M a r . , 1919
T H E J O U R N A L OF I N D U S T R I A L A N D ENGINEERING C H E M I S T R Y
warfare service, military training of Gas Defense Division officers located in New York City and vicinity, and training of boat crews carrying offensive gas supplies. This organization spt?nt a great amount of time doing all kinds of vigorous physical work and exercise under simulated field conditions while wearing gas masks. They rendered most valuable service in pointing out weaknesses of design as developments took place, and especially those uncomfortable features of the masks which were only apparent through long wear. During the course of its activities it built a complete trench system in the Pennsylvania Railroad yards, with an elaborate dugout which matched any of the famous German quarters on the western front. I t carried on a large-scale field test at the Lakehurst Proving Grounds on the A. T. and K. T. masks in which a gas attack under large scale and high concentration conditions was realized. CONCLUSION
As to the production record of the Gas Defense Division, it is interesting to note without further comment the following extract from the War Department: A mistaken impression that delayed production compelled American soldiers to depend on British and French masks has been current in this country. This theory is entirely unfounded. * * * I t may be stated authoritatively that prior to the July counteroffensive against Germany, an American gas mask had been shipped across the Atlantic for every American soldier in France. There is in addition an ample military reserve. * * * The American attacking forces are protected against gas by masks which actual field tests prove give twenty times the protection afforded by German gas masks. The work of this division may be summed up in the statement that American soldiers were provided with equipment which neutralized the best efforts of German chemical knowledge as evidenced by the offensive methods and materials employed. This was accomplished by an organization located three thousand miles from the point of use and source of practical field information. This organization grew from the acorn stage to the great oak in mushroom time. Its growth was due to the patriotic enthusiasm of its personnel: officers, enlisted men, civilian workers, and clerical force. GAS DEFENSEDIVISION CHEMICAL WARFARE SERVICE, U. S. A. 19 WEST 44TH ST.,NEWY O R K C I T Y
TESTING NATURAL GAS FOR GASOLINE CONTENT’ B y G. G. OBERFELL,
s. D. SHINKLE AND S.B. h l E S E R V E
Received January 4, 1919
I n a previous article2 one of t h e writers had occasion t o describe a method for testing natural gas for gasoline content. T h e method described in t h a t article was intended especially for testing casing-head gas which is generally rich in gasoline content. T h a t method consisted in extracting t h e gasoline vapors from t h e gas with oil as t h e absorbing medium and recovering t h e gasoline b y distillation. The method described i n this article employs t h e use of a solid absorbing medium such as charcoal and is applicable t o both lean and rich natural gas. DESCRIPTION O F ABSORBER
The series tube absorber shown in Fig. I is preferably made of aluminum and consists of 4 tubes, B B, fastened rigidly t o t h e supporting plates, C C. The tubes are each 2 2 cm. long and have a n internal diameter of z cm. Each t u b e has a removable per1 Published by permission of the Director of t h e Chemical Warfa% Service. THIS, JOURNAL, 10 (1918), 211.
I97
forated disc, D D, 3 cm. from t h e b o t t o p , which is held in place b y a hollow cylinder fastened t o the disc and resting against a plate, E, at the bottom of t h e tubes. T h e absorption tubes are connected in series by means of tubes attached t o t h e bottom plate E, and t o p plate, F. The plates are held in place b y means of thumbscrews, GG. The absorber is made airtight by means of rubber gaskets, HH, fitting closely on t h e plates a t each end. M E T H O D OF O P E R A T I O N
( I ) FILLING THE TUBES-charcoal or other material of high absorption value should be used. The plate F is removed and each t u b e is filled with t h e absorbent t o within about 3 cm. from t h e top. T h e height of t h e absorbent i n each t u b e is then about 1 5 cm. After t h e tubes are filled t h e plate F is replaced in such a manner as t o connect all 4 tubes i n series, providing this arrangement is desired. B y proper arrangement of t h e plate, 2 of t h e tubes will be i n series ready for test while t h e other z will be by-passed, By t h e latter arrangement duplicate tests may be made with one filling. ( 2 ) A R R A N G E M E N T O F APPARATUS-The following arrangement of - t h e apparatus has been used in tests conducted i n t h e laboratory: Gas + flow meter + calcium chloride d r y meter manometer * absorption tubes --+ manometer --+ suction (when needed). T h e flow meter was used t o control t h e r a t e of gas flow. An orifice flow meter has been used and found satisfactory for rough determination of gravity of t h e metered gas, t h e determination being made as follows: The flow meter is checked against t h e d r y meter, t h e time being recorded for delivery of a certain volume of air, V, with a constant differential height, H, on t h e manometer of t h e flow meter. T o determine t h e specific gravity of t h e gas t h e flow meter differential is maintained a t t h e height H and volume V of gas passed through it. T h e time for t h e gas flow is recorded. The specific gravity of t h e gas is calculated as follows: (Time for gas flow)2 Specific gravity of gas = (Time for air The calcium chloride was used t o prevent possible deterioration of t h e absorbent due t o moisture. Also, during distillation moisture is liable t o condense i n t h e receiving vessel with t h e other vapors absorbed by t h e charcoal and thereby cause difficulty in gravity determinations. The open manometers were placed before and after t h e absorption tubes in order t o get t h e pressure drop through t h e absorber. T h e d r y meter was arranged with a manometer so t h a t t h e pressure of t h e metered gas could be obtained. The temperature of t h e gas was taken b y means of 4 thermometer placed a t t h e inlet t o t h e dry meter. uction was used i n cases where t h e gas pressure was insufficient t o give t h e required volume of gas.
*
*
9
(3) M E T H O D O F D I S T I L L A T I O N A N D G R A V I T
xATIoh’s-The
distillation apparatus and t
a
T H E JOURNAL OF INDUSTRIAL A N D ENGINEERING CHEMISTRY
198
1701.
11,
No. 3
SECTIONTHRU /l-A JtKW. $''NIPAS
70 BE. THILCaPED F11 ONE €No. OTHLP 6ND 7-0 TWO5 CLU00)tE TVBlNa.
2 REQUIRED.
I
PERFORATED
I
t
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( 2 0 PEAtWetaTt0N.r
I~M~.DIFIME~E 1R H E L D IN PLRCI? BY TWIN MetflL CTLlnoEa PLAT6 CT CYLIflDEIL SOLD B R L D
BOTTOM PLBTL.
SECTION FIG. S SERIES TUBEA B S O R B ~ R
for the determination of t h e gravity of the distillate are essentially t h e same as described in t h e previous article.' T h e distillations were made after adding 600 cc. of straw oil (petroleum distillate about 30' Be.) t o !he charcoal in t h e distilling flask. Distillation tests were also made in which zoo cc. of glycerin were added t o the charcoal which was placed in a 500 cc. Pyrex flask. 1
LOC. Clt.
Several methods of distillation have been tried. Direct heating with the flame impinging against t h e flask was unsatisfactory for two reasons: first, i t was difficult t o drive off all the vapors from the absorbing medium, a n d second, in tests of natural gas a large quantity of t h e less readily condensable vapors are absorbed and cause large distillation losses by carrying over some of t h e more readily condensable vapors. Oil baths and also sand baths were found t o be unsatisfactory because the temperat u r e was not sufficient t o satisfactorily drive o f t h e absorbed vapors. Steam distillation introduced difficulties in gravity determinations and gave low yields. The most satisfactory methods so far tried are distilling in the presence of straw oil or in t h e presence of glycerin. T h e advantage of using glycerin is twofold: first, t h e chircoal can be regenerated easily b y washing with water, and second, if t h e distillate were contaminated with glycerin i t would be removed b y washing t h e distillate with water. If t h e distillate were w n t a m i n a t e d with oil, an error would be introduced in calculating t h e yields of gasoline, since separation of oil and gasoline is not practical with such a small
Mar., 1919
T H E J O LrRnTAL O F I N D U S T R I A L A N D E h T G I N E E R I N G C H E M I ~ R P I '
Pf AN FIG.2-EoUIPMENT Compartment A holds dry test meter Compartment B holds tube absorber Compartment C holds orifice meter Compartments D (9) hold receptacles for samples
volume of test. Extensive termine how and thereby
gasoline
as
would
be obtained in a
tests have not been carried out t o de many times a charcoal can be regenerated continue t o be of value for absorption
RECORD CARDOR TESTS Yield pts /IO00 cu. f t . (60' F. and 30 in. Hg) = Distillate cc. X 1000 Cu. ft. gas used X factor X 473 1 Locality: Homer, Ohio 2 Date of test: November 15, 1918 3 Source of g a s : inlet t o gasoline plant 4 Test began: 10.07 AX. 5 Test finished: 10.52 A . M . 6 Test duration, min.: 45 7 Barometer, in. of Hg.: 29.13 8 Pressure of meter. in. of HE: 1.13 9 Total gas pressure in. of Hi:30.26 10 Temperature of gals deg. F.: 64 11 Conversion factor, 60' F. and 30 in. Hg : 1.000 12 Meter reading, finish, cu. f t . : 935.70 13 Meter reading, start, cu. ft.: 925.70 14 Meter readinn difference, cu. ft.: 10 15 Gas rate c u . f t . per hr.: 15 16 Gas used cu. f t . 60' F. and 30 in. Hg: 10.00 17 Absorbeit. kind! charcoal 18 absorbent^ nreliminarv treatment' none 19 20 21 22 23 24 Distillate cc. 60' F.: 9.76 25 Distillate: sp.'gr., 60' F./6q0 F.: 0.6292 equals 92.5 BC. 26 Distillate. color: water white 27 Distillate' odor: ethereal 28 Distillate; Der cent H ~ S O absorotion: I less than 1 Der cent 29 Distillate; 'yields pts.71000 cu. i t . gas (uncorrectGd): 2.06 30 Distillate, yields pts./1000~cu. ft. gas (60' F. and 30 in. H g ) : 206 31 Distillate, yields pals./miIlion cu. it. gas (uncorrected) : 258 32 Distillate, yields gals./million cu. it. (60' F. and 30 in. Hg): 258 REM.4RKS : TEST BY.. CHECK BY
............ .............
tests of this nature. This would of course depend upon several factors, chief of which is the quality of the charcoal. However, charcoal which had been regenerated three times gave satisfactory results. The method of regeneration used is as follows: The glycerin is decanted off the charcoal. The
CASE FOR F i E L D TESTS Shellac all parts Equip lid with hinges and hooks Sre sketch for arrangement of strap handle
charcoal is then placed on a Buchner funnel and washed with about 500 cc. of water. The water is added t o the decanted glycerin a n d filtered. T h e filtrate is evaporated until all the water has been removed. T h e glycerin so recovered is ready t o be used over again. The charcoal is left on t h e Buchner funnel and a stream of t a p water is run through i t for 2 hrs. A t the end of this period the charcoal is placed in a n oven and dried for several hours at 140' C. (usually over night). (4) D A T A RECORDED-The preceding form has been used €or recording d a t a of tests. RESULTS
Tests were made of natural gas for gasoline content. I n Table I are presented the results of tests with t h e series tube absorber using charcoal as the absorbing medium and results of comparative tests with t h e portable oil absorber.' These results show t h a t t h e two methods compare favorably, the yield by t h e portable oil absorber being about 6 per cent low. Comparison is also made with plant production for t h e days during which the tests were made. TABLEI-COMPARISON OF OIL ABSORPTIONMETHODA N D CHARCOAL ABSORPTION
METHQDIN TESTSOF NATURAL GASFOR GASOLINE CONTBNT OIL ABSORPTION METHOD ABSORPTION CHARCOAL Portable Plant
Number of tests averaged..
METHOD Absorber 4 2
.............
Source of gas.. ........................ Gasoline recovered, Be. 60' F./60° F.. ... Gasoline yield, Pts./M. cu. f t . gas.. . . . . . . Gasoline yield, per cent2..
...............
Yield 2 days' product Inlet t o gasoline plant 90.2 90.4 88.6 1.76 1.65 1.55 100.0 93.8 88.1
"Extraction of Gasoline from Natural Gas by Absorption Methods," by G. A. Burrell, P. M. Biddison and G. G. Oberfell, Bureau of Mines Bulletin, 120 (1917). 2 Calculated from charcoal absorption method as giving 100 per cent yield. 1
T H E J O U R N A L OF I N D U S T R I A L A N D ENGINEERING C H E M I S T R Y
200
E Q U I P M E N T CASE FOR FIELD TESTS
The equipment as shown in Fig. a is intended for testing gas wells f0.r flow of gas and for making the absorption tests of t h e gas for gasoline. The receptacle E may serve either as a sample container or as a n absorber. After absorption of gasoline vapors from a measured volume of natural gas in t h e field t h e charcoal containing t h e absorbed vapors is sent t o the laboratory for distillation t o determine t h e gasoline content of t h e gas as described above.
Vol.
11,
No. 3
subsequently recovering t h e gasoline b y distillation. The method possesses several distinct advantages: I-The apparatus is simple t o construct, easy to operate, and is readily portable. a-The method gives information both as t o yield and gravity of gasoline and offers possibility of construction of an apparatus for determination of t h e vapor tension of t h e gasoline. This work was started under the direction of t h e Bureau of Mines and was continued under t h e Research Division of t h e Chemical Warfare Service.
SUMMARY
GASMASKRESEARCH SECTION RESEARCH DIVISION CHBMICAL WARFARE SERVICE,IT.S. A. AMERICAN UNIVERSITY EXPERIMENT STATION WASHINGTON, D. C.
The principle of this method for testing natural gas for gasoline content consists in absorbing t h e vapors in a solid absorbing medium such as charcoal, and
I
ORIGINAL PAPERS METHODS OF VARNISH ANALYSIS
PREPARATION O F T H E VARNISHES
B y W. T. PEARCE
Received June 15, 1918 INTRODUCTION
At t h e present time t h e status of varnish analysis is not good. It is generally agreed t h a t t h e following of a n y of t h e published methods will give results t h a t vary in t h e hands of different analysts and t h a t do not represent either t h e quantities or qualities of t h e materials used. The consensus of opinion among varnish chemists is t h a t a complete chemical analysis would reveal little as t o t h e relative merits of' competitive grades of varnishes. This opinion needs t o be fully investigated. The literature on varnish materials clearly indicates t h e need of more work on t h e physical and chemical properties of resins and t h e need of research on t h e analysis of oil mixtures. Varnish analysis t o date seems t o consist chiefly of t h e following determinations : thinners (turpentine, benzine, etc.), resins, rosin, oil, and drier. Tests for factory control include specific gravity, viscosity, hardness of film, drying test, and panel test. I n outlining t h e work t o be carried out in this laboratory, we thought it wise t o make up a few varnishes, differing widely in composition in order t o investigate t h e accuracy of existing methods. Along with this we have studied t h e problem of identifying and estimating t h e different oils used. ---RESINS-Estimated
No.
........................
2
15.8
Found 13.82 (D) 2 0 . 0 4 (T) 15.65 (B)
3..............................
5..
6..
............................ .............................
17.1
13.0
-ROSIN--Estimated
................................
40.35 19
------OIL---
---'rHINNERS--
Estimated
Found
Estimated
--BENZINE-Found Estimated Found
36.9
8.01
?!I,}
34.3
iZ:hf)(D)
57.7
56.93
48'3
~
34.5 ~
33.0 ~
46.4
$:3 :1?:.}3 (D)(B)
85
Ej:ii)(B)
80
77.66 (B)
80
:z:ttf(B)
40
39.01
17.47 17.23b)
:::%I
;!:E
(D)
1'23
1 15
20
Found
4 :;)
20
..............................
The linseed oil was kept at zooo C. for a hrs. with oxide of lead added. The constituents of t h e varnishes used for the analyses reported in this paper are: No. a-Sierra Leone copal, rosin (colophony), linseed Chinawood oil, turpentine, and drier; No. 3-rosin, oil, drier, and turpentine; No. 5-East India copal (white), rosin, menhaden, Chinawood and linseed oils, drier, benzine, and turpentine; No. 6-East India copal (white), soy bean, Chinawood and linseed oils, drier, turpentine, and benzine; K-Sierra Leone copal and
4.54
R ....................... K ................................
MATERIALS U S E D
4 0 . 9 8 (D) 34.81 (S) 3 3 . 5 6 (B)
Q ........................
M
About 2 0 per cent more of t h e resin was taken t h a n we wished t o use. When it seemed t o have cooked enough we weighed t h e kettle and contents t o get t h e weight of t h e resin left. This loss in weight was between 2 0 and 30 per cent, except in t h e cases where only rosin was used, and then it was nearly 7 per cent. The hot boiled oil (or oils) was then added and t h e kettle and contents weighed t o get t h e weight of oil added. This mixture was cooked in the usual way. A kettle of t h e same dimensions containing a volume of oil equal t o t h a t in t h e varnish was heated t h e same length of time at t h e same temperature t o give t h e loss in weight of the oil in t h e varnish. I n this way we were able t o calculate t o within one per cent of t h e oil and resin in t h e material. The loss in weight of t h e oils was between I and 2 per cent.
20.60 20.53
(B)
:$:::)
38.67 (B)
59.7
21.52 (B)
81
61.33 (B) 78.48 (B)
~
13.8 ~
13.93
f
~
