Soil quality. Determination of some selected phenols and chlorophenols. Gas chromatographic method with mass spectrometric detection

Soil quality. Determination of some selected phenols and chlorophenols. Gas chromatographic method with mass spectrometric detection

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1   Scope

This International Standard describes the gas chromatographic determination of phenols, methyl phenols, di-methylphenols and tri-methylphenols (see Table 1) and selected chlorophenols (see Table 2) by using mass spectrometric detection in soil samples. This method can also be used for other solid samples, such as sediments and solid wastes. This International Standard describes an acidic liquid extraction of soil, followed by acetylation and then liquid/liquid extraction. Determination takes place by gas chromatography and mass spectrometric detection.
With this method, phenols and chlorophenols can be determined at the lowest of mass concentrations ranging from approximately 0,01 mg/kg to 0,1 mg/kg depending on the component sensitivity and the quantity of sample used. In some cases, complete separation of isomers cannot be achieved. Then the sum is reported.

NOTE With this method, other higher methylated phenols can also be analysed provided that the suitability and the validity of the method is proven.

Table 1 — Target phenolic compounds with relevant mass fractions of respective acetylated compounds for MS-detection
Compound CAS-RNa Chemical formula Acetylated compounds
Fragmentationb
      1st mass Relative intensity % 2nd mass Relative intensity %
phenol 108-95-2 C6H6O 94 100 66 26
2-methylphenol
(o-cresol)		 95-48-7 C7H8O 108 100 107 68
3-methylphenol
(m-cresol)		 108-39-4 C7H8O 108 100 107 85
4-methylphenol
(p-cresol)		 106-44-5 C7H8O 108 100 107 92
2,3-dimethylphenol 596-75-0 C8H10O 122 90 107 100
2,4-dimethylphenol 105-67-9 C8H10O 122 100 107 85
2,5-dimethylphenol 95-87-4 C8H10O 122 100 107 90
2,6-dimethylphenol 576-261-1 C8H10O 122 100 107 92
3,4-dimethylphenol 95-65-8 C8H10O 122 99 107 100
3,5-dimethylphenol 108-68-9 C8H10O 122 100 107 68
2,3,5-trimethylphenol 697-82-5 C9H12O 136 87 121 100
2,3,6-trimethylphenol 2416-94-6 C9H12O 136 90 121 100
2,4,6-trimethylphenol 527-60-6 C9H12O 136 10 121 85
3,4,5-trimethylphenol 527-54-8 C9H12O 136 70 121 100
2-ethylphenol 90-00-6 C8H10O 107 100 122 48
3-ethylphenol 620-17-7 C8H10O 122 48 107 100
4-ethylphenol 123-07-9 C8H10O 107 100 122 35
4-propylphenol 645-56-7 C9H12O 107 100 136 25
4-isopropylphenol 99-89-8 C9H12O 121 100 136 28
2-hydroxybiphenyl 90-43-7 C12H10O 170 100 141 23
Internal standards
2-fluorophenol 367-12-4 C6H5FO 112 100 64 58
4-fluorophenol 371-41-5 C6H5FO 112 100 64 18
3-fluoro-2-methylphenol 452-72-2 C7H7FO 126 100 97 29
4-fluorocatechol 367-32-8 C6H5FO2 128 100 75 28
a Chemical abstract service registry number.
b Spectral database for organic compounds (SDBS).
Table 2 — Target chlorophenolic compounds with relevant mass fractions of respective acetylated compounds for MS-detection
Compound CAS-RNa Chemical formula Acetylated compounds
Fragmentation
      1st mass Relative intensity % 2nd mass Relative intensity %
2-chlorophenol 95-57-8 C6H5OCl 128 100 130 34
3-chlorophenol 108-43-0 C6H5OCl 128 100 130 29
4-chlorophenol 106-48-9 C6H5OCl 128 100 130 35
2,6-dichlorophenol 87-65-0 C6H4OCl2 162 100 164 67
2,4-dichlorophenol 120-83-2 C6H4OCl2 162 100 164 66
2,5-dichlorophenol 583-78-8 C6H4OCl2 162   164  
3,5-dichlorophenol 591-35-5 C6H4OCl2 162 100 164 66
2,3-dichlorophenol 576-24-9 C6H4OCl2 162 100 164 66
3,4-dichlorophenol 95-77-2 C6H4OCl2 162 100 164 66
2,4,6-trichlorophenol 88-06-2 C6H3OCl3 196 100 198 98
2,3,6-trichlorophenol 933-75-5 C6H3OCl3 196 100 198 100
2,3,5-trichlorophenol 933-78-8 C6H3OCl3 196 100 198 100
2,4,5-trichlorophenol 95-95-4 C6H3OCl3 196 96,1 198 100
2,3,4-trichlorophenol 15950-66-0 C6H3OCl3 196 100 198 98
3,4,5-trichlorophenol 609-19-8 C6H3OCl3 196 100 198 100
2,3,4,5-tetrachlorophenol 4901-51-3 C6H2OCl4 230 — 232 —
2,3,5,6-tetrachlorophenol 935-95-5 C6H2OCl4 230 79 232 100
2,3,4,6-tetrachlorophenol 58-90-2 C6H2OCl4 230 78 232 100
pentachlorophenol 87-86-5 C6HOCl5 264 66 266 100
a Chemical abstract service registry number.