Determination of Additives in Polymers and Rubbers

Chapter 6: Paper Chromatography

Overview

Wheeler [1] has reviewed the available literature on the applications of paper chromatography in the examination of polymers for antioxidants (Table 6.1). He points out that, as most antioxidants are highly polar, they cannot be efficiently separated on normal paper except by the use of highly polar mobile phases. Consequently reversed-paper chromatography [2-5] or acetylated papers [6-9] have been used to reduce the effects of tailing . Various workers have discussed the determination of antioxidants in rubber extracts [10-14].

Table 6.1: Paper chromatographic separation of amine antioxidants
Acetylated paper, Mobile phase: benzene:methanol (1:1). Spray reagent: 4% benzoyl peroxide in benzene

Systematic name

Trade name

Colour of reaction product

Identification limits before/after chromatographic separation, g

R f values

1 Phenyl- ?-naphthylamine

Neozone A
Nonox A
Alterungsschutzmittel
PAN

Light yellow

5

10

0.64

2 Phenyl- ?-naphthylamine

Neozone D
Nonox D
Alterungsschutzmittel
PBN

Blue-grey

5

20

0.64

3 Diphenyl- p-phenylenediamine

JZF

Yellow-orange

< 1

2

0.56

4 Phenyl-cyclohexyl- p-phenylenediamine

Alterungsschutzmittel
4010

Yellow

< 1

10

0.73

5 Di- ?-naphthyl- p-phenylenediamine

Agerite White
Santowhite
CI Nonox CI
Alterungsschutzmittel
DNP
Antioxidant 123

Pink

1

5

0.55 (Tailing)

6 p-Isopropoxydiphenylamine

e.g. in Agerite Hipar, a mixture of 2, 3 and 6

Yellow-brown

-

-

0.73

7 p, p ?-Dimethoxy-diphenylamine

e.g.

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