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ie ENGIN. Bel 1983
. ) CORNELL UNIVERSITY
| LIBRARIES

NL ITHACA, N. Y. 14853
aye

  

 

Engineering Library
Carpenter Hall
UNIVERSITY OF ILLINOIS BULLETIN

Vol.1 JULY 15, 1904 No. 20

 

Published Fortnightly by the University and entered at Urbana, Illinois, as second-class matter

The Gniversity Studies

Vol | JULY. 1904 No. 7

 

 

_ The Coals of Iflinois; Their Composition
and Analysis

By

S. W. PARR. M. S..
Professor of Applied Chemistry in the University of Illinois,

THE ILLINOIS COMMISSION
TO THE LOUISIANA PURCHASE EXPOSITION

PRESENTED WITH THE COMPLIMENTS

OF THE

COMMITTEE ON MINES AND METALLURGY

COMMITTEE

WALTER WARDER, CHAIRMAN, CaiRO
J.N. C, SHUMWAY. TAYLORVILLE H. M. DUNLAP, Savoy
CopyricuHt, JuLy 1904,
By THe University oF ILinors.
Gniversity of Jllinois

Vol | JULY, 1904 No. 7

 

 

 

 

 

The Anuntversity Studies

The Coals of Illinois; Their Composition
and Analysis

By

S. W. PARR, M, S..
Professor of Applied Chemistry in the University of Illinois

PRICE 25 CENTS

Aniversitp Press
@rbana
Char

BRO
UG
La?
1904
THE COALS OF ILLINOIS.
THEIR CoMPOsITION AND ANALYSIS.

There are two sources of motion on the earth, chemical
action and gravity. They are the initial forms of power and
constitute the prime factors in industrial development. Their
availability in any region is an index of present or potential
activity. Of gravity it may almost be said that it has become
a commodity by reason of its easy transformation into electric
energy; but its range is limited. (Chemical energy in its cheap-
est form resides in the coal and oil deposits of the world. Their
cost of transformation is the great problem of the engineer.
He has been mainly occupied with boilers and grates and stok-
ers, but recently a marked tendency is evident towards a more
critical study of the fuel itself. The investigation presented
herewith of the composition and properties of coal is a con-
tribution in that direction.

Geologically, coal is a mineral derived by process of de-
composition from organic material consisting, in the main, of
cellulose. We know the products of decomposition of this
material when submerged to be carbon dioxide, marsh-gas and
water; hence a chemical change takes place somewhat after
the following equation:

6CsHwO =7 CO2 + CHs + 15H2O + CrsH26O
Cellulose Coal

Now, if we take this hypothetical coal molecule, CxsH2x0,
and examine it chemically, we shall find that under the influ-
ence of heat its most natural decomposition products are coke,
marsh-gas and water, indicated in an equation with their per-
centages as follows :

Crs H260 ss Cy 4+ 6CHs + H,0
Coal Coke Marsh-gas Water
100 per cent. = 69.84 per cent. + 25.40 per cent. + 4.76 per cent.

{291]
4

But in the usual method of analysis a separation is made
between the coke, or non-volatile part, and the volatile matter
as a whole, including in the latter both the marsh-gas and
water; hence we have a procedure represented by the follow-
ing equation:

CHO == Cor + (6CHa + H20)
Coal Coke Volatile Matter
100 per cent. = 69.84 per cent. + 30.16 per cent.

This volatile matter burns, being mostly marsh-gas, the
chief constituent of house-gas; the water is small in amount
and seems to have been in a measure lost sight of, for this vola-
tile material came to have the name “ volatile combustible ”
applied to it. Moreover, water of more genuine characteristics
is always found present. It is hygroscopic and invisible, to be
sure, but it can be removed by drying, as the other water of
composition can not be, and hence the analysis showing only
the one kind, the hygroscopic, has been made to satisfy both
the purpose of the engineer and the conscience of the chemist.
The engineer therefore receives his results in percentages of
constituents labeled as follows :

Ash

Moisture

Volatile Matter
Fixed Carbon or Coke

He calls the first two the non-combustible, and the last two
the combustible, material; and to the sum of the latter, as the
unit of the fuel, he refers the evaporative efficiency of his
boiler, and also his calorific values, on the theory that he ob-
tains the heat units per pound of combustible when making
the calculation to the material as “ash and water free.”

Semi-Brruminous Coat.

In the accompavying diagram (Fig. 1) the characteristics
of this type of coal are more concisely shown and in the rela-
tive proportions of the constituents. The results, moreover,

[292]
5

are not hypothetical, as above considered, but are taken from
an actual sample of “ Pocahontas” coal,' which belongs to the
so-called semi-bituminous type, and constitutes a very large
part of the coal deposit of the Appalachian field.

The outer zone in the diagram represents the constituents
as ordinarily found by proximate analysis, and in tabular form
would be represented thus :

Pe nece Gi eegeterecine 3.49 per cent.
MOISHITO: 4) 054-204 0445 “93
Volatile Matter....... 18.70“ *
Fixed Carbon......... 76.88 “ *
100.00 “«  *
Total non-Combustible. 4.42 “ “
Total Combustible .... 95.58 “  *

Hence 104.62 pounds of coal are required to make 100.00
pounds of actual fuel.

In the next to the outer zone of the figure the constituents
are the same, except that the “volatile matter” is subdivided
into that part which in our hypothetical coal molecule was
referred to as water of composition, as distinct from the
“moisture” or hygroscopic water. This constituent in the
actual coal amounts to 4.21 per cent., leaving for actual com-
bustible in the volatile part only 14.50 per cent. instead of 18.7
per cent. as before indicated. Hence it appears that our report
of analysis as above given should be modified to read thus:

GND os Gok lead fades baa ahaa a tl hh Soe 3.49 per cent.
Moisture .................. Oa
Water of Composition ..... hoes <s
True Volatile Combustible... 14.50 “ = “
Fixed Carbon.............. 76.88 “  “
100.00 “ «
Total non-Combustible..... 8.63 “  “
Total Combustible ......... 91.38 “  <*

 

1 Trans. Am. Soc. M.E., XXIV., 1211.
[293]
ANALYSIS & EASTERN
COALS

yy
fama Gy Fe ;
Py

 

ANALYSIS OF A SEMI-BITUMINOUS COAL
(POCAHONTAS) SHOWING CONSTITUENTS
IN RELATIVE PROPORTIONS

FIGURE 1.
[294]
7

In this case 109.43 pounds of coal are required to make 100.00
pounds of actual fuel.

The inner zone of the diagram shows a still further sub-
division of the true volatile combustible into carbon, hydrogen
and sulphur; but of this subdivision and their ratios we shall
make mention later.

The type of coal thus far considered is common to the
Eastern States and to European countries, and it may be that
analytical processes, at least the so-called * proximate analysis,”
conveyed an element of untruth of not sutticient magnitude to
disturb the method because of the convenience that character-
ized it.

Biruminous Coat.

Let us briefly make a parallel statement concerning the
coals of the Mississippi Valley. We find on working back from
the present structure to the original cellulose decomposition,
that it has proceeded somewhat differently, thus :

6CsHwO; = 7CO2 + 4CH, + 138H,0 + Cos HO

Cellulose Coal

The decomposition of the coal in analysis, therefore, would
be represented thus :

Cas HisO2 = Cx + CsHi + 3H.0

Coal Coke Pentane Water

100 per cent. = 65.58 per cent. +- 19.67 per cent. + 14.75

To carry out the comparison, a second diagram has been pre-
pared, and again this has not been made up from the hypothet-
ical coal molecule just presented, but from the average of results
obtained from ten typical Illinois coals.

As in the first diagram, the outer zone represents the ordi-
nary proximate analysis and by the usual method would be
reported thus :

[295]
ANALYSIS ILLINOIS
COALS

 

ASIFRACE OF TEN ILLINOIS COALS
SHowine ConSTITVUENTS iN
RELATIVE PROPORTIONS.

FIGURE 2.
[296]
Wel UCAccceee ewe sates 8.00 per cent.
Moisture ............. 7.00 “ “
Volatile Matter ....... 35.60 “ “
Fixed Carbon......... 49.40 “ “
100.00 *  “*
Total non-Combustible. 15.00 “ “
Total Combustible.... 8400 “ “

Here we need 119.00 pounds of coal to make one hundred
pounds of fuel.

The next zone shows the relative parts when a division is
made of the volatile matter, and for this type of coal the
analytical data agree somewhat closely with our hypothetical
coal molecule given above. This zone shows the volatile mat-
ter to consist of 14.00 per cent. of inert matter, or, as we have
been calling it, * Water of Composition”, and 21.6 per cent. of
true combustible matter. Hence, instead of the list as given
above, our report of constituents should be:

Mel sa cade ne soaueaocere nes 8.00 per cent.
MGISGUTE su ward wets aie a orcas Too
; Water of Composition ..... 14.00 “
) True Volatile Combustible... 21.60 “ = “
Fixed Carbon.............. 49.40 “  *
100.00 *
Total non-Combustible..... 29,00 ~ =
Total Combustible ......... noe

Hence there are required 141.00 pounds of coal to make 100.00
pounds of actual fuel, instead of 119.00, as by the usual method.

LiaNiTE or Brown Coat.

It is of interest here to present a third diagram showing
the same facts with regard to brown coals,a North Dakota
lignite being used for the analysis.

[297]
ANALYSIS o LIGNITIC
COALS

ns
2
g
a
ld
F
<
L
2
%
Oo
3

 

ANALYSIS OF A LIGNITIC OR BROWN
CoAL SHOWING CONSTITUENTS
IN RELATIVE PROPORTIONS.
FIGURE 3.

298]
8

By reference to the outer circle, which represents the usual
method of analysis, we have results as follows :

SNe ved aa hesinae wks 2.71 per cent.
MOISTURE 250444465005 1412)
Volatile Matter....... 41.91 “ «
Fixed Carbon......... 41.26 “ *
100.00 “ :
Total non-Combustible. 16.83 “  *
Total Combustible .... 83.17 “ = “

Hence, by this showing, 120.28 pounds of coal would be re-
quired to make 100.00 pounds of combustible.

However, upon further analysis of the volatile matter, we
find it to consist of 21.63 per cent. of water of composition
and of only 20.28 per cent. of actual combustible. Hence our
results should be made to read as follows :

 

Pieluaccaleaoiaweues oie mes 2.71 per cent.
Moisture .................. 1412 * *
\ Water of Composition ..... 21.638 "  *
( True Volatile Combustible... 20.28 “ *
Fixed Carbon.............. 41.26 “ *
100.00 “ *
Total non-Combustible..... 38.46 “  *

Total Actual Combustible... 61.54 “

Here there would be needed 162.49 pounds of coal to make
100.00 pounds of actual combustible. These ratios in the three
types of coal, with the differences in the results of the custom-
ary and the proposed method of determining actual fuel, may
be better illustrated in a table, thus :

 

 

 

TABLE I.

No. of pounds required to make 100 pounds| Error of common

* of ‘‘Combustible.”’ method per 100

pounds of actual

Kind of Coal. Common Method. | Proposed Method. fuel.

Pocahontas. ..... 104.62 109.43 4.81
Illinois ........... 119.00 141.00 22.00
Lignite ........... 120.23 162.49 42.26

 

 

 

[209]
12

It is evident from the table that a boiler rated, for example,
at an efficiency of 10 pounds of steam per pound of coal of the
Pocahontas ‘type would have difficulty with a coal wherein 22
per cent. of the so-called combustible was really non-combusti-
ble and inert, to say nothing of the loss due to heat of vapor-
ization and temperature of the same water in the form of
escaping flue gases.

WatTER OF CoMPOSITION AND VOLATILE COMBUSTIBLE.

We come now to the methods for obtaining the factors
above indicated. At first thought, an ultimate analysis of all
the constituents would seem to be the only means for arriving
at these data. But such analyses are almost prohibitive for
technical use, because of the time and. manipulative skill
involved; but more than this it may be questioned whether an
ultimate analysis alone will give the data in the desired form.
Very much depends upon the factor for “available”, that is,
combustible, hydrogen. With this factor at hand, and one for
total carbon, we have all the constituents that can enter into
the actual combustible, with the possible addition of a small
correction for sulphur.

In the data so far presented the factor for the disposable
hydrogen has been calculated from the results obtained by
both ultimate and proximate analysis, wherein the available
hydrogen in bituminous coals was regarded as a part of the
volatile hydrocarbon having the composition represented by
the formula C;H», or, in semi-bituminous coals, by CH. The
formula in each case therefore, for calculating the hydrogen

would be ——— cs © and C— ae Cin which Cand care the total carbon

"a
and the fixed carbon respectively. Therefore (C —c) i
would represent the true volatile combustible, and this value
subtracted from the total volatile matter equals the water of
composition.
Before passing to the consideration of methods for obtain-
ing the total and fixed carbon, a word further concerning the

[300]
13

deriving of hydrogen from these constituents is necessary. That
this method is applicable to certain classes of coals is evident
from Table IT.

Comparison is made between the usual method for arriving

at the available hydrogen by means of the expression (H —3),

C—

5
from the averages of 10 Illinois coals. The others: are calcu-
lated from averages obtained by Lord and Haas.’

and the proposed ratio ( ae The first results are derived

 

 

 

 

 

 

 

TABLE II.
Percentage of
Available Difference
Coals. Hydrogen in
Percent:
H--2 C—c age.
8 5
Average of ten Illinois coals....... 3.76 3.60 — .16
Upper Freeport, Ohio and Penn,..| 3.4 4.20 + .26
Pittsburg, PON i sasdis a sasridionweicmes 4.15 4.28 + 13
Darlington, Penn...............4. 4.10 4.10 00
Hocking aul Ohi ssexesescawes 3.34 3.67 + 33
Thacker, W. Va...............005 4,27 4.39 + .12
Pocahontas, W. Va. (Sample 1)?...| 3.85 3.35 — .50
ae te (Sample 2)?...| 3.97 3.62 — .35

 

From the table, it would appear that the possible error
from thus calculating the available hydrogen would be less
than one-half of one per cent. of the true value, and its effect
as a variable, therefore, in calculating the true volatile com-
bustible would fall within that limit.

It may not be concluded, however, that so uniform a ratio
is applicable to widely varying types of coal. Indeed, there is
good evidence, so far as it has been tested in connection with
Illinois coals at least, that a gradation exists; thus if we let
the volatile carbon be represented by total carbon minus fixed
carbon, or C—c; then

1 Trans. Am. Inst. Min. Eng. XXVII., 266-7.

w=

 

{301]
14

Where C — c = 10 per cent. the available hydrogen = 3
66 be =—_ 15 66 6é gs 6 = t
oe 6a“ = 90) ce bo be “ce = t
be [73 — 95 6c 6“ 6“ 6c = $

A diagram therefore has been arranged as follows to test the
correctness of the above ratios. Fifty Illinois coals have been
located with the volatile carbon for abscissa and that amount
of hydrogen for ordinate which would be required to produce
the heat values indicated by the calorimeter.

Available Hydrogen

 

10 15 “20 25
Volatile Carbon, C — ¢

FIGURE 4.

TotTaL CARBON.

It will be noted that the expression 5 = requires the

 

value for C, that is, the total carbon content of the coal. If
this must be obtained by the usual combustion method we have
made but little progress by the mere development of the above
ratio. It is proposed to obtain the factor for the total carbon
by means of the apparatus shown in Figure 5.

Combustion of the coal is effected in a closed bomb as in
the calorimetric process described further on, by use of sodium

[302]
15

peroxide, NazO2, the product of the combustion being sodium
carbonate, Na2COs. The solution of this material is placed in
the receptacle A, while acid is in B and C. The flask C con-
tains about 25cc. of sulphuric acid, and a carefully measured
volume of air taken at common pressure and temperature. At

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

J

APPARATUS FoR ToTAL CARBON DETERMINATION.
FIGURE 5.

the end, after admitting all the carbonate solution and meas-
uring the volume of gas evolved, the flask C is completely
filled with the wash water from A and the total volume meas-
ured over in the jacketed pipette PP. By subtracting the
initial volume in the flask C, the exact volume of carbon diox-

[303]
16
TABLE III.

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

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[304]
17

ide from the sodium carbonate is obtained. Ihe pressure and
temperature readings are taken and from the subjoined table
the exact weight of the carbon is derived. Great care hasbeen
exercised in the preparation of the table. The computations
were made by three individuals, with comparison of results to
eliminate all possibility of errorsin the final readings.

Fixep Carson.

It will be evident from what has preceded that more than
usual importance attaches to the factor for fixed carbon. A
special study has been made of methods for obtaining this
factor, first because the method recommended by the commit-
tee of the American Chemical Society on coal analysis' is not
altogether satisfactory; and, second, because with western
coals high in sulphur the use of platinum for this determina-
tion is to be avoided if possible.

The report of the committee prescribes heating in a plati-
num crucible over a Bunsen flame 20 cm. high when burning
free. Our objections to the prescribed method may be stated
as follows :

The heat capacity of a Bunsen burner is not measured
alone by the height of the flame. For example, a large sized
adjustable burner with a tube of 10 mm. caliber will give more
heat than a small burner with a tube of 9 mm. caliber, and
burning at the regulation height. The results also are more
variable than they should be. This is more noticeable in west-
ern than in eastern coals, but in any case it is to be expected
that the platinum crucible arranged as prescribed is especially
sensitive to external influences, and especially to differences in
the heat capacity of the flame. In the table following, an aver-
age sample of coal designated Sandoval, Illinois, was used. It
cokes freely, and has ash 11.94 per cent. and moisture 5.51 per
cent, Comparison of results is made with use of a large and
small sized Bunsen burner as above described, and also with

 

1 J. Am. Chem. Soc. NAL, 1122.
[305]
18

the old combination of burner and blast, and with use of a
porcelain crucible in a small furnace of special construction to
be described later.

TABLE IV.

DETERMINATION OF VoLATILE Marrer, SANDOVAL, ILLINOIS, CoAL.

 

Large Bunsen burner............ ) Highest ...,........ 37.21 per cent.
F hi Lowest ............. 35.71
ame 20 cm. high.............. f Vislallore cucscuas “T50
Plat. crucible, Time 7 min....... Average of eight ... 36.52 per cent.
Small Bunsen burner............ Highest ............ 36.73 per cent.
‘ Lowest ............- 35.69
Flame 20 cm. high .............. VWatatiOn cccccsccos, a. Tot
Plat. crucible, Time 7 min....... Average of eight.... 36.13 per cent.
Bunsen flame 33 min............ Highest ............ 37.78 per eent.
‘ Lowest ...........+5 36.53
Blast flame 33 min .............. WalGBOH, isc ssc cx 35
Plat: ertietble ci .e00 cess essay Average of fourteen. 37.13 per cent.
Bunsen flame 34 min............ Highest ............ 37.35 per cent.
Blast flame 33 min.............. Lowest ...........-- 36.69
Porcelain crucible in special Variation .......... -66
PUPNACE: Se ccacsieses ¥ hob era woe whos Average of nine..... 37.10 per cent.

 

 

From this table it appears feasible to replace the expensive
platinum crucible with one of porcelain. The serious deterior-
ation of platinum under the combined effect of red hot carbon
and sulphur makes this end a very desirable one, even if there
were no advantage in the results. On this latter point there
is much to be said in favor of the porcelain crucible. The in-
itial heating up is somewhat more gradual. A bright red is
very easily reached and evenly maintained, and especially is it
true that the full effect of the heat is exerted on all sides, com-
pletely enveloping the crucible.

The form of apparatus is shown in the accompanying
figure.

First, as to the lamp: This simple form of blast lamp has
been in use in this laboratory for the past seven years, and has

[306]
19

proved itself of such general utility as to merit a brief descrip-
tion.

It consists essentially of a Bunsen burner with the blast
entering at the usual inlet for the gas, and the gas entering
through a side tube attached where the air is ordinarily ad-
mitted. The air is discharged through a tip with circular open-
ing 14 mm. in diameter, and is so adjusted as to come about

 

 

 

 

 

 

Coking FuRNACcE
FIGURE 6.

even with the lower side of the gas inlet tube. A wire gauze
is inserted in the tube about 3 of the way towardsthe top. The
lamp is especially adapted for use with blast of constant press-
ure. By adjustment of the air it may be made to burn with a
common Bunsen flame. In connection with the furnace it is
allowed to burn for the first 34 minutes as a strong Bunsen
flame of 12 inches when burning free. During the second
period of 34 minutes it burns as a blast lamp. The combus-

[307]
20

tion, however, leaves the tip of the lamp and takes place en-
tirely within the chamber underneath the crucible. In this
way an excessive amount of fuel may be forced into a small
space by the jet action of the blast. The combustion taking
place in this chamber and the hot gases being turned downward
to escape through the annular space at the side, a very intense
heat is quickly attained.
A cross section is shown through the furnace in Fig. 7.

 

 

SECTION THRU FURNACE
FIGURE 7.

The base B rests on a cast plate with an opening 14 inches
in diameter. The crucible rests on a triangular support which
permits of the free passage of the gases, part of which may
escape through a small opening in the top of C, but mostly
they are required to travel downward between the two walls
and escape at the lower edge of R.

A common glazed crucible of Royal Berlin Porcelain No.
00 is used. Crucibles as true as possible are selected, with well
fitting covers, and these are ground with emery powder until

[308]
21

the lid touches at all points. Crucibles may be used many
times, but if warping occurs the covers may require regrind-
ing,—not a difficult matter and easily accomplished by hand in
tive or ten minutes.

SULPHUR.

We come now to sulphur, a constituent having more im-
portance than is usually ascribed to it; this is especially true
of western coals, in which this element varies from 1 per cent.
to 5 percent. One of its characteristics, and by no means
the least, is the part it plays as a disturbing element in
nearly all the determinations in coal analysis. The Eschka
method is satisfactory, but heat other than from a gas flame
must be used. There is still some question as to the like-
lihood of sulphur being left in the residue, and also as to
the necessity of dehydrating the silica. The use of sodium
peroxide as an oxidizing agent has received considerable atten-
tion, but the violence of the reaction has brought disfavor upon
the method. However, by means of a closed bomb, as in the
Parr calorimeter, there has been fully demonstrated the prac-
ticability of using sodium peroxide for this purpose. Indeed,
over two years ago, Mr. Milton Hersey of Montreal, Canada, in
a communication to the author reported the very satisfactory
use of the residues from the calorimetric process for gravimet-
rically determining the sulphur. Later articles by Sundstrom!
and by von Konek? have advocated the same method.

It is not my purpose now to enter into a discussion of this
phase of the matter, but simply to emphasize the fact of the
completeness of the oxidation, which has been verified very
many times by the writer.

Coupling the sodium peroxide method of arriving at a
combustion with the photometric method proposed by Mr,
Hinds,’ there seem to be possibilities well worth investigating.

 

1 Jour. Am, Chem. Soc. XXV., 184.
2 Zeit. {tir Ang. Chem. 1903, p. 517.
8 Jour. Am. Chem. Soc. XNIIL, 269.

[309]
22

The work with the photometer, however, either as outlined by
Mr. Hinds, or as elaborated by Mr. Jackson,’ was not found
satisfactory. A careful study was made of the variable ele-
ments that entered into the proposition. The method prescribed
a candle of standard power, maintained at a definite distance
from the bottom of the graduated tube in which was read the
depth of liquid through which the outline of the candle flame
could be seen. It was soon found that the strength of the
light had little to do with the matter. A stronger light would
illuminate the liquid to a corresponding degree and cause the
outline of the candle flame to disappear at about the same
depth as a lesser light with a less illumination of the liquid.
As between a common candle and a forty candle power
acetylene light there was no marked difference. Indeed, the
greatest difference was noted when the diffused light was cut
out by diaphragms, in which case the light could be seen
through a greater depth. An extreme illustration of this fact
was afforded by completely blackening an incandescent light
bulb and then cleaning a small spot to show a short length of
the glowing filament. This bit of filament, which afforded no
illumination to the liquid, could be seen through a very much
greater depth than was the case with an ordinary candle, though
its power was far below thestandard. Other disturbing conditions
related to the method of precipitation, whether hot or cold,
whether the barium salt was added in the solid or the liquid
state, whether readings were made at once, or on standing, or
whether precipitations made in the cold were subsequently
heated or not. The control of the conditions regarding the
light has been accomplished with a greatly modified apparatus
in the following manner, as shown in Fig. 8.

The tube graduated in millimeters is placed in a common
flask having a little clear water in the bottom. The flask is
placed on a square of glass resting on a carbon plate about 3 of
an inch thick and having a } inch hole in the center. The

 

1 Jour. Am Chem. Soc. XXIII, 799.
[310]
23

plate is adjusted about 10 inches above the flame of a common
candle. It will be noticed that the reading tube has a round
bottom, This is carefully blown, of clear glass without flaw,
and ground on the outer surface; the whole when immersed
playing the part of a lens. By this arrangement, together with
the diaphragm effect of the hole in the carbon plate, a pencil
of light is secured with the minimum amount of illumination

 
  
 

Fofperietitabim tends. (reeled afi faba

 

 

 

 

 

l J

PHOTOMETER FOR SutpHurR DETERMINATIONS.
FIGURE 8.

being imparted to the liquid. Moreover, instead of the vary-
ing and indefinite outline of a candle tlame there appears a
steady compact point of light. The end reading is thereby
rendered sharp and definite. It is interesting to note that
precipitations made with the barium salt in solution, or with
the sulphate solution hot, transmit the rays from the candle as
white light, while in the case of precipitations made with the
crystals of the salt, the red rays only are transmitted, the illu-

[311]
24

mination of the liquid isin this way still further reduced, and
the sharpness of the end reading is thereby promoted. To
secure concordant results, definiteness of precipitation must be
obtained. This is accomplished by adding the barium salt to
the 100 ce. of solution at room temperature, and after dissolving
completely, heat on the water bath to about 70°. Let stand
for half an hour and bring to the room temperature, when it is
ready to transfer to the photometric tube for reading. With
this device it has been necessary to work out a new table. (Ta-
ble VI). The conditions are purely empirical, but not arbitrary
within reasonable limits, except as to the size of the hole through
the plate and the method of precipitation. The table has been
developed directly from astandard solution of potassium sulphate
having 5.4386 grams dissolved in a litre, thus containing 0.0001
grams of sulphur by weight per cubic centimeter of solution.

Results from use of this method as above outlined, in com-
parison with those obtained under standard conditions, are
shown in Table V.

TABLE V.

SHOWING PERCENTAGES OF SULPHUR.

 

 

 

 

: Residues from Parr
Washings from Mahler : :
Tllinois Coal. aati eeneaeky soos Photo-
(Per cent. ) (Per cent. )
Ls (OGIN;, Pla cc peccverseticaceangaees 2.30 2.17
2. St. John’s, lump.................. 1.55 1.65
8; Pana, slackesie csc vey eens ew astee dee 4.03 4.04
4. Danville, lump ................... 2.16 2.31
D. Ridgely, pea csscncsevcezes aeee es 4.00 4.01
6. Bloomington, lump ............... 2.57 2.68
7. Spring Valley, washed ............ 3.04 3.20
Be, eI WOOG sccrccsrechiavece ners caroaancesn aeeerees 1.53 1.61

 

' With this form of apparatus, the facility with which the
sulphur determinations may be made has enabled us to under-
take an additional factor in the case of each sample, viz., the
estimation of the amount of sulphur remaining in the coke
after the volatile matter has been driven off. The coke is pul-

[312]
26

TABLE VI.

 

 

PHOTOMETRIC TABLE FOR SULPHUR
WEIGHT OF SULPHUR IN GRAMS

PER MILLIMETER DEPTH

 

SULPHUR

SULPHUR

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

ne | incrams| tM! Werams | | in orams | | in GRamMs
200) 0.00/38 |/51 0.00/16! |//7| 0.00204 83 | 0.00270
/95| 0.00140 | /50| 0.00/62 |//6}| 0.00206 | 82| 0.00275
/90\ 0.00/42 |/49)| 0.00/63 |//5 | 0.00208 8/ 0.00277
/85| 0.00145 | 148} 0.00164 |//4 | 0.002/0 80} 0.00280
/83| 000/47 |/47) 0.00/65 | //F | 0.00212 72 | 0.00284
/80| 0.00/50 |/46| 000/66 | //2 | 0002/14 78 | 0.00288
179} 000/150 | /45| 0.00/67 | /// 0.00216 77 | 000292
178 | OOO/S5/ | /44| 0.00/68 |//0 | 0.002/8 76 | 0.00296
177 \ O.00/S! | /43 | 0.00169 |/09| 0.00220| 75 | 0.00300
1/76 | 0.00/15/ |/42| 0.00I7l |/08| 0.00222 7# | 0.00302
175 | O.OOIS! |/4/ | 0.00172 |/07 | 0.00224| 735) 0.00704
/7#\ 000/52 |\/40)| 0.00174 |/06| 0.00226 72 | 0O.OOFO07
173 | 0.00/82 |\/39 | 0.00175 | /05) 0.00228 7/1 | 0.00310
172 | 0.00152 |/38 | 0.00/76 |/04| 0.00230| 70] 0.003/3
“71 0.00/52 |/37 | 0.00/77 |/O3 | 0.002F3/ 62} 0.003/7
/70| 0.00/83 |/36 | 0.00/79 |/02 | 0.00233 68} 0.00320
/69\) 0.00/53 \/95 | 0.00/80 | /0O/ 0.00234 67} 0.00323
168 | OOO1S3 |/IF| 0.00/18! |/00| 0.00236 66 | 0.003727
167 | 0.00/54 |/F3 | 0.00182 II| 200238 65 | 0.00330
166| 0.00/54 }/F2 | 0.00/8F | I8| 0.002359 64 | 00073355
/65| 000/154 |/5/ 0.00185 97 | 0.00240 63 | 0.00340
164| 000/55 |1F70| 0.00/87 96| 0.0024! 62 |} 0.00345
/63| OOO/S5 |/29| 0.00188 | 95 | 0.00243| 6/ | 0.00350
/62| O.O0O0/IS5S |/28 | 9.00/89 94.| 0.00244| 60| 0.005755
/6/\ 90.00/156 |/27 | 9.90190 293 | 0.00246| §2| 000360
/60\ 0.00/56 |/26| 0.00/91 92| 0.00248 58 | 0.00367
159\| 0.00156 |\/25 | 0.00193 9/| 000250 | 57 | 0.00373
/58\ 0.00/57 | 124} 0.00195 | 90| 0.00252} 56 | 0.00380
157\| 0.00157 |/23 0.00196 89} 000255 55 | 0.00586
156) 0.00/58 | /22 0.00/98 88 0.00257 54 | 0.00F9S
155\| 0.00158 |/2/ | 0.00/99 | 87 | 0.00260 | 53 | 0.00400
/54.| 0.00/59 |/20]| 9.00200 86 | 0.00262 92 0.00407
153) 0.00159 | //9| 0.0020/ 85 | 0.00265| S/ | 0.004/3
752| 0.00/60 | //8 | 9.00203| 84] 0.00267} 50} 0.00420

 

 

[313]

 

 
26

verized and burned with sodium peroxide in the calorimeter
bomb as usual, and the sulphur determined in the residue by
means of the photometer. Having determined the total
sulphur in the coal, the difference between these two factors
represents the volatile sulphur. In the analytical tables at the
end these divisions are observed thioughout.

CALORIFIC VALUES.

1st. By calculation: Many attempts have been made to
develop a reliable formula for calculating heat values from
analytical data. The formula of Dulong is the most reliable
and is recommended by the committee of the American Chemical

Society in the following form, 8080C + 34460 (H — 2) + 22505."

The variations between the observed calorific values and the
calculated values as shown in Mahler’s tables’ range from + 3
per cent. to — 3 per cent., though the averages of numerous
results are much closer.

The variations in the work of Lord and Haas above re-
ferred to are not so great, ranging from +2 per cent. to — 1.8
per cent. Kent* has used the factors 3 and 5 times the avail-
able hydrogen derived from ultimate analysis to indicate (when
subtracted from the total carbon) the amount of fixed carbon,
and to the various percentages of fixed carbon he has assigned
certain calorific values. His results while interesting seem to
show greater conformity in the case of eastern than of western
coals.

Possibly quite as good as any method of calculation would
be the one already partially suggested in the discussion con-
cerning the derivation of the factor for true volatile com-

 

1 Jour. Am. Chem. Soc. XX1I, 1130.
2 Contributional "Etude des combustibles. Mahler, 1892.
3 Trans. Am. Inst. Min. Eng., XXVIL., 948.

(314]
27

bustible or water of composition (p. 13). Stated as a formula
{

it would be 8080C + 34500 ie 5 ©) + 9950S in which U is the
total carbon, ¢ the fixed carbon, and S the sulphur, or still
more accurately, 8080C + 34500 (H ) + 2250S, wherein H is the
available hydrogen as indicated by the curve in Figure 4, the
point being located by the percentage constituent of volatile
carbon as shown by C—c. Calculated in this manner the 50
Illinois coals there listed would show extreme variations from
the calorimeter values of about +1.5 per cent. to — 1.5 per
cent. In Table VII. the calculated results thus derived are
compared with observed values by means of the calorimeter.

Concerning calculations in general, however. it is well to
quote Mahler’, who says: “We cannot give a general formula
depending strictly on the chemical composition which will give
the calorific power of substances so complex and varied”; or
Poole, who says:’ “If possible, by all means, have a calorimetric
test. If not possible, use the best analysis available.”

2nd. By observation: The calorimeter devised by the
writer has met with very general favor and is now widely used
both in this country and abroad. It is too well known to call
for detailed description here. However, a few modifications
and improvements have been made and since it has been used
in the accompanying results and also in comparison with quite
a list of determinations with the Mahler-Atwater apparatus, a
brief reference is here given.

Figure 9 shows the relative positions of parts. The can A.A.
for the water has a capacity of 2 litres. The insulating vessels
B.B. and c.c. are of indurated fiber. The charge of coal and
chemical are put inthe cartridge D. Upon ignition, the heat
generated is imparted to the water and the rise in temperature
is indicated on the finely graduated thermometer T. The car-
tridge or bomb rests on the pivot. F and is made to revolve,
thus by aid of the small turbine wings attached effecting a com-

 

 

1 As quoted by Poole, The Calorific Power of Fuels, p. 10. 2 /ézd.
{315]
28

plete circulation of the water and equalization of temperature.
The reaction accompanying the combustion may be repre-
sented by the equation:

56Na.0. + Co5HisOs = 25 Na,CO; + 18 NaOH + 22 Na,.O
Sod. perox. Coal Sod. carb. Sod. hydrate Sod. oxide

With certain substances such as coke, anthracites, petrole-
ums, ete.,a more strongly or vigorously oxidizing medium is

 

 

 

 

 

 

 

 

 

 

 

 

FIGURE 9.

needed than exists in the peroxidealone. This may be secured
by various additions. The most effective are :—a mixture of
potassium chlorate and nitrate in the proportion of 1 to 2 and
this mixture used in the ratio of 1 to 10 of the sodium peroxide;
another effective mixture is an addition of potassium persul-
phate in the ratio of 1 to 10 of the sodium peroxide. Other

[316]
29

substances facilitate the oxidation, notably ammonium salts
and certain organic substances, as tartaric or oxalic acid, ben-
zoic acid, etc. In the work on Illinois coals, while ordinarily
no extra chemical would be necessary, still in certain cases
such as extra slaty coals and coals with excessive volatile

i matter, and also to guard against variations in
the quality of the sodium peroxide, a mixture
as first described above, of chlorate and ni-
trate, has uniformly been used throughout
these tests.

One peculiarity in the behavior of the com-
bustion has been improved ‘by the above mix-
tures. This behavior is probably due to the
fact that there is a tendency on the part of the
particles of coal in immediate contact with
the metal, which is kept cold by exterior con-
tact with the water, to escape action of the
chemical. A further improvement in this
particular is effected by a modification of the
bomb as illustrated in the accompanying fig-
ure (Figure 10). The air space about the low-
er part of the bomb prevents direct contact
with the water. However, upon ignition this
enclosed air expands and part of it is driven
out through the holes below. Later as cooling
and contraction occur the water is drawn into
the air space and rapid cooling is effected but
the period of high temperature for the inter-

FIGURE 10. joy reaction has been prolonged from a few-
seconds to a half minute or more. Other advantages are se-
cured, notably the avoidance of screw threads on the interior
or other opportunity for material to lodge and cause sticking
or difficult removal of the ends.

In Table 7 are given results with this apparatus in
comparison with the readings obtained by use of a Mahler-At-
water apparatus. In the third column as already indicated

(317]

 

 

 

        

  

 

RSSSSHSSSSSSSS

JOLIE TI

A

NY 4
USO
aaa

CALORIMETER BomB
30

 

 

 

 

TABLE VII.
ComPARISON oF CaLoriFic Factors.
Mahler— Parr— Calculation—

No. Mlinois Coal. Atwater Bomb Per-oxide 8080 C + 34500
Calorimeter. Calorimeter. A”
A | Bloomington, lump........... 6566 6530 6687
B | Carterville, washed........... 7174 7185 7027
C | Danville, lump............... 6797 6762 6804
D | Elmwood, lump 7050 6990 7092
E | Moweaqua, lump............- 6152 6135 6256
BE) | (OGM, Peas sine 's ars came wesc oF 6227 6257 6333
G | Pana, slack .................. 5383 5387 5745
H | Ridgeley, pea................ 5922 5964 6193
I | St. Johns, lump..... Sis vietieuse 6917 6911 6769
J | Spring Valley, washed........ 6150 6109 6346
12 Bloomington, 2nd V., slack ... 5510 5637 5742
13 ‘lamp. re 6447 6511 6571
14 es 3rd V., slack.... 6327 6326 6316
15 ss sc" lump.... 7140 7106 7119
24) Buxton, lump................ 6534 6520 6540
37| Centralia, slack .............. 5911 6020 5879
38) Centralia, nut................ 6425 6476 6440
45) Danville, slack............... 6616 6672 6610
60) Eldorado, slack .............. 5743 5777 5854
64, Fairbury, ae idiisiaelwpar s-o8ber bee 5782 5868 5893
65 MUM Pin ccsiacenas verona 6804 6747 6773
75| Harrisburg, lump 7370 7379 7276
126| Sandoval, Tiara Caeigliialadnelcuees 6636 6677 6500
131 Springfield, slack 6653 6635 6589
134 Streator, 2nd V., slack....... 6343 6395 6371
135 iin ‘lump mee eoes 6962 6983 6948
136 et 7th V., slack ........ 6745 6775 6717
137 i ee? lump ........ 7257 7256 7119
140) Trenton, nut................. 5445 5500 5673
141 “ SLAC c csvierdistanssece sates 5808 5947 6008

 

 

 

 

 

under “Calorimetric Values by Calculation” are given results
obtained by use of the formula 8080 C + 34500 (H), in which “H”
is the percentage of available hydrogen as indicated by the
curve in Fig. 4. The samples are given numbers corresponding
with those of the analytical tables at the end. The values are
given in calories per kilo. (Cal. per kilo x 1.8 = B.T.U. per
pound),

The ultimate analyses which have served as the basis for
some of the preceding calculations are embodied in Table
VIII. There is also included the proximate analyses and a
comparison of values obtained by the old and new methods
Results are given throughout in per cent.

[318]
31

 

 

 

 

 

 

 

 

 

 

 

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TILA AT&V iL

[319]
32

The samples for Table IX. were collected between Feb. 8th
and June 8th, 1904. These were obtained at the mines from
the surface of car lots as made ready for shipment to the con-
sumer. Amounts varying from 40 to 50 pounds were taken
and shipped in sacks to the laboratory. In general one sample
of lump or screened nut and one of screenings or slack was
procured from each mine. The term “slack” has been uni-
formly applied where the material included all that passed
through a 14 inch screen.

Immediately upon receipt of the material it was reduced
by quartering in the usual manner. A check sample, buck-
wheat size, was taken, another part was ground to pass through
a 100 mesh sieve and each was sealed ina “lightning” fruit
jar. The analytical results are given in percent. The calorific
values are given in British thermal units per pound of actual
coal as represented by the samples and also in calories per kilo
of actual coal.

 

[Note.—For the collection of many of the samples I am indebted tothe State
Mine Inspectors, and I wish here to express my appreciation of their interest and
efficiency. The general analytical work has been in charge of C. H. McClure, assist-
ed by Chas. Edwards and A. C. Brown, and I heartily commend the skill and faith-
fulness which has characterized their part of the work.—S., W. P.]

[320]
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[328]
NUMBERS OF THE UNIVERSITY STUDIES PREVIOUSLY

ISSUED

[Address all communications concerning the Studies to Editor, University Studies,
305 University Hall, Urbana, Il.]

Vol. 1., No.

No.

No.

No.

No.

No.

1.

vo

Abraham Lincoln: The Evolution of his Literary Style. By Pro-
fessor D. K. Dodge, Ph.D.

The Decline of the Commerce of the Port of New York. By Mr.
Richard Price Morgan.

A Statistical Study of IMinois High Schools. By Mr. F. G. Bonser, M.S.

The Genesis of the Grand Remonstrance from Parliament to King
Charles I. By Henry Lawrence Schoolcrait, Ph.D.

The Artificial Method for Determining the Ease and the Rapidity of
the Digestion of Meats. By Harry Sands Grindley, Sc.D., and
Timothy Mojonnier, M.S.

Illinois Railway Legislation and Commission Control since 1870. By
Joseph Hinckley Gordon, A. M. Introduction by Professor M. B.
Hammond, Ph. D.