Document q6eE3L1bOzpome8dz6Ob4JaR

STANDARD TEST PROCEDURE SO. 555 5.?.COOn}.IC:I Cighl&O. CO. Gas Chromatographic Analysis of Vinyl Chloride Monomer Using the Hydrogen Flame Icnization ____ _______Detector I. SCOPE: This test is used for measuring th2 impurities in vinyl chloride monomer and it nay also be used for other low boiling liquids. H. PRSC1PLS: The principles of gas chromatographic sepr^a^ions aro employrwd utilizing hydrogen flame icni2aticn detection for high sensitivity. IH. SAFETY PRECAUTIONS: Care should be taken in the handling of vii^rl chloride, using adequate ventilation and keeping it from open flames or sources of heat and electrical spark. IV. APPARATUS: 1. Temperature programmed gas chromatograph with hydrogen flame ionization detector and equipped with a Micro Tek universal sample Inlet system. 2. Micro Tek sample cylinders. 3. Micro Tek snap sampler, O.COj? cc (5 micro liter) or smaller when adequate sensitivity can be obtained. U. Recorder, 0-1 mv range with variable speed chart drive. Rreezer for storing samples. V, PROCEDURE! A, Instrument Operation. The operating manual of the instrument manufacturers must be strictly adhered to and the operator should be thoroughly familiar with ttess manuals prior to attempting to run the equipment. Utilizing the Beckman GC2A Themotrac temperature prograntrvsr and Hydrogen flame lenAsatlon detector with a 3/16" x 22' S3 column of 3Oi Carbcrwax 1500/ 1% HyOh on Chrccioeorb Vj 30^0 M, the following conditions should bo used ASV 0005455 '`*Av - I* must be realized that the analysis is only as good as the sample and sampling is one of the most important aspects of any chromatographic work. Ih lower the boiling point,, of the material and the wider the belling point range of the various impurities, the mere iroportant sampling technique becomes* C. Introduction of sample into the instrument. The snap sampler is placed in the sample cylinder and allowed to remain in the liquid with the plunger down for one minute. During this time the chromatograph controls may be sot and checked. Pull the plunger up and down a few times. Transfer the full snap sampler to the universal sample inlet and inject the sample as quickly a3 possible. The analysis is completed ir. the routine manner for gas chromatography, til CALCULATIONS: The area of each peak is determined and from this the concentration of each ccr-.pcr.erit ia calculated and reported in ppm. Various materials found in TCI have shcvma different response (in terr.s of neck height and araa) to ths rl.F. doteetcr. It is, therefore,, necessary'to deterrwind correction factors which rili'be used in tr.e calculation: to obtain correct aoi or weight figures. .y* >rr- * - r-'-