consequently hexa-ethyl-di-si licon was syn- thesized, and it was found to produce very good results indeedo At this point the use of powders other than rouge were tested, but the only ones found to produce the effect were barium sulphate, rouge, and lampblack, being better in the order given* Tests of a great variety of lampblacks and car- bon blacks showed that acetylene black was markedly better than all otherso Shawinigan Chemicals Limited made available a wide range of acetylene blacks, and of these "Super Hyflow" was se]fi cted as best. It is now used as standard. Silicon bonding compounds were then synthesized con- taining silicon chains of one, two, three, and four silicon atoms^ with hydrocarbon side chains up to sixteen carbon atoms. The butyl compound with three silicon atoms was found to pro- duce the most repellent bond, while the butyl compound with only two silicon atoms was found to give the strongest attach- mentj in cases where it is desired that the residual bonding compound should be volatile, the ethyl compound with two silicon atoms, carefully purified from higher constituents was found to give best results. The wax coating was then reinvestigated, and the purification of each ingredient proved to be of the greatest importance. It was found that even the cloth by which the materials are applied must be specially purified to give best results© FHirther complications are also introduced by dif- ferences in the techniques required to produce satisfactory results under such different conditions asj- ...T^i . ' ^iJii. J. '.' >J - 39 (a (b (c (d (e (f (g (h (1 First application on new glass windows 5 Maintenance on glass windows 5 Application to plastic v/indows, both acetate and methacrylate 5 Application to high temperature 5 Application be^ow the freezing point; Application to windows during rain; Possible renewal during flight if continued rain ultimately wets the window; Effects of alcohol or heat used for deicing; Effects of gasoline or oilo At first, different materials or techniques were necessary for each of these conditions; but after a thorough Investigation, with constant modification of the technique, the waxes and the purification methods, a simple kit and a uniform technique were developed which are entirely satis- factory under all conditions. The kit consists of (1) a packet of purified pieces of cloth for the applications, and (ii) two collapsible lead tubes containing respectively the bonding paste and the wax paste o The instructions for use are as follows: clean and dry window with the bonding paste, and polish; rub hard all over again with the bonding paste, and polish; apply the wax, and polish at onceo This treatment leaves an invisible film, free from optical distortion, and provides very clear vision during flight in rain without windscreen wiperso It has the ad- vantages that:- (a) Application is rapid, requiring only a few minutes per window; (b) The base material may be any kind of plastic or any kind of glass (including fused quartz); (c) Plastic windows may be treated wet or dry; glass windows may be retreated wet or dry^ although the original application to glass must be while dry; (d) The coating can be revived in flight either wet or dry with a hand-operated wiper, or with a spray of special wax solution applied in a manner similar to alcohol delclng; (e) The materials can be applied at any temperature from -40<*P to -USS^P; (f ) Curvature of the window does not limit the action as it does in the case of windscreen wipers j 9?. ... ^ 1 a £■ > J, Q .1 & ■ II Ol ci iS 01^2 tifct - 10 '10 t":":oo Bt?Ji-i: » j.«.' J j. ^ \^ _r,-jf-c._f -r ^iiB'-TO oicl'Ji sic 10 f aL--: vj 'jc rt 8W 1 srf • .^ .1: e t rf '9 * I "^ 40 (g) The treatment helps prevent scratching of plastic windows., and produces the visibility of existing scratches I (h) Plight under dry conditions does not reduce the sub- sequent life under rain., and treated windows may re- main dormant in or out of the hangar without damage;; (i) Alternate exposure to rain and to dry air does not accelerate deterioration; (J) So far as is known.r the coating is not affected by any deicing procedure; (k) The coating is not damaged by oil, gasoline, alcohol or glycol; (1) Oil may be removed in flight with the **reviver" spray; (m) The materials needed are cheap, non-corrosive, free from chlorides, and stable in storage. A standard ground test has been developed in v/hich a blower forces air and water droplets against the treated glass in a manner corresponding to flight, at 300 mop»ho, through rain falling at a rate of one inch per hour. Under such test, the initial clear vision obtained by this treatment is re- tained unimpaired for seven hours; then deterioration becomes noticable, and after seventeen hours, performance is the same as for untreated glass. Plight through hail removes the film entirely, but as explained above, the film can be renewed in flight. Tests in flight conducted by the Test and Development Establishment of the K.CoA.Po proved very favourable j, and after extensive service testa the Air Porce has adopted the treatment as standard. ANALYTICAL LABORATORY This laboratory did not of Itself undertake any re- search problems, but it co-operated actively in the work of many of the other laboratories. During the five and a half years of the war, the Analytical Laboratory of the Division of Chemistry made some 50,000 determinations on approximately 17,000 samples. However, the activities of this laboratory can hardly be considered "routine" since the infinite variety of materials submitted for analysis was a continual challenge to the technical ability of the staff and required chemical proficiency of the highest order. These were in addition to analyses of textiles, leathers.^ paints^, detergents,, corrosion products, metals and alloys, etc The laboratory, on request, also prepared . 3il r i.C. or' ^ :t9ilJ .81 OC iiiiC ?1 br 1} £xc'¥i) eveG J- TqabB .. c ^ l: cri BHO. -)J j\'', jfj'r^r HBO !> 9 "IB c: ^"^' i a '.'.; ii 1 ,^ . .:' fc f-^i^^ i- ^ "^ Bs£ 41 bibliographies on a number of subjects for other labora- tories of the Division, SALVAGE At the request of the Department of National War Services, the National Research Council undertook in 1940 to study the question of salvage with a view to determining whether it would be advisable to institute a national sal- vage campaign, and a member of the staff of the Division of Chemistry was asked to investigate this question ami to pre- pare a report. At that time there was considerable public agitation for a salvage campaign^ but some of the controllers of supplies were known to be opposed to it. In the time available it was not possible to conduct an exhaustive enquiry, but each of the principal types of salvage materials was examined (i) as to its statistical position, (il) as to the possibility of obtaining additional supplies through a salvage campaign;, (iii) as to the ability of industry or export markets to absorb any additional sup- plies which might be collected, and (iv) as to methods of collecting and marketing. At the time this survey was undertaken, no real shortages of supplies had developed. The Department of National War Services was advised that under the conditions then prevailing the collection of additional salvage material could be justified only if carried out on a voluntary basis, and that even then the financial returns would probably be small. If collections were made, it would be advisable to include all types of scrap of potential value, and not merely those of one kind, as was then being done. It was found that the collection of heavy iron scrap (in the aggregate of greatest value) and that of the common base motals and paper were already being fairly well t aken care of, but that a moderately favourable situation existed with respect to aluminum, tin alloys, wool and cotton rags, and rubber. If a campaign were undertaken, it was recommended that the col- lection of scrap be handled through established dealers. MISCELLANEOUS INORGANIC INVESTIGATIONS A number of minor investigations in the field of in- organic chemistry were also undertaken in the Divisional Laboratories. 42 Purification of Sea Water At the request of the Navy, several methods of producing potable water from sea water were Investigated© Some work was done on synthetic r^sln Ion exchanger So Eventually a still was developed which operated automatic- ally If the relative humidity was less than 100%, Maximum distillation rates of 60 cco per sqo fto of still surface per hour were obtained. Potassium Tetroxide At the 3ugg3stion of the late Sir Frederick Banting, potassi^jim tetroxide was produced in small quantities for experimental purposes. This material has been used in the ventilation of submarines to maintain the oxygen supply, and has also been considered for use in a special type gas mask in which it provides oxygen Independently of the ex- ternal atraosphere© Carbon dioxide exhaled from the lim-^.s, coming in contact with potassium tetroxide, reacts tc form potassium carbonate and to liberate oxygen. Methods of producing potassium tetroxide were studied in the laboratory, and apparatus for making this chemical on a semi-pilot scale was builto In this apparatus potassium (vaporized by heating a mixture of potassium chloride and sodium metal) was blown by a current of nitrogen, thrdugh a burner^ where, it was mixed with oxygen, into a larger chamber, where it burnedo The product of combustion settled out in the chamber as a fine powder of potassium tetroxide. As this material in its original form was too finely divided for use in respirators and the like, it was granulated by stirring, while warming; Just enough to make the particles coalesce. Asbestos The utilization of Canadian asbestos had been a subject of investigation by the Division of Chemistry for some time before the war. As this was a long term project not likely to have much bearing on the conduct of the war, these activities were soon terminated and the most recent results were published. During the war Canada continued to export consider- able quantities of certain grades of asbestos to neutral countrleso The Department of Trade and Commerce feared that this material might contain quantities of longer fibres that could be recovered and shipped to Germany by pro-German neutrals O J o .t of) 911 i exlj fir JjOELf neecf £.t-r{ lejit-d-uiTi eiri'^' ,^^0c; . . . i^ K2;'5iri:t ^nfc\ lo ineTioc .. . . . .. h ejtif^ eA .eL^. ... .. . . ,- . ., e- "^ /, .. : t oEj? iqI: beblvlb •. oca lol Ibh.' : Ixtxisct^w ctoa[,G'iq rn^bi , , _ & ci- ,_ ". .tsw , _ :oa ^-iBw erict lo d-oi/bnoo sn^ no ^^n' ^^ox/m evBd. o.t xleyi^ [ ;fon daeoo'i Jeon edc^ bn^ Ive^iinlme:' iicc ''-"d" - O'l XB'iifjLfeft Ou :. ^ . j'.too ';•; '^£nifO .; end- ■:' j e'i5 'f.n?=:r ve-cj oelfc ©VBii .... -•?^i-P- ^ - ^ 44 Association Committee to establish a Canadian Code for Head and Eye Protectiono REVIEW OF FOREIGN RESEARCH ORGANIZATIONS At the request of the Acting-President of the National Research Council a member of the staff of the Division of Chemistry undertook, in 1942 and 1943, to prepare a review of the organization of research in the major industrial coun- tries, with particular reference to plans for post-war re- searcho Included in the literature survey were Australia, Prance, Germany, Great Britain, Japan, the UoSoSoRo, and the United States o For each country an attempt was made to give enough of the historical background to permit one to understand how the present system had ariseno The principal research or- ganizations were listed, their fields of activities and avail- able funds were indicated, the relation between the^i (if any) was set out, and references to more complete information were citedo In the case of the United States there were listed the chief research foundations and trusts, the many insti- tutes and associations having laboratory research as a major activity, and the larger private industrial research labor- atories j a brief review of the work of several of these was includedo Special attention was called to the United States Government's research studies made by the National Resources planning Boardo A review was included of the Kilgore bills i*iich, though not ultimately passed, nevertheless reflect the thinking of many Americans. Letters were also written to about a dozen prominent research directors in the United States, asking their views on such questions as (i) the relation between research spon- sored by governments and that of the universities and pri- vately endowed organizations, (ii) means of promoting co- operation between research organizations, (ill) the degree to which planning for research should be carried out on a national scale, Tlv) the advisability of centralizing govern- ment research, or otherwise, (v) the probable trend of re- search after the war, and (vi) how peacetime research should be related to national defenceo The replies received differed widely from one another, as might be expected, but were defin- itely stimulating and helpful© J^^ ""to 'ID y, -■ ^' iit^ild --•lil.v 3nJ 3., ...r\'-. .■n.j'on" f^t f-j^^f R r f" ft' c e •let (tooiloi ^- ■errrA v ■nor.-- ifoiBseei nas' -co "^ >'iq aO ?;. 9^'t, J (111) -m ev o 3 an 1 s 1 J ■ 1 o v: t : i i js 3 x .- f;- b .'^'^IX^ 'ii. C^l ')x;t*iSinB*rxc jo J: ) . elij ^. snoi. J;3.a ou es 45 REPORTS ANS PATENTS Refractories Craig, Jo Wo Chrome for Canada o Trans o Cano Insto Min* Meto 43^ 762-780o 1940, Craig, Jo Wo Refractories Industry in Canadao Journal of the Canadian Ceramic Society, 9, 21-27, 1940o Craig, Jo W. Canadian Basic Refractory Practice? Algoma Steel Corporation,, Blast Furnace and Steel Plant, 16^ 15-18, 1942. Hodnett, Lo Production of Refractory MaterialSo Cano Pato 429,272, Augo 7, 1945. Hodnett^ Lo A Spa lling -Resistant Chrome Refractory, Can© Pato Appo 492,272, May 5, 1942. Hodnett, Lo , Lathe, Po Eo and Perry, Jo S, C. Brucite- containing Refractories. Can. Pat. App. 492,271, May 5, 1942o Lathe, Po E. Basic Refractories in Canada - 1914 and 1939. TranSo Can* Inst. Mint, Meto 43, 83-99, 1940. Lathe, Po E. and Hodnett, L. Refractories for Furnace Linings. Cano Pato App. 509,642, Jan. 7, 1944. Lathe, Po E. and Hodnett, L. Refractories for Furnace Linings. U.So Pat. App. 518,670, Jan, 17, 1944. Lathe, Po Eo , Prince, A. T. Treatment of Siliceous Dolomite. Can. Pat. 425,184, Jan. 23, 1945. Perry, J. So C. and Prince, Ao T. Bonded Refractories for Furnace LiningSo Can. Pato App. 508,655;, Dec. 2, 1943. Perry^, J. So Co and Prince, A. T. Bonded Refractories for Furnace Linings. U.S. Pato App. 565,063, Nov. 24, 1944. Pitt^ N. P., Halferdahl, A, C. and Lathe, Po E. Stabilized Magnesia Refractory. Can. Pat. 411,352, Mar. 23, 1943. Recovery of Magnesia Lathe, Po E. Potential Sources of Magnesia in Canadac 34 ppo, Jane 1941. 2^ zernoj' ^nJ^A ,. d-ertl .[T.80 -1 a. 3 . ^-M .ii nH oHbO aSlii :.ejBlu v'lo toiii-r le: ^ ' ''iboE .hbO .t^^^^^^'^'i^^ arao:, •/•••■■ .T iLoR ..95 ex tPiB Me. I - Bbinn b;:±--3 ©fld-BJ dcrlmoIoCI 3ij. 3 -1:0 driera^B->'T .^ rsnlT'-i , .S '1 , ©-idfiJ J es:^ af^BO S ^L' , ^'"■:. aal q X,'-!-^-'^ ,.qq I'S ,BfcB>iT:BO ill sr-^ i;.:oc:i l£,J: ■ ;-,).''0 1 -4 46 Magneaj-um Pidgeon,, Lo Mo New Methods for the Production of Magnesiumo Transo Cano Insto Mine Meto 47^, 16-34 (1944) o Pidgeon, Lo M« Thermal Production of Magnesiumo Cano Pat* 420.239, May 16, 1944o Pidgeon, Lo Mo Apparatus for Reduction of Volatilizable Metals. Can, Pate 415^,764, Oct, 12, 1943, Pidgeon, Lo Mo Apparatus for Reduction of Volatilizable Metals, UoSo Pato 2,330,142, Septo 21, 1943. Pidgeon, Lo Mo Thermal Production of Magnesiumo Can. Pato 420.240, May 16, 1944. Pidgeon, Lo M. Production of Magnesium and Apparatus Therefore Cano Pato App, 488,487, Dec. 18, 1941. Pidgeon, Lo M. Apparatus for the Reduction of Volatilizable Metals. Cano Pate 420,241, May 16, 1944. Pidgeon, Lo M. Apparatus for the Reduction of Volatilizable Metals. Cano Pat, App. 488,488, Dec* 18, 1941. Pidgeon, Lo Mo Direct Production of Ductile Magnesiumo Cano Pato 420,242, May 16, 1944. Pidgeon, Lo M. Direct Production of Ductile Bfcignesiumo UoS. Pato Appo 427,004, Jan, 16, 1942. Pidgeon, Lo Mo Production of Magnesium and Apparatus Therefore UoSo Pato App. 426,009, Jan. 8, 1942. Pidgeon, Lo M. Thermal Production of Magnesiumo UoS. Pat. App. 426,010, Jano 8, 1942. Pidgeon, L. M. Apparatus for the Reduction of Volatilizable MetalSo UoSo Pato App. 426,007, Jan. 8, 1942. Pidgeon, Lo Mo Apparatus for the Reduction of Volatilizable Metals. UoSo Pato App. 426,008, Jan. 8, 1942. Pidgeon, Lo M. Method and Apparatus for Producing Magnesium. UoSo Pat. 2,330,143, Sept. 21, 1943. f-.yf-^ ^r. ij^ Pi' 6lrfBo:.lIi::T.eI . f - r £ i ' ■! r^>Vl- ,nj^U .>r^r^ -T 'r^ -....^ - ,^^-,^ .-C ip Tf ■I 6.L •q T:olen;='fij. sifctv^'ih- cfA ip 0,7 iB^ .S ,U .nuTl 8 ,mu o-in. q .. 'I .. > 'i o'o '. U 0 f' 47 Pidgeon^, Lo M© Method and Apparatus for Producing Magnesium^ Cano Pato 415^765;, Octo 12^ 1943c Pidgeon^ Lo Mo Apparatus for Producing Magnesium by Thermal Reductione Cano Pato Appo 490<,123i, Pebo 21^. 1942o Pidgeon; Lo Mo Apparatus for Producing Magnesium by Thermal Reduction, U«So Pato App<^ 453o452, March 5, 1942o Pidgeon, Lo Mo Vacuum Apparatus for Producing Magnesium© Cano Pato 420^244, May 16, 1944, Pidgeon^ Lo M« Vacuum Apparatus for Producing Magnesium© UoSo Pato Appo 434,933, March 16, 1942© Pidgeon^ Lb M© Apparatus for Producing Magnesiums Can© Pato App© 492,103, April 30, 1942© Pidgeon, Lo M© Apparatus for Producing Magnesiumo U^So Pat© Appo 442,411, May 11, 1942© Pidgeon, L© M© Method and Apparatus for Recovering Vola- tillzable MetalSo Cano Pat© App© 492,764,, May 20^ 1942^ Pidgeon, Lo M« Method and Apparatus for Recovery of Vela- tllizable Metals© U„S, Pat. App„ 445n714, June 4, 1942. Pidgeon. Lo M© Method and Apparatus for Producing Magnesium^ Carlo Pat© App. 505,201, Aug. 7, 1943© Pidgeon, L„ M^ Method and Apparatus for Producing Magnesium© UoSo Pato Appo 498,206© Aug© 11, 1943© Pidgeon, L„ M© and Phillips, No Wo Po The Production of Anhydrous Magnesium Chloride© Trans© Electrochem© Soc©, 78^ 91-^113 (1940©) Pidgeon^ Lo M« and Phillips, No Wo P© Production of Anhydrous Magnesium Chloride. U©S. Pat© 2,356,118. Aug© 15, 1944© Drying Air for Blast Furnace Use Wolochow,, Do Dry Blast Production© Can© Metals Metl© Inds© 5, 230 --237 (1942)© imijleox .Bff; iBtn- • ITG' 0.^ V b; J .Li.. ^nqh -. j; ,' ■'t'O ':'; »•;*.>; A .l4 ..el^al .IcteM elB^f'M oW 48 TJtillzation of Open Hearth Slag Lathe, Fo E. The Utilization of Sydney Open Hearth Furnace Slag, N.R.Co Publication No. 1028, 88 pp., Nov. 1941, Lathe, F. E. The Utilization of Phosphatic Open Hearth Slag. Part I: Effect of Rapid Cooling on the Solubility of Phosphoric Acid. Jour. Soc. Chem. Ind. 62, 24-28 (1943). Lathe, Fo E. Annotated Review of Recent Literature Prepared for the Committee on Sydney Slag. 77 pp.. May, 1944. Wright, L. Eo , Leahey, A. and Turner, R. C. The Utilization of Phosphatic Open Hearth Slag, Part III The Avail- ability of Phosphoric Acid as Measured by Yield and Phosphorus Recovery in Barley and Clover. Jour, Soc. Chem. Ind. 62, 28-31 (1943). Vanadium Recovery Lathe, F, E. Review of Recent Literature on Vanadium Recovery with Special Reference to Vanadium Iron Ore. 32 pp., N.R.C. Publication No. 1075, June, 1942. Lathe, F. E. Controlled Desiliconization of Pig Iron and Recovery of Contained Vanadium. Proceedings of 26th Conf • , National Open Hearth Com., Am. Inst. Min. Met. Eng., 166-172 (1943). Lathe, F. E. Method of Refining Pig Iron and Recovering Vanadium. U.S. Pat. App. 532,165, April 21, 1944. Nickel, Copper and Platinum Metals Lathe, P. E. The Determination of the Metals of the Platinum Group in Nickel Ores and Concentrates. Can. Jour. Res. B 18, 333-334 (1940). Atmospheric Pollution Katz, M. Atmospheric Smoke Conditions in the Vicinity of McKinnon Industries, St. Catharines, Ont. N.R.C. Report No. C671-45S, September, 1945. Supplementary Reports, November 30 and December 28, 1945. Katz, Mo Investigation of Smelter Smoke Conditions in the Sudbury Region, 1945. Report of the Smelter Smoke Committee, Ontario Department of Lands and Forests, Toronto, Ont., 1946. 8j^ ■■'JBJ JbiiB i • 008 e^i; ..' , : • Si>ei ,enx.L .aVOI .0:^ noictj^' bnj3 noil 3.c^ "io no.! r^BsIno^ t ':eoC h&IXoM.jrcO oc. 'cJ gni-Tsvooej"' /toil ; " ':foM ^rf t.fiJ .M^Gi ,1'. > .::ia. J o'- ^.. ...... r . - . ... . ' - -.QincfA X 1 B ;t a onio i q qsjt . . ? •". 1^ ■ . 49 Katz, Mo and Chapman, P. Ho Trail Smelter Questiono Sulphur Dioxide Content of the Atmosphere 1937 to 1940o Sup- plement to Canadian Documents Series B and BB; King's Printer, Ottawa, 1940, Charcoal for Fuse Powder Greeno Po Go Pinal Report on Carbonization of Rharaus Prangula and Alternative Woods. N.R.Co Report No. C941-45S, March 28, 1946o Deicing and Defrosting Broughton, Jo Wo Effect of Solvents on Octane Number of Aviation Puel. N.R.C. Report No. MP867, Sept. 23, 1942o Griffith, T. Ro Aeroplane Propeller Deicing* NoR.C. Report No. C2839-42S, Dec. 26, 1942. Griffith, T. R. Present Status of Research on Aeroplane Pro- peller Deicingo NoRoC. Report No. C2839-42S, Dec. 26, 1942. Griffith, T. R. Electrically Conducting Composition. U.S« Pato Appo 515,870, Dec. 27, 1943, Griffith, T. R. An Electrically Conducting Article and Method of Producing the Same. Can. Pat. App. 525,591, April 14, 1945, Griffith, To R. An Electrically Conducting Article and Method of Producing the £%me. U.S. Pat. App. 594,800, May 19, 1945. Griffith, To R. and Orr, Jo L. Prevention and Removal of Ice or Prost on Aircraft Parts. Can. Pat. 428,132, Dec. 6, 1945. Griffith, T. Ro and Orr, J. L. Prevention and Removal of Ice on Aircraft and Like Parts. UoS. Pat. App. 493,700, July 7, 1943. Griffith, To R. and Orr, J. L. Method of Making a Heating Device. Can. Pat. 429,005. July 24, 1945. Griffith, T. Ro and Orr, J, L. Prevention and Removal of Ice or Prost on Aircraft Parts. U.S. Pat. App. 562,878, Nov. 10, 1944. ■•" res jj,nii H seHor «^ :3-[. ;■ ihl cO "- ■ Oil enBlqo'io.' ,3S .ceC ,^-: # c< i,U .>aoJ:JiE3q:fiv ,ei \'bm no oeU 10 1 j-nelloqoH .i.'sH --'^ p., ---o - 'ilA no eeU -lol uii-IIo^ •! .G •■d8 a^i^GI ■ , ^ . - si-'iBioiIA lol ctneXloq; " ' ,n>2rate:r8 .UiY* TC oriC 10 ,-'. ieH P ■•. : T rr ilA . ■'■ < '. 'J ■ , ^ . ■ i -V- X ClI acl:^91 ^Ig o"l^^i 2^::i' :>xO ooW JioqeB .:..:.:. »OoHo'*'I oBlBiiuJ-BM iBn.tS '10 eI.i£d-6CI iBolirfsr^" 52 Stedmarif, Do Po and Sterns, So Rain Repellent for Aircraft Windows - Chemical Details of Pinal MaterlalSo NoRoCo Report NOo C51-45S, April 13, 1945o Steciman, Do Po and Sterns, So Rain Repellent for Aircraft Windows - Tests of NoR.Lo 139o NoRoCo Report NOo C403- 45Sp June 25^ 1945 o Stedman, Do Po and Sterns, S* Rain Repellent Instructions© NoRoCo Report NOo C499-45S, July 28, 1945o Stedman, Do Po and Sterns, So Rain Repellent for Aircraft Windows - InstructlonSo NoR«C. Report No. C732-45S, Oct. 12, 1945o Stedman, D. P. and Stems, S. Rain Repellent for Aircraft Windows - General Description and Useo N.RoCo Report NOo C907-45P, March 1, 1946. Stedman, Do Po and Sterns, So Rain Repellent for Aircraft Windows - Materials In Kit. N.R.Co Report No. C933- 45P, March, 1946 « Salvage Lathe J, Po Eo Proposed National Salvage Campaign. 30 pp.. Novo 1940. Miscellaneous Inorganic Investigations Brown, A. Go Test of Desslcants to Specification J.C.N.AoAoPo -Po -218, N.R.C. Report No, C1814-44S, Peb. 26, 1945. Brown, A. G. Impact Tests on Hardened Lenses. N.R.C. Report NOo C203-45S, May 13, 1945* Brown, A. G. and Stegmeyer, 0. Effect of Excelsior on Cor- rosion of Metal PartSo NoR.C. Report No. C877-43S, July 20, 1943o Puddlngton, I. E. Purification of Sea Water, N.R.C. Report NOo C1299-42S, July 20, 1942. Puddlngton, lo E. A/S Recorder Paper, NoR.C. Report No. C418-44S, June 7, 1944o Puddlngton, I.E. Design for a Comf ortometero NoR.C. Report Noso C829-44S, Aug. 24, 1944, and C1519-44S, Dec. 22, 1944, s:e -• T- r'XjOvlBd Q o qq 05 oXigii/iq^iBO e3Bvl83 XartuJ: eno-t: it e^Jtrte e v nl .;: . x;.e^; .tM itioqefi cOoHoPI ,e'>eneJ r-eno^iiiPi. no B.:.*ao'r doBaii:! «v „.\ t6I -ToO nc leoxS "to >roe'i'12 .0 c,Ti:>'/;offise^^ ^'" ' -A nitwoTH 42S^"i^'V60 oO['I ;i^.o::&H =Oo?icIl ^ciJ-'ib*! iBcteM : d-'ioqoH .OoHcW ^'led-BW v.&u "jO noJ::t-BoiliiL4 oG; . ;/l oI-^^'9I ..V 6-:/;L ,.3^^:^ 3X^0 :oa@H oO.HoH ri©d-6iJCJ-*io'irrfoO b -lo'-t xi^i .Mit.ir^ 53 VanWinaen, A« Superfine AsbestoSo U, So Pat. App, 379,641, Pebo 19, 1941o VanWlnsen, Ao Superfine Asbestos and Method of Manufacture Cano Pate 430,679, Octo 16, 1945. Wolochow, Do Thermal Studies on AsbestoSo II: Effect of Heat on the Breaking Strength of Asbestos Tape and Glass Fibre Tape. Can. Jo Res. B19, 56-60 (1941). Wolochow, D, Thermal Studies on AsbestoSo Ills Effect of Heat on the Breaking Strength of Asbestos Cloth Con- taining Cotton, Can. J. Res. B19, (1941). Wolochow, D. Spinnable Material in Group Pour Asbestos Pibresc N.RoC. Report No. C1155-43S, Aug. 30, 1943. Wolochow, Do Comparison of 3R Asbestos Pibres. N.R.C. Report No. C1296-43S. Sept. 21, 1943. Wolochow, D. Comparison of 3R Asbestos Pibres. N.R.C. Report Noo C1406-43S, Oct. 8, 1943o Wolochow, Do Spinnable Material in Group Pour Asbestos Pibres. NoR.C. Report No. C1412-43S, Oct. 12, 1943. Wolochow, Do and White, W. Ho Thermal Studies on Asbestos. It Effect of Temperature and Time of Heating on Loss in Weight and Resorption of Moisture. Can. J. Res. B19, 49-55 (1941) o Review of Poreign Research Organizations Lathe, Po Eo The Organization of Research in Selected Countries. 90 pp., Dec, 1943o Zii .(IJ^^- ,^.^. e o :t a ed s A ^iiic " q i/o 1 0 ctl I b 1 ^ f- J a^T -^ f ■ ' .- v:i ' e ► Bo:tE9aeA no ealxjj.-fP; iBirfo:.... .H oV; .6^1 -r-JiA*" e8oJ no ^ni:^Be¥. lo amlT bnB 9tx'.j"s-t eBsH oL ,nBO oetucJsloM lo nolrt^T'io^i;: aiio X d 3sInBE':rO no ^XBe ' " :^ivQfi j^9ctot)I?8 at ffo^T-eEs:-! lo no^ ' "^ o.ed:ti3j o£i-%I : oOe.. -i^qq -- >*-. ■■■0 54 ORGANIC CHEMISTRY EXPERIMENTAL EXPLOSIVES ESTABLISHMENT History of the Establiafhment The evolution of the High Explosives Sub -Commit tee on the Advisory Committee of Industrial Chemists has already been outlined in the Historical Introductiono Under its sponsorship, research on explosives was started in several universitieso Out of this research came several new ex- plosives or promise of new methods of manufacturing existing explosiveso No matter how promising laboratory tests may be, it is absolutely essential, in the case of a new explosive, to prepare several thousand pounds for field tests or, in the case of a new process, to carry it through the pilot plant stage in order to discover and solve manufacturing problems o The High Explosives Sub-Committee brought the need for such an explosives pilot plant to the attention of the National Research Council, who, in the spring of 1942, rec- ommended to the newly formed Army Technical Development Board that such facilities be provldedo The Board thereupon allocated one hundred thousand dollars to the projecto About this time, it was learned that the Department of Munitions and Supply were considering the construction of a propellant development building and laboratory, but had not passed beyond the initial layout planSo It occurred to some of those Interested that, if this plant were also needed, it might advantageously be combined with the experimental high explosives buildlngo After thorough investigation, this sug-- gestion was approved by the Army Technical Development Boardo It was the opinion of those interested in the plan that the project should be a permanent one and that, for this reason, the establishment should not be situated beside a war-time plant, which might be dismantled after the waro It was also thought that it should be wholly under government control and, therefore, that it should not be placed on pro- perty of a private explosives manufacturer* Visits were made to similar establishments in the United States and it was found, from their experience, that explosives development laboratories should be situated close to a weapon proving range o A suitable site was therefore sought, and found, adjacent to the Artillery Proof Establish- ment at Valcartier, Land was made available there in February 1943 o #"5 Yi^iSQiXB BBrf £i cfe I'll oriC '...... . ..:!jf)r^I lo .._-...... -. , ^. . l£T:sv9S ni ' ^ Levleclqr.e no r:oT:£e*;e'i -xe '*v6n I. .V. v.. . . . . rio'ix-ieeai eiri.T lo •t>.'0 Snirfelx© ^ni:'i'iJJOB*i.r/:iBrn lo 8^n^Id•em wen lo etl;' I'a ^ecf-^Bfn Ecteei viouBToc :oiq woil ^'^ ^.eviEoIqxe wen s 'lo a* -jXsiJne. ^ al (v^ro ejBQct- oioll r^nsauoft:}- . ■LtHBlq doJlq arlct dguc-iriJ o^ o oct .as -0 8*1 -SI^QI lo sriliqa Qi: rf-nemqoloveC iBolnnoeT .p i^ ij^^u'i'... noqjjeTedct' biBoQ. eriT ofce^- ■ <• -•"i' -'■i aeJ: . ^..^.. :. . .... 0^09 tciq 9rlci"o:^ e^ .iori;:^ be'i^n.jd 6jto te i d^n eni;t ia q stl en:i -j &n ct £■ en -i b a I g b w :t I ^ er.; .. ...'•■* s- . 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In the meantime 5, the expanding program in explo- sives development and research had made reorganization neces- sary and towards the end of 1942^ the National Research Council had set up an Associate Committee on Explosives to coordinate all work on explosives development,, to supervise the extra mural research on explosives^ and to supervise the new Experi= mental Explosives Establishment© In the meantime, too, pre- liminary plans and cost estimates had been prepared by the staff of the Division of Chemistry and funds had been made available through the Army Technical Development Board in January 1943 o At the request of the Canadian Government , the United Kingdom provided an expert research director from Wool- wlch Arsenal to guide the establishment through its initial stageSo After his arrival in April, plans went ahead more rapidlyj construction was started in late summer, 1943, and continued throughout most of 1944© While construction at Valcartier was in progress, the nucleus of a technical staff for the new establishment was collected at the National Research Council in Ottawao Since it was virtually impossible to obtain men with training in the field of explosives manufacture, because of the existing demand for such men by industrial firms, an effort was made to familiarize the initial staff with explosives practice by sending them for various periods of time to places such as Nobel and DeSalaberryo In this connection., very excellent co- operation was received from Defence Industries Limited and from the various plant managers© Coincident with this training period^ the staff pre- pared plans and blueprints for the pilot plant manufacture of the newer high explosives© With the assistance of DdoLo en- gineers, plans were prepared for the Installation of the sol- vent propellant presses in the nearly completed buildingo Three surplus presses from Defence Industries Limited, Nobel, were secured and delivered to the siteo Laboratory furnishings^ such as work benches, fumehoods, equipment.^ and chemicals, were planned and ordered for the laboratorieSo Plant equipment, consisting of motors, mixers, controllers, and countless other items, were placed on order and eventually secured from numerous sources© The staff likewise participated in experimental work Insofar as facilities and conditions at the National Research Council would permit© The first experimental work undertaken by the staff, while in Ottawa, was the development of a cli- matic storage cabinet y^iich could be used for the testing of ammunition and explosives under conditions of heat and humidity likely to be encountered anywhere in the world© A standard type of construction and control mechanism was sought, which would- 9-J Bnibioo 0 -. . u ev i e o i qx i ■" -I -, f.-< ..,■■,- io iTBOcr Jx/oj;*ii'OiaJ ;■ liJfTT nem re.aalJ ;iico . s e ©'130 T:q a 1 -; b w sm jfierariaiXcr^s.:^'-'; v, ejB fi oBlq \0 ■■> *^a bnjB bed-inrfJ £6. -3 io edrs Xoo X ;ti eev. ©ffcf 7Cf iic: > ..iiTiai) :nl f ,.*:... 1^- . .^dofl jei B . rj-B'ieqo ■im anBiq ei,foi:T.Bv oxlct mo rl to e^lUo w b'Ijjh Bfi-: r ■ .oe Olid- Io fiolr^Bi eimr obIbo Lnario bnB ;t. p^ rtn ■"""■" .' r^diio ^ftvv .itJf.'nTxi. p! i^in'sevt? iiiie -JT.flq .;«.>.; esfid" p-reei.il5 ni c- tn©v- moil - . ..oTfiT >AievJ:j .B a lew .ILfl .,£ eiloned" foi/B .t 10 1 beieh" .. i/mlq A in: ..a ^lOCtO;. f^thCiOO ■i9i)io no bODBlO . .lijoe ne^ . iCiii 2f 10 w. i a;tn 1X0 & to clriemqolev :ue A ..iiXiQw 7-'^bfi;' - XBlosnl ■/ Tx on jj-qO Bdi v6 ' LaL'mmB oo b):iB nol:foifi^^noo 'Io 56 be flexible, automatic and reliable^ Two experimental units were constructed, and one in particular was subjected to a six months* test period^, which illustrated its inherent soundness of designo Particular attention was devoted to developing a simple cycle control mechanism which would per= mit the automatic alteration of the test conditions between predetermined limitSo Considerable success was achieved in this direction and very satisfactory units are now in opera- tion.o Apart from experimental work, the group took an a ctive interest in all published papers and two of the members com- piled a very extensive card index of all explosives documents and reports. Late in 1944 members of the group began to spend more and more time at Valcartier and the job of fitting out the various buildings was commencedo By the spring of 1945 the three presses were in place and the laboratories were furnishedo As soon as the rolling house was vacated by the contractor, the rolls and auxiliary equipment, including an automatic deluge system, were installedo The climatic test hut was furnished with three test cabinets and all put in operation. Control and recording gear for five more cabinets were placed in positiono By VJ'-Day numerous dummy batches of propellant had been worked up in the kneaders and extruded in the presses to check the operation of the equipment. Some minor changes had been found necessary. A few batches of *'live" propellant had been processed and further batches were going through from day to day. The Experimental Explosives Establishment was sug- gested by the High Explosives Sub -commit tee, was financed by the Army Technical Development Board, was administered at first by the National Research Council, and finally was turned over to the Army - on September 1, 1945, it became Wing C of the Canadian Armament Research and Development Establishmento Although it was not^ strictly speaking, an activity of the Division cf Chemistry, the divisional staff made large and important contributions in the formulation of plans for it and the Division of Chemistry gave it a home until the premises at Valcartier were ready for occupancy. ETHYLENE OXIDE In addition to its use as a raw material in a wide range of organic syntheses, ethylene oxide shows considerable promise as a fumigant^ bactericide, and insecticide. In all a I. t d"n0m.. itee. lIA nT ^af;! 57 these fields the chief obstacle to a much wider use of ethylene oxide is the present restricted available supply and costo At the present time no ethylene oxide is produced in Canada c, while Canadian imports of ethylene glycol (the most widely used derivative of ethylene oxide) for antifreeze purposes alone amounted to more than a million gallons a year in 1939o An Investigation of the vapbur phase oxidation of ethylene to ethylene oxide with air ovdr a silver catalyst, begun In the Division of Chemistry in 1938^ has ltd to the development of an economical process for the production of ethylene oxide and ethylene glycol from readily available hy-= drocarbon fractions such as oil refinery gases,, without re- quiring the isolation of the ethylene* The critical problem in the oxidation of ethylene to ethylene oxide is temperature control of the catalyst surface in order to prevent complete oxidation to carbon dioxide and water « When the ethylene is diluted with methane and ethane another problem is presentedo Methane and ethane are themselves oxidized to carbon dioxide and water^ under the optimum conditions for the oxidation of ethyl- ene to ethylene oxide, and also promote the complete oxidation of ethylene. In the process developed at the National Research Council^, close temperature control of the catalyst surface to- gether with the addition of controlled amounts of ethylene di- chloride to the reactor feed have suppressed the oxidation of the paraffins and have made possible the economic production of the ethylene oxide by the air oxidation of ethylene in hy- drocarbon feeds containing as low as 10% ethyleneo The chief new features of the process are:- 1« The ability to utilize ethylene in a mixed hydrocarbon feed containing 10 to 90% paraffins. The hydrocarbon feed may also contain small amounts of hydrogen^, carbon monoxide or acetylene^ 2. A new silver catalyst prepared, under special conditions^ by the thermal decomposition of silver oxalate in the presence of calcium oxalate, and to v^iich is subsequently added a controlled amount of stannous oxide as a promoter© 3o A new, fin-type, catalyst support, affording close tem- perature control over all the catalyst surface « 4o The addition to the reactants of controlled amounts of ethylene dlchlorlde, less than 0o005% by volume of the total gas entering the reaction tube^ for the specific purpose of suppressing both the oxidation of the para- ffins and their tendency to promote the complete oxidation \ ij lo ^c.^ meic LTfliJs 6 9'T. eri:t 58 of ethylene o The ethylene dichloride rate required to give optimum conversion to ethylene oxide has been found to be a linear function of the amount of methane plus ethane in the feed, and to be independent of the amount of ethylene present© Estimates indicate that the raw material costs^ depending on the mode of operation, will be 0o8 to 2o3 cents per pound of glycol when the process operates on methane- ethane -ethylene mixtures obtained by processing depropanizer residue gas, or its equivalent, in standard refinery equip- mento Sufficient data is not yet available to estimate the operating costs, but it may be pointed out that there are no fuel costs involved in the oxidation atep^ since the re- action is strongly exothermico The process has been successfully tested on a la- boratory scale at a Canadian refinery over a period of seven monthso Plans have been prepared for a pilot plant in Turner Valley, Alberta© ETHANOLAMINES In 1943, following preliminary experiments in the National Research Laboratories, a pilot plant for the pro- duction of ethanolamines was erected and put into operation at the plant of the Canadian Aniline and Extract Company in Hamilton, Ontario o This work was undertaken to supply di- ethanolamine for research on explosives at the University of Toronto and for pilot scale production of new explosives at Valle:fl61do. The reaction between ethylene oxide and aqueous ammonia gives a mixture of mono-, di-^ and triethanolamines, the proportion of each constitutent depending upon the ratio of ammonia to ethylene oxide o Since the most valuable pro- ducts in this case were the mono- and diethanolamines, it was necessary to use as large an excess of aqueous ammonia as was commensurate with reasonable production^ in order to keep the triethanolamine formation to a miniraumo The process as finally installed can be divided into two main parts - (i) reaction of ammonia and ethylene oxide followed by recovery of the ex- cess ammonia, and (ii) fractionation of the resulting aqueous solution to give mono-, di-, and triethanolamine© >Bl S a arc -TQ '^r{i\ '11 - - ■ - r-. - o (~f .0 -■^-KB 6TfC^ ■;<'^'.? 1.0 59 Reaction and Ammonia Recovery A jacketed stainless steel autoclave^ available in the plant p was charged with aqueous ammonia (28%) and then warmed to 30=35®Co to ensure rapid reaction of the ethylene oxide o Ethylene oxide was vaporized and passed into the solutlono During the addition,, "wiiich required about two hourSp the reaction mixture was vigorously stir- red and cooledo On completion of the reaction^, the excess ammonia was recovered by slowly heating the contents of the autoclaveo The ammonia was thus driven out and was absorbed in a simple recovery unit built from drums and piping available in the plant o Providing the autoclave with a reflux head prevented the distillation of mych water during this periodo The re- covery was about 90 to 95% efficient and the ammonia obtained suitable for recuse (25 to 28%) o Following the **blowlng" of the ammonia^ the auto- clave was cooled and drained to give about 150 IbSo of mixed ethanolamlnes in about 500 IbSo of watero Each batoh re- quired approximately six hours to prepare© Fractionation of the Ethanolamlnes The fractionating equipment for separating the ethanolamlnes consisted of two continuous stripping columns and one batch stlllo All these units, together with their receivers,, condensers^, and other auxiliaries^ were built In Hamilton from readily available materialso A second batch still of small capacity was also used at times to purify diethanolamlne for shipment to the University of TorontOo All these stills were operated under vacuumo In the first stripping column the water content of the ethanolamlnes was reduced to about 5% without appreciable loss of monoethan- olamlneo In the second stripping column 65 to 75% of the monoethanolamine was removed, the separation was not complete because only 70 poSdo steam and 27 inches of vacuum were avallableo The final separation was effected in the batch stlllo The diethanolamlne obtained was almost colourless and had a melting point of 24 to 25°Cof but before shipment it was redistilled to bring it up to a melting point of 26 to 27®Co The monoethanolamine obtained as by-product was con- verted to di-n and triethanolamlnes by further treatment with e thyle ne oxi de « E. 60 Triethanolamine was obtained as the residue from the batch still and hence was of poor quality^, marketable only to a slight extent in spite of the severe shortage of this material at the timeo It could^ however ^^ have been improved by installing equipment to permit its distillation under high vacuumo This process was operated for several weeks on a 24-hour day; 6-day week basiSo The daily output was of the order of 270 IbSo of mono-, 200 IbSo of di-,- and 140 IbSo of triethanolamineo in alio some six tons of diethanolamine were supplied to Defence Industries Limited© FREE RADICAL REACTIONS An investigation of the mechanism of chemical re= actions usually reveals that what we normally write as a simple reaction is actually a series of very rapid reactions involving free atoms or free radicalSo Such processes are commonly referred to as elementary reactionso A knowledge of such elementary reactions is of the utmost importance in obtaining an understanding of ordinary chemical processes, particularly since these elementary reactions are in them- selves complete entities and may appear as steps in numerous complete reactionSo Numerous elementary reactions of importance in the field of organic chemistry have been investigated by the Physical Chemistry Section in accordance with the policy of continuing fundamental research during the period of hos- tllitieso Fundamental data of this type are of value to chemists working in such fields of applied chemistry as petroleum and synthetic rubber technologyo RUBBER The wartime activities of the Rubber Laboratory involved a great number of rubber products i the research, compounding^, and testing problems undertaken were so varied as to d ef y complete description© The Rubber Laboratory cooperated in the rubber conservation program instituted by the Rubber Controller by attendance on committees^ by giving technical advice^, and by undertaking research to find means of replacing natural rubber in various product So There was cooperation with the Polymer Corporation Ltdo.^ Sarnia, and the War Production no ni ©ox: lo. ^-hR eiBw ' n / 1 0 , B V i:I<:,ffO to-1? eq .5 6 i; ■ /moo 1^" <3 61 Boards Washington^ In work on government manufactured syn- thetic rubber o Many research problems were undertaken for the Armed Service s^, for the Department of Munitions and Supply^ for the Inspection Board of the United Kingdom and Canada^ for the British Admiralty Technical Mission, and for companies in Canada and elsewhere o Acceptance tests of rubber products were carried out for the Inspection Board and for the Armed Services ac- cording to a specification when availableo Ivlany new speci- fications were prepared for special products, and recom- mendations were made for revision of current specifications as shortages In materials occurred, or when the product was required to function under conditions not previously en- countered© Numerous vulcanizing Jobs were carried out for other National Research Council Divisions and for the Armed Services, consisting mostly of small^, sometimes intricate^ moulded parts for experimental apparatus o In the majority of cases this entailed designing special moulds^ and often required the development of new rubber compounds to meet the varied and exceptional conditions of service© Synthetic Rubber The substitution of synthetics for natiural rubber brought many research probiemSu As a preliminary to com- pounding research, a program to calibrate the test equipment and procedures of all the contributing laboratories was under- takeno The Rubber Laboratory cooperated in this calibration^ T^ich was coordinated by the Polymer Corporation Synthetic Rubber Technical Advisory Committee o The result >^ obtained were about midway between the extremes found m the re^^it: of the various laboratories© This was felt to be an indica- tion of well calibrated equipment « Various compounding studies were made for this committee^, some of which are sum- marized below© An early problem was the slower rate of vulcanization of GR-S synthetic rubber as compared with natural rubbery thlSp If not overcome, would tend to slow down production© As part of this investigation the Rubber Laboratory was re- quested to determine the effect of dl -isopropyl xanthogen di- sulphlde accelerator in producing rapid cures of pure gum GR-S stocks at room temperature© It was found that some im- provement could be attained through the use of a relatively low quantity of sulphur in the mix with one part of piper idlne and one part of di-lsopropyl xanthogen dl sulphide « v;r.A J zis a "Tew JUp 62 An attempt was made to Improve the characteristic, low tensile strength of pure-gum^, GR-S compounds by the use of selenium as the vulcanizing agent instead of sulphur in this respecto The possibility of improving the characteristically low^ pure-gum. tensile strength of GR-S by using special ac- celerators of vulcanizatioti was also investigatedo The ac- celerators tested were BJP, Tuada, Selenac, and Tetrone Ao None of -^hese accelerators caused a significant improvement in the tensile strength. One of the more extensive projects in connection with the use of OR-S rubber was the investigation of various materials added as softeners which might reduce the tough= ness and improve the tackiness of the rubber i, and thus allow It to be processed as easily^ and as rapidly^ as natural rubber. The materials added v/ore natural rubber^, balata, gutta percha, Vistanex^ Plastogel^ and p-nitrosodimethylaniline. In some cases the process -ability v/as slightly improved, but none of these materials was found to produce a tackiness in the synthetic rubber compound approaching that produced in a similar nat\iral rubber compound. Various oxidizing agents and heat treatments were also investigated as to their effect on the tackiness of GR-S. Sone improvement was found for the rubber itself but m all cases the Incorporation of carbon black during compounding largely destroyed any tackiness that had been produced by the reagents tried*, In cooperation vMiih the Unitod States \7ar Produc- tion Board, studies were made cf the effect of storage on OR-S in the raw state. As the synthJtic rubber production increased^, it became necessary to determine the conditions under which the rubber might be stored for a considerable period of time without deterioration, so that stock piles might be built up. GR-S rubber was stored for one year at four temperatures^ 30**^ 80®^ 1^0®, and 160®Po ^ and tested every three months to dettjrmine any change in the original pi^'operties. It was found that storage for periods up to 12 months at 30 ®P. and 80"?. had no deleterious effecto Storage at 160®P. adversely affected process-ability as well as the physical properties of the vulcanized rubber. The adverse effect on processability of storage at 120**P. for 12 months was relatively slight. It was, therefore, concluded that GR-S could be successfully stored for a considerable period of time at all temperatures -encountered in the United States. (j^ "-f j_ U o .. ,j ' -', ■- ■6^j;o "vol fix 1 1 . 3 B '. wo II. & t ■ "- *:" i; ' fir ^ -■. - enillfiBlYi; ;tifcr ;.jje ill ee:viiL_ rri: beo.['; Job J 'a J .L^ .:i • - -' •■ ■- -■•• e.cf-t tol t-n, .'2 .a-HO nocfiflo 'I ^oubc-zH no e nolztojj'Lc enolctJ:i\ i elcfcie. e.eliq iioo . d-B TBe^ en. bB.iBerf bnfi 1.1^- Si .^ . ,. . ^ i^Biod-fi oJ:t D£ - 1.1 : a?. .,..tB eir: ?• ;Xw .. jBm ii seen ca ctl .'lacfcfiri ac Bctctcr^ 10 e nl ) ^non ,:3 erl:t i;mla b !■ bnB no .. 6 i'iu'i > :-&Icf beK . -HI) • -£ii bnir lid J.'/ t'Jj ■ J J , "^ ......... .- ... »r.' -^- %t; .. .,_..« 3y 9 •.3.b en iiom oiq r ^' ^B 8£i:;nom SI - ^^'!le ^tBrid" bebi^ ui oiri^c: a aw boliaq ©Id-: .. .. „ .. r r ^f ■•!;■.; -.^ -510 .Eed-Bd'2 bo.-tinlT ^ tni.oo ^/ 65 Cooperative United States-Canadian investigations were made of butyl rubber carbon black stocks o Butyl rubber has a slower rate of cure than natural rubber^ and various accelerators and accelerator combinations were tested in an effort to increase the rate of vulcanizationo It was found that 1% to lo5% of Selenac gives satisfactory accelerationSp particularly the higher amount o It was found possible to produce butyl rubber cements that would slowly vulcanize at room temperature through the addition of relatively large amounts of lead peroxide and GMP acceleratoro At the request of the Department of Munitions and Supply, a literature survey was made regarding the possibility of producing synthetic rubber from alcohol o It was found that a plant for producing synthetic rubber from alcohol can be built more quickly than a plant using petroleum as a raw material o The production of rubber from alcohol, however, is more costly than from petroleum© In cooperation with the Division of Biology^, tests were made of Kok-Saghyz and milkweed rubbers as substitutes for natural rubber© Milkweed rubber containing some natural resin was found to give at best a tensile strength of only 1500 IbSo per sqo ino In a tread type compoundo It would thus not be particularly promising when used aloneo In admixture with GR-S it acted as a softener and gave some Improvement in processabilityo A rubber free from resin would be a satis- factory rubber substitute but the cost of purification would be prohibitive 9 Kok-Saghyz rubber j, grown in Canada by the Experimental parm^, proved to be almost equal in quality to natural rubber although its cost is higho Its molecular weight appears to be somewhat lower than that of natural rubber© Studies were made of blends of natural and GR-S rubber^ and of fillers in natural and synthetic rubber, in cooperation with the National Research Council Radiology Laboratoryo Many fillers in rubber were observed to give characteristic X ray diagramso Stretched natural rubber gives a pronounced characteristic X-ray interference diagram, where- as, comparatively speaking, GR-S gives noneo Mixtures of natural rubber and GR-S prepared in the Rubber Laboratory were observed to give X-ray interference diagrams, under cer- tain circumstances, even when only ten percent of natural rubber was pre sent « The X-ray examination thus gives an idea of the degree of dispersion of natural rubber in GR-S and it would appear that the mixing of the two rubbers does not pro- duce an absolutely homogeneous product but leaves small units of unchanged natural rubber dispersed in the OR -So ©nolltB^iri--^ ^-^v^ HI'-' evl: ;tBrf:r I^riijo .: -tecfcfi t •. lo ©cf uiio I ■-ifl^nYS ,^ .-. q b ^1,1 '.._>!'■ " .J Bill , .... aloTu -} ^ ,. ... -^ - - 'lOin Tir . - o- Qudi bj. _ . 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Q^ XSololb&H iL:-£iiJoD nc^-'jeeen IsnoJ .i d-i :eqooo ■ ©vlsj.:! t- ' ■' ':Si:^ a' --dod &Q\^l'g T.e6mj^i i ... ■ ;,afii..-- _^ ^_ 'ido - e'xsriw -^mBTjiBlr ^fone^'.c^ r'{3:^(Ll rsi- X .oJ:.tEi'-ie.io£''"j[jajrio L q & Xio:^Miort) its ,1 io noiBioqeib lo 86 jfirf lo oiq don 2 9oL a' '-^ -^ ' ' - ed:i JiiriJ •"::. f^Ixjow ao-lnji IlBmp &evi .:!Oii Yiad-itlo,- ..- eoub 64 Laboratory Teat Methods Laboratory test data were obtained In conjunction with road teats of synthetic rubber recaps on Army truck tires, and a valuable correlation was thus made available* The road performance was found to be closely related to the modulus of the rubber o The specif Icatior for camelback, prepared as a result of this work, called for an increased moduluso The modulus and other requirements in this specification tended to make the manufacturers' products more uniform, and a general improvement in quality resulted© An improved correlation of laboratory abrasion resistance testa with road wear vsas obtained by modifying the standard test by extracting the test specimen with an ethanol-toluene mixture before abrading ito It was found that softener from the rubber was coating the abrasive in the abrasion machine and vitiating the results*, The extrac- tion removes this softener and enables a good correlation with road wear to be obtainedo A method was developed for the identification of rubber in sludge in aircraft lubrication systems « Rubber dissolved from oil hose can thus be distinguished from other types of sludge© Rubber Applications Acetylene black was studied as a reinforcing agent for OR-S in tire t reads « Some advantages for this type of filler were indicated because of the lower hysteresis and con- sequent lower heat development resulting from its use© Static is readily discharged in an aeroplane tire containing ace- tylene blacko A study of lime hydrate, a by-product of acetylene manufacture, showed it to be a useful filler in insulating compounds© In cooperation with the National Research Council Electrical Engineering Laboratory and the Directorate of Scientific Research and Development, Naval Service^, the physical and electrical properties of insulation made from three different types of raw GR-S were investigated© The OR-S insulation compounds were prepared by a number of dif- ferent wire and cable manufacturers for examination by the National Research Councilo The electrical stability of the rubber insulant was found to be related principally to the water soluble ash content of the r aw GR=So Sarnla GR-S of ■srp . - ' . y i. fl e B jb C' 8riT b &br: e i bt: .laiii er[:t ' vjj:i*ij.fp ill jivoii'evo'iciTij. I^'ienag IC' rro t <-^ a I eiioo f . e>ad>j-. v^ nA n.r.roi-'j.onBrl;Je •- ' STOB erfif Ov+ ..B;iV bBO'1 rfctiW lo noi: Tiericto moil ;.. « rf .i 'r r; 1. b h ' • O [OY^b B P ^'^,•n A •A 111 o6> nl i0dcfju"i 'noo bns ei3 6T:oJsv'r^ Tev j;^£u2 oeeu ecri ; -eoB gniniB^^rii, IlonuoO rioiBse^H lo e;tBicctcry nioil 9f)Bxrf nol lo a»HD BlxiiB^-. E 3W >ioBld ©n^j.' v^ C' e J A -•■- oB/jBe-rr^ e-iicf al e-HC toI - Boecf Jberf^Bolbnl eiew TalXil •: . nofiiqclsvel: ^B©r{ lewoi .l-nsupoe OT.9B fiB nl bsQiBi-'otilt xIlb&e^L el ed'BiiDYri oinxl lo 6?cij £ ecf o^ ct.^ I oBtn/Joqmoo oo-^-iorfBJ sniieenlgnS lBoii.:tooI3 .., , — ..uqoIeveCI ft fib r{o*i£ee&H oiliclnslog ..t lo BeliTsqoiq iBcx'f^toels .brte iBcieij'jriq v/BTC lo aaqiji^ .^ns'reTtllJb 8©7r{::t ' •'"■ " ^•T: -,qtfroo nolctBlijenl S-HO sIcfBo briB eilw cfnei^l oil . .i.TJLroO doiBsaoH lBnoi::tBVI . - OG ^jnjLol aBw ;tnBlxrenl ledcfifi WB 1 orfzf lo -r^9^^n:oo daB elcfflos isjfBW 65 exceptionally low ash content has "been prepared for evaluation in this connectiono A specification for rubber glands^ or packings^ used in hydraulic mechanisms in aircraft^; was prepared for the RoCoAoPo Such glands must be resistant to the various oils and fluids used in aircraft,, and also flexible at low temperatures encountered at high altitude So Studies were made of the best synthetic rubber compositions for this pur- pose., and useful knowledge was obtainedo A standard rubber gland material was prepared and, in cooperation with the Gas and Oil Laboratoryp was tested in various aircraft hydraulic fluids and oils. This work resulted in specifications for fluid and oil that would function satisfactorily and at the same time not be injurious to the rubber o Numerous tests of glands prepared by the various rubber manufacturers were made against specification requirements for the RcCoAoPo In cooperation with the Royal Canadian Air Force numerous types of rubber hose for conveying oil^ fuelp coolant ^ etco:, were tested with a view to producing a single general spedif ication which would cover all types of service and re« duce the number of production items necessary in aircrafto In cooperation with the RoCoEoMoEo a number of types of rubber repair patches for synthetic rubber inner tubes were evaluated. Amongst other physical characteristics^ the flexing resistance of the patch was determined. Methods of application of a satisfactory repair were investigated© A number of manufactured products for use as anti*^ skid deck paints were investigated for the Naval Serviceo A specification for a composition containing a plastic and a coarse mineral aggregate w as preparedo Acceptance tests were carried out on a considerable number of lots of this type of material. A niomber of experimental hard and soft rubber parts were prepared for non-metallic land mines© These were de- signed by the Directorate of Engineer Development to avoid detection by electrical means. In cooperation with this same Army Branch;, pressure tests were carried out on lOOO-ft. lengths of tubing to hold explosive o Such tubing, when thrown out, filled with explosive, and exploded^, could be used as a means of neutralizing land mines© Rubber belting for use in the track assembly of snowmobiles was found to shrink excessively in the longi- tudinal direction when wetted. Investigation showed that .l:fBul£V^' 10 1 surrl" n^ 9*'I©W ' ed:f F t^i..'- a-^TO*^ ilA ru. -. f _. ;t ::o'i etc a ,:tlBir»Ti£ nL lo lacfrrif/n e o '-^ o,. '-t- A vOotv • > -r ■lv;;;-J "• eJ^ a Taw ■'<-■,.; e>,.) 10 -i ..an, eon: if. X O '.'',* ew 66 the cause of this shrinkage was the tension placed in the belting during manufacture o This shrinkage^ which was irregular and unpredictable^ created difficulties in the assembly and maintenance of the snowmobile o Knowing the cause of the shrinkage it was possible to suggest means of overcoming the difficultyo An investigation of the creep or set occurring in snatch plugs, used in wireless sets^ was carried out for the Canadian Signals Research and Development Establishment o These are electrical plugs containing five terminals em- bedded in rubber, the rubber being used to add resilience and to make the plug fit tightly into its socket with some elastic deformation of the rubbero When the change to syn- thetic rubber was made, the rubber was found to have undue creep, or set, so that the plug after some time in the in« stallation would come out of its socket too readilyo An accelerated.o compression-set test and a test to determine the force required to pull out the pl"ug were devised.^ and suggestions were made as to the best .type of natural or synthetic rubber compound to use in order to overcome the difficultyo The Rubber Laboratory cooperated inroad tests of bogie wheels for Ram tanks carried out by the Army En- gineering Design Branch of the Department of Munitions and Supply, and by the Inspection Boardo It was found that bogie wheels in which the solid rubber tires had the highest resilience were superioru This is because resilient rubber has relatively low hysteresis and consequently d evelops less heat on the roado For certain positions on the tank it was found not possible to use synthetic rubber bogie wheels be- cause of the somewhat lower resilience than natural rubber and consequent higher development of heato RUBBER GOODS Development work on various items of protective equipment of viiiich rubber was a constituent was carried out in various laboratories of the Divisiono It was found that the considerable drop in the bursting strength of fire hose caused by mildew can be prevented by treating the hose with zinc naphthenate© A test was developed to evaluate the shock absorbing pro- perties of various types of sponge rubber for crash heleratSo Rubber socks for field experiments were prepared from latex by the Rubber Laboratoryo A portable tent flooring for cold weather use was urgently required^, and a suitable material 8BW 'io ^iihem ooneiixaei nj ■^ ■b©t"'j!:;9Cf bfiii Bnol:tin 7 arid- bcisj. ■f — '^- Id sd:i b^M\ aesX eqolevo •'-. •.ecfcfiri I; • c; lo ■©fits aOOx :.t '9-9 ill ©cf rrao v/ei a/Tt ©IdB?.L 'dniX'; Ocxy i; iicf uadadve'iq . 9q 67 was recommended In the form of fabric equal in weight to that used In ground sheet s^ but coated on both sides with an all-reclaim rubber compound <. Technical assistance was given in comment ng the manufacture of gas masks in Canada, and all manufacturing problems were solved before the war started Skin irrita- tion may be produced by contact with rubber in gas masks or other equipment ^ the Rubber Laboratory prepared rubber compounds for toxicity tests by the Chemical Warfare Labo- ratories in order to detect the irritating ingredientc In an attempt to find a substitute for natural cellular rubber in life jackets and in other buoyant pro-^ ducts, many different materials were examined. During the Investigation a thin-walled^ alr--filled Neoprene bubble was developed in cooperation with the Viceroy Manufacturing Companyo These bubble s^ tightly packed together > were shown to be of use as a buoyant material A number of designs for automatically inflatable life Jackets were also developed These jackets were made of a waterproof, air-tight;, rubber and fabric construction^ and consisted of a number of compartments sealed from nne another and inflated from carbon dioxide bullets by pulling a cordo Successful trials were made by the Naval Se vlceo A considerable amount of work was performed in testing rubber coated and plastic coated fabrics for use in ground sheets, rsdncoata^ ponchos ^ muzzle covers^ hospi- tal sheeting, etc. Numerous tentative specifications were written to cover the production and testing of such materials PLASTICS The National Research Council was called upon to give advice to the Services regarding the selection of the most suitable type of plastic for innumerable items of equipment. This work, involving extensive physical testing of plastics and of plastics products, although unspectacular, was an important contribution in the evolution of efficient service equipments Among the items investigated were: transparent acrylics for aircraft enclosures j battery box materials; mess trays; combs; shaving kits; razors; radio antennae Insulators; caps for water, gasoline, and oil containers; service buttons; badges, and web strap tips; and parts of hand grenades and smoke boxes.. In each case the testing ensured that a plastic material of adequate properties was usedo va fM-i- ^ i 1 0 J.. Zi C - 9n'- n. , - ' "I BO.i':*:c-- . I TB X i/o B d" C' sq fe nu d ^>; ., :^ lio , <=»£-* J 68 After extensive testing, formulations of melamine - o( -cellulose were adopted by the Navy for plastic mess gearo Bayonet scabbards of various plastics were tested^ a design using Injection^moulded cellulose acetate -butyrate., was shown to have adequate resistance to extremes of temperature and to have toughness much superior to thermosetting plastics o Some testing was carried out m connection with plastic motor- cyclists- crash helmets and modifications in the specification were suggested^ this helmet of sisalphenolic material appears to have possibilities with regard to the development of a better miner -s helmet. Testing, carried out to determine the possible usefulness of thermoplastic tubing for fluids in air- craft, showed that low temperat\ire embrittlement is a limiting factor in most cases; this fact, together with solvent re- sistance considerations, suggested only limited usefulness in view of the small weight advantage compared to aluminumo Considerable assistance was given the Army regard- ing the correct adhesive to use in the manufacture of bullet- proof glass that would withstand extremes of temperaturei ethyl cellulose was eventhaily adoptedo At the request of the Army, an identification disc composed of asbestos paper and phenol«formaldehyde resin was fabrlcatedo This disc was virtually indestructible by fire and had good water resistanceo It was never adopted, howeverp due to commercial production difficulties, A laboratory test„ which was later adopted as standard, was developed to determine the amount of acidity developed by urea resin glues during the curing cycle « Some work was done attempting to use dimethyl urea as an adhesive for wood wastes. Considerable assistance was given to the industry in the manufacture of casein, A large number of composite-type periscope prisms had been produced by the Industry when bubbles began to ap- pear in the field of vision. It was demonstrated that the defect occurred in the laminating adhesive used to cement the glass protective plates to the acrylic body of the prism. The effect, probably due to loss of plasticlzer, might have been avoided by adequate preliminary testing. Considerable testing was done In connection with the plastic prism holders for the periscopes of tanks. Of box-like construction, these holders must have certain specific properties;, and plastic construction was adopted In Canada early in the war, the plastic being chosen to fulfil the requirement that the holder must shatter completely so as to be readily replaceable and not jam the periscope v(*ien struck se . X 30-'- /-' ■i::q8 ■ Tew L 1:0 dn :. - '^^^■^^'^ OCT r^J: &bi; 'ar:esoq du* e tn-j TO J .i, ^j-^'rq ■ :.-.. ^ . o >.i3ecf 10 c3:inBo "■■ 'usCq Brief c . . pel 'iiau'iod fiofiw ©q.. j.Mt.h cd'i ed 69 by enemy fire© The holder must also be of vapour proof con° struct! on so that there will be no opportunity for internal fogging of reflecting surfaceso A long series of tests was carried out to check this last point,, smd tests were also made to compare various methods of silveringo Practical firing tests were arranged which demonstrated the superiority of the plastics type holder over an aluminum alloy type in that it shattered more satisfactorily when struck by rifle fireo A problem of quite considerable interest was that of waterproofing military maps so that they could be given operational markings with ordinary pencil (colored or other° wise), and so that such markings could be erased, as troop positions changed, without injury to the mapo Previous solu- tions only partly solved the diff icultieso that iSp gave water- proof maps from which marks were erased only after damaging the map, required special pencils, or required the use of sheets of plastic which could only be, at best^ insecurely attached to the map© The answer developed was that of lac- quering the maps with a heavy coating of plasticized poly- vinyl chloride - acetate, including in the lacquer a pigment p such as barytes, of refractive index substantially the same as that of the plastic and of suitable particle size (3 to 26 microns )o Such a coating is transparent ;, readily takes markings in pencil, allows repeated erasure without damage to the map, and provides excellent waterproof ingo The procedure is moderately expensive but may also have peacetime uses where similar properties are desired© After the principles involved had been established, commercial development was turned over to the Aulcraft Paint and Varnish Company who produced a very satisfactory commercial product© In the manufacture of large, wooden^ laminated timbers a considerable amount of time is lost due to the fact that the member must remain in clamps for a considerable period after the flue is applied© This time may vary from eight to twenty-four hours© High frequency electric heating has been used to hasten the process, but, while this is quite satisfactory, the initial cost of equipment is high© In an effort to confine the heating to the glue line,, and to el- iminate high frequency equipment, considerable experimental work was done using carbon black mixed with the glue to make it electrically conducting and then applying ordinary 60 cycle alternating current to this glue line© To make the glue line a more uniform conductor the method was later modified by applying the carbon black to an open mesh fabric such as mos- quito netting© This method showed some promise for commercial use© X^i- '■ X6 ed'j 0 7 :tjjo .haliiJBO ^ : ':. il ctBnct •J J8ff.. eifiBP ©^refiw Bee -J '-^i bevlovnl: <- ■i'6vo ter. ■ : ■'■V .s t&ossb^ Ten J .vf.>e*i'. ^ . ,,. - jTqie^Bv/ lo iw 8?^i3itJ8n iBiioI.-tBieqo 0? bcsB ^ (eeiw srio 'rrol:Jleoq •jr^f 'loo'tq . ^qAiiTi erfct aiq lo e;teerf8 t JborIoa;t:tB .'XtJ j^nliei/p •fXtiid BB rioj.fB ^■i:i iro vfBf(;j bB ^qBm ©rfd •:^Biei>om al iq iBJlin.te .0 n3ec/ ibBfi T:o mo r • to b'- >s.l XqaB al B uL-idcfrnl^ :ri:? i&d-lfl Jbolieq oD-oBleliJBe f.r( 0;tBnj • \ jb Bjam 2i- nco mriolliit/ ©lom £ TB o Off 't ;art .t y I qq b 70 Prior to the establishment of the structure labor- atory considerable work was done on the moulding of plywoodo This was given a great impetus by the announcement of the Vidal bag-moulding processo Models of a tail assemblyp.a gasoline tankp and an engine nacelle were madOo After the supply of natural bamboo was cut off by Japan ^'s entry into the war^ attempts were made to produce cylinders from ply- wood which had strength properties approaching those of bambooo It was found, when birch veneer was coated with urea -formaldehyde cold-setting adhesive and wrapped about a mandrelp that after the resin cured compressive strength equal to that of natural bamboo could be obtalnedo Diffi- culty was foundp however , in maintaining this strength when two pieces were splicedo The work was initially done at the request of the British Admiralty, yrho use bamboo in quantity in the manufacture of anti-aircraft kites© LUBRICATING GREASE = FUNDAMENTAL STUDIES Late in 1938, under the sponsorship of Imperial Oil Ltdo , an investigation was started of the more funda- mental properties of lubricating grease, and this project was continued during the early years of the ware The work was concerned mainly with the physical properties of soaps In organic media, although some attention was given to prac- tical problemso The results of this work have been disclosed in publications listed at the end of this Section© ALKALOIDS In addition to direct war research, the Organic Chemistry Laboratory continued Its investigations in the field of alkaloidso During the period 1940-41 two alkaloids were synthesized;, the chemical structures of two others were completely unravelled, and that of another partially soo Furthermore, close to twenty new alkaloids have been discovered and reported* In connection with the determination of the structure of new alkaloids, the bast is usually degraded^ and it often gives rise to a methyl= and dlmethyl^quinolineo Since only about 40% of the possible methyl^ and dimethyl- qulnolines were k;nown, it was seldom possible to identify such a degradation producto Such a case was encountered, and the synthesis and characterization of all these quinolines was therefore undertaken and completed© o '^ 10 (if:.! 3"-. .be- B . X^ edcf O^ji i. ^ .. ■ V '( 1 010 T lo e rswiv^ flu \ilrlnB.sjp BiTf eie^^' -tJ-Cttt'^ TlOCffl 3 tjlT rajblV iti^vLiinBrft " i Bi/p © eqBoa lo 8 0 q ed'i rfS^iw :" M.A aJblolB^flB ' oOfe i^etevooeJ^ i t- -It cenli?:?^:.. 3fi^ ,_. .0 Mell :o iB.ffnf J!>nB ^JbeIi9v.!*T0i, yJ-'©-'^^-^'!^'^^ .jjodB xino eon IB -: «w 3X ,,rtwoii^ eae^v Renilonlx/p -- t3B.^B'i;sob ^ rfoiJ'B 71 During the period 1932-42 a systematic study was made of the alkaloids of the Pumariaceous plantSo This work was important "both chemically and botanically because it con- stituted the first systematic investigation of the alkaloids occurring in the various species of one genus of plants o Work started before the war on the synthetic pre- paration of plant hormones was also completedo MICRO ORGANIC ANALYSIS In research work in the field of organic chemistry the amounts of some substances isolated are often very small o As these substances are usually obtained in quantities in- sufficient for analysis by ordinary methods,, they must be analyzed by a special system known as Pregl' s micro-analytical methodSo Before the war^ all such substances obtained in these laboratories were sent to Germany to be micro-analysedo With the outbreak of hostilities, it became Imperative to have our own facilities, so a micro-analytical laboratory was established., and, to familiarize him with the technique involvedj, one man was sent to New York University for a summer course in micro- analysiSo The services of the National Research Council Micro- analytical Laboratory are available to research departments in those Canadian Universities not equipped for such work© STARCH Beginning in 1938, considerable assistance was given to a potato starch plant at Grand Palls^, NoBo; in* ad- apting to their process American made machinery " chiefly con- tinuous centrifuge So Equipment of this type was formerly sup- plied by Germanyo Considerable assistance was subsequently rendered in checking the quality of the product© Investigations of the physical and chemical pro- perties of starchp which had been in progress for several years were terminated during the early years of the waro Interesting relations have been noted in the falling off of the viscosity of starch pastes with intensive drying of the granules prior to pasting* Thermal degradation of the starch granules, as is practiced in the preparation of dextrin^ has yielded some very valuable information on the probable mech- anism of dextrin formatlono This work was extended to some of the lower molecular weight hydrocarbons, and the rate of thermal decomposition, as obtained by the amount of gaseous products formed, was followed for dextrose, maltose ^ cello~ biose, and sucrose. Some work on the behaviour of starch fractions on the film balance was also started© IV ,edT;r Au e'TCl 9<'l Join DO c. I i BruE -11/0 ov ^"O^Oillf Hi B 1 0 e i ■ .• T til ... . 8 .-•r:^i eA v 1:+ frioal nwo • F10 cf B J I a n i -jy I Bn b SBw e^ ■ '" -Ijb '£14. ^noo ^Ileiii-: yld-nei/peedi B>'9I eno' a^ ' ' ' -t ^nld-qB • t^ a — ^ r> ^r; OillO ^i O o "to actij-T i -•oil© J .f{r.oeJb iBftr'tericf iiiiol e;is'5jj£)0'iq i;8 hnij ^eeolcf ;j i;..- r.. rjii:^ no BiJOlcJOBll 72 PEAT Peatp in its various formSp ia one cf Canadians most abundant materials^ With the interruption of the European supply d\iring the war^, Canadian peat was used in a small way for soil conditioning^ for stable littePo for packing material, andp for a brief period^ it was exported to one of the larger United States magnesium plantSo In Europe, its chief use has been for fuel in areas where coal and wood are not readily available and labour is cheapo The only really large scale fuel development seems to have been In the UoSoSoRo Efforts to develop its use as a fuel in Canada have not yet proved economicalo The two great difficulties ihich have retarded its development are the high moisture content (up to 90%) p and the small scale of operations which has kept up its cost of recoveryo It appears that any major industrial use of peat must be on a scale sufficiently large to warrant low-cost mechanical recovery^, and must be of such a nature that the high moistixre content is not a disadvantage o For use as a fuel, the scale of operations would be large enough to warrant the use of mechanical handling equipment j but the drying difficulties were never surmounted -' artificial drying was too costly and natural air drying too slowo This, then, leaves the utilization of its chemicaj. constituents without predrylng as the only probable means of exploiting this abundant natural resourceo It was with this in mind that a study of peat was undertaken in the Division of Chemistryo Peat is a complex mixture of various materials, including waxes^ alpha-cellulose, hemicelluloses, lignin^ humlc acids, and asho The proportions vary considerably between different deposits and between different depths in the same deposit© In commencing this work it was thought that if some segregation of these various components could be effected, it might be possible to isolate materials of higher unit value than the peat mixturec As it was desired to accomplish t his objective without passing through the' uneconomic drying operation, treatment with an aqueous solu-- tlon was Indicatedo Two such treatments were known which might be applicable, namely, treatment with an alkaline solu-^ tlon to extract humic acids, and dilute acid hydrolysis to effect some degree of saccharif ication aSp for example ^ in the Schoeller process for the treatment of weed waste© f? "■ b:~ •'• riBcne J3 .-^ ©no otf i^oow Jbna i:t n: need Of! 7 £)nB / no . m ."iaeq lo ..30- ooJ- eBW giti-^T:!) ilCI ,loal - bn u - ylt.isjd :^L di^'^'- ... 'xeev/^ted 1 - > ^rriBS erid" )e 'li ^Ba'^ .. i^d-oaTie 8a ^irtir lerfgifl qiTIOOOB Oit ' -tcnooexiu 3w ncld" ' -^rlsim 73 Alkaline Treatment Humic acid extraction was tried firsts using dilute caustic soda solution^' this worked very well except that the subsequent filtration was slow and diff iculto Ammonium hy- droxide was tried nextp as there is a large production of am-- monia available in Canadao This worked much better andp in the course of this work^ it was noted that the solid residue from the extraction dried quite rapidly and became considerably tougher than raw dry peato This observation suggested that, if it were possible to dry peat rapidlyp it might be economically possible to work on it with other than aqueous solutlonso Several repetitions confirmed the original observation^ and It was found that peat would dry, though slowly, at temperatures almost down to the freezing point o Treatment at an elevated temperature, on the other handp weakened the tough structure « Since a use for the humic acid extract had not yet been developed, drying experiments were performed on alkali- treated peat without separating the hiiraic acldo Again the mass was found to air-dry quite readilyo Other alkalis were tried, but sodiiim carbonate was the only one found vfriich could compare with ammonia in effectivenesSo The effect of adding other chemicals was investigated and ferrous sulphate was found to add strength to the dried product and to prevent shrinkage cracks o The final preferred process was to add to wet peat^ as recovered from the bog^, ammonia or sodium carbonate solu- tion until the peat slurry was r.eatral or very slightly alk- aline, then to add about OoSjS (based on dry weight of peat) ferrous sulphate in solutiono When the resulting pasty mass was formed into blocks about two inches square., it hardened and dried appreciably in air within three days • or within half that time if air was blown over the surface by a fano The product then contained about 10^ moisture o After a further ten days, drying was as complete as practicableu The product obtained had the following properties j; density^, about loOj fuel value „ 9000 BoToUo per Ibo 5 ash content.,, 5 to 6%j and moisture content, about 4%o This product is quite re-' sistant to handling but disintegrates if exposed to rain for any length of timeo It should make a very satisfactory fuelp except that to produce one ton of dry material^ about ten tons of wet peat have to be handledo In areas where other fuel costs are high, it might be produced cooperatively,, and it is certainly much superior to the usual hand-cut peat blockSo '^V oc;j|)OT[q erlT ^rt evBff J-soq J^ew 'io 8no:t jbifiB :.:Y-^^^ ■ '-^ be:jiJtoi:q ec' MrAuZTi rf .t ,dsld ff"iB ejeoo ^B6q - ..ri lBf./eir sxlj' oj Tioi'reqi/E rioirrn Tln.tB:f^e'^ e^ u ^.^ oE:iooIcf 74 Acid Treatment Experiments were also carried out on the hydrolysis of wet peat with dilute acldr, although apparatus for high pressure treatment was not available o Iz was found that a substantial percentage of reducing sugars could be obtainedo although the amount was less than from pressure treated woodo However, large scale harvesting of peat should be obtainable in many parts of Canada^ whereas wood waste is not so widely available in the tonnage required for alcohol production© After concentration of the sugar-containing liquor,, both al- cohol and butylene glycol were obtained qualitatively by enzyme action but no actual yield figures were obtainedo MISCELLANEOUS ORGANIC INVESTIGATIONS Low Temperature Grease At the request of the Meteorological Service s^ sources were investigated for a grease which would give ade- quate lubrication at temperatures down to -60**Po or -70**Po for use with radio- sonde equipment o The pre- war lubricant used was a French oil prepared from porpoise fins and dis^ cusslon with all oil companies had failed to find anything suitable to replace their minute and dwindling supply© After a number of other sources failed to provide suitable lubricants, it was decided to test the use of fractions refined from ordinary fuel cilo This is a residue from the thermal cracking of petroleum and it was hoped the heat treatment might have destroyed those molecular types resulting In poor viscosity indices and high freezing con stituentSo In general, the paraffinic constituents are those with high freezing points, and it was hoped that this class in particular would largely be destroyed by the cracking o since the aromatic constituents responsible for poor viscosity indices can be removed chemicallyo This was found to be entirely correct and from suitable fractions remarkably good oil can be securedo As first taken from the fuel oil by distillation, the material is naturally very crude .„ on standing in the air a tremendous amount of gum forms, oxidation tests are very bad and- owing to a high aromatic content .c its low temperature properties are useless o However^ sulphuric acid treatment removes large amounts of aromatic constituents and heating to 250® with sodium metal removes gum forming and other undesirable constituentSo After acid and sodium treatment., the oil is ex ijOB ...t6o 75 clarified with bentonite and distilledo The product is an entirely stable pale yellow oil of slightp agreeable odor,, forms no detectable gum even after several years^, and remains very fluid down to remarkably low temperatureso Tests by the Meteorological Services showed that their very delicate mechanisms remained properly lubri- cated down to "80®Po In order to retain this light oil in small bearings it is made up in the form of a thin grease using lithium stearate and a specially developed selenium compound is also added to produce low starting frictiono This grease was also tested in anti-aircraft shell timers at the request of the Inspection Board and at °89**Po the mechanism was delayed by only a half secondo A small supply of this grease was sent to the Fuse Division of the Inspection Boards, together with all details of its produc- tion; it is understood that further work was undertaken else- where o The Kinetics of I^olymerization Reactions An article on the kinetics of polymerization re- actions was prepared^, in 1940^ in collaboration with Dro Ho Mark, to form a contribution to the series of monographs on High Polymeric Substances edited by Buck^, Mark^ Houwinkp and Whltbyo The manuscript was submitted to Professor Houwink of Leyden, but publication was delayed owing to the invasion of Hollando In addition to a discussion to the theory of the chain reaction in polymerization and of the kinetics of poly- merization reactions^ the manuscript contained an account of experimental kinetic investigations of styrene^ of acrylic acid and its derivatives^ of vinyl acetate, and of some miscellaneous hydrocarbons© Butadiene Towards the end of 1943, in cooperation with the Biology Divisionp work was undertaken on the production of butadiene from butylene glycol© This process was at that time receiving considerable attention from the United States Department of Agriculture as a possible source of butadiene for synthetic rubber o .11 edT ■ IBM no flO 76 In the National Research Laboratories an effort was made to develop a continuous process for the esteri- fication of butylene glycol and the subsequent pyrolysis of the ester to butadieneo In the course of this work glycol esters were prepared from a large number of acids but none showed much promise of commercial applicaticno Pair yields (60 to 70^) of butadiene were obtained from the adiplc acid derivative by pyrolysis at relatively low temperature (350° to 400®),, but work was stopped when no method was found for preventing the simultaneous pyrolysis of adipic acid to cyclopentanoneo However^ this pyrolysis of the adipic acid ester is probably the most convenient laboratory method yet found for preparing butadiene of high purity© Vitamin A Assay After the Invasion of Norway, which had been prac- tically the only source of cod liver oil for Canada.,, it be- came necessary for Canadian producers to manufacture cod liver olio Since cod liver oil is 'priced according to its content of Vitamin A a id Vitamin D, these have to be assayed on every batch of oil producedo The assays are made by the manufacturer but they have to 'be checked^ The Dominion Experimental Farm undertook to determine the Vitamin D Content of these oils and the National Research Council agreed to carry out the determination of Vitamin Ao This Involved saponifying the oilSf isolating a fraction containing the Vitamin A,; and de-- termlning the Vitamin A content spectrophotometricallyo The first two steps were carried out in the Division of Chemistry and the last one in the Division of Physicso On the average^ four samples of oil were received per montho Barium Phosphopyruvate A request came from England for the preparation of phosphopyruvic acid in the form of its bari^T*' c-oito The first attempt to prepare this salt by the use of a method given m the literature led to very poor resultso The method was then modified and the substance was subsequently obtained in fair yieidSo It Is prepared by the action of phosphorus oxychlorlde on pyruvic acido The product is converted to the barium salt and the salt is purified by a lengthy process of repeatedly dis- solving in dilute acid and reprecipltating by proper adjustment of the pHo Starch A poiarlmetric method for the estimation of starch 77 In wheat was extended to other materials in collaboration with the Association of Official Agricultural Chemists and adopted as a tentative method by the Association© Isothiocyanates Arising from the isolation of a sulphur-containing plant substance, some related compounds were synthesized in order to study the connection between the sulphur grouping and bitter tasteo Chlorohydrins and Glycols The reaction of sodium hypochlorite with e thylenic compounds was studied© <<-Cyano-phenylglyceric acid was pre- pared and its decomposition products were identified© During this work it was found that sodium hypochlorite is an efficient reagent for nuclear chlorlnation of certain aromatic acids and aldehydes© Some physical constants of 233-butylene glycol were determined© Fatty Acids Work on the occurrence of ll:12-eicosenoic acid In a vegetable oil was completed© The acid was identified by means of derivatives and degradation products© REPORTS AND PATENTS Ethylene Oxide Cambron, A© Oxidation of Ethylene to Ethylene Oxide© NoRoC© Report Noo C161-39p August 16^, 1939© Cambron, A© and McKimp F© L© Wo Oxidation of Ethylene to Ethylene Oxideo N©R©C© Report No© C125-40S, June 28, I94O0 Cambronp Ao and McKim^; P© L© W© Production of Ethylene Oxideo UoS© Pat© App© 500,360p Aug© 28, 1943© Cambron, A© and McKim, P© L© W© The Production of Ethylene Oxide© Can© Pato App© 516^428, July 19.. 1944© Cambron, A© and McKim, P© Lo W© Apparatus for the Production of Ethylene Oxide© Can© Pato App© 516^,429, July 19^ 1944© aniTf/' ^afi oO^Ho^A ^QbixO BA '•rrsO \:j •l-^Q. 78 Cambrorip Ao and McKinip Po Lo Wo Apparatus for the Production of Ethylene Oxideo UoSo Pato Appo 556^279,, Septo 28^ 1944o Cambron^ Ao and McKim^ Po Lo Wo Silver Catalyst and Method of Preparing Sameo Cano Pato Appo 516p430p July 19 ^ 1944 o Cambron, Ao and McKinip Po Lo Wo Silver Catalyst and Method of Preparing Sameo UoSo Pato Appc 556^,280, Septo 28^ 1944o Carabron^ Ao ^ McKinip, Po Lo W o .^ Shane ^ Go and Mohun, Wo Ao The Production of Ethylene Oxide by the Direct Oxi- dation of Ethylene in the Presence of Methane and Ethane ^ NohoCo Report NOo C2931-42S,, Jam ll^, 1943o Ethanolamines Cambron;, Ac Production of Ethanolamines „ Cano Pato 429^4185 Augo 14, 1945o Cambron^ Ao and Mohun^ W^ Ac The Production of Monoethanolamineo NoRoCo Report NOo C3162-42S^ Jano 29., 1943o Cambron,, Ac. Mohun,, Wo Ao and Eastham^, Ac Mo The Praction-^ ation of Ethanolamineso NcRoCo Report NOo C1263-43S, Septo 20,, 1943o Mohun^, Wo Ao The Production of DiethanolaminOo NoRoCo Report NOo C1262'-43S;, Septo 20., 1943o Mohun. Wo Ao Continuous Rectifying Column for Aqueous Ethan^ olantneso NoRoCo Report Noo C3383-42Sp Pebo 18^ 1943o Mohun^ Wo Ao and Simard^, Ro Jo An Investigation of the Factors Affecting the Yields of Ethanolamines,, NoRoC© Report NOo C917°44Sp Septo 12n 1944o Free Radical Reactions Darwentr Bo deBo and Steacle^ Eo Wo Ro The Mercury Photo- .fiensitlzed Reactions of Propane at Low PressiireSo Jo Chemc Physc, 13,, 563=571 (1945) o Gunning^ Ho Eo and Steacle, Eo Wc Ro The Mercury Photo- sensitized Polymerization and Hydrogenation of Butadiene o J„ Chemo Physo 12, 484-493^. 1944o 8' .i^L-^d^ J^^yi :^nlfXLh. oO.H,.VT o 0 ■: H : VI L^*-t; A ^ ._., ,,(,, -■':jO 79 Gunning, Ho Eo and SteaciSp Eo Wo Ro The Reaction of Methyl Radical with Butadiene and Isopreneo Published as OSR„ 15 PR"7"3c, June 15, 1945o Gunning, Ho Eo and Steacie^ Eo Wo Ro The Mercury Photosen- sitized Reaction of Propylene and Isopreneo Jo Chemo Physo, 14^ 57=61, 1946o Habeeb., Ho, LeRoy, Do Jo and Steacie„ Eo -Wo Ro Zinc Photo- senitlzed Reactions of EthylenOo Jo Chemo Physo 10, 261"267p 1942o Harris, Go Mo and Steacle, Eo Wo Ro Reaction of Hydrogen Atoms with Acetoneo Jo Chemo PhySo 13y 554-559 (1945) o Harris^ Go Mo and Steacie^ Eo Wo Ro The Reaction of Hydrogen Atoms with Di -methyl Mercury^ Jo Chemo PhySo 15. , 559-562 (1945) o LeRoy, Do Jo and Steacie. Eo W. Ro The Mercury Photo- senltized Reactions of Ethylene o Jo Chemo PhySo 9p 829-839 (1941) o " LeRoy, Do Jo and Steacie^ Eo Wo Ro Activation Energies of Elementary ReactionSo Anno Tables of PhySo Constants, Section 6026p (1942 )o LeRoy. Do Jo and Steacie, Eo Wo Ro The Mercury Photosen- sitized Reactions of Ethylene at High Temperature So Jo Chemo PhySo lO;, 676-682 (1942) o LeRoy.. Do Jo and Steacie, Eo Wo Ro The Cadmium (^P^) Photo- sensitized Reactions of the Lower OlefinSo Jo Chem© PhySo lOi, 683-685 (1942) o LeRoy;, Do Jo and Steacie o Eo Wo Ro The Mercury Photosen- sitized Polymerization of AcetylenOo Jo Chemo PhySo, 12^ 117-124 (1944) o LeRoy, Do Jo and Steacie j, Eo Wo Ro The Reaction of Hydrogen Atoms with Acetyleneo Jo Chemo PhySo , 12p 369-373 (1944)o LeRoy^ Do Jo and Steacie, Eo Wo Ro Determination of Nitric Oxide using Solid ReagentSo Indo Eng„ Chemo, Analo Edo .o 16, 341 (1944) o Steacie^, Eo Wo Ro Atomic and Free Radical ReactionSo ACS Monograph NOo 102,, Reinhold Publishing Corpo, 1946o .{OP^::l) ectnB.'tSiioO JC ■HeJ a TciTeJ G YoHaJ ■ r ne^idlJXH lo aoij (J^^GI) cSVo- '; .f "■■ bS ...,.-'. 20A o6:i^GI. ■ YoHsJ ..^A oflal 80 SteaclGp Eo Wo Ro and Dewar^ Do Jo Mercury Photosensitized Reactions of Propaneo Jo Chemo Physo , 8^ 571 (1940)o Steacie., Ec Wo Ro ;, LeRoy^ Do Jo and Potvin^ Ro The Cadmium Photosensitized Reactions of Propaneo Jo Chemo Phys„ 9p 306'-314 (1941) o Steacie.0 E,. Wo Ro .. LeRoy.o D. Jo and Potvin^ Ro The Cadmium Photosensitized Reactions of Propaneo J< Chemo PhySo, 9^ 306-314 (1941) o Steacie, Eo Wo Ro . in collaboration with Noyes. Wo Ao Jro^, Taylor.o Ho So^,, Teller,, Eo and Westo Wo The Primary Process in Photochemistry. Annals of NoYo Acado Scio^, • 41p 169-240 (194i)o Steacie^ Eo Wo Ro and LeRoy, Do Jo Experimental Methods of Determining the Activation Energies of Elementary Re- actionsc Chemo Reviews, 31,, 227-293 (1942 )« Steacle;, Ec Wo Ro and LeRoy, Do Jo The Polymerization of Ethylene Photosensitized by S^^i Cadmium Atoms'o Jo Chemo Physo.o 10, 22»=34 (1942)u Steacie;, Eo Wo Ro and LeRoy., Do Jo The Quenching .of Cadmium Resonance Radiation (3261 A) by Hydrocarbons and other Gaseso Jo Chemo PhySo , ll^, 164-171 (1943)o Steacie.o Eo Wo Ro and LeRoy D. Jo The Resonance Emission of Calcium Hydride Bands in Cadmium Photosensitized Reactions of HydrocarbonSo Jo Chemo PhySo;, 12 ^ 34"36 (1944) o Rubber Chilcott, Jo and Griffith., To Ro Pure Gum and Tread Stock Buna S - Smoked Sheet Blend Vulcanlzates for X^-ray Laboratoryn NoR-Co Report NOo C1594' 43S, NoVo lie, 1943o Griff ithp To Ro Synthetic Rubber Compoundingo Cano Chemo & Proco Indo 27^ 444--445 (1943)o Griffith, To Ro Synthetic Rubber from Alcoholo NoRoCo Report NOo C2344--41S, Mar^ 27^ 1942o Griffith,. To Ro Synthetic Rubber from Alcoholo NoRoC„ Report NOo C156°42S,, Apr,, 14^, 1942© 08 b:-- .,e^y.vi froj- Xo^ ,j 0 . n ,j j^i i e-i.T. .■: ;:t nn 81 Griffith^ To Re Preliminary Report on Kok-Saghyz and Milk- weed Rubber o NoRoCo Report NOo C2982-43S<) Jano 11 o 1943o Griffith^ ToRo Milkweed Rubbers (2nd Group of 1943 Samples) Further Reporto NoRoCo Report No. C1905'=43So Jano 5^ 1944o Griffith;, ToRo Proposed Cure for Camelback for Road TestSo NoRoCc Report Noo C628=44S,, July 15, 1944o Griffith, ToRo Specification on Synthetic Rubber Glands for Hydraulic and Shock Absorber Mechanisms on Aircraft o NoRcC, Report NOo C1897'=42S, Septo 30, 1942o Griffith^ TnRo Two and One-half Inch loDo ^ Single Jacket Cotton^ Rubber Lined. Fire Hoseo NoRoC. Report Noo C248--44S, May 11, 1944o Griffith, ToRo Cone°Shaped Covers for Puseso N^RoCo Report NOo C1415- 42S, Augo 1, 1942o Griffith, ToRo Specification on Insulating or Splicing Tapeo NoRoCo Report NOo C2582 ■42S. NoVo 30,, 1942o Griffith, ToRo Description in Specification form of Fabric Reinforced Rubber Hose Suggested as a Substitute for Linen Hose,, Forestry "'TpOo IIoR« Co Report NOo C2614-42Sy Deco 9. 1942« Griffith., ToRc Specification on Rubberized Fabric for Black- out' CurtainSo NoRoCo Report NOc C510-^41S. June 4, 1941o Griffith. ToRo Specification for Cements for Particular Useso N.r'cCo Report NOo C3448-42S. Febo 23^, 1943u Griffith, T.Ro Specification for Cement General Purpose « NoRoC. Report No. 03447-423 Febo 23. 1943o Griffith, ToRo Leather and Peat Products as Blowing Agents in Sponge Rubber o NoRoCo Report NOc C147-45S, May 4„ 1945o Griffith, ToRo. Chilcott, Jo and Perrin, G.E. Milkweed Rubbers (2nd Group of 1943 Samples) in Buna S Tread Stocko NoRoCo Report No. C1904-43Sn Jano 4,, 1944o 18 b n ' uSi*^ roi ^oil ->fi .0 H .Saghyz Rubbers Evaluation of Recent Specimens^ Effect of Washing and of Anti-copper Treatments^ N.,RoCo Report Noo Co903-43Sp Jano 3p 1944o Griffith., ToRo and Perrin, GoEo Interim Report on Compounding Tests on GR-i (Butyl Rubber) in Connection with War Production Board Program TTOo 60 No Re Co Report Noo C1965--43S^ Jano 14, 1944o Griff ith^o ToR. and Perrin, GoEo Second Interim Report on Compounding Tests on GR-1 (Butyl Rubber) in Connection with War Production Board Program No. 60 NoRoCo Report NOo Cx966-43S, Jan^. 14., 1944o Griffith,, ToR. and Perrin^, G.Eo Pinal Report on Compounding Tests on GR«1 (Butyl Rubber)^ NoR.Co Report NOo C2004 ■43S,. Jano 22, 1944o Griffith, ToR.. o Perrin,, GoEo and Chilcott,, Jo Milkweed Rubbers (3rd Group of 1943 Samples) interim Report Is Purified Milkweed Rubber and Detritus^ NoRoCo Report NOo C1906 •43S. Jano 5, 1944o Griffith, ToRo, Perrin, G,.Eo and Chilcott, Jo Milkweed Rubbers (3rd Group of 1943 Samples) interim Report II j? Milkweed Resin. NoRcCo Report No,, C1912-43S., Jano 5^ 1944 • Griffith;, ToRo and Storey^ EoBo Tests of Syntheliic Tire Re- tread CompoundSo NoR^Co Report NOo C2305='43So Mar^ 23,, 1944o Griffith, ToRo and Storey^, EoBo RoCoAoPo Synthetic Rubber Specification,, Sheets Tubing^ Extrusions. Molded PartSo NoRoCo Report NOo C1252»43S, Septo 14, 1943o Griff ith^ ToR. and Storey^ EoBo Specification for Marine Deck Coverings, Non-Skido NcR Co Report No., C87- 44Sy Apro 17, 1944 o Griff Ithi, ToRo and Storey,, EoBo Rubber Belting for Snowmobile Tracks. NoRoCo Reports NoSo C1551'-'44S Jan,, 9^ 1945 j C1557-44S,> Jano 6, 1945 5 C1724-44S« Pebo 9, 1945^ and C15-45S, Apro 5, 1945o Griffith,, ToRo and Storey, E„Bo Elastic Webbingo NoRoCo Report NOo C2031-43S,, Jano 29 „ 1944o 4 83 Griffith^ ToRo and Storey^ EoBo Compression Rubber,-, Under- carriage. MosquitOo NoRoCo Report NOo 0227-443^^ May e, 1944o Griff ithp ToRo and Storey. EoBo Compression Rubber. Under- carriage^ MosquitOo NoRoCo Report NOo C1009-44Sy Septo 29p 1944o Griff ithi, ToRo and Storey. EoBo Tests on Air Seal Puncture- proofing Mater laio NoRoC. Report Noo C296 -42S^ Apro 27 p 1942 o Griffith,, TnRo and Storey,, EoBo Rubber Conservation in Oxygen MaskSo NoRoCo Repom NOo C1521 42S, Augo 14, 1942 o Griffith, ToRo and Storey, EoBo Effect of :,„3-Butylene Glycol on Natural and Synthetic Rubber CorapoundSo NoRoCo Report NOo C1520-44S5 DeCo 26,, 1944o Grifflthp ToRo, Storey. EoB,,, Barker C.Mo and Desmarais, JoRo GR»S for Wire and Cable Insulation-. NoRoCo Report NOo C828-44S,, Augo 26.,, 1944o Griffith,, ToRof Storeyp EoBo,, Barkery Co Mo and Barkley. Jo Wo Do Effect on OR-S of Storage in the Raw Stare , Assoco Commo on Synthetic Rubber Research Report No. OSR 26o Griff ithp ToRo^ Storey., EoBo and Barkley, JoWoDo Hose,; Alr« craft o NoRoCo Report No. C616-45S; Auge 16^ 1945o Griffith, ToRo^ Storey,, EoB,,., Barkley J„W D. and Barker, CoMo Investigation of Tackiness in GR S Compounds AssoCo Commo on Synthetic Rubber Research Report NOo 0SR-18r, June 27, 1945 o Griffith,, ToRo; Storey,, EoBo and Beatty. HoWo Synthetic Rubber Camelback„ NoRoCo Report NOo C1158-44S Novo 23 r, 1944 o Griffith, ToRo, Storey. EoBo and Desmarais. Jo Hose,, Air-- crafto NoRcCo Report No. C1299--44S,, NoVo 17, i944o Griffith, ToRo;, Storey, EoBo and Ellement,, LoMo Synthetic Rubber Electrical Insulationo NoRoCo Report NOo C1959- 43So Jano 12 „ 1944o ■M , vv T . A ,M 0 ■liiiO \xJ ■ rn 84 Griffith, ToRop Storey, EoBo and Ellement, LoMu Effect of Ethylene Glycol and Butylene Glycol Solutions on Natural and Buna S Rubber CorapoundSo NoRoCo Report Noo C1522- 43Sj, NoVo 1, 1943o Griffiths; ToRo, Storey.. EoBo and McGilvray^; PoMo Tests on Synthetic Tire Retread Compounds. NoRoCo Report NOo C380'-44S^ June 1,, 1944o Griffith;, TcRoo Storey, EoBo and McGilvray, P„Mo Modified Abrasion Test for GR-S Tread Compounds,, Assoco Commo on Synthetic Rubber Research Report NCo OSR-S^ DeCo 7^ 1944o Griff ithp ToRo^ Storey, EoBo and McQllvray, PoMo Abrasion Loss of Footwear CompoundSo NoRoCo Report NOo C495-= 45S;, July 19i, 1945o Griffith., ToRop Storey. EoBo and McGilvray, PoMo Synthetic Rubber Compounds for use in Glands for Hydraulic and Shock Absorber Mechanisms on AircrafCo NoRoCo Report NOo C521-44S;, June 21 , 1944o Griff ithp ToRo, Storey, EoBo and McGilvray, PoMo Deck Coverings^, Non-skid ^ Marine, NoRcCc Report NOo C106-44Si, Apro 20.0 1944o Griff Ithp ToRo, Storey, EoBo and McGilvray, PoMo Snatch Plugs NoRoCo Report No,, C594 44S, July 8. ^ 1944o Hall;, RoHo Acetylene Black in Butyl Rubbero Cano Chemo & Proco Indo 29x> 858^^560., 1945o Hallp RoHo and Griffith,,, ToRc Electrical Properties of Super-Pine Lime Hydrate in Natural Rubber, GR-S, and GR-Io NoRoCo Report NOo C1997-43S^ Jano 21^ 1944o Sheppardp JoRo Preliminary Study of Dl-isopropyl Xanthogen Dlsulphide as Accelerator for Buna So NoRoCo Report NOo C2306-='433.o Marchl^ 1944o Sheeppard;, JoRo and Chilcotti, Jo Bardol^ Dinaphthalene^ Thio- phenep Chlormethylnaphthalener, Tests on,; NoRoCo Report NOo C606-43S,, June 1<, 1943o Sheppardp JoRop Chilcott^, Jo and Griffith; ToRo Preliminary Calibration of Canadian Rubber Laboratorieso NoRoCo Report NOo C884^'43S^ July 21p 1943o f-0 .cll ■vrr ni'TQ :g ? i.tlix' 1.3H eao. ■e©ri3 85 Sheppard^ JoRo. Chilcott,, Jo and Griffith^ ToRo Selenium in Pure Glim Buna So NoRoCo Report NOo 0723 433^ June 29c, 1943o Sheppard, JoRo^, Chilcotto Jo and Griff ith. T.Ro Some Charac- teristics of Pure GuK Buna S Vulcanizationo NoRoCo Report NOo C855-'43S, July 16,, 1943o Sheppardi, JoRop Chilcott,. Jc ^ Perrin^ GoEo and Griffith,, ToRo Report by National Research Council^ Ottawa,, Canada in Cooperation with War Production Board Program NOo 2 (GR-S, Buna S)^ NoRoCo Report NOc Ci391"43S. Octo 5., 1943o Sheppardp JoRor Chilcott^, Jo i, Perrin,, GoEo and Griffith,, ToRo Further Report by National Research Coi^cil^ Ottawa^ Canada^ in Co-operation with War Production Board Pro- gram NOo 2(GR='S, Buna S)o NoRoCo Report NOo C1482-43S^ Octo 21, 1943o Sheppard;, JoRo and Perrin.n GoEo p^Nitrosodimethylaniline in Pure Gum Buna S Stocks. NoRoCo Report Noc C1317-43S,, Septa 22p 1943o Storey, EoBo Hose.o Aircraft© NoRoCo Report NOo C77"45S5 Apro 17.0 1945 o Storey, EoBo Snatch Plugs o NoR-Co Report NOo C1943-44Sr, Apro 4^ 1945, 'o storey, EoBo Peat Resin Product in GR-S CompoundSo NoRoCo Report NOo C352«45S„ June 20, 1945 o Storey.o EoBo and Barkley, JoWoDo Repairing of Synthetic Rubber Inner Tubeso NoRoCo Report NOo C616-45S , Augo 16, 1945o Storey^ EoBo and Barkleyo JoWoDo Hose^ Aircrafto NoRoCo Report NOo C1714-44S,, Pebo 9^ 1945o Storey, EoBo and Barkleyo JoWoDo Gum Cushion Stocks., NoRoCo Report NOo 039-453^. Apr^ 16p 1945o Storayp EoBo and McGilvray^, PoMo Synthetic Rubber Snatch Plugs for NOo 19 Seto NoRoCo Report NOo C1414°44Sp Deco 12^ 1944o Wianless;, GoGo and Griffith,, ToRo Study of Milkweed and Kok- Saghyz Rubber as a Compounding Ingredient for Buna So NoRoCo Report NOo 05=433, Apro 1^ 1943o r IP, 86 Brown^ AoCo Teats on (Plastic) CombSo NoRoCo Report Noo 0869-453^ Jano 22 „ 1946 o Browiip AoGo Tests on Melamine Tabiewareo NoRoCc Report Noo C266-43S, May 30^ 1945o Brown^ AoGo Tests on Plastics (Service) Underwear BuutonSo NoRoCo Report NOo C289- 43S. May 3^ 1943o Brown^ AoGo Spray Tests of Periscope Upper Prism Holders (Plastic), 0 NoRoCo Report Noo C1543°34S^ Novo 5. 1943o (See also Tapp^ JoSo. NoRoCo Report Noo C3170-42S^ Jano 29;, 1943) o Brown;, AoGo Impact s^ Tensiles and Water Absorptions on Prepared Samples of PlasticSo NoRoCo Report Noo C417'-43S;, May 17 ^ 1943 o Brown, AoGo Development of Waterproof Map;, Surfaced for Operational Maifcking In any Weather o NoRoCo Report NOo C556'-44S, July 3o 1944o Brown^ AoGo and Lashley. Ro Tests on Plastic Tubing for Alrcrafto NoRoCo Report NOo C2113°43S„ Pebo 16p 1944o Brown;, AoGo.^ Michael, Go and MacKay^ Eo Tests on Luclte and Plexlgias to Speco DTD339Ao NoRoCo Report NOo C314°44Si; May 19, 1944o Gallay, Wo Plastics Researcho Cano Cherao and ProCo Indo 25^ 635-538 (1941) o "^ Gallay^, Wo Plastics in Engineeringo Engo Jo 2p\ 72«77p 103 (1944), Gallay^ Wo Plastic Laminated Materialo Cano Pato 424c, 938 r, Jano 9., 1945o Gallay.o Wo and Brown,, AoGo Plastic Bayansb Scabbards,, NoRoCo Report NOo C680-43S; June 23. o 1943 o Gallay, Wo and Graham, Go Go Production of Laminated StruC" tures., UoSo Pato 2^393,100,0 Jano 15., 1945o Gallay, Wo and Graham,, Go Go Laminated Structure So Cano Pato Appo 516^244. July 13, 1944o twolQ ' J l>-t;a. *:? oCi *i u 'i'lisL , ^o^"^ uodO . on ■ •'> ■■? r, VV 87 Gallayp Wo and Graham^, Go Go A New Method for Resin-Bonding of Woodo Chemo Indo 54^ 196-198 (1944) o Gallay^ Wo and Grahanio GoGo A New Gluing ProcesSo Modern Plastics^ 21p 126-129, 168, 170, 172 (i944)o Tappp Jo So The Composition and Method of Manufacture of a New and Peculiar Core Used in Radio SetSo NcRoCo Report NOo C613-41S,, June 11, 1945o Tappp JoSo Tests on Crash HelmetSo NoRoCo Report NOo C3122- 42Sp Jano 26, 1943o (See also Brown., AoGo,, NoRoCo Report NOo C1859-'43Sp Deco 23, 1943) o Tapp, Jo So Water Absorption Tests on Plastic Periscope Com- ponentSo NoRoCc Report NOo C2607-42S;, DeCo 2, 1942o Lubricating Grease Oallay.o Wo and Puddington, loEo The Effect of Certain Ad- dition Agents on the Physical States of Sodium SoapSo Cano Jo Reso B21, 211-'218, (1943) « Oallay^ Wo and Puddington. loE., The Physical States of An- hydrous Sodium Soaps'o Cano Jo ReSo B21^ 202-210 (1943) o Oallay^ W^ and Puddlngton, loEo Sedimentation Volumes and Anomalous Plow in Lyophobic SuspensionSo Cano Jo ReSo B21^ 171-'178 (1943) « Oallay^ Wo and Puddlngton, loEo Surface Tension of Sodium Soap Dispersions in Mineral Oils© Can© Jo ReSo B21,, 225--229 (1943)o Oallay, Wo and Puddlngton, loEo The Effect of High Shearing Stresses on Recrystalllzation of Sodium Soaps in Mineral OllSo Cano Jo ReSo j^2^ 103-108 (1944) o Gal lay. Wo and Puddlngton, loEo Low Temperature Saponifi- cation in Anhydrous SystemSo Cano Jo ReSo B22, 76-89 (1944)o Oallay, Wo and Puddlngton, loEo The Recrystalllzation of Calcium Soaps in Mineral OilSo Cano Jo Reso B22, 173-181 (1944) o ,:- .t ■< .t1 ITfG' ■-1 ^ ~ i. -0 J- V. i LA Lis.(=- SCTBOC . -ill rfSB'^X' r: edk T .qqsT -, diJj H-al ^^'-t>;rrr^Di;^ ,.■ "/lO bns.- £ exnjj .. " o V o xtB ■:■. ,F 'M .\ ..enolc. '^ Irrs .,Vv nnri: no ^ - \li\SiLBQ li-.,. ,t ySi:::^ - ciSJ^ ^'iT 7f I ■ iVi no f:'{:aE9irc ^ ~v |. ^tL' WO J ,^itf 3 .. lo riclrtBsXlIjG; ■ X ^ s .^ a. \j BtH 1 jt^l-^X) 1:8 I o ^ 88 Gallay^ Wo and Puddingtorip loEu Sedimentation Volumes and Rigidity in Suspensions of Sodium Soaps in Mineral OilSo Cano Jo Re So B22.o 16-20 (1944) o Gallayp Wo and Puddington, loEo The State of Dispersion of Calcium Stearate in Mineral OilSo Cano Jo ReSo B22 ..; 161'-172 (1944) o Gallayp Wo and Puddington loEo Wetting Power in Caiblum Soap - Oil SystemSo Cano Jo ReSo B22^ 155-160 (1944) o Oallay^ Wo and Puddington., loEo Plow-Pressure Relationships in Calcium Soap - Oil SystemSo Cano Jo Reso 24., 73 80 (1946 )o Gallayp Wo and Puddlngtonn loEo The Composition of Aluminium Stearateo Cane Jo ReSo 32 6. o i55='160,; 1948o Gallay, Wo and Puddingtono loEo Lubricants n UoSo Pato 2^594^ 907,, Pebo 12 i, 1946o Gallay^ Wo and Puddington^n loEo The Recrystallization of Sodium Soaps in Mineral OilSo Caiiu Jo ReSo B22 ■> 90-102 (1944) o Gallay^ Wo. Puddington,, loEo and Tapp, JoSo Pibre Structure In Dispersion of Soap in Mineral Oilo Can< Jo ReSo B22p 66--75 (1944) o Gallay, Wo ^ Puddington, I0E0.0 and Tapp.., Jo So Wetting Power in Sodium Soap - Mineral Oil SystemSo Can^ Jo Reso B21p 230='235 (1943) o Gallay, Wo .0 Puddington, loEo and Tapp, JoSo Summary Report on Lubricating Grease -- Parts I„ II.., Ill and IVo NoRoCo Report NOo C1272-'42Pp July 1942o Alkaloids Manske. RoHoPo The Alkaloids of Pumariaceous Plant Sj> XXIV ? Corydalis ochotensis Turezo Cano Jo ReSo BlBo 75^79 TmUT ' o Manske^ Rt^HoPo The Alkaloids of Pumariaceous Plant s^ XXV 2 Corydalis pallida PerSo Can,. Jo ReSo B18, 80-93 (1940) O Ljr X -''^ <-.v,'. W 'to .to.rrtiJsiiliB.'.t '■ :b€ iC 'Tiu2 C ,T- '-^ ,:■ i i J f,- J I^ cm. rr^M 89 Manskep RoHoFo The Alkaloids of Rumariaceous PlantSo XXVI§ Corydalls clavlculata (L) DCo Cano Jo ReSo B18^ 97-99 (1940)o Manske^ RoHoPo The Alkaloids of Pumariaceous Plant So XXVII A New Aikaloido Che 1 lanthif oljne ^ and its Constitutiono Cano Jo Re So Bx8„ 100-102 (1940^ o Manske^, RoHoPo The Alkaloids of Pumariaceous PlantSo XXVTIIg Corydalis n.g:bilis PerSo Cano Jo ReSo Bx8y 288- 292 (194( ManskOp RoHoPo The Alkaloids of Pumariaceous PlantSo XXXg Aurotensineo Cano Jo Reso BlSf, 414'-417 (1940) o Manske^ RoHoPo A New Source of Cocositolo Cano Jo ReSo 319.9 34-37 (1941) o ManskOp RoHoPo The Alkaloids of Pumariaceous PlantSo XXXIg Corydalis montana (Engelmo) Brittonc Cano Jo Reso B20<, 49'^52"Tl942TI " ManskOp RoHoPo The Chemistry of QulnolineSo Chemo Revo 30.9 113-=>i44 (1942 )o Manske^ RoHcPo The Chemistry of IsoqulnollneSo Chemo Revo 30p 145-^158 (1942 )o Manske, RoHoPo The Alkaloids of Papaveraceous PlantSo XXXII 8 Stylophorum diphylliim (MlchXo ) Nuttoo Di cranes trlmna f ranche t ianum (Praln) Pedde and Glaucium serpleinieldro Cane Jo ReSo B20., 53-56 (1942 )o ManskOp RoHoPo The Alkaloids of Pumariaceous PlantSo XXXIII s Corydalis cheilantheifolia Hemselo Cano Jo ReSo B20o 57-60 (1942)o Manskeo RoHoPo The Natural Occurrence of 3-Methoxy-Pyrldln©o Cano Jo Re So B2p,, 265<-2e7 (1942 )o Manske^ RoHoPo The Alkaloids of Pumariaceous PlantSo XXXV§ Corydalis platycarpa Makino o Cano Jo ReSo B21o 13-- 16 (1943 )o Manske^, RoHoPo An Alkaloid from Menispermum canadense La, Cano Jo ReSo B2ip 17='20 (19437^ a i >M M vxxx -i I, 90 Manske^ RoHoPo The Alkaloids of Pumariaceous PlantSo XXXVI Corydalls thalictrlfolla Pranch<) and the Constitution of a new Alkaloids n Thalictrif olineo Cano Jo Reso B21,o 111=116 (1943) o Manske^, RoHoPo The Alkaloids of Pumariaceous PlanuSo XXXVTIf Dactylicapnos macropapnos Hutchinsono Cano Jo Re So B21, 117-118 ( 19451 o Manske, RoHoPo The Alkaloid-? of Papaveraceous Plant So XXXVIII g Bocconie^ Arborea WatSo Cano Jo ReSo B21o 140- 143 (1943TI Manske^ RoHoPo and Marion Lo The Alkaloids of Pumariaceous PlantSo XXIX^ The Constitution of Cryptocavineo JoAm© Chemo Soco 62^ 2024-2044 (1940) o Manske^ RoHoPo and Marion Lo The Alkaloids of Lycopodium SpecleSo Is Lycopodium complanatum Lo ^ Cano Jo Reso B20p 87-92 (1942) o Manskep RoHoPo and Marion Lo The Alkaloids of Lycopodium Specieso III^ L: B21„ 92.-96 (1943 Specie So III^ Lycopodium annotinum Lop Cane Jo Reso ' ITo Manske, RoHoPo and Marion Lo The Alkaloids of Thermopsls rhombifolla (Nutto) RichardSo Cano Jo Re s o B2l7 ~ 144-148 (1943) o Manske, RoHoPo and Marion Lo The Alkaloids of Lycopodium SpecieSo Vg Lycopodium obscurum Lo Cano Jo ReSo B22.9 53»55 (1944) o Manske, RoHoPo r Marion, Lo and Ledinghara^ AoEo The Alkaloids of Papaveraceous Plant So XXXIV g Hunnemannia furmariae- folia Sweet and the Constitution of a New Alkaloid^ Hunnemanineo Jo Amo Chemo SoCo 6£o 1659-1661 (1942)o Mansle^ RoHoPo o Marion, Lo and Leger^ Po The Synthesis and the Characterization of the Monomethyi- and the Dimethyl- quinolineso Cano Jo ReSo B20^ 133°152 (1942) « Marlonp Lo GelseminOo I^ The Degradation of Gelsemine to 2p3"dimethylindoleo Cano Jo ReSo B2lp 247-250 (1943) o Marionj, Lo The Synthesis of Of,N-Dimethylanolobineo Jo Amo Chemo SoCo 66^ 1125-1127 (1944) o d B X r J 1 •_ ,J >T^ enBi.i o 1 a Iff A 91 Marion, Lo The Alkaloids of Sedum acre Lo^, Cano Jo Reso B25;, 165=166 (1945) o "^ Marion, Lo and Graasie^ Vo The Synthesis of l°Roemerineo J. Amo Chemo Soco 66 ^, 1290=1292 (1944) o Marlon^ Lo and Manske,; RoHoPo The Alkaloids of Lycopodium Specie So lis Some Degradation Experiments with Lycopodineo Cano Jo ReSo B20,; 153-156 (1942)o Marionp L« and Mansleo RoHoP* The Alkaloids of Lycopodium Specieso IVs Lycopodium tristachyum Fursho Cano Jo ReSo B22p 1-^4 (1944) o Marion.^ Lo and Manske^ RoHoPo The Alkaloids of Lycopodium Specie So VI g Lycopodium clavatus Lo Cano Jo Reso B22,9 137-139 (1944)o "~^ Micro Organic Analysis Marlon, Lo and Ledingham^ AoEo Micro-analysis of Gaseous HydrocarbonSo Indo Engo Chemo ^ Analo Edc IS^ 269 (1941) o Starch Gallayp Wo and Puddington,, loEo The Hydration of Starch below the Gelatlnization TemperaturOo Cano Jo ReSo B21, 179'=185 (1943)o "" Tapp, Jo So Bird Continuous Centrifuge in Starch Manufacture, NoRoCo Report NOo C213-40S^ Augo 9, 1940o Peat Storeyp EoB© Peat Resin Product in GR-S CompoundSo NoRoCo Report NOo C352"45Sp June 20, 1945o Miscellaneous Organic Investigations Easthara, AoMo and Cambron, Ao New Method for Preparing But- adiene « NoRoCo Report Noo C3505-42S, March 3^ 1943o Easthamo AoMo and Cambronp Ao Apparatus for the Rapid Analysis of Butadiene Samples© NoRoCo Report Noo C3503-42S^ March 3^, 1943o isM ofeci r .J ■ I' ^aoI'isM . t> ; I L . ."I « 'J 3iiM ;10ltJE?M o^^ IBM 0 92 Hopkins, CoYo Report on Starch in Flour© JouPo AoOoAoCo 23p 489»491 (1940) o Hopkins, CoYo Taste Differences in Compounds having the NCS Linkage o Cano Jo ReSo 620^ 268-273 (1942)o Hopkins, CoYo Patty Acids of Hare"'s Ear Mustard Seed Oilo Cano Jo ReSo B24.o 2il«220, September, 1946o Hopkins, CoYo and Chisholm, Mo Jo Chlorination by Aqueous Sodium Hypochlorite o Cano Jo ReSo B24.o 208-210, September, 1946© Hopkins, CoYo and Chisholm, Mo Jo < -Cyano-^ -Phenylglyceric Acido Cano Jo ReSo 624^ 89=92, July 1946o Hopkins, CoYo.o Chisholm, Mo and Michael, Ro < -Cyano-^ -Aryl" acrylic AcidSo Cano Jo ReSo 623^ 84-87, (1945) o Katz, Mo and Mark, Ho The Kinetics of Polymerization Reactionso NoRoCo Report NOo C15-=40S, Apro 15, 1940® i-71i\ -^^ I^JBO 95 D, PROTECTION OF PERSOMEL AM) Ei^UIPMENT SPECIFIC ATI ONS5 TESTING, AND TEST METHODS The routine testing of equipment and supplies for the Armed Services was a function of such agencies as the Inspection Board of the United Kingdom and Canadao Howeverp considerable testing was done by tne Division of Chemistry of the National Research Council before suitable facilities were established by the Inspection Board or because the Research Council possessed special equipment or experience requisite to the tasko In general^, the Research Council did not undertake routine testing when other suitable laboratories were availableo The burden of this routine work fell par- ticularly heavily upon the Textile, Rubber., Corrosion^ Leathsr and Plasties^ and Protective Coatings Laboratorieso A number of oases arose in which no specifications existed or in which existing specifications required modi- fication due to the necessity of using substitute materlalSo In such cases the Research Council was often called upon to provide a suitable specif icationo This in turn often re- quired the development of test methods appropriate to the case under consideration. Such activities occupied a considerable part of the time and effort of the Textile^ Rubber^ Corrosion^ and Protective Laboratories^ and constituted an extremely valuable^ alt^iough unspectacular^ contribution to the national war effort. The specif ligations prepared numbeir" several hundred and the tests performed number well over ten thqusando Although some reference will be made in what follows to particular as" pects of this workf, no effort will be made to discuss it in full. Advisory Panels on Textiles^ on Leather,, and on. Rubber were set up under the National Research Council Co- ordinating Committee on Protective Equipment,, for the purpose of examining the technical requirements of specif Icationsg to ensure that they were in order. All specifications re- ceived from the Directorate of Interservlce Research and Development were transmitted to the members of the appropriate Panels when necessary, meetings of the Panel were held to discuss them^ and suggested changes wsre incorporated in new specifications. In all the work a very close liaison was maintained with the Directorate of Interservlce Research and Development. bf: 'A -IZ i £i : . pw:.. I ^.■' . • T i. *^r id'y -.A e3''v/:i.fa ttli-^ war .a 94 • TEXTILES Parachutes When it was realized^, early in the war<> that there would be a shortage of silk for parachu-ce canopleSo and of linen for harness webbing „ a Committee on Substitutes for Parachute Materials was formed^ under the auspices of the National Research Council^ with representation from the manu- facturers and from the Air Force o An investigation was made of the properties required in parachute materials^ and various possible substitutes were tested for strengths for elastic properties,, for weighty for effect of lights and^ in the case of canopy cloth^ for air permeabilityo It is fortunate that two years before the war there had been introduced on the market a new synthetic textile fibre •= nylon - from which a light material with high strength and good elastic properties could be produced, and which in this time of emergency proved to be the ideal material for parachute canopieso It was found possible to construct from it parachutes which were not only lighter f, but also stronger^ than the previous silk oneso In these parachutes the canopy and shrouds were of nylon^ and the harness webbing of cottono It speaks well for the work of the Committee that these new materials were first adopted officially in Canada^ The development work was handicapped by lack of definite information regarding the stresses to which the para- chute is subjected when it open.„ hence decisions had to be based largely on full-scale field trialSo Until recently the important question of impact strength had been neglected and work is in progress to compare the impact strength of nylon with that of fortisan - the only material with a reason- able degree of elasticity and at all comparable in strengtho The parachutes studied included those for flares as well as those for personnel© Since the requirements for flare parachutes were less critlcalo It was possible to sub'- stitute rayon by using a somewhat heavier fabric and reduc- ing the strength requirements to a minlm\imo With the assis- tance of the Aeronautical Laboratoryr, a gauge was built to register the opening shock loads of the flare parachutes,, but the gauge was found to have too low a range for the purpose^ and the work was not continued because existing flare para- chutes had proved satisfactory. i^p • no-tla^xT' ^^d foiirow YlI-sioi'Tlo n^ 1" o li '^pI "^ cf £) 6 q Of r'. 0 c ' Idw c .1 :i:.r^ine »C:^:. iix -exoB-ifctq. . eiiJ'flo.Qi.eq e/i. S iO . .. i ^91 95 Routine Teats for the Subcommittee on Wool Throughout the war years^ testing work was con- tinued for the Sub-Committee on Wool of the National Sheep Committeeo This involv ed t e stingy each year^ about 300 samples of wool clipped from sheep in experimental flocks in the Westo These samples were all tested for clean yield of wool, for fibre diameter^ and in some cases for fibre length and other special characteristicso Aviation Medical Research » Protective Clothing Problems assigned to the Textile Laboratory by the Subcommittee on Protective Clothing of the Associate Committee on Aviation Medical Research had to do mostly with the comfort of certain items of clothingo The first essential was to develop and standardize methods of evaluating f abrics and clothing for comfort p and methods of measuring thermal in- aulationo This was done in collaboration with the Ontario Research Foundation and the Banting and Best Institute of Medical Research, The National Research Council co-operated with the United States authorities^ in standardizing thermal Insulation test methods^ by measuring the thermal insulation of samples already measured by themo The thermal insulating properties of various fabrics were the chief subject of investigation. It was found that heat losses due to radiation could be reduced by applying a bright flexible metallic coating to cloth 5 and apparatus for the continuous electroplating of cloth was built and operatedo Later, when it was found that double pile fabrics afforded the best means of attaining the insulation required, with a maximum of flexibility and a minimum of weighty work was largely confined to a study of the properties of these double pile fabrics, which were finally adopted as standard for lining air-crew suits. Quilted materials were also studied, but it was found that the required degree of Insulation could be obtained only by sacrificing flexibility or llghtnesso The early work showed that the thermal insulation of double pile fabrics was dependent upon their thickness; the construction of pile fabrics was therefore studied with a view to obtaining maximum resistance to compression without loss of insulation or lightness. The materials investigated included fabrics with piles made from mohair c, alpaca, cotton (candle-wick), rayon, and Aralac, in single and double pile construction, as well as the sharling formerly used in air- men's Jackets. The effect of various factors, particularly ■'p eii;? 10 ".i q eerie iBrzc. 00c ikic £c*X 'I**?' Bfid :tij : 10 1 .-^e 8K 3- =10 'i moo erid nolJsIJLfsni: I.Cii- JO nj , ) olo i ,v ©Icfifob eseri^ lo fc:e bijjoo £10 l:fBlij an: M i: ^ . r / . O J Olj i'Ol e ^eeen^folrf::'- -^ d^hv bi^'tbuii . :tiLrorf;tiw nalEae'iamco ou r[o:t;tco ,BOBqiB ^riBdom i Yl'IBliJOXCtlBq Hc?T ^ ei©w ■ fc i :r fieri -'-i-- eri^ /iOitBj , _ ^U! ■ ■^ ■■ 6f»':? IxeC XBfn be , d% , . i .■.■ .'T •^fi'«■cn,.■ -^ ^_'-5 r Cfi/Cf . ■•'■■• .-.■•" . ed -. - - -^ lo eric? ;V JE? U^ ''J a em 96 that of humidityp were studied in connection with the com- pressibility of these materiaiSo The best ground construe- tion had to be determined as well as the most desirable quality of wool for ito It was also necessary to initiate water absorption studies of these fabric So Not only was it important to study the behaviour of the double pile fabrics, but it was also necessary to investigate the type of cover °all used over the double pile^ and to investigate the variations in the properties of the coverall with wind conditionso This was an extensive piece of work requiring determinations under a wide variety of conditions o The permeability of coverall fabrics was shown to be important only with high winds > with low wind velocities the effects were independent of the type of coveraxlo The relationship between wind velocity and protection afforded by coveralls of various permeabilities was completely invest tigatedo With this informationo it is possible to evaluate any fabric with regard to wind protection© This study is still being pursued to determine the effect of wind on any free space behind the coverall materials and thence to cal- culate the thermal insulation in areas where the clothing is looseo With reference to this problem., the effect of air leak- age,, or ventilation, through clothing is one that deserves further study; information on warmth of clothing will not be complete until such experiments are carried outo A study had to be made of the behaviour of the interlining materials during dry cleaning, launderlng.o and service. By varying the methods of determining thickness it was found possible to gauge fairly accurately the effective thickness of the material during service use,, and hence to determine its insulation effectiveness, which had been shown to depend upon thickness© Methods for evaluating the flotation properties of filler materials in life Jackets were also studied© In this connection, the compression characteristics of milkweed,, kapok^o and polystyrene fibres were determinedo Tests on the waterproofing properties, of various materials were also carried out for the Subcommittee on Pro- tective Clothingo A project has been started for the purpose of determining the role played by various factors iri'^con- trolling the water repellency of materials but this in only In Its Initial stages so that there is nothing to report as yeti, i^rivl 97 Investigations for the National Research Council Coordinating Coimnittee on Protective Equipment (Research) One project undertaken for the Coordinating Com- mittee on Protective Equipment was the study of the present general service sock for the purpose of recommending a better wearing sock;, and of determining the best method of reducing shrinkage « The study involved testing the pro- ducts of fourteen different manufacturers, and developing proper test methods for shrinkage and for determining damage to socks resulting from any treatment given to re- duce the felting properties of the woolo It was the re- sponsibility of the Subcommittee working on this problem to make recommendations regarding the best method of pro- ducing this shrink resistance and regarding the standard- ization of sock constructiono Although it has not yet been possible to make any decision regarding the best method of producing an anti-shrlnk sock,, definite recommendations have been made regarding improved sock constructiono Samples made according to these recommendations have been tested, and it has been found that by using the proper type of wool and by proper mechanical construction a very great reduction in shrinkage can be effected^ so that chemical anti-shrink treatments sire no longer necessary in order to meet the specificationso Another investigation for this Committee indic- ated that no apparent advantage in preventing stains is obtained by providing a v/ater repellent finish for clothing when the clothing is used under conditions in which the type of soiling is predominantly of an oily or greasy nature. This would be expected to be the case with overalls worn by mechanic So On the other hand, there is evidence that the use of a water repellent finish is a very great advantage in re- ducing the tencency to stain by aqueous types of dirt. While only one of the soils used in the present investigation was of the aqueous type., the results obtained;, together with data gathered from previous work along this line, indicate quite clearly that for aqueous types of soil the use of a permanent water repellent finish (Velan) is advantageous. Another investigation indicated that a satis- factory rotproof vamp-lining fabric could be produced by substituting a permanent --type cellulose finish containing a rotproofer for the previously used starch-type f inlsh^, which was known to promote the rotting of the liningo The rotproofers used in this investigation were commercial pre- parations in which the active ingredient is phenyl mercuric A C' -- .vr 1 ,■' p , j . 'J ?£ o t i ; o -L J J3o , r. i J" 0 OC £ •'O i i J J 6 em vnl •\ 7.j^ 1 ,oeJB ed^ nerfw ^ .... - ^ v^ airlT > erfzt nO :io em £ :->^ iici^nl"! yaelleqe J;J 1o ■^d ntB^e OCT Y--^©^"" ... J ^'-nfo ' cil b^Bij ^::ZtGB erf:t ''to 6. . ; C e iljLfB©'! 9f{.t. ,. SQY^ ;o ."•f , r : .-' ^j-ow EiLTolveiq , . . . .. ...33 BLroeiipB lol rtBxiJ Vj-' iBe./o X (iii:5laV) lie in 11 d-xie. iieq ei' ■ lattBw oLijni 'eeaji; Ycf mo\v eJ:iBi:;v,.. . . . ., .. 9Ei/ ddi d-jBdd- eon ai)iv 9 el e^fi •"61 ai egBctnfivbB i-B' ov eXlriV; ••:till) lo seq^: - BBw xiol^Bgld'eeval ^nr: B:tBJb ri:rlw 'lerlcfegoi .benxirjao e.:txi;p ||[fBol£)ni .enxl slrict ,1nenBmieq b lo seij' arf.-t Xlos • 8JJ0 63BCfilBVfcB ycf f)oo;/ii)OT:q e "^iO L' i« 99 The outbreak of war in the Pacific ^ at the end of 1941^ gave additional impetus to research in the field of rot- proofing^ especially in the United States where large research programs were quickly set up by various agencies - Oog© Army Quartermaster Depot s^ the Bureau of Standards ^ and the De- partment of Agriculture o The National Research Council has been constantly in touch vrlzh these agencieso Since the be- ginning of 1942 there has been an ever-^growing list of items requiring rotproofingo One instance of such a material., manufactured in Canada in very considerable quantity, is waterproofed duck^ used for covers for motor transport vehicles, Several million yards of this material have been produced in Canada during the last four yearso When the material was to be used under conditions in which microbiological attack might occur •» for example „ in the trt)pics =- it was essential that it have an adequate degree of rotproofnesso The publication by the Scientific Liaison Bureau^ Melbourne ^ Australia^, of the confidential "Report on the Condition of Service Material under Tropical Conditions in New Guinea** drew the attention of Service supply agencies to the great need for proper pack« aging and adequate protection a gainst the ravages of moisture and microbiological attacko Although this report may have presented the story of the deterioration of Service material in the tropics at its worst o there was little doubt that^ as long as hostilities in the tropics continued^, there was the possibility of this type of deteriorationo Laboratory work in this field was theref ore .piir- sued with increasing intensityo A large amount of information on rotproofers was colle cted and compiled in an index covering the composition and properties of most of the rotproofing com- pounds on the marketo The first requirement for a program of investi- gation was to have reasonably satisfactory methods for assess- ing rotproofnesSo In general^, use is made of two methods j one involves the use of pure cultures of one .or other of the cellulose destroying fungi^ and the other involves burial of the treated material in biologically a ctive soil under con- trolled conditions of temperature and moisturoo Arrangements were made for carrying out the pure culture tests in the Division of Applied Biologyr, while the soil burial tests were conducted in the Division of Chemistryo As information on the efficacy of various rot- proofing agents was collected^ it became possible i^ the case of certain of these compounds, for example , copper naphthenate^ to dispense with the biological tests, and to assess* the degree ■7BW o e.. ii)HJ c; "*^ ci.ifc'iu ffi o O t-ji i 1 10 c t: q .1 o T no '^ ■• '' ^ ^^. ' .... -. .- - lu I e't«:?w 8d"ee:t I.eJi'^-.. r 4^f> 31 ew a V 1o odj 100 of rotproofness of the treated, materials by means of a chemical analysis for the amount of rotproofer pre sent o The National Research Council has cooperated with the American Association of Textile Chemists and Colorists in the work of their subcommittee on test methods for assessing microbiological attacko Much helpful information has been obtained from research organizations in the United States in connection with work on the estimation of various rotproofing agent So The types of rotproofing agents studied include aromatic phenolic derivatives^ organic and inorganic- copper compounds, dihydroxy-dichloro-di phenyl methane i, organic mercurials 0 and chromium treatments. The aromatic phenolic derivatives are not sufficiently permanent due to their vol- atility and water solubility j the inorganic copper is too water soluble and appears to c ause appreciable photochemical tendering of cellulosic fabrics j of organic cooper soaps such as the oleate, oleo s tearate^, and naphthenate.o the latter has been most used on this continent owing to the adequate supplies of naphthenlc acid from the petroleum industry - it has been found quite satisfactory in use | where the rotproofer comes in contact with rubber^ zinc naphthenate must be substituted for the copper compound^ copper tannate has been successfully applied in Canada to the rotproofing of sewing thread^j di" hydroxy-dl chl or o>di phenyl methane has been widely used and found to possess satisfactory properties when used In con- Junction with waterproofing waxes 5 the organic mercurials are not particularly effective by themselves and are rather easily removed by weathering., but when used with copper naphthenate they prevent the growth of copper tolerant bacteria, which^ although harmless to cellulosic materials., remove the copper and leave the fabric open to attack by other organisms 5 the so-called ^•mineral khaki" treatment, obtained by precipitating iron and chromium hydroxides or carbonates in the fabric.; has been found to be extremely fast to leaching and to offer con- siderable protection against actinic degradation., but to be poor protection against cellulose destroying fungi and bacteria< It cannot be too strongly emphasized that it is necessary to carry out weathering tests on rotproofers in order to determine their stability under conditions of usoo In many instances rotproofers have been placed on the market with- out due regard to this needo While it is customary to sub- mit rotproofers to the action of leaching with running water^ the importance of the effect of combined exposure to sunlight ^ rain, and wind has frequently been overlookedo In this con- nection there is also the possibility that certain types of 61. a^ Bi'ti lebi ■3 o:f .;a 101 rotproofing compounds may cause degradation of cotton fabrics due to catalytic actinic actiono For this reason the National Research Council has attached considerable importance to weathera.ng testSo A limited series of such tests were carried out during the summer of 1944 o These dealt chiefly with the re-^ sistance to weathering of copper naphthenate^ oleate^, and "tallate**;, and of copper hydroxy naphthenateo It was found that copper naphthenate and copper hydroxy naphthenate both shov/ed good fastness to weathering when present in association with waterproofing waxeso The weathering characteristics of the other compounds was of a considerably lower order© Recommendations and specifications have been pre^ pared regarding the rotproofing of numerous items of Service equipment;; including tentage, cordage^ sewing threadj> paper^ linen fire hose, insect netting^ and cotton duck for haver- sacks, kit bags., hammocks, and assault boatso Waterproofing Resistance to water is important in a -number of Service items such as protective clothing, cotton duck covers of all kinds, and canvas for assault boatSo The textile laboratory's early a ctivities in this field had to do with the setting up of test methods for assessing the water re- sistance of heavy fabrlcso As the demand for heavy waterproofed ducks for tran- sport vehicles increased^ the textile laboratory was instru- mental in arranging for the production in Canada of this material^ which had formerly been imported from the United StateSo The laboratory cooperated w ith the Army in the production of water repellent battle dress^ andc, in cooperation with the Rubber Laboratory^ work was undertaken for the RoCoAoPo on the develop- ment of an improved plastic-coated fabric for raincoatSo Flameproof ing Work in the field of textile flameproof ing was con- fined chiefly to giving advice on methods of treatment and methods of testo Early work carried out by the textile laboratory had to do with flame resistant treatments for cotton clothing worn by workers in munitions factorieSo Recommendations were made covering the use of mixtures of borax and boric acid 1 « T 102 applied at the end or the laundering operationo Since other types of water soluble^ flame resistant materials were on the market^) it was of interest to determine the possible damaging effect of all the commonly used water soluble f lame -pr oof ers when applied repeatedly to cotton garments after launder ing^ for it was considered possible that the effect of heat in the finishing operation might promote chemical tendering© It was found that certain of these materials ° eogo ammonium sulphamate caused considerable degradation when applied repeatedly to the same fabric© A considerable amount of testing was carried out on antiflash hoods and gloves treated with borax=boric acid mixture 3 p and recommendations regarding suitable amounts of the flameproof ing mixture were made to various manufacturers© Much attention has been given to methods of testing flame resistance© The usual type of test,, involving the ap- plication of a flame to the lower edge of a fabric,, under con<- trolled conditions, was regarded as inadequate in the case of materials which in use might be subjected to the action of a flame impinging on their surface© Hence a surface burning test was devised and has become a standard method© Assistance was given to the industry in applying permanent flame resistant treatments employing mixtures of chlorinated paraffins or aromatics in conjunction with antimony oxide© Experimental cotton coveralls for tank crews were developed, in collaboration with the Chemical Warfare Labor- atories, using vinylacetate-vinyl-chloride copolymer with antimony oxide,, a treatment developed by the United States Chemical Warfare Service© Bacteriostatic Treatments At the request of the Associate Committee on Army Medical Research^, laboratory and plant-scale studies were made of methods of testing army blankets to provide a fabric pos- sessing a bacteriostatic or bactericidal surface, which would prevent the dissemination of airborne infection from blankets in hospital wards and dormitories© The problem was also of interest with respect to the possibility of producing a bac- tericidal fabric for use in ordinary items of combat clothing© r^ , 3pf ;■ 'iO 0 0 "iei:ui;j oX'"icifi.i b lo egJDe tewoi e E lo nol^oB eri-t oct l^e^loe. «(r yncnlctn.f? fi'revi Qwe-jo ilnB".-' 'T-^'^ s^IlB'^L'evc "■ ■:^ )-t r f- ©bsfti e'levf ss,; ■■aoq Dii'dst ^.r e.te>inBJcf mo "to oel-- -ojad 8 31; ., -.':^'i ., -..^ > • -■- ^-^ O rt' 103 Methods of treating blankets after laundering were worked out which were satisfactory for this purposoo These methods were a decided Improvement on those formerly available o Laundering and Dry Cleaning Assistance was given to the Armed Services in setting up their laundry and cleaning activities, and exten- sive assistance was rendered in solving various problems which arose concerning the laundering of Service clothingp Close contact was maintained with the laundry and dry cleaning industry during the war^, although it was necessary to discontinue research for private industryo It was con- sidered advisable to continue the test bundle service,, since this gave a measure of the washing efficiency of laundry and dry cleaning plants^ and was., therefore^ of importance from the point of view of prolonging the life of clothingo The referee service has also been maintained and has been of value in bringing to light certain shortcomings of wartime textileso One such difficulty has had to do with an apparent reduction in the quality of dyestuffs used in consumer clothing^ despite the fact that it has been well established that there is no need for such a reduction© Work was completed on the development of a modified short formula for use in the laundering of white cottons, using silicated alkaline builders. This formula was put to use in a number of plants throughout Canada „ and has effected a con- siderable saving in time and washing supplies, in addition to its beneficial effect in reducing the amount of mechanical action suffered by clothing during washingo Substitute Materials In adrl-'tion to the work on parachuteSc already dis= cussedr other problems arose due to shortages of various tex- tile fibreso Work on cordage substitutes arose as a result of the critical shortages of hard fibresp such as manila and sisalo Substitute rope, of cotton, satisfactory for certain purposes^ was developed in cooperation with the industry© Another problem^ initiated at the request of the Inspection Board;9 had to do with finding a substitute for the silk fabric used in ammunition exploder bagSo Recommendations be' 1 ^ >• 'Bib 'r|)BaiI.6 ©cJJ •i QTt rfn r '■■ 07 104 regarding the use of a fabric woven from spun viscose yarn and carrying a special finish had been received from the United Kingdomo Considerable work was carried out on this project in cooperation with the industry- with particular reference to the finishing treatment, ^niiich employed a con= stltuent (urea formaldehyde resin) designed to suppress de- terioration of the viscose yarn caused by nitrous vapours© The rate of burning of the fabric was also controlled by the use of ammonium dihydrogen phosphate o The suitability of cotton as a substitute for the silk and linen thread pre- viously used in these bags was investigated^ and its use for this purpose was recommendedo Considerable work was carried out on the relative buoyancy properties of Canadian milkweed as compared to Java kapoko At a packing density equal to that used in life- saving equipment (3 pounds per cubic foot)i, the buoyancy of milkweed was found to be equal to that of kapok after im- mersion periods up to forty-eight hourso The loss in buoyancy over longer periods of immersion was slightly greater for milkweedo The effect of buoyancy of mechanical shock was also studiedo There is no doubt that Canadian milkweed can be used as a substitute for kapok in buoyancy equipment but^ unfor- tunately,, no action was taken in this mattero Studies were also made of the buoyancy properties of cat--tail floss (typha)^ Bubblfil (viscose filaments carrying entrapped air)^ and water repellent cotton fibre© Cat=tail floss was tested as a sub- stitute for kapok and considerable promise was shown© Miscellaneous Investigations Early in the war an investigation was started to determine the reason for the deterioration of cotton fabrics at the water-line when they are partly immersed^ It was found that the effect was apparently due to the selective absorption of ions by the cotton, resulting in an acidic reaction at the water-linoo Work was also initiated on a study of the con" stitution of woolj the wool was broken down by acid hydrolysis under various conditions and the relative proportion of liberated amine acids was determlnedo Both of these projects were aban- doned because of the pressure of urgent war problems o At the request of the Navy an effort was made to prolong the life of awnings used on shipboard;, which had de- teriorated very rapidly in the pasto An examination of the old canvas indicated that weakening of the cotton was due to acid damage rather than to oxidation or mildewo Substantial lengths of canvas were treated (a) with cutch^, (b) with a cellulose acetate coating., or (c) with sodium bicarbonate :;:."; i r ."^evow jfcxJ./-'- llTX-V TJifi scr^tcfBl aod'Joo la iioi oBirfoIcfciL: Ti % ji-^agij:.! lo ^: ■f'T B'i9nt OT eJ^Bm Esw jiolle lib yvbH eriJ , ,tiinirrT£.*'.B r o^ &i^b 8 sw n o i ;? ' ' ^ :i s. o v.- B rl:tl»v (a; ~do:ikjr iiti?^ (.9) ^j- 105 followed by calcium chloride ^^ which left calcium carbonate deposited on the fabrico These samples were subjected to service trials but were not returnedo so it was not possible to compare the relative merits of the three treatmentSo However i all reports from the ship on which the pieces were under test indicated that after two and a half years of service they v/ere still in good shape o Tests were made to compare the degree of ventila- tion of standard bell tents with those fabricated from canvas proofed against fire^ rot, and moisture^ and to determine whether there is any hazard to personnel,, or effect on their efficiency ;, due to carbon monoxide, carbon dioxidOo or lack of oxygen resulting from occupying such tents when closed and heated under winter conditions,, The ventilation rate was de- termined by observing the rate of decay of gas concentration after release of measured amounts of sulphur dioxide con- densed in glass bulbs^ The hazard to personnel was assessed by analyzing the air in the tents at definite intervals during the period in which they were occupied^ and also by the ex- amination of blood samples collected from the men before and after occupying the tentSo There was no marked difference shown by the use of the proofed canvas^ even under winter con- ditions, with a low outside wind velocity., the heater in operation^, and the tent inhabited by six meno LEATHER AND ALLIED PRODUCTS A considerable amount of work was done in the Division of Chemistry in connection with leather products and equipment for the ServiceSo The bulk of the work was concerned with the chemical and physical analysis of various kinds of leathers used In Service footwear, such as vegetable- tanned sole leathers^ chrome-vegetable-retan upper leather ^ and chrome -tanned upper leatherc Prom the laboratory viewpoint ^ comparatively good and uniform quality leathers have been produced throughout the waro In one case only, the laboratory confirmed the sus-- picion of the Inspection Board that a tanner was incapable of obtaining a satisfactory product^ and his allocation of hides was redistributed by the control authorities to those who could Similar analyses were carried out from time to time on garment leathers (chrome -tanned horsehide or dowhide) for such items as glove 3^0 mitts,, and flying helmetSo Various leather washers •- eogo washers for torpedoes^ fuse cap washers for ""Hfllla^ and hydraulic leathers for the buffer mechanism of twenty^-five- pounder and other guns - were 106 continually being tested to ensure a satisfactory product^ free from constituents which might have a deleterious effect on the lifetime or performance of the stores involvedo During the period of acute fat shortages, tanners had great difficulty in obtaining suitable stuffing greases for Army upper leather^ and physical tests on proposed mix- tures enabled the quality to be maintainedo Shoe polishes,, dubbinSp and other waterproofing materials for Service boots were frequently testedo Since the establishment of Service boot rebuilding depots,^ analyses of the various oils (straight and sulphonated fish oils,, mostly) used in revivifying the leather have been carried out to ensure a uniform and satis- factory products The causes of the cracking of chrome-tanned shoe vamps, and the causes of shoe insole deterioration were invest igatedo A technique for the measurement of the real density of leather was dovelopedo Abrasion resistance measurements on soleing materials have frequently been madeo While It is recognized that abrasion is only one of the factors involved in the wear of soleing materials, and while the small variations in abrasion resis- tance between different sole leathers are not very significant,, useful results have been obtslned from such measurements in establishing, in a general way. the relative values of various synthetic soleing materials.,, and in indicating the superior wearing qualities of such materials over the average leathero At the request of the Department of Munitions and Supply work was undertaken to produce a substitute for leather shoe sole So The material found most satisfactory for this purpose was fabric coated with polyvinyl butyralo Sufficient layers of this material laminated under heat and pressure gave a sheet of any desired thickness^, which had a flexibility similar to leathero Wear tests on the product showed that it outwore leather by a factor of about twoo At the request of the Navy to develop a rubber shoe that would not slip on wet decks ^ various designs were cut in soft rubber., and the angle at which they slipped on a piece of wet steel; when weighted with a fixed load, was notedo A "V" design eventually was recommended^ Various minor problems encountered by the Services were investigated from time to timeo 107 CORROSION Corrosion is a relentless enemy against which an unremitting struggle must inevitably be fought - in war even as in peace o During the war the solution of specific pro° blems submitted by the Armed Services occupied about three quarters of the efforts of the Corrosion Laboratory^ the balance of the time was directed toward more fundamental in«= vestigations of corrosion phenomenao Fundamental Research Just prior to the outbreak of war^ the laboratory began an experimental s tudy of cadmium and zinc coatings on steelo Panels were exposed at the Atlantic and Pacific coasts at the half^tide position^ and other panels were exposed in the laboratoryo Cadmium plating and zinc plating were found to be about equally resistant to tap water | cadmium piating was the more resistant to sea^water at half-'tide position© A study was made of the corrosion resistance of low-alloyp high-strengtn steels in sea-water,; exposures being made at both sea coastSo At the same time a study was made of the aea-water corrosion resistance of five aluminiim alloys said to be quite resistant to sea-watero It is thought that this work should be extended because marine growths appear to have a bad effect on certain a lloys^ while others survive with but little or no attacks The type of growth and its incidence appears to be importanto The evidence is quite clear that anodizing contributes no significant advantage to these alloys in resistance to corrosion by the seao Of course^, anodizing is an excellent base for paintSo One of the chief research activities of the lab-- oratory is the devising of new and better corrosion test- methodSo A new apparatus for continuous, completely sub- merged testing of metal specimens in liquids has been devisedr, its merits have been evaluated^ and a description of the ap° paratus has been publishedo Preliminary work was done on a stirring corrosion testo Some work was done on methods of testing with humidity effects^, but this was set aside pending provision of more space o Another very important field of research is that of corrosion Inhibitorso A search is being made for better inhibitors for antifreeze liquids^ mostly with negative re- sults so faro Inhibitors of corrosion of ordinary pipes by water presented a number of important unsolved problems^ in particular, the published work on the effects of sodium 108 hexametaphosphate ("Caigon") appeared to be quite inadequate o An investigation revealed the important fact that sodium hexametaphosphate has littlec, if any^ inhibitive effect in still or stagnant water - it is only active when the water Is in motiono Purthermoreo the amount of sodium hexameta- phosphate that gives best inhibition is considerably greater than that alleged in published articleSo These articles,, unfortunately, present no quantitative datao When there is inhibition, the potential of iron against a calomel half cell dropSo A few preliminary experiments have been made with sodium nitriteo A number of inhibitors will be studied in this connection - eogo sodium silicates^ phosphates, lime^ soda asho caustic , chromates^. and organic compounds o Metal cleaners w ere tested for corrosion effects^ and some work was done to determine the relative efficiency of cleanerSo This latter problem seems to have two aspects^ namely^, rate of cleaning,., and amount of permissible contamin= ation of the cleaner before discardingo The first aspect was solvedg it was found that consistent and reproducible results could bo obtained using steel panels which had been annealed by heating to 600**Co and cooling overnight in the furnace | the panels were then pickled to remove scale^ and finally were polished electrolyticallyo With such surfaces^ the times,, or rateSn of cleaning of oiled surfaces in the various cleaners were closely reproducible.o usually checking within 15 seconds© The second aspect of the problem requires development of a test for cleaniinesso Many cleaners contain wetting agents which make it possible to wet oils with water p so the water break test fails to measure cleanliness in such caseso Incomplete studies were made of metal spray- coatings on steel;, exposed in the sea at Miami,, Ploridao The object was to learn whether zinc protection blocks on ships may be replaced by patches of zinc spray-metal^, applied re- peatedly over old sprayed metal without more than wire- brushing the previous zinc surface o Time has not permitted further work on this project o Experiments were done on electrolytic polishing of duraluminumo Invariably the electrolyte etched the work during removal from the electrolyte and before washing could b© accomplishedo Pulling the work through a layer of Nujol on the surface of the electrolyte reduced the etchingo Further work is planned on this problemo Very considerable test work was done,, early in the war^ on temporary protective coatings,, that is., on oils^ e'j '-lO ^ f'. 109 grease Sp and waxes o These results were later very useful in making approvals and in preparing specificationSo Upwards of a hundred of these materials were testedo Specific Problems for the Armed Services Early in the war the problem of a specification for dishwashing compounds for aluminum ware was presentedo Such proprietary compounds usually consist of mixtures of soda ash^, sodium metasilicate„ trisodium phosphate^ and sodium pyro-phosphateo Investigation showed that soda ash is the ingredient cheifly responsible for corrosive attack of aluminum^ and that increasing the sodium metasilicate content of the mixture to 25^ almost completely prevents this attacko Many corrosion tests for the Armed Services were made on innumerable items of equipment such as ball bearings,, flash lights,, automobile lights^ water filter barrels^ web° bing hardware p silver plated ware^ coffee urns^ strapping for shipping boxes,,, camouflage materials,, and fuso boxeso A long'-term study was undertaken of drums of various metals containing aviation gasolineo The preliminary studies were useful in choosing metals for gas tanks on patrol- torpedo boatSo An extensive experimental study was made of the corrosion of steel by used crankcase oilo A number of antifreezes were submitted for cor- rosion tests and., in cooperation with the Army, a practical road test was run on trucks to make a comparison between ethylene-glycol-type antifreeze and calcium-chloride-type antifreezco The latter proved to be very corrosive© Experimental studies were made of protective coat- ings for bomber exhaust manifolds of low carbon steelo On the basis of experiments, the Lp^boratory suggested considera= tion of the use of a single base coat of f erro-enamel.,, which could be applied inside as well as outside the manifold after fabricationo It is understood that this was used later in the United States as a substitute for unavailable alloyso Considerable attention was given to coating smoke cups for tuenty^five^pounder guns, a problem submitted by the Inspection Boardo Howeverc, before proven success was attainedp a modified method of filling solved the difficultyo A problem in rusting of large calibre shells was also i^studiedo 110 Corrosion of corrugated steel huts for storage of shells near Montreal was invest igstedo Measurements showed that the steel should last long enough without further pro- tective treatment o Some work was done for the Chemical Warfare Labor- atories on corrosion by acids and by war gaseso Some attention was given to electrical insulation of dissimilar metal jointSo Insulation of ship^s propellers by using a grease loaded with mica between shaft and pro- peller was found ineffective in laboratory trialso During the last two years of the ware work was done on packaging of metal articles for export to tropical regionSo The Corrosion Laboratory early advocated testing of final packages in humidityo All containers^, except tin cans or galvanized cans soldered closed, let moisture get in- side | once insidep it cannot get outp andy in timOp the article rusts.o even though coated with a rust preventativeo Rust pre° vention of metal articles is better with a heavier coating of rust preventative than with most wrapperso However^ mechan- ical protection of the coated article is considered requisiteo Tropicalization of trucks has been considered by the Laboratoryo Carburetors are made of die-cast zinc^ which^ in sea-water and sea airo corroses very rapidly in contact with the variety of dissimilar metals comprising a trucko A high temperature paint was found to give considerably enhanced protection to the zinc, and is now understood to be used in practiceo The ball and socket joints of front steering wheels also corrode,, so the Laboratory made up.c and teste dp a cor- rosion-inhibiting grease for this useo This grease has also baen suggested for factory application to all nuts and bolts of vehicles,, in peace as well as in war^ as bolts and studs break due to rusting, particularly in the Pacific tropicso Brakes and brake drums also presented a serious problem of deterioration^, the drums being alleged to perforate in a month opposite rivets of the llningo Tests were started in this latter connection but the alleged perforation effects could not be substantiated in laboratory simulated trialso A number of problems encountered during operations were investigated, such as the corrosion of the lifting cables on aircraft engaged in North Sea patrolo This was found to be due to soldering flux,, carelessly left by workmen assembl- ing the worko In a number of cases of plane crashes^ the Corrosion Laboratory was asked to investigate certain aspects of the case to help determine the cause of the accidento in Specific Problems for Commercial Firms In 1940 the Laboratory studied the problem of severe sporadic corrosion of rivets in the hull of the 5000<= ton train ferryp "Charlottetown"c It was found that the badly corroded rivets showed Neumann lines in polished and etched sections., an evidence of finishing at too low a temperature - so low^ that stress relief did not occur suf- ficientlyo It was recommended that any future rivets be finished at as high a temperature as possible and that the rivet lines be sandblasted^ spray-coated with metallic aluminium^ and then painted^, in order to try to prevent further deteriorationo This was done^o but the "Charlotte-^ town" was sunk less than a year later^ so there was no opportunity to learn the effects of the spray coatingo It was learned subsequently that zinc should have been used because it repels fouling better than does aluminumo Recently the problem of severe corrosion by cold brines in the new type of overhead-icing refrigerator cars of the Canadian National Railway was presentedo Some pre- liminary suggestions were made which should eliminate some of the deterioration^ and work is continuing on this problemo Another problem recently presented by a commercial firm concerns treatment of mine hoisting cables with the flrm-s proprietary rust preventative o Preliminary experiments have been outlined in this difficult and awkward problemo Upwards of one hundred reports were issued each year by the Corrosion Laboratory so that it is impossible to give a complete bibliographyo Some of these are listed among those at the end of this Sectiono PROTECTIVE COATINGS The importance of protective coatings in the pro- duction of war equipment was indicated by the large volume of enquiries received by the Protective Coatings Laboratory of the National Research Councilo This Laboratory was frequently called into consultation by the Armed Forces regarding various aspects of paint design^ specif icationp and use^ so that fre- quent meetings,, discussions and job inspections were necessaryc Many of the recommendations required lengthy investigations and laboratory trials« The employment of substitute materials also necessitated much investigation and proving in the Laboratoryo T 1ja:1:' I , i'iU.; i , Jo ara c ' e :> lie b i u o n^- ■ ri-:>B9 F-- '-^ - f ---'^^ '■ y -t^nr^- orr aicfj :jii;t ^^ Olid ' •:>r. 6)1 in bi C V • >-* 112 A large volume of approval testing was carried out for the British Supply Board and for the Inspection Board of the United Kingdom and Canada.,, from 1940 to 1943 o As part of this work it was necessary in some cases to design spec- ial apparatus and to prepare new test procedureso Experience accumulated by the Laboratory enabled the staff to offer useful recommendations leading to the revision of specif icationso For example ;, investigations of priming paints for shells re- sulted in a recommendation to adopto for this purpose., an entirely different type of primer which would eliminate much of the trouble previously caused by premature corrosiono Supervision of paints for motor transport con-- stituted one of the most important war functions of the Laboratory on account of the great volume of production^ whichp up to the end of 1944p totalled 745.000 vehicles^ valued at over two billion dollarso Thousands of gallons of vehicle paints were used daily throughout the period of the war^ and many problems arose in connection with their useo Investigations were necessary in connection with the approval testing of paint, the standardization of colourSn the deter° mination of duralDllity in service n the adjustment of dif- ficulties in use., the cleaning and preparing of the metal for painting, and the selection of priming and finish paints and of special paints for wood bodieso As paint is one of the chief materials relied upon for camouflage of buildings and permanent ground instal- lations, camouflage paints and camouflage materials were studied in detailo Paints were selected suitable for Canadian use on coastal defence installations^, buildings^, and air fields J these included types for application to concreteo and to asphalt roadways.o as well as to wood and to metalo Specifications were written to control their purchase and inspectiono Experiments were conducted.o and recommendations made^ in respect to camouflage painting of motor vehicle s^, packing cases, galvanized roof s^, Airforce buildingSn and run™ wayso When the use of steel wool for camouflage purposes introduced painting problems, since this material must be well protected by paint to prevent its destruction by cor- rosionc, the Laboratory made recommendations as to paints and painting procedures,, carried out tests of paints,., and adjusted difficulties in early productiono This made pos-- slble the production of considerable quantities of steel- wool camouflage nets in Canada in 1942o Recommendations were made as to methods of finishing other camouflage materials such as paper garnlshingj, camouflage cloth^ camouflage netSc, and tentSo Accelerated weathering tests were conducted on a number of these materials o Close 113 study was directed to the matter of Infrared reflectivity of camouflage paints, so that^ when the Army requested In-- formation early in 1943,, the Laboratory was well prepared to deal with the mattero Infrared reflectance standards had been assembled,, and equipment for measuring infrared reflectance had been set up and calibratedo In this con-^ ^ nectlon a number of samples of paint from production w^-ne tested;, and recommendations were made to manufacturers as to choice of pigments and manufacturing methods o In 1943 a request was received from the Depart- ment of National Defence for a material which would make canvas to itage resistait to water,, flame and mildew, and would aloo be satisfactory for comouflageo A survey of commercially available materials was made without finding one that was entirely suitablec Accordingly, development work was undertaken to formulate such a material and to provide test methods for determining its effectivenesso When satisfactory samples had been prepared in the Labor- atory. International Paints (Canada) Ltdo co-operated by making pilot plant plant batches from the most promising formulae c The development erf suitable materials and test methods permitted the writing of a specification for the preservative compound in collaboration with the Textile Laboratoryo The preservative material chosen consisted of a chlorinated hydrocarbon base containing fire retardent pigments such as antimony oxide o Practical trials of the material on Army tents, carried out by Army personnel under the supervision of the Laboratory staff, demonstrated that the treatment was satlsfactoryo More recentlyc, a large sample was supplied to the British Army Staff in India for experimental worko Proper painting of landing barges constructed of plywood was an important problem on which the advice of the Laboratory was requestedo After a study of the construction of the vessels and of the conditions of useo a painting scheme was prepared and put into effecto The Laboratory also assisted in providing decontamlnable paints for use on folding boats and pontoons when the existing specifiC'= at ions were found to be unsuitable o Occasional inquiries regarding the usefulness and availability of luminous paints were received through^ out the war periodo Shortly after commencing work on phos- phorescent paints, it was realized that there was an urgent necessity for a method of measuring the brightness or lumin- osity of the paint coatings and the duration of such bright- nesso There was also need for the establishment of minimum JO 114 requirements for brightness and for the preparation of a specification which would include all of the essential features of a phosphorescent painto It was soon discovered that physicists had not yet been successful in devising a simple and rapid method for measuring the brightness of sur- faces at such low levels of brightness o The use of the MacBeth photometer was tedious since the observer must spend at least forty minutes becoming dark-adapted before taking a reading^' furthermore,, the accuracy obtainable was un" satisfactoryo Considerable time was spend endeavouring to reproduce and to improve a photographic method originated by the United States Army, but it was eventually abandoned^ About this time new methods were introduced in Great Britain and in the United State So The American apparatus was based - on the use of photoelectric cells ^ this method was not con- sidered acceptable because the relationship between the human eye and the photoelectric cell at low levels of bright- ness is not adequately knowno The British method proved satisfactory and was adopted© It consisted essentially of a modified MacBeth photometer with a built-in device for subjecting the sample to a standardized irradiation with ultraviolet light o It did not, however^ eliminate the nee-- essity for becoming dark-adapted before making measurement So The necessary apparatus was constructed by the Optics Labor- atory and., after a study of available commercial products^ a specification (No,. PR-2) was prepared to cover a luminous paint having high initial brightness and to cover one having long af ter^-glowo Extensive work was carried out on fire retardant paint for shipSo Methods for the removal of heavy^ oil-paint coatings were studied., and ships at Halifax were inspected to determine the condition of the painted areas with respect to fire hazardo Recommendations for stripping and refinishing were madeo Specifications for fire retardant paints were written^ methods of test were compared,, and commercial products were evaluatedo Other Naval paints considered included an interior coating for drinking water tanks., interior anti- condensation coatings, insulating varnishes., and exterior camouflage paints o A detailed study of gloss requirement s^ gloss standards, and measurements of gloss was carried outo Aircraft finishes of many types were investigatedo A major project was the selection of a suitable coating for the interior of plywood gasoline and alcohol tankSo This study was completed in collaboration with the Structures Laboratory of the Division of Mechanical Engineeringo c .' i J:^it. 115 Protective coatings for tropical use were studied in detailp particular attention "being given to the evaluation of rotproofing coatings for woodo The evaluation of wood preservatives and rot resistant materials had always been difficult and time'-consumingo During 1944 the Protective Coatings Laboratory developed a new method of test for such substance Sc involving the determination of loss in tensile strength of wood veneer strips dipped in the preservative and subjected to soil burialo By this means a numerical index of the efficiency of rotproofing agents can be obtained, In addition.., performance testing of packaging waxes^ mildew- proofing lacquerSi, and canvas preservatives was carried outo TREATMENT FOR "TRENCH MOUTH" In the clinical treatment of "trench mouth"^ officers of the Dental Corps had observed that Fowler's solution (ioeo i% arsenious oxide in water^, neutralized with potassiiim hydroxide) and hydrogen peroxide -- both of which are old remedies of none too great effectiveness - when mixed together, became much more effective than would bo expectedo Efforts were made to utilize this discovery^, but the mixture was found to have defects which could not b6 corrected^ It etched the teeth badly in its original condition; if made sufficiently alkaline to prevent etching^ the peroxide decomposed and the mixture was not effective; and, if made neutral., or faintly acid enough to be stable^ etching reappearedo When the matter was referred to the National Research Council^p it was felt in the Division of Chemistry that further study in the light of the above observation might lead to a solution of the problemo The etching was clearly caused by the fact that arsenates, produced from arsenites in Fowler "s solution by oxidation with the hydrogen peroxide^, are isomorphous (that l3, crystallize in identical form) with the phosphates of the teetho Thus a solution containing arsenate,, placed in contact with the teeth, removes a layer of phosphate,, and deposits in its place a layer of arsenate^ This is later removed as a foreign substance by the saliva, and the effect l3 repeated at each use of the solutiono A study of the underlying causes shows that there is only one way of combatting this difficulty;, namely.n the use of a solution actually supersaturated with respect to tooth substance y largely calcium and magnesium phosphateSo Since such supersaturated solutions can be prepared only by special methods^ it is clear why earlier efforts had not succeededo 116 The ultimate objective was a useful treatment in tablet form butj, since the need was urgent r, a recipe was first provided which involved mixing a number of separate solutionso By this procedure it is quite easy to secure several-fold super saturation and, fortunately, in the case of calcium phosphate such supersaturated solutions are ade- quately stable^ if mixed only as needed for immediate dis- pensingo The development p however p of a dry powder which would dissolve to provide a supersaturated solution was hardly expected to be successfulp since it is axiomatic that solids will not dissolve past the saturation point© After much experimenting^, however ;, it was discovered that a mixture of sodium or potassium phosphate with a calcium salt such as the benzoate would readily produce solutions considerably supersaturated© ThiSp no doubt, is due to the organic nature of the calcium benzoate g it apparently dis- solves as intact molecules and ionises later only after adequate dilution has been secured to prevent immediate pre- cipltatlono The next recipe therefore used these salts but still required that the preparation be left as a more or less loose powder, for when this powder was pressed into compact tablets the intimate contact resulted in the pro- duction of insoluble calcium and magnesium phosphates o The powder was therefore packaged in capsules, to be dissolved in peroxide at the time of dispensing© A large number of tests were then made on methods of preparing a tablet which would still remain soluble after long storage© It was found that a frothing agent added still greater efficacy to the mixture p so different ways of incorporating this frothing agent were tested in attempts to stabilize the tablet© The best method found was to coat all particles of the powder with the frother by adding it to the powder as a benzene solutionp rather than by incorporating it by grinding© These coated grains could then be mixedo without further grinding, and pressed into tablets© The stability of the tablets produced in this way was tested by subjecting them alternately to a temperature of 60**Co for forty-eight hours, and then to 98% humidity at 20®C© for an equal period© After fifteen such cycles they were found to retain over 90% solubility, although they had swelled and crumbled slightly© Yet one drop of liquid water will cause a tablet to set immediately to a hardness resem- bling concrete© Sn.. ■ erIT '>*•«-. ni ^ ■11 a If' el 3Y < -t •:: BT 117 All clinical tests during this work were conducted by the Canadian Dental Corps o The Department of Pensions and National Health made a valuable contribution by studying the toxicity of this form of arseniCo Prom these toxicity studies it would appear that the minim\am lethal dose for man would be about one tablet every day for a week 5 and since each patient is issued only one tablets, already dissolved in peroxide^ there seems no danger of accident in this re- spect o Although many thousands of cases have now been treated with this prescription, no single case of any re- action attributable to the arsenic has yet been notedo Many cases of sensitivity to the peroxide are found but these are readily adjusted by using it rather weaker, and the symptoms rapidly disappear after discontinuing its use© In many cases twenty-four hours" treatment will arrest,, and very markedly improve ^ serious conditions of the mouth; and only rarely is treatment as long as a week neededo Patients who cannot eat are frequently comfortable after one day.o that is.^ after four applications of the treats mento Many conditions other than that commonly known as "trench mouth", benefit markedly.^ for example, several cases of Vincent's infection of the tonsils have been cured by its usee Indeed.o many inflammatory conditions of the mouth ap- pear to involve organisms against which this treatment is beneficialo MISCELLANEOUS INVESTIGATIONS Anti-Dim Materials Anyone who has had his spectacles fog over in the winter-time upon entering a warm room will understand how serious the fogging of goggles or gas mask can be for a soldier or airman in combat o Ant i -dim materials commonly in use are all soluble substances and are^ therefore ^ removed readily as soon as condensation occurso During the defrosting Investigations it was noted that the polyethers of myricyl alcohol have properties v^ich make them valuable as anti-dim agent So If the ether chain is not too long^ that is,, if it Is less than about forty units long, these ethers are hardly soluble in water at alio They are., however., quite active antl-'dims with any chain length above about eight unitSo Consequently.-, within this range, effective anti-dims may be obtained which are sufficiently insoluble that one application of material may be used over long periodSo The Chemical War- fare Laboratories tested these materials and found them very satisfactoryo ail p, p rfv ;;! ^Xl erit .rl Tf^vo .a ecf x^^ p'^tf -l-j/^B evict '^e'^'\r» 118 Plastic Armour Early in the waro at the request of the Navy^ an attempt was made to improve the plastic armour then in use as a substitute for steel armour plateo This plastic armour con- sisted of a mixture of gravely limestone^ and asphalto About a year of continuous effort was spent experimenting with various shapes and mesh sizes of the gravely different types of gravel and different ways smd means of fabricationo In addition to this, a new type of non^etallic armour was de- veloped, which consisted of crushed rock bonded with sodium silicateo REPORTS Textiles Bayley^ Co Ho The Effect of Light and Air on the Accuracy of Cuprammonlum Fluidity Measurements on Textile Cottono Bayleyp Co Ho Effect of a Permanent Water Repellent Finish (Velan) on the Removal by Laundering of Stains Pre- dominantly of an Oil^Soluble Type© NoRoCo Report Noo C2286-43S, Maro 18^ 1944o Bayley, Co Ho Notes on the Dry and Wet Chlorination Processes for Pre-shrinking Woolo Report to NoRoCo Co-ordo Com* Protecto Equip o p DeCo 8;, 1944o Bayley^ Co Ho Improved Fabric for Vamp Linings and Doublers for ShoeSo Report to NoRoCo Co-ordo Como Protecto Equipo5 July 25p 1944o Bayley, Co Ho Camouflage Dyeing of Army Clothingo Report to NoRoCo Co-ordo Como Protecto Equipo p Septo 18^ 1944o Bayley^ Co Ho Investigation of Improved Fabric for RoCoAoF. Raincoat So Report to NoRoCo Co-^ordo Como Protecto Equipop Maro 28^ 1945o Bayleyp Co Ho Dry Cleanability of Co Wo Ao Co Cap Peak Stiff enerso Report to NoRoCo Co^ordo Com. Protecto Equipo,, May^ 1944o Bayleyp Co Ho Examination of Four Types of Tents as Requested by Chiefs of Staff Sub-Commo on Protective Equipment, (in connection with the 1943=44 winter trials) « NoRoCo Report NOo C548-44Sn June 28^ 1944o VLB ri'C zV. ^ a -■'<: . ill J 'A*' '^ ' ■(■ 1 -3 Elnr 119 Bayley^ CoHo Kaumagraph Markings on GS SockSo Report to Co«=ordo Cqwo Protecto Equipo « Novo 27^ 1944o Bayley^ Co Ho Report on the Situation in Great Britain and Canada with Respect to Tentage Ducko Report to NoRoC* Co°ordo Conio Protecto Equipo , Deco 8;, 1944* Bayley^ CoHo Notes on the Copper-Iron (''CupronO Process for the Rotproof ing of Cotton TextileSo Report, to NoRoCo Co-ordo Como Protecto Equipop DeCo 22^ 1944. Bayleyo CoHo Notes on the Rotproof ing of Cotton and Linen Sewing Threado Report to NoRoCo Co-ordo Como Protect. Equipo , Jano 23p 1945o Bayleyp CoHo Notes on the Rotproof ing of Woolo Report to NoRoCo CO"Ordo Como Protecto Equipo ^ Pebo 8, 1945. Bay ley, CoHo Situation in Canada with Respect to the Use of the Iron°Chromium (Mineral Dyeing) Process for the Rot- proofing of Cottono Report to NoRoCo Co-ordo Com. Protecto Equipo , Maro 31, 1944o Bayley, CoHo Rotproofness Tests on Cotton Thread Treated by the Cutch"Copper-Ammonia ( »CCA' ) "Process, N.RoCo Report NOo C1695-^44S, Pebo 3, 1945o Bayley, C.Ho Plameproof ing of Cotton Textiles used by Muni- tions Workerso NoRoCo Report NOo C822°41S, July 2, 1941, Bayley, CoHo The Souring Operationo Laundry & Dry Cleaning JouTo Cano 19^ NoVo ^ 15-17, 21 (1939 )o Bay ley, CoHo Modified Short Pormula with Silicated Alkaline Builderso Laundry & Dry Cleaning Jouro Cano 20, March 8="9, 30 (1940). Bayley, CoHo Standards for Military Worko Laundry & Dry Cleaning Jouro Cano 20p Septo^ 8-11 (1940) o Bayley,, CoHo Laundering Coloured GoodSo Laundry & Dry Cleaning Jouro Cano 21j, July, 8-10 (1941) o Bayley, CoHo Dry Cleaning - Laundering - Cotton Textiles. Cano Chemo & Proco Indo 26p 47-50 (1942) o Bayley, CoHo War°time ProblemSo Laundry & Dry Cleaning Jour< Cano 22^ Octo, 9p 20-21 (1942). 9IX eeaooi'i t ■ no .qi/0 ) aoi^-^i- OCT .-^^LoqeH teellJxeT aoc - . - - -- lo 82XJ erlct ort cfoeqeeH rtitlw arcnBO nl nol^fltrr? •mod oi)io-»oO cO^HoW o^ 710 ■ o(6c9.r) IS , Vj. ai oVoK ,,§£, iiJ^O , i. ©nilfijll^ be-Jj80Xlie rfdXw sXifarro'^ ;fiod« i ^..•> - r. :1. c(o^ei^ ^'-'-^ -^qea (,02 ^fT^r. .-• .(1^91) C: .. •<.XJJu .^2 oH^O oii oiiiol. snJtnBs'O y*^^ ^ "^' ' ..errxelcO' . , S^9I) iS-L 120 Bayley^ CoHo Questions and Answers - a monthly featiire in the Laundry and Dry Cleaning Journal of Canada of since May 1943o Bayleyp Co Ho Detergent Properties of Soaps Containing Bentoniteo NoRoCo Report NOo C585=4535 Augo 17^ 1945o Bayley^, Co Ho and Larose,, Po Testing Defence Textileso 1941 Manual of the Textile Industry^ Po 78o Bayley, CoHo and LarosOo Po Research on War Uses of TextileSo 1943 Manual of the Textile Industry., po 85o Bayleyp CoHo^ Rose^ GoRoPo and Weatherburn^ Ao So ThQ Applic- ation of Dust-laying Oils to Wool, Cano Jo Reso P24p 224-^231 (1946) o Bayleyp CoHo^, Rose,, GoRoPo and Weatherburn^ AoSo Chemical Aspects of the Application of Dust°laying Oil to Cotton© Cano Jo Re So P2j4^ Septo 348-359, 1946 o Bayley, CoHo and Tweedie^, AoSo Examination of the Rot Re- sistance of Various Mineral Dyed Ducks of Canadian Manufacture o Report to NoRoCo CO'=ordo Como Protect© Equipo , Septo lis. 1944o Bayley, CoHo and Tweedie., AoSo Comparative Launderabilities of Certain Cotton Uniform Cloths of Canadian and UoSoA© Manufactureo NoRoCo Report Noo C890-45S, Pebo 1, 1946© Bayley, CoH© and Weatherburn, MoW© Observations on the Growth of Some Coppertolerant Pungi on Cotton PabricSo Can© Textile JouTo 62^ Maro 9., 34'=36p 46 (1945) and Amer© Dyestuff Reporter^ 34^ 247=248 (1945) o Bayleyp CoH© and Weatherburn^ M©Wo A Study of the Effect of Leaching on the Rotproofing Efficacy of Copper Naph- thenate© Amero Dyestuff Reporter, 34p 457-460, 471-473 (1945)© Bayley, CoH© and Weatherburnc, MoW© The Effect of Weathering on Cotton Pabric Containing Certain Copper Rotproofers© Can© Jo Reso P24^ 193-202,, (1946)© Bayley, CoH© ana Weatherburn, MoWo The Effect of Weathering on Rotprpofed Cordage© Amer© Dyestuff Reporter, 35, 218p 235-236 (1946)© 051 IsoImsi-fO nS.A _niucfi©ri^BeW bfiB o'^oH.,0 <^eeoH ^.F.O velrcS eai^tillc^. - -'-.-i/Bj i^viJBiBq::.: . aiLeewT Lns cKoO c.^oIybS oA 08011 Jbni? nBlfcsnaO lo edctoiD m'lcllnTJ rxo:f;toD nlBiieO lo „e ■ " pOe'^. ^eei^-'OesO uOlf ;t^oq©H oOofl.P! .eTj/loBlDiJe;/! iI^woiO ©rict no anoxaBvieeoO ^WcM jfla^iaierfitBeW i)nB oHV.O ,X9*T*S ofiBO -.eolndBS no:t:foO no Ignjj^ ^naielo JieqqoO ©mo2 lo oiemA i?nB (5^S.:} a^ ,^S--^S .9 ibT,! .26 ,TXfoL elf^-sT lo cfoollE ori;t lo rbu^E A oW^M ,^Ai'::iJCfi9r{:yBeW baB oHoO r^YelY^e^ -riqBK teqqoO lo Y-^J^oillS 3nlioo*iq:fofl eilcf no ^irio&ed 3ni:ierf;tBeW lo ^toallS ©oT oWoM .n r;.rd'i©rid-BeW bna „K oO c^el^JE^S oeieloo'iq:tofl leqqoO ni.Bu*^i©0 ^nliiltiJnoO oI'icfB'^ no:^.+oO no gn i lerlitfift W lo ;t 0 sllH. erfP o W o M ,, niirrfi an ^ BeW nriB ., M 0 v el •^ bS „5£ q©H llif^faaYCT o'leii^A „e3Bfc'ioO f)eloo'ic 121 Bayley^ Co Ho and Weathorburn^ Mo Wo The Effect of Accelerated Weathering on Cotton Thread "Proofed by the Cutch-Copper= Anmonia Prooeaa and the Chrome ProceaSo Report to NoRoCo Co-ordo Como Protect* Equipo., Maro 24., 1945, Bayley, Co Ho and Weatherburn^ Mo We Investigation of the use of Ammonium Humate in the Rotproofing of Cotton Fabric o NoRoCo Report NOo C922'-45S<, Marc 23^ 1945o Bay ley., Co Ho and Weatherburn., Mo Wo Copper-S^Hydroxy-quinoline as a Rotproofing Treatment o NoRoCc Report NOo C77-46S5 Apro 17 p 1946 o Bayleyp Co Ho and Weatherburn. Mo Wo The Cupron Rotproofing Treatmento N.RoCo Report NOo C916-45S5 Mar, 12, 1946. Bayley, Co Ho and Weatherburn^ AoSo Chemical Aspects of the Application of Dust-laying Oils to Woolo Cano J. Reso F25, 402=412 (1945), Larosep Po Tensile Strength Tests, Cano Textile Jour. 57, NOo 1, S5 (1940). Larose„ P. A New Form of Abrasion Testero Cano Jo Res. A18, 161-164 (1940). Larose, Po The Breaking Strength of FabricSo Jo Textile Insto 32, T167-T178 (1941) o Larose n P. Pectic Substances in Cottono Cano Jouro Reso Bi9, 61-64 (1941). Larose o Po Lea Keratines© Revue Trimestrielle Canadienne^ 27, 271-284 (1941). Larose, P. The Water Absorption by TowelSo Amer. Dyestuff Reporter 31^ 105-108, 123-124 (1942) o Larose, Po Expansion of Textile Research, Cano Textile Jouro 60p Octo 22^ 15«16 (1943). Larose, P. Application of Statistics to Textile Manufacturing* Can„ Textile Jouro 62, Jam 12^ 39, 42, 43 (1945). Larose, P. Standard Regain of TextileSo Cano Textile Jour© 62, July 13, 42, 51 (1945). he;:^ <.B&H oZ o.ibO re' 'll>;;tft3YQ .. ror ; t»woT vcf no ''7 CI 122 Larosop Po Newer Fibres, Cano Chenio & ProCo Indo 29, 476-479 (1945) o Larose, Po Variation in Thermal Insulation of Double Pile Fabrics with Thicknessc NoRoCo Report NOo C465»42S5 May 6^ 1942^ AoCoAoMoRo Report NOo C2460e Larose^ Po Compressibility and Thickness of Pile Fabricso NoRoCo Report NOo C2075'-42So Octo 19^ 1942^ AcCoAoMoRo Report NOo C2337o Larosep Po Compression of Milkweed, Kapok and Polystyrene FibreSo AoCcAoMoRo Report NOo C2404o Larose^ P. Compressibility of Double Pile FabricSo AeCoAoMoR. Report NOo C2406o Larose, Po Compressibility and Recovery of Candlewick FabricSo AoCoAoM«Ro Report Noo C2407o Larosep P« Thermal Insulation of Interlining Fabric with Coverall MaterialSo AoCoAoM«Ro Report NOo C2411o Larosep Po Compression and Recovery of Insole MaterialSo AoC.AoM,Ro Report NOo C2430o Larose^, Po Compressibility of Worn Flying Suit Liningo AoCoAoNoRo Report NOo C2469o Larose.o Po The Effect of Moisture Content on Thickness, Compressibility and Recovery of Pile FabricSo AoCoAoMoRo Report NOo C2498o Larose, Po Thermal Insulation due to Protection Given by Coverall Materials of Various Permeabilitieso AoCoAoMoRo Report NOc C2611o Larose,, Po Test Methods - A Revised Compressibility Method© AoCrAoMoRo Report NOo C2687o Larose^o Po The Measurement of Compressibility of Double Pile FabricSo AoCeAoMoRo Report NOo C2688o Larose ^, P. Change in Thickness of Double Pile Fabric with Moisture Contento AoCoAoMoRo Report NOo C2654o Larose p P« Thermal Insulation of 1/4" Cork and l/2" Wool Double Pile FabriCo AoCoAoMoRo Report Noo C2936o e n ©TV d^ E -f: I o 'i tm^ - r. ii^ . f . .0 A ix-J ^ ri^ilYf grrln.,^ ._ 10 r ■TT f -f "t r . p. ■'^r I o r^ r ii'' "*■ 2 .?. c :.'^ ,t < 'Tit' fi ,/i J4..A -U ,A .i^o:i^9M ^s^ >.ii^ ©Xdi/oG lo \, ell's -qJ h'5 !9i . 123 Larose^ Po Sock Shrinkageo NoRoCo Report NOo C78-46Sp June lOp 1946 o Larose^ Po and Burton^ AoCo Comparison of Methods of Measure- ment of Thermal Insulation of PabricSo AoCoAoMoRo Report NOo C2410o Larose, Po and GoodingSp AoC» Test Methods and Ratings, AoCoAoMoRo Report NOo C2419o Puddingtono loEo Properties of Cat^tail Plosso NoRoCo Report No. C1877°42Sp Septo 29^ 1942o Rose, GoRoPo and Bayley^ Co Ho Strength Tests on Cotton Duck, Cano Textile Jouro 58. Augo 15 ^ 31-32 (1941) o Tweedie, AoSo and Bayley^ C,Ho Preservation of Cordage o Amero Dyestuff Reporter, 33, 373=374, 378=379 (1944) o Tweedie, AoSo and Bayley^, CoHo Deterioration of Plame- proofed Cotton PabriCo Cano Textile Jour, 60, Aug, 27, 31, 33 (1943), Weatherburn^ MoW. and Bayley^ Co Ho Hydrolysis Method for the Determination of Copper in Copper-Naphthenate- Treated MaterialSo Cano Chemo & Proco Indo 29, 52 (1945) Weatherburn^ AoSo^) Weatherburn. MoWo and Bayley, CH, Deter- mination of Copper and Zinc in their NaphthenateSo Ind, Engo Chemo p Analo Ed« 16 ^ 703 (1944) « Leather and Allied Products Brown^ Ac Co Tests on Greases for Stuffing Upper Leather, N.RoCo Report NOo C210'43S, April 22^ 1943, Brown^ AoGo Analysis of Dressing Compound for Militia Boot Upperso NoRoCo Report Noo C8-44S, April 4, 1944, Brown, AoGo Waterproofing Tests on Mitt Leatherso NoRoC, Report NOo C683"45So Septo 24, 1945, Brown, AoGo Tests of Various Pormulations of Visole (Synthetic) Soleingo NoRoCo Report NOo C165-44S, April 28, 1944, Brown, AoGo and Wood, Wo Tests of Samples of Shoe Polish to Speco lGP-'48o NoRoCo Report NOo C416-44S, June 7, 1944, , ) . Vi , oijni .bt \JLlq^/l "I.:. c l ■- . V t. ^ a e 1 0 • :: 1 V lo 2 n C 1 J B I JJflllO'^I 124 Gallay. Wo Substitutes for Sole Leathero Jo Amo Leather Chemo Assoco 38^ 250-255 (1943) o Gallay^ Wo Replacements for Shoe Leathero Cano Chemo & Proco Indo 27p 551-554 (1943) o Gallay^ Wo Synthetics in ShoeSo Modern Plastics 21 « 95=98„ 180p 182 (1944)o "" Gallay Wo Shoe Sole Materialo Cano Pato 424^,9380 Jano 9^, 1946 o Gallay^ Wo and Tapp., Jo So Deterioration of Shoe Upper Leather, Jo Amo Leather Chemo AssoCo 36^ 513=525 (1941) « Gallay o Wo and Tapp. Jo So Determination of the Real Density of Leathero Jo Amo Leather Chemo Assoco 37„ 140-150 (1942)o Tapp, Jo So Available Information on Dubbin^ NoRoCo #6o NoRoCo Report NOo C1919'=41S, Octo 30, 1941o Corrosion Broiighton, JoWo Tests of Aviation Fuel Stored in Drums Treated with Various Finishes by Corrosion Research Laboratoryo NoRoCo Report Noo MP'-1981^ Septo 25, 1945o Cohen„ Mo An Apparatus for Measuring Corrosiono TranSo Electrochemo SoCo 87^ 221°226 (1945) « Cohen, Mo Sodium Hexametaphosphate as a Corfosion Inhibitor for Ottawa Tap Water^ TranSo Electrochemo SoCo 89, 193-207 (1946) o Cohen, Mo and Halferdahlo AoCo Tropicalization of Motor Vehicles - Interim Report IIo NoRoCo Report NOo 01855-443, March 6, 1945o Cohen.o Mo,, Puddington,, loEo and Halferdahl^, AoCo Tropical^ ization of Motor Vehicles - Interim Report TIIo NoRoCo Report C45-45Sp Apro 11, 1945o Cohen.n Mo, Stegmayer^ GoMo and Half erdahl, AoCo Tropical- ization of Motor Vehicles - Interim Report IVs Re Corrosion of Brake DrumSo NoRoCo Report Noo C412-45S, June 25 „ 1945o ■n oj :r- r-. 125 Halferdahlp AoCo^ Michael^ ToHoGo and Griff ith,. ToRo • Insula- tion of Magnesium Alloys from Steele NoRoiCo Report Noo C450-44S, June 14,, 1944 (mimeographed) o Half erdahl^, AoCo and Stegmayer^, Go Mo Experiments under Fouling Conditions of Aluminum and Steel Panels Having Metal Spray and Paint CoatingSo NoRoCo Report NOo C4"44Sp April 4^ 1944o Halferdahl, AoCoo Stegmayer,, GoMo and Hennessy^ Eo Tests on Rust Preventive Oils and GreaseSo NoRoCo Report NOo C1500-43Sp Octo 29<, 1943 (mimeographed) o Migurska,. Ko and Halferdahl, AoCo Preliminary Corrosion Tests with Perchloric Acid and with Fuming Nitric Acido NoRoCo Report NOo C803-44S., Ai;igo 21p 1944o Stogmayerp GoMo and Halferdahl, AoCo Corrosion Tests on Rust Preventive Oils^ Waxes and Greases after Condition- ing with Airo NoRoCo Report Noo C1576'=44Sp Jano 10^ 1945 (Mimeographed) o Stegmayerp GoMo and Halferdahl^ AoCo Interim Report on Packages for Tropical Shipment exposed to Humidity Testo NoRoCo Report NOo C1599-44S. Jano 16^ 1945o Stegmayerp GoMo and Halferdahlp AoCo Humidity Tests on Packages ■= Further Test Results on Vapour Transmission© NoRoCo Report NOo C1708-44S, Febo 6, 1945o Stegmayer. GoMo and Halferdahl, AoCo Laboratory Testing of (a) Monel Metal and Everdur Metal suggested for over- head icing tanks in refrigerator cars; and of (b) Farbertite, Tygon linings and asphalt for the bottom of flues in refrigerator carso NoRoCo Report NOo C905='45Sp Febo 25^ 1946 « Thomasp JoFoJo Corrosion Researcho Cano Chemo & ProCo Indo 26^ 169'-171 (1942) o Thomasp JoFoJo The Effect of Dishwashing Compounds on Aluminumo Cano Jo ReSo Bol9p 153-157 (1941) o Thomas p JoFoJo Inhibition of Corrosion of Aluminum and Other Metals in Soda Ash SolutionSo Cano Jo ReSo B21p 43°53 (1943)o -a I * ,,oa •T^ >^ ' i; li y.'l-! ( ■ 126 Thomas^ JoPoJo Report of Experiments on the Corrosion of Steel by Used Crankcase OilSo Part Is The Effect of Treatment of the Oil with Magnesium and Other MetalSo NoRoCo Report NOo C94<-40Sp June 3^ 1940 (Mimeographed) o Thomas, JoPoJo and Halferdahl. AoCo Comparative Corrosion Resistance to Sea-Water of Low^-Alloyp High-^Strength SteelSo Cano Chemo & Proco Indo 29., 43-48 (1945To ThomaSi, JoPoJo and Half'erdahl^ Ac Co Corrosion Resistance of some Commercial Aluminum Alloys in Sea°Watero NoRoCo Report Noc 01042^ 43S. Augo 1942o (Mimeographed) o ThomaSo JoPoJc and Halferdahlo Ac Co Preliminary Corrosion Tests on Metals^, Alloys and Protective Coatings in the Construction of Aviation Gasoline Containerso NoRoC« Report NOo C1113-'40Po March, 1941o Protective Coatir^a Hopkins, CoYo Pire Retardant PaintSo Report for Naval Service^ NoRoCo Report NOo C812='43S^o July 10^ 1943o Hopkins n CoYo Rust Preventive Compounds « NoRoCo Report No© C3545°42Sp Mar© 11^ 1943o Hopkins r, CoYc Adhesion of Paint to Galvanized Iron© NoRoCo Report NOo C824"42Sn June 15, 1942o Hopkins. CoYo Insulating Impregnating VamisheSo NoRoCo Report NOo C360-43S, May 17,, 1943 « Hopkins., CoYo Modern Methods of Paint Testingo Official Digest Pederation Paint and Varnish Production ClubSp NOo 215 0 94-^101 (1942)o HopkinSo CoYo Paint Research -= War Problems in Manufacture^ Application^ Specifications and TestSo Cano Chemo & ProCo Indo 26,. 227'-229, 247 (1942) « Hopkins^ CoYo Paint Researcho Can© Paint and Varnish Magazine, 19^ NOo 3.o PPo 13p 16o 53 (1945) o Hopkins, CoYo Accelerated Weathering Tests of Enamels on Steel and Correlation with Outdoor Exposuroo ProCo Ao So To Mo 40, 289-294 (1940) o rj'' C-jir ' o- r.- H. /I z^edB Y ,0 C'^v •> 0\\ - jre.'■■ '- ^ r' ... . i.i'i^- '■•13'.. es 128 Treatment for "Trench Mouth** Stedman, DoPo Periodontia Corapositiono Can. Pat. Appo 527,025, May 23, 1945. Stedman, D.P. and Sterns, S. Development of Treatment for »Trench Mouthy N.R.C. Report No. C310-45S, May 17, 1945o Mlacellaneoua Investigations Gallay, Wo Plastic Armour. N.R.Co Report Nos. C1598-41S, Sept. 24, 1941 and C1825-41S, Oct. 20, 1941. Gallay, W. First Report on Non-Metallic Armoiir. N.R.C. Report Noo C2663-41S, January 1942. Gallay^ W. Second Report on Non-Metallic Armour, N.R.C. Report NOo C360-42S, April 1942. ''^^. ,8a^'-0I'!-0 .Oil J'l'-qeH •0,/i,M :M rior RI^- '"9'=J"0 ,80v: :t-- ,0«H*;i .ijjoimA ol^teBl^l .t \:eIIbO ("I 129 Eo CHEMICAL WARFARE EVOLUTION OP ORGANIZATION WITHIN CHEMISTRY DIVISION^ NATIONAL RESEARCH COUNCIL During the First World War no investigations on chemical warfare ^o either offensive or defensive ^ were carried out in Canada^ nor was there any manufacture in Canada of offensive or defensive supplies or equipment o Furthermore^ Canada was one of the signatories of the 1925 Geneva Protocol outlawing gas warfare^ so thatp in the years following the armistice of 1918,, the subject was permitted to become chiefly one of academic interest o About 1934"5o after the Manchurian incident of 1932 and the changes in the German government, it began to appear desirable that some thought be given to chemical warfare and, at the request of the Department of National Defence c, a member of the staff of the Division of Chemistry was author- ized to devote some time to reviewing the technical literat- ure in this field and to keeping informed regarding new de- velopments^ for 5 while there was no thought of Canada build- ing up a military establishment for carrying out this type of warfare, it was definitely in the national interest to give thought to defensive measures against it© In 1937 the Department of National Defence con^ sidered the assembly of respirators in Canada and the manu- facture of at least some of their components© In 1938 the Department of National Defence asked the National Research Council to send a member of its staff to England to inspect the various plants making respirator components and assembling complete respiratorso While in England he also attended a course at the Chemical Defence Experimental Station at Porton. On his return to Canada it was considered that our knowledge was now sufficient to warrant the Canadian manufacture of respirators, importing only a few of the components from the United Kingdom© This work was taken in hand by the Department of National Defence with our staff member acting as consultant,, and a small laboratory was set up in the National R/^aearch Council to test the respirator containers and tie active charcoal used therein* During this time o\ir contacts with the Department of National Defence were becoming more numerous^ and to Improve liaison, an Associate Committee on Container Proofing J.) o.; -'J ,0 ^r.o ^ Ly '.. ^ Ir{T *=>L OCT : 130 and Research was organiaedo Its terms of reference covered only the defence aspect^ and the chief attention was given to the manufacture of respiratorSo The advent of war found the respirator production programme well advanced and the National Research Council with the nucleus of an organizationo The Research Council staff had also gained some experience in 1938 by the preparation of small amounts of mustard gasj, chloracetophenonec, and brombenzyl cyanide ^ for use in summer training of troops at military campSo About April 1940p plans were made to start a reference libraryo This took in charge the small number of British chemical warfare reports which up to that time had been kept in the Council's administrative section and it also received from National Defence a large number of Army specifications^, such as those for paints and chemicals© Efforts to augment this collection were not immediately satis= factory^ for at that time no direct liaison had been estab- lished in London, however^, this condition soon improved© Air Raid Precautions literature was also acquired and indexed© At the start of the war^ offers of assistance poured in from all pacts of Canada - in particular, from the universitieSo As needs became clearer^ it was possible to utilize the services so offeredo In the chemical warfare workp some fifty to sixty projects were initiated in the first two years of the war© Out of this work came valuable assistance on subjects of immediate interest and also a supply of well'-trained scientists^ who subsequently joined the staff of the chemical warfare organizationo After Dunkirk,, the growth of the Chemical Warfare Section of the Division of Chemistry accelerated,, and so did its activities© A number of the staff members went into uniform and were seconded back to the National Research Council to carry on with their work© Many new aspects of chemical defence were consideredi and knowledge of the work was spread by bringing into the Associate Committee representatives of the Army,; of the Navyc, and of the Air Force © A number of staff members were sent to the United Kingdom at various times to become familiar with the work being carried on there^ and to inform workers there of Canadian plans and investigationSo Early in 1941,, the Associate Committee was dis^ solved and the Laboratory staff became the Research Estab° lishment (CoWo) under the Army^s Directorate of Technical Research© This may be considered the formal separation of the chemical warfare group from the organization of the n-e e ■ cilil .8 ^^bV 131 Division of Chemistryo However, some civilian members of the establishment remained on the Research Council payroll for some time^ and other members of the Divisional staff continued to give considerable assistance in the laboratory worko Actually^ the co-operation between the Division of Chemistry and Chemical Warfare Laboratories was so close at all times that for many of the projects it is'^diff icult to say whether they were carried out by the Chemical Warfare Laboratories or by the Division of Chemistryo In the account which follGwSp investigations have been included in the Divisional history for which considerable scientific direction was provided by the staff of the Division of Chemistry - funds and laboratory assistants were frequently provided by the Chemical Warfare Laboratories and there was., of course^ a continual exchange of scientific information between the officers of the Chemical Warfare Laboratories and Research Council staff engaged on related proJectSo After the fall of Prance^, a need arose for a site for large-scale chemical warfare experimentSo since the United Kingdom had previously carried out such work in French Algeriao A Field Experimental Station was eventually e3« tablished at Suffield^, Alberta^ as a joint United Kingdom- Canadian enterprise o By May of 1941,, the staff of the es- tablishment had increased to about twenty^ and very con- siderable growth was in prospect^ in particular^ with respect to the Field Experimental Station at Suffieldo The estab- lishment was then reorganized^ becoming the Chemical Warfare Laboratories of the Directorate of Chemical Warfare and Smokeo Change~over was completed by December 1st of that yearo One member of the Division of Chemistry staff con- tinued to be engaged part time for about two years in check- ing production of asbestos-wool pads and In development of improved oneso Most of this work was done in the plants of the companies producing these pads^ it was a matter of ob- taining the asbestos in a state of subdivision such that it gave the desired filter^ properties when mixed with the woolo The effect of mustard gas on concrete was studied on behalf of the Chemical Warfare Laboratories^ and extensive tests were made of a number of products recommended as linings for concrete mustard gas storage tankSo The Divisional Work- shops made up special pieces of equipment^ as required., and the Divisional Stores supplied the numerous requirements of laboratory apparatus and chemicals not sufficient in quantity or value to warrant special outside purchase o ,^_. -> ^ Jti. .-J ^^3 C\l 1 :.■ ' C7\ I 132 At various times diiring the war^ requests were made for the investigation of carbon monoxide in army work- shops, tank hangar Sp and aircraft ^ and for the determination of carbon monoxide in the blood of men and animals exposed under various conditionso Visits were made to a number of research centres in the United States and reports were pre- pared on developments in carbon monoxide detectors^ instru- mentSp and related problemSo Other projects carried out by the Chemistry Division for the Chemical Warfare Establish- ment are described in the sections followingo While chemical warfare was not resorted to during the war, except in the use of smoke screens^ it is possible that this omission was due wholly to the enemy^s laiowledge that we were well prepared and in a position to retaliateo Since it was not the policy of the United Nations to initiate chemical warfare ;, Canada ^s expenditures on this work were really a very cheap form of insurance « As the record shows <, the Division of Chemistry provided the scientific nucleus from which the Chemical Warfare Laboratories evolved^ sup- plied the laboratory space , obtained equipment andc when the Army finally took over the section^ continued to afford it space^ equipment loans^ and considerable specialized scientific directiono RESPIRATORS In the preceding section it was shown how the Chemical Warfare Laboratories grew from the pre°war plan- ning for respirator productiono At the opening of hos=> tilltiesp a small proofing laboratory was in existence at the National Research Council and mass production problems had been largely solved, in vfliich latter connection the Rubber Laboratory had made a considerable contributiono The outbreak of war in 1939 caused an immediate re-survey of plans, in order to produce in Canada such com- ponents as the active charcoal and filter pads, which it had previously been planned to import from the United Kingdomo The filter pads were first investigatedo These pads, consisting of a mixture of wool and asbestos fibre., are used in respirator containers to prevent the passage of particulate smokes^ which would penetrate a container filled with charcoal onlyo Fortunately^ the Division of Chemistry had been working on both wool and asbestos^ so < ■ > ' T' '. x'l rrivjqflni oj 133 that staff members wore immediately available to start pre- liminary investigationso Within a few days contacts had been made with industrial companies equipped to produce this type of material and in the next few weeks experimental filters were produced at the National Research Laboratories,, while one company prepared to go into productiono Pro= duction began early in 1940 and by the spring of that year a second company was producing experimental ba^tcheSo When v/ork was undertaken to develop an improved wool-asbestos filter, the penetrometer used to test the filtering ef^ flciency of the pads proved to be unsatisfactoryo The Division of Physics was requested to design a more sensitive type and this new instrument became available in the spring of 1940o Active carbon had not been made in Canada prior GO 1939 because there was not enough demand for it to war- rant starting a plant hereo The field had been thoroughly investigated by at least one company and found unattractiveo Once war started, however, interest in producing revivedo IWhile decisions regarding its manufacture rested with the Department of National Defencec, the National Research Council was concerned in a consulting capacity and obtained and tested several brands of American manufacture o Late in 1939, while in the United Kingdom re-= garding medical research. Sir Frederick Banting learned that the authorities there had become alarmed at the possibility of the enemy using arsine gaso In discussing gas defence generally, it was learned that, since about 1938^ several European neutrals had been exploring the possibility of placing orders for respirators in the United States and thaty among other things, they had asked concerning a charcoal which would be effective against arsinOo A copper impreg- nated charcoal, which would be useful for this purpose,^ had been developed in the United States during the First World War and could, it was learned, be obtained through regular commercial channelso A trial lot was ordered at once and a request was sent to Ottawa to place a confirming order o Meanwhile, the laboratory staff in Ottawa had been preparing to run proofing tests against arsine^ in addition to the gases already used in proofingo The copper impregnated charcoal gave excellent results when received and, in general, behaved better and more uniformly than the silver treated charcoalo 134 This work was very timely for a final decision had been made to manufacture charcoal in Canada and the chemists in charge of this work were sent to the National Research Laboratories for preliminary trainingo CARBON MONOXTDS CONTAINER DSVELOPIGNT Protective Container for Carbon Monoxide in Air at High Humidity In order to protect personnel against carbon monoxide in tank landing craft and other situations where a consider- able hazard from this gas exists^, it was considered highly desirable to investigate the minimum requirements of drier and hopcalite ( an efficient oxidation catalyst for carbon monoxide) in a small contained which could be attached to the face piece of an assault respirator and would thus afford good protection under the prevailing atmospheric conditionso Hopcalite is very readily poisoned by water vapour^ which is strongly adsorbedo Therefore^ in order to avoid the use of excessive amounts of catalyst and to maintain the dimensions of the protective container within practical limit Sf, it is necessary to have an efficient drying agent in the aystemo The geometry of a catalytic bed consisting of layers of various drying agents and hopcalite ^ to provide adequate protection against high concentrations of carbon monoxide in air of high relative humidity^, was investigated under air flow conditions sufficient to meet the requirements for the maxi- mum rate of ventilation of the lungs in men at worko The best results were obtained with magnesium per- chlorate as the drying agent o For a container four inches in diameter, a layer of 2o0 inches of magnesium perchlorate with 0o5 inch of hopcalite will provide protection for over thirty minutes against toxic carbon monoxide concentrations., at a flow rate of 64 litres per minute ;, in air at 80% relative humidity© The Oxidation of Carbon Monoxide by Silver Permanganate on Various Metallic Oxide Carriers Although hopcalite 0 a mixture of manganese dioxide and copper oxide i, is used widely in conjunction with various protective drying agents in carbon monoxide respirators and ic 0 f^ciT i. , .1 1 .1 , « ^ ^ ? . 135 detector instruments^ it has many disadvantageso The life of the catalyst is roughly equivalent to the life of the drying agent, as hopcalite is rapidly poisoned "by water vapour o Furthermore^ the heat liberated in the presence of relatively high carbon monoxide concentrations in a respirator container of this type may raise the temperature of the ef= fluent air to the point where some cooling device is neces^ sary to protect the wearero Thus^ at a concentration of 0o35% carbon monoxide^ the heat developed in a small container of the assault respirator type^ during oxidation at a flow rate of 32 litres per minute^ is sufficient to raise the temperature of the effluent air to 75^0^ and at concentra- tions in excess of 0o50^p the temperature may rise to over lOO^Co The activities of a considerable number of prepara- tions were therefore investigated in order to develop a compound which either would serve as a catalyst or would react stoichiometrically with carbon monoxide^, in moist as well as dry air, and which^ when incorporated in a protect-^ ^'■e container^, would afford adequate protection and greater com^ fort to the wearer than present hopcalite containers of stan- dard design© It was found in preliminary studies that^ of the various compounds investigated, silver permanganate showed the highest activity towards carbon monoxide in racist airo The activity increased vihen this compound was distributed on an oxide carrier o Consequently,, a thorough study was made of various metallic oxides as carriers for silver permangan- ate^, with special reference to the following factors in re- lation to activity and useful lifeg-= (a (b (c (d (e (f (g (h (i Carbon Monoxide concentration Height of catalytic bed of material Plow r ate (ioeo space velocity) Moisture content of granules Size of granules Temperature and relative humidity of influent air Induction period Aging at various temperatures Ratio of catalyst to carrier Among the more efficient carriers investigated were diatomite silica, kaolin^ chrysotile asbestos^o and the oxides of copper, zinC; lead^ antimony^, molybdenum, tin, titanium^ iron, cobalt;, zirconium, and ceriumo These silver permanganate preparations may be subdivided according to their carriers into two braod classes as followss- 136 (a) mixtures which require about 8 to 10^ of adsorbed water for optimum active life^ such as those con= taining diatomite silica, kaolin^ or finely ground asbestoSo (b) mixtures #iich are most active when little or no ^ adsorbed water is present in the granuleso The reaction between silver permanganate and carbon monoxide is stoichiometric b^it the velocity of this chemical reaction may be increased greatly by the presence of a carrier^ which, in this respect^, acts catalyticallyo With the proper type of carrier^, relatively high space velocities may be employed with complete oxidation of carbon monoxide to the di oxide .0 until about 80^ of the permanganate has been con- verted to the manganite stageo Thereafter, the efficiency falls off owing to a sintering of the active surfaceo The effective life of the catalyst (breakdown time) is Inversely proportional to the carbon monoxide concentra° tion and space velocity and is directly proportional to the height of catalytic material through ^ich the gas stream is passedo There is an incraaae in active life with decrease in average particle size down to about 0o9 mmo diameter ^ below which there is no further improvement in activity^ Although the optimum range of temperature for longest life would appear to lie between 24° and 40*^00 . the catalyst is still active enough at 0°Co for respirator requirementSo Special attention has been directed towards those metallic oxide preparations which showed sufficient stability^ after prolonged aging at elevated temperatures,, to warrant consideration for practical purposes such as use in respirator containerso Many catalysts )fl^ich showed a high initial ac° tivity towards carbon monoxide, when freshly prepared^ were eliminated from further consideration because of a slow de- composition reaction,, resulting in the liberation of oxygen^, the rate of )«diich increased at higher temperatureso In this category may be placed those catalysts containing the oxides of aluminium, silicon,, titanium,, cadmium^ cerium^, vanadium^ nickel, and manganese o The most efficient catalyst discovered thus far is one containing 69 mole percent zinc oxide and 31 percent silver permanganate, dried to less than 0c5% adsorbed watero After prolonged aging at 60*^00 this catalyst showed a life corresponding to several hours for efficient removal of 0o5^ carbon monoxide in moist air under standard test conditions 'ir. 137 -^ in the assault respirator containero This performance is considerably better than that shown by equivalent hopcalite containerso The investigation is being continuedo • The work was then transferred to the Chemical War- fare Pilot Plant to prepare this zinc oxide catalyst on a pilot plant scale and to fill a considerable number of re- spirator containers for physiological and service testSo TOXIC SUBSTANCES Oxido-biS'^/j'^chlorodiethyl sulphide The first problem on toxic substances which was undertaken by the Organic Laboratory at the request of the Chemical Warfare Laboratories consisted in the preparation of oxide-biS"/^ ^chlorodiethylsulphideo This substance is a by°product which accompanies mustard gas prepared by the action of hydrogen chloride on thiodiglycolo It is also a vesicant and a better knowledge of its properties was desir- able. Although it is relatively easy to separate the mustard gas from the reaction mixture^ it is extremely difficult to purify the oxi do => compound which is the main by-product o Several attempts were made,., therefore,; to synthesize the substance by other methods ^ but all of these proved fruitless 5 since the main phase of the study had for its object the preparation of the disulphone of oxido<-bis°/f -chlorodiethyl° sulphide p a direct synthesis of this compound was attempted from mustard sulphone but no success had been achieved when a more pressing problem caused the work to be abandonedo Nitrogen Mustards It was known that before the collapse of their country the French chemists had devoted considerable effort to the study of tri -(/^ -chlor ethyl) -amine and its vesicant propertieSo The French were also known to have had the large stores of this vesicant,, which was commonly called "French mustard'% and the Germans were in possession of these store So It also became known that the Germans were manu- facturing large quantities of a nitrogen mustard which was apparently not French mustardo This was suspected to be bis- (/? "ChlorethyD-methylamine and chemists in England^ the United States.,; and Canada immediately turned their attention to this substance o Part of this work was done in the National Research LaboratorieSo Bis-(/f -chlorethyl) -^methylamine can be prepared in the laboratory by the action of ethylene oxide O J' J LJ Ton 138 on methylamine and subsequent chlorination of the producto It has to be handled with extreme care because of its action on the skin and on the eyeso Several kilos were prepared in the Laboratory to supply various workers at the Research Council, and at Canadian universities^ who had volunteered to study the substance o Only one mishap occurred during this work and it^ fortunately^ was without serious resultSo Its rate of hydrolysis in water,, its rate of reaction with itself^ and its chemical properties were studiedo Means were sought to stabilize it^ for at room temperature it re- acts with itself to form an innocuous compoundo The search for substances capable of reducing the r ate at which the ni- trogen mustard decomposed was only partially successfulo It was eventually abandoned because of the discovery that a homologue of this nitrogen mustard^, which was just as toxiCp was itself sufficiently stable torender the use of stabil° Izers unnecessaryo Various compounds partially similar in structure to the two nitrogen mustards referred to above were synthesized in the Laboratory and submitted to the Physiological Section of the Chemical Warfare Laboratories for toxicological assayo For instance, such substances as the following were prepared in the Laboratoryj- lo Ethyl N-/^ -dichloroethyl carbamate 2o /^-dichloroethyl'-nitroso -amine 3o /? -chlorethyl N"/3-chloroethyl=N=nitroso carbamate A short investigation into the preparation and properties of .tri-(/? -chlorethyl)»amine, the so-^called French mustard^, was also carried outo An extremely toxic gas was discovered in the United States by Dro Kharasch but^ unf ortunately^, this gas decomposed so readily on standing that it could not be stored with safetyo However, the intermediate compound obtained just before the final step in the synthesis is quite stable„ Several attempts were, therefore, made in this Laboratory to design a means whereby the last step in the synthesiSo which is a nitro- sation reaction, could be carried out in the shell just before usee The nitrosation reagents are so toxic to mice that it was not possible to observe the extent of the reaction nor its rate ,9 because the animals died as readily from exposure to the vapor of the reagent used as they did after exposure to the gaso 139 VENTILATION AND ANTI-^-GAS PROTECTION IN ARMOURED TANKS Carbon Monoxide and Gun Fumes At the request of the Directorate of Chemical War- fare,, an investigation was undertaken in December 1941 at Camp Borden on the carbon monoxide content of the atmosphere in various types of armoured tanks under general operating conditions and of carbon monoxide ^ nitrous o and ammonia fumes^ generated daring the firing of the guns under battle condltionSo The concentration of these gases at the breath- ing level of the personnel in the tank during firing of the Besa^, Browning^ two'-pounder^ and six-pounder guns was studied under various rates of fire in order to evaluate the potential hazard to human life from this source o Whenever <, it was de- monstrated that; in the type of tank under examination,, the gas conditions with the existing ventilation were dangerous at the maximum rate of fire likely to prevail in battle^ an auxiliary ventilating system was installed and its effective^ ness testedo Under normal operating conditions., without the firing of the guns^ the carbon monoxide concentrations attained from seepage of exhaust fumes in the various types of tanks^ travel' ling alone or in convoy^ were generally below 100 parts per million and did not constitute a danger to human healtho The concentration of gases discharged inside a tank during the firing of the armament depends upon the calibre and type of gun.o rate and direction of air movement in the vicinity^, rate of fire^ and total number of rounds of am- munition expendedo Higher carbon monoxide concentrations were found during the firing of the Besa machine gun (7o92 mmo ) than during that of the Browning gun (0o30 ino ) under similar conditionso If the ventilation rate inside the turret is appreciable i, the gas concentration tends to drop quite rapidly in the reloading intervals betv/een firings but under other conditions dangerous amounts of carbon monoxide may accumulate© Under similar weather and other operating con- ditions j, the carbon monoxide hazard was found to be apprec- iably greater in the Ram I tank than in the Valentine VII for equivalent firing rates o Thus,, in firing six rounds of two-pounder (AoPo Shotp Cordite) and 750 rounds of Browning accumition (SoAo Ball 30 06) in ten minutes there was re- corded an average carbon monoxide concentration of 0o85^ and a maximiim of 0ol02^ in the Ram I tank compared with 0o017% and Oo 023^0 respectively, in the Valentine VI lo he, en 7 ;>c ens ^ » .- r 'V c. r^f J- snoi »fi.j ^bi^r j.aj uej o r *- o ' T f- f ;10':* ei / Xx -•61 ?. ; ifpg -A ^) 140 As the above and other data indicated that the Ram I tank was inadequately ventilated^ a modified ventilating system was installedo This system resulted in a considerable improvement in carbon monoxide conditions, but it was deemed advisable^ for adequate removal of fumeSp'to provide ventila- tion at a rate of at least 200 cuofto per minute in the main turreto It was found that the nitrous fumes released during the firing of the guns were not in sufficiently high concen- tration to constitute a hazard to the health of the crewo Further tests disclosed that the ventilation system of the Ram II tank was also inadequate to reduce the fumes to a safe level during the firing of the armament^, including the six-pounder gun^ from a stationary positiono The carbon monoxide concentrations exceeded the danger limit of 0o05^ in all tests and frequently rose to values above OolO^o Re- commendations to correct these conditions were madeo Anti°gas Protection of Personnel The object of this work was to develop a method of either collective or individual protection for the crew members of tanks against gun fumes or outside gas attacks o The investigation was carried out mainly along the following lines J (a) the development of a gas filtering unit with in- dividual ducts leading to oeach crew member 5 (b) the degree of protection afforded by air at various flow rates delivered at a slight positive pressure to a loose-fitting transparent plastic mask covering a portion of the operator's faceo Ex= perimentfe were carried out in a gas chamber v/ith various chloroacetophenone vapour and lethal concentrations of sulphur dioxideo With a volume of 3 to 4 cucfto of filtered air per minute for each operator., complete protection was afforded by drafts of air from various types of orificeSc, without the use of a mask^was also investigatedo It was found that the effective zone of protection in this case was extremely limited.,, even at flow rates as high as 20 cucfto per minute for each operatoro Further studies of gun fumes and anti=gas protec=^ tlon were carried out at the Chemical Warfare Field Experi- mental Stationp Suffield. Albertao The project consisted not only of chemical tests to determine the concentration of gases released under various operating conditions but also of clinical and physiological tests to determine the effect of the gases upon the tank personnels The results indicated that dangerously high concentrations of carbon monoxide and ammonia were released during the firing of the armament of the Ram II tank and the average carbon monoxide content of 141 the main turret could not be reduced to the safe level of less than 0o05^ by volume without the use of an auxiliary exhaust fan ventilation systemo In the absence of forced ventilationp rapid and prolonged firing of the six-pounder gun impaired the health and efficiency of the crew by causing a marked increase in the carbonmonoxyhaemoglobin content of the blood and by other physiological effects© Complete protection was afforded against both gun fumes and non-persistent gas attack by use of an "anti^-gas protective unit"p which supplies four cuofto of filtered air per minute to each crev? member o COMBUSTION PRODUCTS OP FLAME-THROWERS In connection with the physiological effects of flame-thrower attack on animals in various types of bunkers (as reported by the Experimental Station, Suffieldg Alberta) ,, it was considered important to study the combustion pro= ducts of various types or compounds having widely different Ignition temperatures,, since the fuel ignition temperature for long range f lame ° throwers appears to have some bearing on the ability to maintain a burning rod in lengths of about 150 yards or more© A measured quantity of the charge was injected under pressure into a specially constructed combustion chamber of about eight cUofto capacity and the mixture ignited si- multaneously by a small hydrogen flameo Gas samples were collected at definite time intervals and the concentrations of carbon monoxide,,, carbon dioxide o and oxygen in the com- bustion products were determinedo The combustion of acetone, methyl ethyl ketone ^ dioxane, phenetole^ and ethyl formate was found to yield considerably higher percentages of carbon monoxide than the combustion of gasoline ^ the standard flame-thrower fuel^, under similar conditionso The addition of iron pentacarbonyl to gasoline also resulted in an increase in the carbon mon- oxide content of the combustion productSo As there is a correlation between the carbon monoxide formed and the fuel Ignition temperature i, it was suggested that liquid fuels having a high ignition temperature be substituted for gas- oline in flame-thrower testSo 160^ .(■noo em r Id. ed i> ■. A b ^/B e Jxj< 142 ANALYSIS OP AIR FOR TOXIC PmiES The Estimation of Low Concentrations of Nitric Oxide and Nitrogen Dioxide The accurate determination of low concentrations of "nitrous fumes" in air is of importance in gun fume problems^ testing of respiratorSp physiological experiments on toxicity, and in many other fieldSo As little as 40 parts per million by volume may be decidedly toxic to human beingSo As it has been well established that the oxidation of nitric oxide in air or oxygen follows a termolecular law^ and as it can be assumed that in very dilute gaseous mixtures all the nitric oxide molecules which have undergone oxidation are in the disocciated form of nitrogen dioxidep the problem resolved itself into finding a method fo'r determining the relative proportions of nitric oxide and nitrogen dioxide in an air streamo The methods finally adopted were the determination of total oxides (nitric oxide plus nitrogen dioxide) and of nitrogen dioxide simultaneouslyo The gas sample for total oxides was collected at a measured flow rate by a water dis-- placement method and the oxides in both the gas and water phases were converted to nitrate with acid hydrogen peroxide solutiono The nitrate was then reacted with phenol disul= phonic acid and estimated quantitatively in a photoelectric colorimetero The nitrogen dioxide was determined by passage of the gas sample at a measured flov/ rate through an absorp- tion train of high efficiency^ containing 10% potassium iodide dolutiono The iodine liberated In this reaction was estimated by titration with standard sodium thiosulphate^ 0o002 N. using starch indicatoro As a test of these methods^ a study was made of the rate of oxidation of nitric oxide in an air stream in the con° centration range of about 0o75% to less than OolO% by volume o The values for the absolute reaction velocity constant Ky calculated on the basis of a third order reaction^, were found to be in good agreemen-c with those reported in the literature© Rapid Determination of Low Concentrations of Ammonia in Air Field trials of the Light Type respirator with a new model container disclosed that ammonia could be detected in the inspired air and in a number of cases the concentra- tion of ammonia proved high enough to be objectionable to 143 personnelo This seemed to be true particularly of charcoal respirators in which the nitrogen content of the charcoal was relatively higho As the problem involved the testing of a consider- able number of charcoal containers to determine the effect of various treatments in eliminating this objectionable feature in the charcoal^ a rapid and accurate method capable of detecting as little as one milligram of ammonia per cubic metre of air was desirable o After some unsuccessful trials with potentiometric methods, a suitable and rapid procedure was evolved by measuring the change in conductivity of a definite volume of O0OOI6 N sulphuric acid solution^ maintained at con- stant temperature, in an absorber containing a sintered glass disc of fine porosityo A measured volume of air from the charcoal under examination was passed through this solu- tion and the change in conductivity was determined by a Wheatstone bridge galvanometer, using platinized plat:Inum electrodes having a knovm cell constanto Tests on the char- coal in these special Light Type containers showed ammonia concentrations as high as 25 to 35 milligrams per cubic meter in the effluent air under high humidity conditiotiSo Treatment of the charcoal with water followed by heating in a stream of air at 170-180°Co was found to be effective in removing nearly all of the volatile ammoniac MINIATUliS INC3NDIARY BOMBS -' This investigation was initiated to determine the feasibility of a proposal submitted to the Inventions Board of Canada for the production of small incendiary bombs which would Ignite by gentle percussion or shock when sensitizedo In view of the fact that millions of these pellets could be broadcast by plane over enemy territory^ numerous small fires would result and would devastate effectively the forests and agricultural cropSo The idea seemed to be a distinct improve- ment on the incendiary leaflets used early in the war and.o for the purpose in hand^, considerably better than large thermite or magnesium bombSo Although an effective miniature bomb was developed quite rapidly, its use against the enemy was rejected, at first, on humanitarian groundSo Later., however^, after field trials at the Experimental Station. Suffield^, Alberta, a modified version of this pellet was adopted© ©J! 144 The bombs consisted of small nitrocellulose plastic rodSp spheres,, and cubes^ coated with a red phosphorus emulsion in acetone, and sensitized by an immersion method in a mixture of sodium chlorate., ace tone p and water© Ex= tensive tests were carried out to determine the best means of coating the nitrocellulose plastic in order to obtain pellets which would ignite readily when thrown on surfaces such as grass and soil and yet which would not be too dangerous to handle o Various concentration factors were studied in order to evaluate the limits of sensitivity and the question of rapid drying while falling through the airo In the method of preparation finally adopted^, the pellets,, although safe to handle in the moist conditionp become sensitive in less than one minute ^Nh.en falling through the air or when dried in an air streamo The bombs then ignite even when thrown into a bed of soil from a height of only five feeto One million of these.,, in the form of cylinders 1/4 inch in diameter and 1/4 inch in length., weigh about 650 pounds and cost about $450 to $500 to manufacture o ANTI-GAS FABRICS AND CLOTHING' In September 1939p the Department of National Defence asked the Textile Laboratory of the Division of Chemistry to co-operate m work on ant i- gas protective clothingo There wa3.9 therefore, a very close association between the Textile Laboratory and the Chemical Warfare Laboratories all through the war«v'^ Good facilities for the examination of textiles were available in the laboratories of the National Research Council but it was necessary to extend these greatly tot ake care of the traried types of work required in connection with pro= tective clothingo It was necessary^ firsts, to provide ad° ditional equipment for laboratory studies of permeable and impermeable protective clothingo It was later necessary to organize and supervise pilot plant and full-scale plant in^- vestlgations^, chiefly in the field of permeable clothingo A considerable amount of co-operative work was carried on with outside firms in the field of impermeable clothingo The term "impermeable" is here used to designate fabrics carrying a continuous coating of some vesicant=resistant material | such fabrics were used in the manufacture of anti-gas capeSp boot So etCo The term "permeable" is used to designate fabrics impregnated with some chemical substance whichp by reacting chemically with vesicants^ prevents their passage through the fabrics such fabrics retain their porosity to air^ whereas 145 the impermeable type do noto It was finally decided by the Chemical Warfare Laboratories that a small pilot plant for processing fabrics and garments should be set up 5 the Textile Laboratory was responsible for designing and equipping the plantp and also for its operation in the early stageSo Later the plant was turned over to the Development Section of the Chemical War- fare Laboratorieso The Textile Laboratory has carried out investiga-= tions and tests on many types of equipment o These include? battle dress serge j; protective wrapping material 5 butyl coated fabrics^ neoprenei capes^ glovesj webbingj adhesive tape I decontamination mitts 5 anti-gas suits 5 eyeshieldsj rayon fabric for ground sheets^ anti°dimming cloth^ mois- tureproof cellophane; oilskin jackets; stockinettes; anti» gas respirator fabric; parchment paper; elastic webbing 5 rubber sponge; fearnought flannel; detector gas sleeves; helmet curtains; leather samples; pliofilm; aprons; suits^ including trou3er3<, jackets and hoods; naval coats; zippers for anti-gas valises; haversack duck; capes; and bags for contaminated clothingo Work on Impermeable Type Fabrics Methods for Measuring Penetration Timess The method first used for measuring penetration times of liquid mustard and Lewisite was that developed by the Chemical Defence Experimental Station^, Porton, Englandc, involving the use' of a metal diffusion cup and using a dilute solu- tion of potassium permanganate as indicator o This method was found to be unsatisfactoryo The indicator gave incon- sistent results and was replaced by a solution of alizarin red adjusted to a pH of 60 lo The brass cups used in the Porton method were replaced by flanged glass cups mounted in batteries of twelve in a thermostatically controlled water bath,, all connections on the off side of the cups being glass to glasso This method was similar to that finally adopted by the United States Chemical Warfare Serviceo Penetration Time Limits; The problem of setting up permissible penetration time limits for impermeable type fabrics was a difficult one^ since it involved an attempt to correlate laboratory penetration t imes with those which would be expected to cause injury under field conditionso It was therefore necessary to work in close co-operation 146 with the Physiological Section of the Chemical Warfare Laboratories in order to choose probable safe laboratory penetration times for the various types of impermeable fabrics used in the manufacture of anti=gas capeso " CO"Operation with Canadian Manufacturers of Anti-gas Fabrics g When the manufacture of anti-gas fabrics was begun in Canada in 1940^ the manufacturers possessed little or no experience in this fieldo This difficulty was complicated by the fact that high initial production was requiredo The Council co-operated with four firms but only one of these appeared to possess the necessary knowledge and technical control to produce a satisfactory range of anti-gas fabrics, A fair amount of this type of fabric was processed by a second firm but great difficulty was encountered owing to their lack of proper technical controlo Co-operation with these firms involved the carrying out of hundreds of tests on experimental production runs^ together with numerous con° sultations and plant visitSo One troublesome property of oll^dressed fabrics was their tendency to undergo spon-^ taneous combustion where the aging of the polymerized oil coating was incomplete© Two plant fires from this cause were investigated and recommendations were made to prevent their re^-occurrenceo The Textile Laboratory was requested by the In° spection Board to undertake the setting up of an adequate system of inspection for these manufactured fabrics and to perform all the necessary testingo In the course of this work thef Laboratory issued approximately 2500 routine in- spection reports covering the manufacture of sixteen million yards of anti-gas fabrico Investigation of other types of Impermeable Fabrics Considerable work was carried out on the investigation of other types of impermeable fabrics n namely^ those having various types of synthetic resin and synthetic rubber coatingSo The Inability of the oi^^-dressed coatings to withstand low temperatures made it desirable to investigate coatings which would remain flexible at temperatures of 0*Fp and lower o In thi-? connection the outstanding properties of butyl rubber^ both with regard to flexibility of low temperatures and to high protection against mustard gas and Lewisite, were early recognisedo Unfortunate ly^, adequate supplies of butyl rubber became available only at the end of the production of anti= gas fabrics in Canada^ but there is little doubt that any future production would make use of butyl rubber o 147 Work on Permeable Type Fabrics Laboratory Investigations^ The various methods for measuring penetration times of permeable fabrics, as developed at Porton, were tried out and it was finally agreed to adopt the standard Congo red penetration method at 30°Co The lab- oratory facilities v/ere therefore extended to carry out -ohese tests on a large scaleo Owing to the fact that the impregnants used are use- ful by virtue of their content of active chlorine ^ it was obvious that there was a danger of damage occurring^ espec-^ ially in the case of cotton fabrics. A considerable amount of work was therefore carried out on the effects of various impregnants on wool and cotton under conditions of acceler- ated agingo At 65% relative humidity impregnated cotton cloth showed high rates of loss of impregnant and of breaking strength after twelve weeks ^ storage i, whilst in the case of wool the loss was considerably lessc An investigation was also imdertaken of the effect of other types of Impregnating chemicals, with particular reference to their stability and to probable damage to the fabriCo Included in this investigation was the effect of different types of dyes and cloth finishes j In general^ sulphur dyes had an adverse effect on the stability of the impregnantSc Associated with this oroblem was the effect of washing and dry cleaning on impregnated garments 5 experi- ments were conducted to determine whether or not they could be cleaned without reducing the impregnant content below a satisfactory levelo Work on the laundering of one type of impregnant treated cotton fabrics v/as extended to include laundering with various types of detergents. Including soap, soap plus alkali , and sulphated fatty alcohol. T^^'=! ro suits indicated that the sulphated fatty alcohol c au3ed_less reduction in mustard penetration time than was the case with soapo The use of soap plus alkali appeared to offer little advantage o Development of Plant Impregnating Processes t (a ) Solvent Suspension Process: Work on impregnation was com- menced on a laboratory scale in 1941o In 1942 substantial contract demands were raised by the Department of Munitions and Supply for impregnated battle dress for use by the Canadian Army overseaso The laboratory operations were therefore extended to pilot plant scale and one thousand 148 suits of Army battle dress and a thousand pair of socks were impregnatedo The finished garments v/ere tested and found quite satisfactoryo Some of the factors which influence the degree of impregnation v/ere investigated. The speed of centrifuging^. the concentration of the impregnating solution, and the type of material had the greatest effect o The duration of centrifuging had little influence o The omission of the centrifuging process^ together v/ith a suitable r eduction in the concentration of the impregnating solution^ gave a uni- forme readily-controlled prcducto It was found that the degree of impregnation can be calculated from the increase in weight of the treated material with an accuracy sufficient to serve as a processing ehecko Pull commercial production was then con-anenced in the dry cleaning plants of Langleys Ltdr ^ Toronto^ and Vails Ltdo J, Ottawao Some 400^000 suits of battle dress were pro-- cessed throughout the duration of these contracts. Reports have been issued giving details of layout and operations at these plant So It was found that pinned-on pieces offered a satisfactory method of sampling the product for inspection* (b) Solvent Processes s-» Investigations were also made of trichlorethylene. perchlorethylene^ tetrachloroethane and pentachloroethane with regard to their possible use as solvents in the impregnation processo Tetrachloroethane appeared to be the most suitable solvent investigated* The Laboratory also looked into the effect of steam pressing on the impr6gnant content of the treated materials^ and into the effect of increased chlorinated hydrocarbon content on the properties of impregnated materlalo (c) Aqueous Processes s~ During 1942 and 1943 the trend in anti-'gas Impregnation of clothing was in the dir- ection of aqueous processes rather than processes involving solvont solutions or solvent suspensions of the impregnants. Work on aqueous processes was begun at the fabric processing pilot plant late in 1943 « Owing to the unexpected deterior- ation of a batch of brown --sulphur -dyed drill impregnated by the British aqueous process,, a study was made of the causes of tenderingo This was found to be due to the effect of the Impregnant on the sulphur dye in the fabric o 149 Storage and Wearing Tt*ial»sg Representative samples of "battle dress treated with one type of impregnant were examined after six and twelve months^ storage for appearancd^ impregnant content^ and chemical damage to the cotton sewing threado The garments were found to be quite satisfactoryo Samples of impregnated battle dress were subjected to wearing trials and garments were withdrawn for examination at intervals of one^ two three. o and four months o There was a gradual loss of protective value caused by mechanical re- moval of impregnant); higher chlorinated -'paraffin content tended to reduce this losso Miscellaneous Investigations on Impregnated Clothing g Samples of four fabrics, exposed to the vapour of methyl- dlchlorosillcane for thirty minute So attained varying degrees of water repellancy,, depending on the type of fabriCo Light- weight cotton materials having a fine weave... such as mer° cerized cotton or tarantule,, gave the best results,; followed closely by wool serge c The results with cotton denim were decidedly inferioro Laundering destroyed much of the water repellent quality of wool serge and of cotton denim but did not appear to affect mercerized cotton or tarantule o Sllicane treatment followed by impregnation is applicable only to wool serge material and even here it is doubtful if the slli- cane is of any value o Battle dress serge impregnated with charcoal was tested for mustard and Lewisite vapour penetration times and for the effect of laundering and dry cleaning upon the subsequeht penetration tlmeo It was found that a negligible amount of carbon was removed by the aqueous detergent solu° tlonso A much smaller amount of carbon was removed by Stod- dard solvent than by trichlorethylene or perchlorethylene^, but the cloth retained its original vapour resistance best in the case of cleaning with trichlorethylenOo Velanized battle dress serge. Impregnated by two different processes, showed a slightly greater overall pro- tective value against mustard vapour as compared to the non-- velanized Impregnated fabriCo The water repellancy of velanized battle dress serge was slightly reduced by impreg- nation, somewhat more so than in the case of non-velanlzed serge. The results of accelerated aging test Indicated that the stability of the impregnants was somewhat greater in the case of the velanized sergeo 150 PROTECTIVE COATINGS A number of investigations in connection with chemical warfare were carried out by the Protective Coatings Laboratory of the Division of Chemistryg Gas Detection In the month of October^ 1939 o an urgent request was received from the Royal Canadian Navy for the prepara- tion of a pilot batch of gas detector paint for immediate use on HoMoCo shipSo A specification for this material was obtained and arrangements were made with a local paint company to manufacture the varnish vehicleo As soon as the materials were received,, they were processed on the labora- tory paint mills, mixed according to the specification with the active agent and solvents, packaged in one-quarter pint •cans, and labelled^ This is believed to be the first batch of gas detector paint manufactured in Canadao Development work in connection with detector paint was then continued in co -operation with the Chemical V/arfare Laboratories, and specifications were prepared covering detector paint in various colours and compositionso Another of the early projects was the development and testing of detector powders for application to uniforms and other fabricSo Their use was later discontinued but not before satisfactory formulae had been developed and com« mercial ^production had commencedo A brief study was conducted to determine the dele-" terious actionj, if any^, of chromium compounds in detector paint So The Laboratory assisted in the development of a suitable detector paint for application to detachable paper *'sleeves" and a highly satisfactory product was put into pro= duct ion by the Canada Paint Company as the result of the combined effort r Some 30;, 000 gallons of this particular paint were manufactured and millions of the sleeve protec- tors v;ere made up by contractors and distributed to the Armed Porceso In connection with the contracts for thi item^ the Laboratory assisted further by conducting approval tests on many batches of the paint and by investigating occasional difficulties which arose from time to timeo Approval tests were also carried out on the active ingredient for incor- poration into the painto Colour standards were prepared for both the yellow and khaki types of painto 151 It is essential that detector paint contain no tur= pentine or aromatic solventSo The Laboratory developed test procedures for detecting the presence of small amounts of such liquidSo Early in 1943. the use of detector paint on steel plates was begun, and the Laboratory co^-operated in preparing the specification for the priming paints the detector paint, and the method of applicationo Chemicals and Smokes Assistance was given to the Royal Canadian Navy in the procurement and inspection of the special paint remover required for the removal of paint from ships in case of poison gas contaminationo Instructions for its use^, in-" eluding the necessary precautions , were supplied to Naval Service o Inspection tests were also made of ^many samples of various chemicals and compositions for smokes Including zinc oxide p aluminum powder n and calcium silicideo Interior Coating for Gas Shells The interior of gas shells must be coated to prevent interaction between the metal and the cheraicalo This is highly important from the standpoint of safetyu Manufacture of an enamel for this purpose was commenced by a Canadian paint company in 1943^ following instructions supplied from Great Britaino The Protective Coatings Laboratory was as- signed thi6 duty of carrying out the rigid inspection tests and found that serious problems were occurring in its manu- facture,, Responsibility for correcting these difficulties was then assumed by the Inspection Boardo A similar project had been undertaken previously^, namely- production of a lining for storage tanks for war gaseso A promising material for this purpose was developed in conjunction with one of the leading resin manufacturers and samples were submitted to the Chemical Warfare Labora- torieso It was founds however^, that rather than run the risk of Imperfection in the coating, due to improper applic™ ationv it was preferable to use chemically resistant con- tainers which required no coating© t^^t r . -■ .'. .ioXr.\ 152 .APraroix MISCELLANEOUS PAPERS °^"\°?i o;. jr«ly«*hylene Glycol Et>,« ana Octadecvl at^^u .^-^J^oi. litners of Po4-,^t „ Jan, 13, l9°Ji\^^=°'>°l^» N.R.C„ Report ^Nof'cgfl^l^l^^ Uos/patf^'^Ssrior^r"?^ «"<^ ''^'hods of Por», , ;>304, 109, July iQ^ j^g^^ 'J" 01 j-ormlng Same„ fJraen, P„o„ Wartime r« = Of Chemistry ^a^fr""?^ Activities of the D, . . ^blication^No. ''?^2%°r' '^^^^^=^ °o-oil N^^R^Jc^f °" Hopkins c Y A J Hopkins, CcYo JJtm *.. jy/vxns, CoYo and Licrht- a ,, No: lSll°"?^,r "°*-"^-l''938!4T''!j^H* Substitutes ^"«l: (Mimeographed), " ^^ """^C' Publication Hopkins ^.Y„ ^„^"'* OaUagher G„ a Pur.f„ can, J, Hes. B19*'li|!SlT &'??!^^ °^ ^^"^^'- Marion L tvi d H-" m. ^'^"'l^^^'^^nU Distyrene. c.n. j. Marion L Th T ^' can, '/Re°3"*iS,°y^l%^r?l^I.T2i^^^^.HX^ 155 Marlon, L„ and Aahford w a n Potaaslum Alooholatea in thl t^Pl^^^tion of the Use of Indoles, can. j, Hel/^^%|^*^«3l3 oi> Substlt^Lf Marion, L„ and MoRae T . . Michael t w n »# , Puddlngton, IE am*- " ^^' ^^^^^ Stopcook'oreaaea T ?" *J?® Preparation of mo-v, rn Puddin^ton X K Tt '°" ^" ^^O^f^^S^--^-^ m=ro3co;e"Hot"1:as°e"/ L^r"^r^R\\^-^3^| \°p%-°^^^'^ Puddington„ I E ^. ^' ^^'^^^ ^^944), Puddlngton, I E ^1 , — " ^^^"^^^ fl944)„ Puddlngton i e ah otodman D F t t — v-Li^*o;o Tapp, J,s Th« r . ' ^°° 2°' 1943,