T/CSES 132-2023 Soil determination of polychlorinated naphthalenes by gas chromatography-tandem mass spectrometry
T/CSES 132-2023 Soil determination of polychlorinated naphthalenes by gas chromatography-tandem mass spectrometry
Basic Information
Scope
Scope: This document specifies the gas chromatography-tandem mass spectrometry method for the determination of naphthalene isomers (2-8 chlorinated naphthalenes) in soil. This document is applicable to the determination of 1,4-dichloronaphthalene, 1,2-dichloronaphthalene, 1,4,6-trichloronaphthalene, 1,2,3-trichloronaphthalene, 1,3,5,7-tetrachloronaphthalene, 1,4,5,8-tetrachloronaphthalene, 1,2,3,5,7-pentachloronaphthalene, 1,2,3,5,6,8-hexachloronaphthalene, 1,2,3,4,5,6,7-heptachloronaphthalene, and 1,2,3,4,5,6,7,8-octachloronaphthalene in soil. When the sample quantity is 10 g and the dilution volume is 50 μL, the method detection limit for 2-8 chlorinated naphthalenes specified in this document is 5 ng/kg~9 ng/kg, and the determination limit is 20 ng/kg~36 ng/kg. Main technical content: Method principle: After extraction, concentration, purification, and dilution of polychlorinated naphthalenes in soil with organic solvents, they are separated and detected by gas chromatography-tandem mass spectrometry based on retention time, characteristic ion mass-to-charge ratio, and abundance ratio for qualitative analysis, and quantified by isotope internal standard method. Precision: Six laboratories tested 12 samples of 2-8 chlorinated naphthalenes with added concentrations of 50 ng/kg, 250 ng/kg, and 450 ng/kg. The relative standard deviations within laboratories were 0.9%~33.9%, 0.4%~18.9%, and 0.6%~22.8%, respectively; the relative standard deviations between laboratories were 6.2%~28.4%, 3.2%~10.9%, and 4.4%~13.4%, respectively; the repeatability limits were 10 ng/kg~20 ng/kg, 30 ng/kg~120 ng/kg, and 80 ng/kg~150 ng/kg; and the reproducibility limits were 10 ng/kg~40 ng/kg, 40 ng/kg~130 ng/kg, and 100 ng/kg~200 ng/kg. See Table B.5 in Appendix B for details. Accuracy: Six laboratories tested 12 samples of 2-8 chlorinated naphthalenes with added concentrations of 50 ng/kg, 250 ng/kg, and 450 ng/kg. The average recovery rates of the added substances were 62.1%~147%, 83.5%