Methods for Testing Coal Tar, and Refined Tars, Oils and Pitches

Publication Date: March 1913. ACS Legacy Archive. Note: In lieu of an abstract, this is the article's first page. Click to increase image size Free fi...
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T H E J O U R N A L OF IATDUSTRIAL A N D EA;GIA'EERING CHEMISTRY

Mar., 1913

Weight

N

3 8 13

4 19 21 8 6

1s 23 28 33 38 43 48 58

TABLEV-DESPAREZ Average Average sucrose solids 18.80 20.59 19.92 19.31 15 . 7 8 1 1 67 14.55 16.20 16.67 16.80 15.20

2 1 3 2 1

16.55 18.16 17.36 17.20 13.15 14.14 12.45 13.40 14.13 14.55 11.so

average purity 88 00 86.38 87.10 88.75 83 3 3 8 4 86 85 5 0 83 00 8 4 67 86 50 78 00

I95

Owing t o the comparatively recent appearance of our first paper on this subject, no reference will be made a t present to the methods in which no change has been made. T.4 R

B . Specific Gravity.-The

special Hubbard type specific gravity bottle, referred to in the previous paper, was not illustrated. I t is now shown on the accompanying drawing No. 2 . C. Free Carbon.-In place of the Knorr extraction

We believe t h a t these results show with sufficient force the necessity of fully taking into account the weight of the individual beets in all studies on composition. CARKEGIE INSTITUTIOX O F WASHIXGTON

METHODS FOR TESTING COAL TAR, AND REFINED TARS, OILS AND PITCHES By S. R. CHURCH Received November 20, 1912

Under this title, the writer has given1 a description of the methods used in our laboratories for testing the raw materials and products of t a r distillation. It was intimated that certain of these tests would undoubtedly be revised from time to time, in response t o suggestions from our own chemists as well as from others engaged in the examination of these materials. It is our present purpose to describe the tests that have been revised since that paper appeared. I t may be well also t o call t o the attention of those interested in testing tars, oils and pitches, a paper by

7hermem e f c r

.

Hook

8.8 S. WJ're

Mica memo'

(C

SPEC/NC GRA V / T Y

aorrLc

EXTRACTOR foff FREE CARBON

apparatus, we have adopted the extractor illustrated in the accompanying drawing No. 2 . This apparatus the writer first saw in use in the Underwriters' Laboratories, Chicago, and it has already been described.= I n it we'use the same filter papers as described in our former article. The filter cup is suspended from two hooks, soldered on to the upper side of the flask cover. ' The advantages of this extractor over the Knorr or Soxhlkt apparatus in making this determination are convenience, compactness, rapidity of operation. E . Viscosity.-The time of flow of IOO cc. a t 60' C. (140' F.) is taken, instead of 2 0 0 cc. as before. The quantity of material placed in the viscosimeter is the same, that is, sufficient to cover the fixed measuring points. PITCH

A/R 5 A TH F O R M EL T / N G POINT T € S 7: Arthur R. Warnes and W. B. Southerton, before the Midland Junior Gas Association,* entitled "Investigations on Coal Tar and Some of I t s Products," and to "Methods for the Examination of Bituminous Road Materials," by PrCvost Hubbard and Charles S. Reeve.3

* THISJOURKAL, 3, 227. J O W . Gas Lzghtine, etc., Feb. 27. 1912. 3 Bull. 38, Office of Public Roads, E. S . Department of Agriculture, July 27, 1911.

C. Melting Point.-(3) For pitches from 7 7 " C. (170' F.) upwards, a n air bath, as shown in the accompanying drawing No. 3, is substituted for the bath of cottonseed oil formerly used. With this oven, shorter hooks are used, so that the pitch cube is suspended on a line running approximately through the center of the observation windows, the thermometer bulb being a t the same level. The temperature of the oven is raised j" C. ( 9 O F.) each minute, as usual, and the temperature recorded by the thermometer a t the instant the pitch drops to the bottom of the oven, is considered the melting point. To make H J . Can-Curr. THISJOGRSAL.

4, So. 5

196

T H E J O C R N A L OF I N D U S T R I A L 4 X D Eh’GI.VEEKISG

results by this method comparable with results obtained in water or oil, 6. j ’ C. ( 1 2 ’ F.) should be added to the observed melting point. E . Evaporation Test.-Reference was made to the use of a circular oven (of the type E. and A., 2073 D) having double walls, circulating fan and self-contained burner. Results obtained with this oven have not been entirely satisfactory, and an ordinary drying oven, lagged with asbestos, as before described, is still used for this determination. C R E 0 S O T E 0 IL-SP

E C 1.4 L TESTS

C. Sulfonation Test.-The method before described, which was a modification of Dean and Bateman’s method,’ has been discarded in favor of a modification described by Bateman’ as follows: Apparatus.-Babcock’s Official Milk Tester, with four bottles. Description.-Ten cc. of the fraction of creosote to be tested are measured into a Babcock milk bottle. To this is added 40 cc. of 37 times normal acid, I O cc. a t a time. The bottle with its contents is shaken for two minutes after each addition of I O cc. of acid. After all the acid has been added, the bottle is kept a t a constant temperature of 98°-~000C. for one hour, during which time it is shaken vigorously every ten minutes. At the end of a n hour the bottle is removed, cooled, and filled to the top of the graduation with ordinary sulfuric acid, and then whirled for five minutes in a Babcock separator. The unsulfonated residue is then read off from the graduations. The reading multiplied by two, gives per cent. by.volume directly. (Each graduation equals one two-hundredths of a cc.) I t is important that the acid be of the proper strength. Fuming sulfuric acid is too strong, and ordinary concentrated acid too weak, a mixture of the two being required to obtain the necessary 80.07 per cent. SO,,which constitutes 37 times normal. A steam bath or steam-jacketed oven should be used for maintaining the bottle a t a temperature of 98’I O O O C. RESEARCH DEPARTMEST BARRETT MANUFACTURINGCo. NEW YORKCITY

THE COMPOSITION OF SALINES IN SILVER PEAK MARSH, NEVADAa By R. B . DOLE, with analyses by WALTON VAN WINKLEAND A. R. .UERZ Received November 12, 1912 DESCRIPTION

Silver Peak Marsh, comprising the lowest part of Clayton Valley, lies in Esmeralda County, Nev., about 2 0 miles west of Goldfield and 2 ; miles southwest of Tonopah. I t is about I O miles long northeast and southwest and about 4 miles wide, its area being about 32 square miles. I t is most readily reached by means of the Silver Peak Railroad, which ‘connects with the Tonopah and Goldfield Railroad a t Blair Junction and runs south to Blair, a small mining town near the western edge of the marsh. The marsh is a salt playa entirely devoid of vegetation and covered for the most part with a white crust of sodium chloride. 1 2

3

U. S. Dept. Agric., Forest Serzue Circular 112. U . S. Dept. Agric., Forest Seraice Circular 1Bl. Published by permisslon of the Director, U. S. Geologlcal Survey.

CHEMISTRY

Mar., 1913

Tracts 3 or 4 acres in extent rising gently I t o 3 feet above the general level appear as rough brown sunbaked patches without a covering of salt. The most noticeable topographic features are Goat and Alcatraz “islands,” two groups of steep limestone hills near the southwest end of the playa. The surface of this alkali flat is usually dry, though it is sometimes covered by a foot or more of water after excessively heavy rainfall. The ground-water plane is, however, always high, and holes a few feet deep anywhere on the flat enter mud, many parts of the marsh being too soft to bear the weight of a horse. The present drainage basin of the valley has an area of 570 square miles. EXPLORATIOX

I n the spring of 1912 fourteen borings 8 to jj feet deep were put down in different parts of the flat by the author for the purpose of exploring the surficial deposits. The upper layer, 5 to I O feet thick, consists of brown mud containing a great quantity of finely crystallized salt. The strong brines in it circulate very slowly as the mud contains a large proportion of clay. The mud along the west shore bears nodules TOTAL SALTSAND POTASSIUM I N BRINESFROH SILVER PEAKMARSH. NEV.. JUNE, 1912

Examinations by 4 . R . Merz. Quantities in grams per 100 cc. unless otherwise designated Potassium expressed as

..............

.............. 6 . . . .....................

11 . . . . . . . . . . . . . . . . . . . . . . .

~

................ ................ ...............

........................

12 13 ........................

14 14

............... ........................ ........................

15.5 21 40 27 35 10 20 27 16 31.5 40 11 17

33.28 33.13 33.75 32.25 32.05 26.56 32.90 32.97 4.15 4.61 3.38 26.82 26.21

0.91 0.77 0.75 0.74 0.55 0.61 0.59 0.64 0.12 0.13 0.11 0.66 0.66

1.74 1.47 1.43 1.41 1.05 1.16 1.12 1.22 0.23 0.21 0.21 1.26 1.26

1.10 3.30 0.93 2.80 0 . 9 0 2.67 0.89 2.76 0.66 2.07 0 . 7 4 2.78 0.71 2.15 0.7’1 2 . 3 4 0.14 3.36 0.16 3.43 0.13 3.80 0.80 3.00 0.79 3.01

30.99

0.69

1.31

0.83

- _ _ - - - -

Average, exclusive of samples from boring No. 13

......................

2.69

of calcareous tufa, which apparently have been formed by deposition of calcium carbonate from the hard waters entering from Mineral Ridge. White tufaceous materials, but no definite beds of salt, underlie the muds in the same locality to a depth of a t least 41 feet. Throughout the rest of the playa east of the “islands” the muds are underlaid by salt clays intermingled with well-defined beds of clay containing crystals of gypsum and beds of crystallized salt containing saturated brine. COMMERCIAL POSSIBILITIES

The records indicate that the northeastern twothirds of the playa is underlain a t a depth of about 2 0 feet by beds j t o I j feet thick of crystallized salt mixed with some clay. Besides these beds practically all other strata to a depth of jo feet contain appreciable proportions of salt that readily dissolves in the waters percolating through them.