Quantitative Analysis with X-Ray Spectrometer

Aldehyde efficiency. Mole percentage conversion to butadiene. 1 Inmate efficiency. Alcohol efficiency percentage. Aldehyde efficiency percentage. Prob...
0 downloads 0 Views 507KB Size
OCTOBER 1947

773 t,he gases f l o through ~ ~t three-Lv This stopcock normally conne with the gas-product collecting tank, but' it can also he used for diverting the gas stream a t an?. instant into a gas-sampling bottle so that t h r catalyst performaric~ran tie checked at, any time. .ifter fluwing through thr thrrr-n-a?-~topeock. the gas is conducted to an automatic nierrur!. , allows tbe gas to flon. prrssurrregulator, t 7 that from the system at atmospheric pressure into an evacuated tank, \'. The gaaes, as they are CUILected in t h r tank, are sampled by means of a Toepler pump and analyzed. T h r tank is tht'ii brought up to atmospheric pressure by means of nitrogen from cylinder Yand is purged for sonic' time into a hood before rc~-evaciiatinghv i r e i n h

niaiutained a t t h r desired trriiperature by mea~isi i i furiiace E , The t,eniperature of the furnace i controlled b y means of a microswitch operated in conjunction \ t h a mercury relay. The back EXPERIXIENTAL RESULTS pressure caused by material flax across the unit is indicated by manonicter F. Directional f l o ~arrows on the line connecting l i t d t i frorn forty runs of 8 h(JUI'S' tluratioii u s t d t o st:rrldF with t,he catalyst tuhtt are in both directions, since the line serves ardize the first catalyst testing unit aria shown in Table I. two purposes. First, tht, hac*kpressure from the unit is exerted I n the calculation of the ultimate efficiency prrccJritage, the through the line to F during operation, and secondly, the line varries nitrogen gas tliat it; uwd t o purge t h e unit before and molrs of rtAaetc.d acrtaldt.2iydr arcs divided by 0.92 because, in aftrr each test run. TtiP iiitrogrri is by-passed a c r o . manometer ~ plant oprration, rthanol is convrrtrti t o acetaldehyde by a sepaI ) through this dual-purposc linr to the reactor. ratr rcwcntion n-hivh is approximately 9 2 5 eficirrit. The ulThe converter-makc, flo\vs from the reactor in furriaw E into tiniatcs c.firit.nc*y is thercJforr rsprtAsseci 011 thr h I hr sPparation unit at point G. Here the converter-makr rnters R cooling coil immerstd in iri. \rater that ip circulatrd by a ('enrrifugal pump, H , from t h e icr watrr reservoir, I . -111 thr conskiisable materials i'riini t hr. converter are coridrrised iri this coil n u d flow into an unpackrtl sertion of the separation column at point J . :\t thi.: point t h t . liquid materials flon- down into the \vhiir thr uncondenscd gases flow up into iiwtionating column, h-, t l l t l lvater scrubher, L . l\'attir is admitted t o I, by mrans of an ,i,ific~ feeder, .If,oprrattd b y maintaining a caonatarit differential prtwurc across the foedt~i,orifice t)y means of riitrogrn pressure iri cylinder S,whirti is cwntrcilled hy niercurv bubbler 0 and dif:'rwntial pressure niaiio~nrtrrP. -1thrrniomcbter placrd a t the ve.5 to sho\v that thr butadiene fractionated out of ction. The hutadienr and 0th yaws f l o i ~fivm the t o p of the water icruhhrr into a hydroq-laminr hydwchloride iolrition scrubher, 0. From 0 thcs gas f l o w through drying :uhe R and then over a iiiei,c.ury-fillrd mariometcr, AS. which s h o w r t i e pr.(,ssurc in t h c *ystrm at that point. From thv riianomt~tc~r q

Quantitative Analysis with the X-Ray Spectrometer JOHA C. It.

thv following variables have been considered: (1) pressurr, (2: time, (3) voltage, (4) recording paper, ( 5 ) electrolyte, (6) drvcaloping agt,nt, and ( 7 ) interfering ions. PRESSURE

Sufficknt pressure must be obtained for intimate contact; howw r r , too much pressure could dt+troy the film or possibly seal over