Additives, determination chromatography

The neutral surfactant is measured after fixing of the ionic substances on a combined anionic/cationic ion exchange column. Volatile substances in the eluate are determined by gas chromatography and nonvolatile substances are measured gravimetrically. In the bulk of the neutral compounds phosphoric acid triesters may be present. This part is additionally determined by atom emission spectroscopy. 

H3PO4 is being used for transamidation in such a case XRF determines higher phosphorous concentrations than justified on the basis of the phosphite additives. Ion chromatography may then be required. 

Gas chromatography has been used to determine arsine in hydrogen-rich mixtures. The arsine was detected on a column containing dioctyl phthalate on polyoxyethylene-glycol as adsorbent with hydrogen as the carrier gas. The limit of detection as arsenious oxide was 0.001 mg. In addition, determinations of down to 4.2 x 10 gl of arsine in silane on various columns have been developed , using dry nitrogen as carrier gas and a... 

The time expenditure per sample is about 24 hours for the wet-chemical procedure, with 2.5 hours being the effective working time. In contrast, using ion chromatography requires only 20 to 25 minutes, including calibration time, for each sulfate determination [52]. In addition, ion chromatography has the advantage that short-chain alkyl sulfonates and sulfates do not interfere with the sulfate determination and chloride and orthophosphate can be detected in the same run. 

Chemical assay is preferably performed by gas—hquid chromatography (glc) or by the conventional methods for determination of unsaturation such as bromination or addition of mercaptan, sodium bisulfite, or mercuric acetate. 

In addition to the above techniques, inverse gas chromatography, swelling experiments, tensile tests, mechanical analyses, and small-angle neutron scattering have been used to determine the cross-link density of cured networks (240—245). Si soHd-state nmr and chemical degradation methods have been used to characterize cured networks stmcturaHy (246). H- and H-nmr and spin echo experiments have been used to study the dynamics of cured sihcone networks (247—250). 

Polymerization-grade chloroprene is typically at least 99.5% pure, excluding inert solvents that may be present. It must be substantially free of peroxides, polymer [9010-98-4], and inhibitors. A low, controlled concentration of inhibitor is sometimes specified. It must also be free of impurities that are acidic or that will generate additional acidity during emulsion polymerization. Typical impurities are 1-chlorobutadiene [627-22-5] and traces of chlorobutenes (from dehydrochlorination of dichlorobutanes produced from butenes in butadiene [106-99-0]), 3,4-dichlorobutene [760-23-6], and dimers of both chloroprene and butadiene. Gas chromatography is used for analysis of volatile impurities. Dissolved polymer can be detected by turbidity after precipitation with alcohol or determined gravimetrically. Inhibitors and dimers can interfere with quantitative determination of polymer either by precipitation or evaporation if significant amounts are present. 

In Table 1 some of the properties of raw synthetic hj -l,4-polyisoprene (Goodyear s Natsyn) and natural mbber (Hevea) are presented along with references that contain additional thermal, optical, electrical, and mechanical property data. Some properties of synthetic /n j -l,4-polyisoprene (Kuraray TP-301) are also given. Molecular weights and mol wt distribution are determined by gel-permeation chromatography (gpc) (11). 

Recalling that a separation is achieved by moving the solute bands apart in the column and, at the same time, constraining their dispersion so that they are eluted discretely, it follows that the resolution of a pair of solutes is not successfully accomplished by merely selective retention. In addition, the column must be carefully designed to minimize solute band dispersion. Selective retention will be determined by the interactive nature of the two phases, but band dispersion is determined by the physical properties of the column and the manner in which it is constructed. It is, therefore, necessary to identify those properties that influence peak width and how they are related to other properties of the chromatographic system. This aspect of chromatography theory will be discussed in detail in Part 2 of this book. At this time, the theoretical development will be limited to obtaining a measure of the peak width, so that eventually the width can then be related both theoretically and experimentally to the pertinent column parameters. 

H. J. Goites, B. M. Bell, G. D. Pfeiffer and J. D. Graham, Multidimensional chromatography using on-line coupled microcolumn size exclusion cliromatography-capillary gas chromatography-mass spectrometry for determination of polymer additives , J. Microcolumn Sep. 1 278-288. (1989)... 

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