Escambia's new research center, situated on a 45 acre tract, is a two story, steel-frame, brick faced structure. The building has 55,000 square feet of floor space. It has 12.000 square feet of bench laboratory space. Each of

the 13 four-man laboratories is equipped with hot and cold water, steam, compressed air, vacuum, electricity, and in some cases, nitrogen. Two are temperature and humidity controlled. Laboratories and offices are air-conditioned

Much Research Needed When Entering N e w Areas

Research has played an important role in Escambia Chemical Corpora­tion's entry into the plastics and petro­chemical fields. To carry out this re­search, Escambia established a research center at Wilton, Conn. This new facility will be used exclusively for re­search on chemicals. Included are derivative!! based on acetylene, propy­lene, and isobutylene; pharmaceutical intermediates, synthetic organic chemi­cals, and new chemistry of nitrogen. Special emphasis is placed on vinyl chloride polymers and copolymers, acrylics and their intermediates, methyl methacrylate, and methacrylic acid.

The center, designed in the shape of a rough cross, has one wing directed to bench laboratory work, one to pilot plant activities, one to plastic technical service work, and one to administra­tive functions. Extra space is avail­able for expansion. At present the per­sonnel total approximately 50, half of whom are professional personnel. Eventually the center will have over 100 people.

Escambia was organized in 1954 by United Gas Corporation and Electric Bond and Share Company. In 1956

the first units of a plant were com­pleted in Pensacola, Florida, and com­mercial production of ammonia, nitric acid, and nitrogen fertilizer materials began. Early in 1957 a second plant which produces polyvinyl chloride res­ins was completed. The following year a methanol plant was placed in com­mercial production. A semi-works plant for methacrylic acid based on a process developed by the Escambia re­search group is now in operation.

Analytical problems are submitted to a chemical analysis group or an instru­ment analysis group, depending upon the nature of the problem. Instruments available for analyses include a mass spectrometer; recording ultraviolet, in­frared and visible spectrophotometers ; and a variety of gas chromatography analyzers. Several of the latter were designed and built in the laboratory for anah'ses for which standard commer­cial instruments are not applicable. The chemical analytical facilities in­clude equipment for functional group analysis, elemental organic microanaly­sis, and polarography. Conventional techniques have been modified by the use of automatic titrators and combus­tion equipment.

To meet the need for a rapid analysis of trace components in vinyl chloride monomer, the gas chromatographic analyzer shown was constructed. Its l imit of detectability for trace impuri­ties is on the order of 10 parts per bil­l ion. A two-cc. sample of liquid is run through a one-half inch column and impurit ies are collected in the cold trap. The operator is turning the valve which routes collected impuri­ties into a one-quarter inch analytical column

VOL. 32, NO. 10, SEPTEMBER 1960 · 1 1 9 A

LABORATORY OF THE MONTH

Lab of Month

This specially designed Karl Fischer apparatus is used for the determina­tion of water in a variety of reaction mixtures. The introduction of re­agents and drainage of the flask are accomplished by means of sealed-in capillary side-arms. Dry nitrogen is used to pump the reagent solutions and the apparatus is completely pro­tected from atmospheric moisture

Complete titration curves are obtained automatically with the recording titrator shown. It is used primarily for the nonaqueous titration of mixtures of strong and weak acids such as solutions containing nitric and acetic acids used in Escambia's methacrylic acid process. In the application shown, however, the instrument has been adapted to auto­matically titrate fractions from a chromatographic column. This is accomplished with a switch actuated by movement of the recorder pen and permits titration of the solution only when the pH is below a preset value. Ha If-titration curves are obtained, each representing a separate fraction

The Plexiglas housing surrounding the microbalance mini­mizes the effects of drafts and minor temperature changes. The balance, which is sensitive to 2 micrograms, is essen­tial for the many problems handled using micro techniques

1 2 0 A · ANALYTICAL CHEMISTRY

•

<

This gas chromatographic analyzer was designed and built in the laboratory, specifically for the analysis of a gas mixture consisting of argon, nitrogen, carbon monoxide, carbon dioxide, nitric oxide, nitrous oxide, and nitrogen dioxide. Two ovens containing three columns and a single detector are in the cabinet on the right. An external trap converts nitrogen dioxide into nitric oxide in which form it is analyzed. Approximately fifteen minutes is required for an analysis

A dual-column laboratory-constructed gas chromatography instrument is shown. One column is used to analyze a complex mixture of organic acids resulting from the oxidation of isobutylene with NO,. Typical components include a-hydroxyisobutyric acid (monomer and dimer), oxalic acid, α-acetoxy isobutyric acid, α-nitrato isobutyric acid, and tetramethyl glycolid. The acids are con­verted to their methyl esters with diazomethane prior to analysis. Approxi­mately thirty minutes, including esterification, is required for an analysis. The accuracy obtained is ± 2 % relative. The second column in the instrument is used for the analysis of traces of ethanol in methanol

OUTSTIRS OUTLASTS OUTSELLS

|ÂU£2ÂAt i l i& l !13 Stirs thickest liquids. Won't stall, won't burn out.

I2IMÉÉÎKÉI^SM^^^MI Not Q stock motor,

but special heavy duty Waco motor. Many labs

operate this stirrer 24 hours a day, 7 days a

week, month after month.

U U l f l J e t t b U I Cools motor, permits contin­

uous use. Outlasts others, saves replacement.

U J ^ ^ U i H l a f i J j & U i l U i f l I n d u c t i o n t ype motor is safe for stirring flammables.

• M f t H Î g l With one 300 and one 600 R.P.M.

% " shaft. These speeds cover the vast major­

ity of stirring needs.

Order Today on Our Guarantee N - 1 0 2 3 5 Waco stirrer with brass mounting

rod and 6 foot cord $25 .25

Ν - 1 0 2 3 5 - 1 Stirrer chuck for Waco stirrer for V4" stirring rods $ 1.65

Write for free Catalog No. N-9, describing 38 different stirrers for every stirring job.

Circle No. 21 on Readers' Service Card

WACO

LOW COST

$2525

WILKENS-ANDERSON CO. 4525 W. D I V I S I O N ST. CHICAGO 5 1 , ILL.

V O L 3 2 , N O . 10, SEPTEMBER 1960 · 1 2 1 A