PD ISO/TS 17182:2014

Foreword
1 Scope
2 Normative references
3 Principle
4 Interferences
5 Reagents
6 Apparatus and equipment
7 Sampling
8 Procedure
9 Calculation
10 Test report
Annex A (informative) - Typical concentrations of the
        standard solutions
Annex B (informative) - Example of gas chromatographic
        conditions
Bibliography

Provides the gas chromatographic determination of phenols, methyl phenols, di-methylphenols and tri-methylphenols and selected chlorophenols by using mass spectrometric detection in soil samples.

This International Standard describes the gas chromatographic determination of phenols, methyl phenols, di-methylphenols and tri-methylphenols (see Table1) and selected chlorophenols (see Table2) 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 0,01mg/kg to 0,1mg/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. Table1 Target phenolic compounds with relevant mass fractions of respective acetylated compounds for MS-detection Compound CAS-RNa Chemical formula Acetylated compoundsFragmentationb 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). Table2 Target chlorophenolic compounds with relevant mass fractions of respective acetylated compounds for MS-detection Compound CAS-RNa Chemical formula Acetylated compoundsFragmentation 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