Analysis of acrylic polymers using combined Zeisel reaction-gas chromatography and infrared spectrometry

Manual of Plastics Analysis

“…In the distillation technique 64 the polystyrene (0.5g) is dissolved in chloroform or ethylene dichloride (20 ml) in a stoppered flask and the solution is poured into an excess of methyl alcohol (110 ml) to reprecipitate dissolved polymer. The polymer is filtered off and washed with methanol (120 ml) and the combined filtrate and washings gently distilled to provide 200 ml of a distillate containing only styrene monomer and any other distillable component of the original polystyrene sample.…”

“…This technique has also been applied to the determination of alkoxy groups in acrylate esters. 60 Anderson et al 64 have used combined Zeisel reaction -gas chromatography to analyse acrylic copolymers. Acrylic esters were cleaved with hydriodic acid and gas chromatography was used for analysing the alkyl iodides so formed (Method 62).…”

“…Infrared spectroscopy has been applied to the determination of free and combined vinyl acetate in vinyl chloride-vinyl acetate copolymers. 67 This method is based upon the quantitative measurement of the intensity Anderson et al 64 have described an infrared procedure for distinguishing between copolymerised acrylic and methacrylic acids in acrylic polymers containing more than 10% of the acid. This method is based on precise measurement of the wavelength of the carboxylic acid absorption maximwn at about 1700 cm-l (5.88 u).…”

Short-cut fused-peak resolution method for chromatograms

“…However, all three are capable of giving consistent KL results for solutes which exhibit multiple sorption mechanisms. The implications of this study and, largely, the earlier studies of 14,16,17) are evident. In particular, bulk solution thermodynamic quantities for testing theories of nonelectrolytic mixtures (15) or for determining hydrogenbond association constants (5, 6) can now be obtained with greater confidence for systems which were previously considered to be too troublesome and error prone.…”

Functional group analysis

“…Esters. Ester groups in acrylic polymers have been determined by cleavage of the esters with hydrogen iodide (Zeisel method) to give alkyl iodides which were then determined by gas chromatography (2).…”