Publication

PD ISO/TS 17182:2014

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

Current

•

Published:

31 Dec 2014

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-RN^a	Chemical formula	Acetylated compounds Fragmentation^b
			1^st mass	Relative intensity %	2^nd 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-RN^a	Chemical formula	Acetylated compounds Fragmentation
			1^st mass	Relative intensity %	2^ndmass	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.

Product Details

Descriptors

Composition

Quality

Soils

Appearance

Soil testing

Soil classification tests

Soil sampling

Field testing

Ground water

Land use

Soil surveys

ICS Codes

13.080.10 Chemical characteristics of soils

Committee

EH/4

International relationships

Identical to:

ISO/TS 17182:2014

ISBN

978 0 580 76247 5

Publisher

BSI