Two Convenient Forms of Receiver for Fractional. Distillations under

pine tar oil its characteristic smell was replaced by that ofthe oil. The latter result suggested that mineral oil of the paraffin oil or light engine...
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T H E JO17RS.-1L O F I S D L * S T R I . I L

Sepi.. 191 j EXPERIXESTS

O S

THE

DEODORIZATION

OF

DRYER

GASES

On passing clrler gas through several bottles of n-ater its odor was practically all removed. I n t h e same way t h e odor was destroyed b y mcans of a solu-. tion of calcium hypochlorite (bleaching powder) containing I p a r t of available chlorine in 1000. B y leading t h e gas across pine t a r oil its characteristic smell was replaced b y t h a t of t h e oil. T h e latter result suggested t h a t mineral oil of t h e paraffin oil or light engine oil class might ha\-e sufficient solvent effect on t h e odorous substances t o make their use in a scrubber possihle. T h e effect of mineral oil was not in1-estigated because of lack of time. T h e action of heat on dryer gas was observed using t h e same a p p a r a t u s as for t h e digester gas. I t was in this case necessary t o draw t h e gas through t h e t u b e furnace. T h e results are given below: EFFECTOP HEAT ox T e m p . in furnace

' F. 40

T e m p . of gases a t point where odor was noted

I50

52

7i0

60

72

4.50

86 86 86 84

;SO 6.50 7.50 8.50

ODOR OF DRYER GASES

~ - A T U R E OF

40° F.

350

THE

Sweet, slightly irritating, burned

'g:

Irritating, acrid, slightly burned Very irritating, acrid, burned

Y.50 I 050 I IS0 1250 I150

93 116 I20 116

( S o t quite so irritating or acrid, only slightly

14511

122

j

ITTII

129

, V e r y irritating b u t not quite so burned I

burned Only slightly irritating a u d acrid, no burned odor . -

~

~

Less irritating t h a n a t I550O F Practically no irritatina odor 18511 S o odor of any kind S o sulfur compounds were present in these gases I6.ill

17511

147 154 163

Esperimenl s were made t o ascertain if dilution with air, before leaving t h e stack, could be carried t o such R degree t h a t t h e dryer odor would be unperceptihlc. Gas a n d air were passed separately through in. t u b e : meters and t h e n mixed in a 4 f t . length of and t h e odor noted. T h e d a t a obtained, f o l l o ~ ~ - s : K a t e of flow, cu i t . per tnin. Ilryer pas Air 12

I?

12

Dilution of dryer gas t o air 1 : 20 I ' 60 1 : 400

CESTRALTESTING LABORATORY CITY O F SEW YORK -~

TWO CONVENIENT FORMS O F RECEIVER FOR FRACTIONAL DISTILLATIONS UNDER DIMINISHED PRESSURE By

ODOR

Slightly burned

[

nc :leaned. X concrete floor with n freqLlLed t a r coat or one of asphalt would be a n e n t on the IT-ood. great i m p l . In conclusion, we n-ish t o acknowledge our indebtedness t o N r . Osborn for his invaluable suggestions, advice a n d inspiring interest in this investigation. We also wish t o t h a n k 11r. Thomas D. Banks, Superintendent of t h e Garbage Reduction Plant of Columbus, 0.. for valuable assistance. a n d hIr. George n'oocl. Assistant Engineer in t h e Department of Street Cleaning of this city. for aid in carrying out t h e experimental work a n d for t h e sketches accompanying this paper. T o N r . Charles Crew, of this laboratory, n-e are grateful for t h e performance of analytical determinations.

Intensity of dryer gas odor Very strong Strong Distinct

T h e results s h o ~t h a t no reasonable a m o u n t of dilution with air is effectiye in causing t h e dryer gas odor t o become negligible. O D O R S . i R I S I S - G F R O M P E R X E A T I O S OF T H E R E D U C T I O S

TVORKS STXL-CTLTKE TVITH L I Q U I D S . E T C .

Brief mention m a y be made of t h e odors resulting iron: t h e permeation of the buildings of reduction works x i t h liquids. etc. The wind passing over t h e plant may in this w a y t a k e u p considerable odor, even n-hen n o garbage is present or in process. T o eliminate this source of trouble garbage plants should be of t h e most sanitary construction t o permit n-ashing and prevent material lodging in crevices. T h e cement of concrete floors is readily attacked b y t h e stick liquor a n d garbage, a n d wooden floors are sometimes p u t down. As m a y be easily understood, these soon become of a 7-ery objectionable nature a n d can-

TAYLOR BOGEKT Received June 16, 1915

h1ARSTOS

Having had occasion recently t o carry out many fractional distillations of t w o or three liters of liquid a t a t i m e , under reduced pressure, t h e writer could not find upon t h e market a n y form of receiver which would permit t h e taking of a large number of fractions, of varying volume. without interruption of t h e distillation. T o meet this need, t h e forms described below were del-ised ar,d have proven very serviceable. Possibly, other chemists confronted with similar problems, also m a y find t h e m of use. .APP.AR.ATUS I is constructed entirely of glass resistant t o t h e action of chemicals. well tempered, and sufficiently strong t o withstand t h e full atmospheric pressure. Ordinarily, t h e connections with t h e end of the condenser (or distilling t u b e ) , a n d v i t h t h e lower vessel into r h i c h t h e fractions are t o be drawn. will be made xvith perforated rubber stoppers; b u t , if desired, t h e y can of course be made with ground glass joints. I n detail, t h e a p p a r a t u s consists of a cylindrical receiving chamber, d , graduated in cc. a n d with a funnel stem through which the distillate collected in -4 m a y be removed a t will b y opening the plain cock F . On one side of this receiving chamber, near the ' t o p , is t h e U Frc. I opening B , for t h e end of t h e condenser F r o m t h e t o p of t h e receir ing chamher . I , the t u b e C passes t o t h e p u m p P a n d t o the outer jacket E of t h e funnel stem. On this t u b e C, there is a plam cock a t H . a n d a 3-way cock with offset ports a t D . By turning this 3-way cock 9 0 ° , connection is established b y means of a perforation in t h e stem of t h e cock, between t h e

7 86

T H E J O U R N A L OF I N D U S T R I A L A N D E N G I N E E R I N G C H E M I S T R Y

outer air a n d , through t h e outer jacket E , with t h e lower receiving vessel. I n t h i s w a y , atmospheric pressure can be restored t o t h e lower vessel without i n a n y way affecting t h e v a c u u m t h r o u g h o u t t h e rest of t h e distilling system. T h e lower vessel can t h e n b e removed, or i t s contents drawn off, as t h e case m a y be. T h e effect of t h i s arrangement of t h e 3-way cock, therefore, is t h a t i n one position only does i t make connection between t h e p u m p a n d t h e lower receiver; a n d in one position only, between t h e l a t t e r a n d t h e outer air. I n all other positions, it merely seals t h e t u b e at D. T h e manipulations are as follows: T h e e n d of t h e condenser (or distilling t u b e ) is inserted through a rubber stopper i n B , a suitable receiving vessel is a t t a c h e d t o t h e funnel s t e m , also b y means of a rubber stopper, t h e p u m p is connected at P , a n d t h e entire a p p a r a t u s evacuated, t h e 'stopcock F being closed, t h e stopcock H open, a n d t h e 3way cock D being t u r n e d so a s t o establish connection between t h e p u m p a n d , through t h e outer jacket of t h e funnel stem! t h e lower receiving vessel. When t h e first fraction has been collected i n d , a n d i t s volume read, i t can be r u n i n t o t h e lower receiving vessel simply b y opening t h e stopcock F . If t h e first (or a n y subsequent fraction) proves greater t h a n t h e graduated capacity of A , t h e l a t t e r can be filled a n d drawn off a s m a n y times as m a y be necessary; or, if preferred, t h e stopcock F m a y be left open during t h e taking of t h e fraction, allowing t h e distill a t e t o r u n right on through A F i n t o t h e lower receiver. After t h e first fraction has all been r u n into t h e lower receiver: t h e stopcocks F a n d H are closed, a n d t h e 3-way cock D t u r n e d so as t o close t h e connection between t h e lower receiver a n d t h e FIG.I1 p u m p a n d open t h a t t o t h e outer air. This allows t h e air t o flow into t h e lower receiver, a n d t h e l a t t e r can t h e n be removed, emptied Meanwhile, a n d replaced, or a new one a t t a c h e d . t h e distillation has not been interrupted in a n y way nor t h e v a c u u m affected, a n d t h e distillate is accumulating i n A . When t h e new receiver is connected below, it is first evacuated b y turning back t h e 3-way cock t o its original position, after which stopcock H c a n be opened again, a n d t h e fraction accumulated in il drawn off as before. If t h e new receiver a t t a c h e d below is large in comparison with t h e capacity of t h e p u m p , a n d t h e operator SUSpects t h a t ' l e a k s may be altering t h e pressure in t h e distilling system (since t h e p u m p is cut off at H ) , he can test t h i s for himself a t a n y moment, without losing a n y of t h e evacuation of t h e lower receiver already gained, b y turning t h e 3-way cock so as t o seal t h e t u b e at D , waiting a moment until t h e pressure gauge has fallen again t o t h e initial pressure i n t h e distilling sys-

,'

1

,

Vol. 7, NO.9

t e m , a n d t h e n slowly opening t h e stopcock H . Any loss of pressure will t h e n be immediately apparent. I n case t h e r e h a v e been leaks a n d t h e pressure has changed, stopcock H is left open until t h e desired .evacuation is restored, after which it is closed and t h e exhaustion of t h e lower receiver resumed. W i t h this a p p a r a t u s , a n y number of fractions m a y b e t a k e n , of a n y desired volume. B y using a separat o r y funnel, or similar vessel, as t h e lower receiver, t h e fractions can be drawn off a t will without removing i t at all. T h e writer has found 2 5 0 cc. a very convenient size for t h e receiver. An a p p a r a t u s of this capacity is a b o u t 1 5 in. high over all, a n d t h e diameter of A is approximately z i n . , so t h a t it is easily held b y an ordinary Liebig condenser clamp. A P P A R A T U S I 1 is a somewhat simpler form, for use in laboratories which, like t h a t of t h e writer, happen t o be equipped with more t h a n one p u m p . T h e 3 way cock D may be set as indicated either in Fig. I or Fig. 11. I n this t y p e of a p p a r a t u s , after t h e removal of t h e first fraction, t h e lower receiver is evacuated b y connecting t h e auxiliary p u m p with t h e hollow s t e m of t h e 3-way cock, after which it is t h r o w n again into t h e distilling system b y turning t h e 3-way cock back t o its original position. Both forms of t h e receiver are manufactured b y t h e Emil Greiner Co., j j F u l t o n S t . , Xew York, N.Y . COLUMBIA UNIVERSITY, NEW PORK CITY

A SIMPLE AUTOMATIC-ZERO BURETTE By A. T. MERTES Received May 7 , 1915

Most automatic-zero burettes discharge t h e overflow f r o m t h e b u r e t t e into a receptacle separate from t h e main reservoir, a n d t h i s excess is either t h r o w n away or is poured back into t h e main supply. For solutions t h a t have been carefully standardized, this practice is inconvenient a n d m a y be a source of error. T h e accompanying drawing shows a n automaticzero b u r e t t e t h a t discharges t h e overflow back into t h e main reservoir. I t has t h e a d v a n t a g e t h a t i t m a y be protected from t h e carbon dioxide of t h e air, a n d hence is especially a d a p t e d for use with s t a n d a r d acid a n d alkali solutions. I t consists of a large Woulfe bottle having a b u r e t t e a t t a c h e d t o i t s neck b y a clamp. T h e b u r e t t e has a side aperture which connects, b y means of rubber t u b i n g , t o a goose-neck-shaped glass tubing, A , a b o u t 5 m m . in bore. This is b e n t in such manner t h a t t h e ring of t h e pinch clamp encircles i t a n d is t h u s prevented from rotating. Half way between t h e b u r e t t e a n d where t h e connection tube, A bends'down i n t o t h e liottle a n inner t u b e , B , is fused. This inner t u b e is about I m m . i n bore. It connects with a short a r m , C, forming a T with t h e main tube. T h e lower ext r e m i t y of t h e inner t u b e B is fused t o t h e outer t u b e a t D i n such a way t h a t it opens outside this t u b e . This prevents air bubbles t h a t m a y be drawn through t h e inner t u b e from rising in t h e main supply tube. T h e t o p of t h e b u r e t t e is closed b y a cork, E , through