Research in Organometallic Problems U
W. L. GILLIL.IND,
UniFersity of Jlaine, Orono, 3Iaine
T
HE accompanying photographs show research equipment
Special precautions are taken to avoid contact with air, which would result in autoxidation, and to secure quantitative reaction studies. The automatic generation of carbon monoxide is especially convenient for metal carbonyl preparation, iT-hile nitric oxide is used in making nitrosyl derivatives and in other reactions.
devised and used a t the University of Naine for research in organometallic problems. These studies involve preparing and handling the alkyl derivatives of zinc, phoqphoruq, mercury, and arsenic, a3 well as nickel carbonyl and various Grignard reagents.
UPPER
ACID FEEDI S T O LEFT. DETAILOF AUTOMATICCARBON MONOXIDE GENER.4TOR; FORMIC FLASKS ON RIGHT; PURIFYING TOWERS ASD ESCAPE VALVEON LEFT
GESERATISG
VIEW OF Gas GESERATORS;CARBOSMOSOXIDEON LEFT, SITRIC OXIDE ox RIGHT, UPPER RIGHT. GENERAL METERBATHIS FOREGROUSD
OF GAS-GEKER.~TING APPARATUSAT CPPERRIGHT,SHOWING DISPLACEMEST METERS LOWERLEFT. EXTESSIOS FOR MEASURING Gas
LOWERRIGHT. EXTE~WIOK OF APPARATUSAT LOWERLEFT, SHOWING (RIGHT)MERCURY COMPRESSIOSPUMPTO REACH3 ATMOSPHERES’ PRESSURE AND (LEFT) MERCURY FALL PUMP. Y-ICKEL C . 4 R B O S Y L IS IX PREPARATIOX (LIQUID IS BULBIX CENTER) 474
AUGUST 15, 1940
ANALYTICAL EDITION
PPPER LEFT. A 250ML. REACTIOS FLASK WITH SPECIALSTOPCOCK SYSTEM TO ALLOW ALL BORESA X D COSSECTIOSS TO BE SWEPT WITH ISERT GAS BEFORE .kDl!ITTING
ACTIVE LIQUID,
UPPERCESTEX. PREPRATIO^^ O F T R I M E T H Y L P H O s P H I pi E : 470 GRAMSOF ZIKC M E T H Y L( R I G H T ) ABOUTTO BE ADDED TO R E ~ C T I OFLASK. S XOTE A4RR.iNGEJIEST5 FOR SWEEPISG
UPPER RIGHT. ZEREWITEXOFFSETUP FOR ACTIVE HYDROGES ASD REACTIVECARB O N Y L D E T E R M I S ATIOS,
USISG
ETHYI,
ETHER .is SOLVEST LEFTCESTER. PREP.: I N COLUMSOUTFIT. BEENSIPHOSEDTO A I WHICH RIGHT CESTER. PH ACTIOS OF NITRIC LOJTERRIGHT. DET SHOWISG P~RIFYING PORS, AND A M T h e p h o t o g r a p h (right center) of JTL . Gilliland was t a k e n in a d a r k e n e d room b y t h e light of t h e reaction. T h e vapors of nickel carbonyl give a slight initial reaction with p u r e nitric oxide. After t h i s is complete, t h e resulting mixture will autoxidize o n c o n t a c t with air,, producing voluminous white f u m e s of nickel n i t r i t e : or i t will Ignite rvirh a hriiliant flash upon being
lighted. T h i s Rash c1ni.s not r ~ p r e s e n toxidation b y air b u t a reaction h e t u r e n t h e cunatituents of t h e gas mixturf,, and'can be produced in t h e absence of a ~ r . T h i s is t h e first picture ever t a k e n , using as a spurce of light this reartion, which u-88 discovered a year ago a n d reported a t t h e Boston meeting of t h e
AXERICAXCHEMICIL SOCIETY.
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