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Mechanical Engineering, Seichi Konzo, M.S., University of Illinois Topographic Mapping in Cooperation with the United States Geological Survey. This report is a contribution of the Analytical Chemistry Division.

February 15, 1948

Digitized by the Internet Archive

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http://archive.org/details/chemicalcharacte132rees

CHEMICAL CHARACTERISTICS OF BANDED INGREDIENTS

OF COAL

O. W. Rees, W. F. Wagner, and W. G. Tilbury

Abstract

Data are presented on certain fundamental chemical characteristics for four sets of banded ingredients and whole coals from Illinois representing three ranks — high volatile bituminous A, B, and C. Evidence is shown of variation by rank of the banded ingredients, vitrain, clarain, and durain. Evidence of variations by rank of fusains is more erratic. Comparison of characteristics of Hsiao fusains with those of hand-picked fusains indicates that the hand-picked samples contain rather large proportions of more reactive materials. Variations in reported analyses of banded ingredients appear to be due partially to the influence of varying rank, but also to variations in the selection of samples.

IN THE work on Illinois coals in this laboratory, considerable attention has been given to studies of the physical and chemical characteristics of the banded in- gredients, vitrain, clarain, durain, and fu- sain. The Stopes classification (15) of banded ingredients is based on macrovisual appearance. It is of interest, therefore, to compare these visually selected ingredients to learn whether each shows more or less specific chemical characteristics. It is also of interest to learn whether each ingredient, secured from coals of different ranks, varies in chemical characteristics as do the source whole coals.

Published analyses for the banded ingredi- ents show wide differences in chemical composition for each ingredient. Probably the composition of each ingredient, at least of vitrain, clarain, and durain, is influenced by the degree of metamorphosis undergone; but how far this may account for reported differences and how much may be due to variation in the selection of ingredients, source plant materials, etc., is a question. Recently Lowry (6), in summarizing chem- ical information on the banded ingredients, showed clearly the wide differences in re- ported analyses for each ingredient. Mar- shall (7) attempted to correlate analyses of anthraxylon with type and rank variation in coal seams. Fisher et al. (3) studied hydro- genation characteristics of the ingredients. Sprunk (13) summarized the influence of physical constitution of coal upon its chemi-

cal properties. Many other investigators have contributed information on various phases of this problem, but space does not permit a complete summary.

This report presents the results of studies of certain chemical characteristics on four sets of banded ingredients from the three ranks of coal — high volatile bituminous A, B, and C — represented in Illinois. The work represents an effort to obtain infor- mation on variations of chemical character- istics of ingredients as related to rank of source coals, and in addition to secure in- formation on differences due to variability in visual selection, particularly of the fu- sains.

Tests on Coal Samples

Four sets of samples, including whole coals and banded ingredients from Gallatin, Franklin, Macoupin, and Henry counties were studied. These represent coals of high volatile bituminous ranks A, B, C, and C, respectively. The whole coals were channel samples, cut down, crushed to pass a 4-mesh sieve, and sealed in sample cans in the mines. The banded ingredient samples were hand- picked in the mines, the selection being made macroscopically. These samples were crushed to pass a 4-mesh sieve and were sealed in sample cans in the mines. In the laboratory, samples were air-dried, crushed to -20 mesh size in a Braun type 6CP pul- verizer, and further pulverized to smaller sizes in a ball mill.

[5]

BANDED INGREDIENTS OF COAL

Several tests were used to compare chem- ical characteristics of the banded ingredi- ents. Proximate analysis, calorific value, and total sulfur were determined on -60 mesh samples according to standard A.S. T.M. procedures (1). Reactivity index was determined by the C.R.L. reactivity test (11, 12). Determinations were made on -40 +60 mesh samples in both oxygen and air, and results were indicated as T15 and T75, respectively. Free swelling index tests were made on —60 mesh samples ac- cording to a tentative A.S. T.M. method (2). Moisture characteristics were deter- mined by the equilibration method described by Stansfield and Gilbart (14) and later used in this laboratory (10).

Further studies were made on the hand- picked fusains. Fusain determinations were made on these samples by the Hsiao method (■/). The inert portions (Hsiao fusains) remaining after nitric acid oxidation of the hand-picked fusains were studied for re- activities by the C. R. L. method, and mois- ture characteristics were studied by the equilibration method. Proximate and ulti- mate analyses were made according to A.S. T.M. standard methods.

Analyses

Proximate analyses, total sulfur, and cal- orific values for whole coals and hand-picked ingredients are summarized in table 1. In general, analytical values for the vitrains, clarains, and durains vary in the same way as do those for the corresponding whole coals. Moisture and calorific values are of particular interest in considering variations due to rank. As-received moisture values for vitrain, clarain, and durain increase with decrease in rank, as do those for the whole coals. Moisture values for the fusains show an exception in regular increase with de- crease of rank of the corresponding source coals; that for the Franklin County fusain is higher than that of the fusain from the lower rank Macoupin County coal. Fusain moisture values are distinctly higher than those for other ingredients.

Calorific values on the moist mineral- matter-free basis, for all ingredients, de-

crease with decrease in rank of the source whole coals. In general, calorific values on the dry mineral-matter-free basis for vitrain, clarain, and durain show this same trend, although values for vitrain and clarain from Henry County are higher than those for the same ingredients from Macoupin County. This is also true for the corre- sponding whole coals. Fusain from the Franklin County rank B coal showed the highest calorific value on the dry mineral- matter-free basis. With the exception of the fusain from the Gallatin County rank A coal, calorific values (dry mineral-matter- free) for fusains are higher than for other banded ingredients and whole coals. This is in accord with the findings of Parr, Hop- kins, and Mitchell (8) in a study of Illi- nois fusains. However, the work reported by these authors covered fusains from high volatile bituminous B and C coals but not for fusain from high volatile bituminous A.

Reactivity and Free Swelling Indices

Table 1 gives reactivity indices for the samples studied. The T15 and T75 values for the whole coals decrease with decrease in rank. This same trend is exhibited also by the banded ingredients. Reactivity in- dices for ingredients and whole coals from the same source are similar. Results ob- tained by the C.R.L. test are probably more nearly a measure of the reactivity of the most reactive portion of mixed samples. Sherman et al. (12) gave evidence of this. Macroscopically picked ingredients may be mixtures containing portions of various other ingredients as impurities. This may account for the similarity of the values for samples from the same source. The fact that ingredient reactivity indices decrease with decrease in rank of corresponding whole coals is further evidence of variation of ingredients with rank.

Table 1 also gives free swelling indices for whole coals and banded ingredients. These values do not show progressive de- crease with rank as do the reactivity indices. Samples from the highest rank coal from Gallatin County show the highest free swelling indices. Samples from the next

BANDED INGREDIENTS OE COAL

Table 1. — Analyses of Hand-Picked Sample:

Whole coal

Moisture (as-received), %

Gallatin

Franklin

Macoupin

Henry

Ash (dry), %

Gallatin

Franklin

Macoupin

Henry

Volatile matter (dry, ash-free), %

Gallatin

Franklin

Macoupin

Henry

Fixed C (dry, ash-free), %

Gallatin

Franklin

Macoupin

Henry

Total S (dry), %

Gallatin

Franklin

Macoupin

Henry

Calorific value, B.t.u.

Moist mineral-matter-free

Gallatin

Franklin

Macoupin

Henry

Dry mineral-matter-free

Gallatin

Franklin

Macoupin

Henry

Free swelling index

Gallatin

Franklin

Macoupin

Henry

Reactivity indices, °C. Tis (in oxygen)

Gallatin

Franklin

Macoupin

Henry

Tib (in air)

Gallatin

Franklin

Macoupin

Henry

5.1

8.0

14.0

19.3

10.0 10.3 11.9 11.0

43.1 40.6 45.0 44.0

56.9 59.4 55.0 56.0

3.19 1.69

5.23 4.77

14,098 13,377 12,022 11,486

14,989 14,701 14,349 14,694

7.0 3.0

4.5 4.5

207 182 160 164

254 229 188 186

Vitrain

4.4

9.2

15.3

17.2

8.1 4.3 3.4

7.5

42.8 34.1 43.3 41.6

57.2 65.9 56.7 58.4

2.42 1.04 3.32 4.76

14,371 13,170 11,920 11,667

15,108 14,576 14,194 14,383

6.5 4.0

3.5

210 184 160

258 245 190

Clarain

3.6

8.0

13.4

18.2

10.3 4.9 4.3

11.0

41.1 37.3 47.0 44.9

58.9 62.7 53.0 55.1

2.74 1.37 4.16 4.32

14,361 13,386 12,248 11,633

14,975 14,633 14,284 14,644

6.5 3.0

3.5 3.5

211 187 159 163

254 240 190 185

6.0 16.2

11.4

'7 '.5

43.2 43^6

56'8 56 '.4

i!i6

3*85

13 ',827 12,131

14,849 14,739

3*.5

180

175

218 193

17.8 21.1 20.3

25.2

18.9

8.6

10.0

14.1

28.6 15.2 19.6 26.9

71.4 84.8 80.4 73.1

4.26

4.20

6.20

10.46

11,719 11,634 11,428 10,397

14,985 15,155 14,812

14,847

1 + 1.0 2.0 1 +

211 186 179 170

258 228 222 208

I 10

tl 8 O

BANDED INGREDIENTS OF COAL

GALLATIN COUNTY FRANKLIN COUNTY MACOUPIN COUNTY HENRY COUNTY

{.'*}

,*y

30 40 50

RELATIVE HUMIDITY-

60 70

PER CENT

ig. 1.

Moisture characteristics of whole coals

CALLATIN COUNTY FRANKLIN COUNTY MACOUPIN COUNTY HENRY COUNTY

. — •""•

**"

30 40 50

RELATIVE HUMIDITY

60 70

-PER CENT

Fig. 2. — Moisture characteristics of vitrains

BANDED INGREDIENTS OF COAL

u a.

GALLATIN COUNTY FRANKLIN COUNTY MACOUPIN COUNTY HENRY COUNTY

/ /

) 20 30 40 50 60 70 80

RELATIVE HUMIDITY— PER CENT

Fig. 3. — Moisture characteristics of clarains

100

highest rank coal from Franklin County show the lowest. Values for the two C rank coals appear to be similar for both whole coals and banded ingredients. Fusain is non- swelling, and values greater than 1 shown in table 1 indicate the presence of small amounts of swelling ingredients in the hand-picked fusains.

Moisture Characteristics

Figures 1 to 5 show graphically the re- sults obtained. Samples, ground to pass a 14-mesh sieve, were brought to equilibrium at different humidities, and moisture con- tents were then determined by heating in a vacuum oven at 105° C. for 3 hours. These

I 8 u cr

H in 6

FRANKLIN COUNTY HENRY COUNTY

20 30 40 50

RELATIVE HUMIDITY-

60 70

PER CENT

Fig. 4. — Moisture characteristics of durains

BANDED INGREDIENTS OF COAL

W Q O

-"-

GALLATIN COUNTY

FRANKLIN COUNTY

MACOUPIN COUNTY

HENRY COUNTY

20 30 40 50

RELATIVE HUMIDITY

60 70

PER CENT

Fig. 5. — Moisture characteristics of hand-picked fusains

values were plotted against the correspond- ing relative humidities. For the four sets of samples studied, the interrelations of mois- ture-humidity curves are similar. In gen- eral, vitrain curves are highest, clarain and whole coal are next, durain is somewhat lower, and fusain is decidedly lower up to high humidities where the curves rise steep- ly. Comparisons of the moisture-humidity curves for the four whole coals studied, as well as for the corresponding handed in- gredients, show wide differences. Curves

for vitrains, clarains, and durains have the same general shape and occupy the same relative positions as do curves for the dif- ferent rank whole coals. The fusain curves (fig. 5) do not occupy the same relative positions.

These comparisons appear to show that moisture characteristics indicate variations by rank in vitrain, clarain, and durain as in the whole coals. Indications of variation by rank of fusains are not clear.

ui 6 Q.

GALLATIN COUNTY FRANKLIN COUNTY MACOUPIN COUNTY HENRY COUNTY

30 40 50

RELATIVE HUMIDITY

60 70

-PER CENT

Fig. 6. — Moisture characteristics of Hsiao fusains

BANDED INGREDIENTS OF COAL

Further Studies on Fusains

The question of purity of banded ingredi- ent samples made it desirable to study the characteristics of more carefully purified samples. The relative inertness of fusain to nitric acid (-/) makes possible its purifica- tion, whereas no such means of purifica- tion of the other ingredients is available. Therefore further studies were made on the fusains in an effort to learn whether dis- tinct differences in chemical characteristics of the hand-picked fusains were due to the presence of various amounts of other in- gredients or to the influence of rank varia- tion of the source coals.

Determinations were made by the Hsiao method (-/) on the hand-picked fusains. Furthermore, since fusain is quite friable, similar tests were made on the close-sized reactivity samples (-40 +60 mesh) to de- termine the loss of fusain in sizing between close limits:

% Hsiao Fusain in

Hand-picked	-40+60 mesh
fusains	fusain
61.5	31.6
79.3	46.8
65.0	44.1
49.0	28.2

County

Gallatin . . Franklin. . Macoupin Henry. . . .

This tabulation shows that the hand-picked samples fall far short of being 100% fusain, as judged by the Hsiao fusain determina- tions. Close sizing further reduces the fusain content of -40 +60 mesh samples. The question then arose as to whether re- sults obtained on samples selected according to the Stopes classification by visual appear- ance are to be interpreted as representative of fusain or of mixtures in which fusain may in some cases be the lesser constituent as judged by chemical characteristics.

Hsiao Fusains

Since the Hsiao determinations on the four hand-picked fusains showed the pres- ence of considerable amounts of oxidizable material, it was thought that residues from nitric acid treatment might be more similar in characteristics. Accordingly, such inert portions were prepared from the four sam-

ples of fusain available. Five 10-12 gram portions of each sample were refluxed in 200-240 ml. of 8 N nitric acid for 7 hours. The inert residues were purified by remov- ing alkali-soluble material with 1 N sodium hydroxide, followed by repeated centrifug- ing and final washing with dilute hydro- chloric acid and water. The samples were then dried by exposure to the laboratory atmosphere (with frequent stirring) for 8 or 9 hours, and then various determinations were made. The nitric acid inert residues prepared as outlined are referred to here as Hsiao fusains.

Analyses. — Table 2 presents the results of proximate, ultimate, total sulfur, and calorific value analyses. Samples available were too small to permit duplicate determi- nations in most cases. These analyses show much closer agreement than did those for the hand-picked fusains. However, certain differences are apparent even in these sam- ples. The ash for the Gallatin County sam- ple is higher than for the others. The car- bon value for the Henry County sample was distinctly lower than those for the other three. Nitrogen values are similar. Sulfur values for three of the samples are not very different ; that for the sample from the low sulfur Franklin County coal is definitely lower than for the others.

Dry ash-free volatile matter and fixed carbon values and dry mineral-matter-free (unit coal) calorific values for the samples from Gallatin, Franklin, and Macoupin counties are very similar. The sample from Henry County shows higher volatile matter, lower fixed carbon, and lower calorific val- ues than the other three.

To summarize, it is evident that the vari- ations of analytical results for the hand- picked fusains were due, in large part, to the presence of other more reactive materials in the samples. Although the Hsaio fusains show comparatively small variations in cer- tain characteristics, these variations do not appear to correlate with the ranks of the corresponding coals.

Reactivity index and specific surface. — Table 2 shows that reactivity indices for these samples are decidedly higher than for the corresponding hand-picked samples.

BANDED INGREDIENTS OF COAL

Table 2. — Analyses of Hsiao Fusains

County

Hsiao Fusains

Hand-picked Fusains

Ash (Dry), %

Gallatin 5.1 18.9

Franklin 2.3 8.6

Macoupin 3.8 10.0

Henry 2.4 14.1

Volatile Matter (Dry, Ash-Free), %

Gallatin 13.6 28.6

Franklin 13.5 15.2

Macoupin 13.8 19.6

Henry 14.8 26.9

Fixed C (Dry, Ash-Free), %

Gallatin 86.4 71.4

Franklin 86.5 84.8

Macoupin 86.2 80.4

Henry 85.2 73.1

Total S (Dry), %

Gallatin 0.42 4.26

Franklin 0.21 4.20

Macoupin 0.52 6.20

Henry 0.46 10.46

B.t.u. (Dry Mineral- Matter-Free)

Gallatin 14,103 14,985

Franklin 14,076 15,155

Macoupin 14,145 14,812

Henry 13,969 14,847

T ° C

Gallatin 285 ~' 211

Franklin 263 186

Macoupin 243 179

Henry 266 170

T,6i °C.

Gallatin 326 258

Franklin 310 228

Macoupin 319 222

Henry 313 208

Hsiao

Fusains

C (Dry, Ash-Free), %

89.64 89.56 89.13 87.62

H (Dry, Ash-Free), %

2.47

2.44 2.57 2.43

N (Dry, Ash-Free), % 0.68 0.66 0.55 0.87

O (Dry, Ash-Free), %

6.77 7.13 7.21 8.61

Sp. Surface Sq. Cm. Gram 5490 4610 4170 5310

Earlier in this report attention was called to the fact that reactivity indices for ingredi- ents and whole coals from the same source are quite similar. This is true even for the fusains. Since fusain is considered the most inert of the ingredients, its reactivity index would be expected to be higher. It was sug- gested that, since the C.R.L. method prob- ably measures more nearly the reactivity of the most active constituent of a mixture, the values found were representative of the most reactive constituent in mixed samples and not of the particular banded ingredient supposedly being tested. If this were true

in the case of the fusains, removal of the more reactive material should have given residues whose reactivity indices were defin- itely higher. This is exactly what happened in the Hsiao fusains.

Some differences in reactivity indices for the four samples are apparent. T15 and T1:> values are highest for the sample from the highest rank coal. The T15 value is lowest for the sample from Macoupin County, and the T75 value lowest for the Franklin County sample. No definite correlation with rank is apparent.

BANDED INGREDIENTS OF COAL

It was thought that differences in re- activity indices might he due to differences in specific surface of the samples. Sherman et al. {12) showed that increasing the spe- cific surface results in lowering reactivity index when studying the same coal. Accord- ingly, specific surface determinations were made by the Lea and Nurse method (5). Table 2 shows that the sample from Galla- tin County with the highest T15 and T75 values had the highest specific surface; the sample from Macoupin County with the lowest T15 value showed the lowest specific surface. Although a study of the relation of surface to reactivity should be made on the same coal, the authors wished to determine whether there might be such a correlation for these samples. As the relation here is the reverse of that to be expected, it seems reasonable to assume that differences in reactivity index for these samples are due to more fundamental causes.

Moisture characteristics. — Results ob- tained by the equilibration method are shown graphically in figure 6. Comparison of figures 5 and 6 indicates that moisture- humidity curves for the Hsiao fusains are more similar than are the curves for the hand-picked fusains. All samples (fig. 6) show a gradually increasing moisture con- tent with increasing humidity, but there is practically no indication of high moisture take-up at high humidities such as that exhibited by the hand-picked fusains.

At present there is no definite explanation for this difference between the Hsiao and hand-picked fusains. Previous data (9) indicate that the differences in moisture characteristics cannot be due to the presence or absence of water-soluble salts. It seems reasonable to suppose that possible changes in porosity or surface characteristics, or both, resulting from nitric acid oxidation might account for the differences in moisture characteristics between hand-picked and Hsiao fusains.

In an attempt to secure further informa- tion regarding banded ingredients of Illi- nois coals, some work has been done with

the electron microscope. Through the co- operation of G. L. Clark, of the University of Illinois, electron microscope pictures at various magnifications were made for one set of banded ingredients and for the four Hsiao fusains. This work appears promis- ing but has not progressed far enough to permit definite conclusions to be drawn.

Acknowledgment

Appreciation is expressed to F. H. Reed, G. H. Cady, and G. R. Yohe for helpful suggestions, to F. K. Bursack for assistance in making chemical analyses, and to C. C. Boley, B. C. Parks, and J. M. Schopf for help in securing samples.

Literature Cited

(1) Am. Soc. for Testing Materials, 1943 Sup-

plement to Standards, ft. Ill, pp. 1-26, Method D271-43.

(2) Ibid. Pt. Ill, pp. 154-7, Tentative Method

4720-43T.

(3) Fisher, C. H., Sprunk, G. C, Eisner, A.,

O'Donnell, H. J., Clarke, L., and Storch, H. H., U. S. Bur. Mines, Tech. Paper 642 (1942).

(4) Fuchs, W., Gauger, A. W., Hsiao, C. C,

and Wright, C. C, Pa. State College, Mineral Indus. Expt. Sta., Bull. 23 (1938).

(5) Lea, F. M., and Nurse, R. W., J. Soc.

Chem. Ind., 58, 277 (1939).

(6) Lowry, H. H., J. Geol, 50, 357 (1942).

(7) Marshall, C. E., Fuel, 22, No. 6, 140

(1943).

(8) Parr, S. W., Hopkins, H. C, and

Mitchell, D. R., Ibid., 10, No. 4, 181 (1931).

(9) Rees, O. W., Land, G. W., and Reed, F.

H., Ind. Eng. Chem., 33, 416 (1941).

(10) Rees, O. W., Reed, F. H., and Land, G. W.,

111. State Geol. Survey, Rept. Invest. 58 (1939).

(11) Sebastian, J. J. S., and Mayers, M. A.,

Ind. Eng. Chem., 29, 1118 (1937).

(12) Sherman, R. A., Pilcher, J. M., and

Ostborg, H. N., A.S.T.M. Bull. 112, 23 (1941).

(13) Sprunk, G. C, J. Geol., 50, 411 (1942).

(14) Stansfield, Edgar, and Gilbart, K. C,

Trans. Am. Inst. Mining Met. Engrs. 101, 125-43 (1932).

(15) Stopes, M. C, Proc. Roy. Soc. (London),

B90, 470 (1919).