From Determination of Additives in Polymers and Rubbers

2.9 Solvent Extraction Ultraviolet Spectroscopy

Straightforward UV spectroscopy is liable to be in error because of interference by other highly absorbing impurities that may be present in the sample [59-62]. Interference by such impurities in direct UV spectroscopy has been overcome or minimised by selective solvent extraction or by chromatography [60]. However, within prescribed limits UV spectroscopy is of use and, as an example, procedures are described next for the determination of Ionol (2,6-di- tert-butyl- p-cresol) and of Santonox R (4,4 ?-thio-bis-6- tert-butyl- m-cresol) in polyolefins [63-66].

Certain additives, e.g., calcium stearate and thiodipropionate, do not interfere in the determination. Other phenolic antioxidants, e.g., Ionox 330, Topanol CA and Santonox R, do interfere.

2.9.1 Ionol in Polyolefins

A polymer sample (20 g) was weighed into a 250 ml round-bottomed flask and 50 ml of chloroform was added. A water-cooled condenser was connected and the flask was placed on the electric heating mantle and brought gently to boiling point. The solution was refluxed for 30 minutes at a moderate rate. After cooling, the chloroform solution was carefully decanted into a 100 ml volumetric flask (using a filter if necessary) and stoppered immediately. A further 40 ml of chloroform was added to the contents of the round-bottomed flask and a second extraction of the polymer was carried out. When cool, the contents were filtered into the volumetric flask containing the first extract. The residue was washed with sufficient chloroform to dilute it to the mark. The...


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Topics of Interest

2.10 Solvent Extraction Visible Spectroscopy 2.10.1 Phenol Antioxidants A very popular method of estimating antioxidants in polymer extracts is by coupling or oxidising them to form coloured products...

The analysis of additives in polymers has been reviewed by several workers [1, 2]. A variety of analytical techniques have been considered. 7.1 IR and Raman Spectroscopy 7.1.1 Instrumentation Further...

4.1 Santonox R (4,4 ?-thiobis-6-tert butyl m-cresol) in Aqueous and Non-aqueous Extractants Ultraviolet spectroscopy is applicable to the determination of phenolic antioxidants in aqueous and...

2.2 Solvent Extraction 2.2.1 Polyolefins The scheme outlined in Figure 2.1 has been proposed for the solvent extraction and examination of PE [1]. Some useful solvents are listed in Table 2.2. Figure...

[concs] Concentrations AAS Atomic absorption spectrometry ABS Acrylonitrile-butadiene-styrene AC Alternating current AC Atomic composition AED Atomic emission detector AFS Atomic fluorescence...