T/CSES 133-2023 Soil determination of short chain chlorinated paraffins by gas chromatography-mass spectrometry
T/CSES 133-2023 Soil determination of short chain chlorinated paraffins by gas chromatography-mass spectrometry
Basic Information
Scope
Scope: This document specifies the gas chromatography-mass spectrometry method for determining the total mass of short-chain chlorinated paraffins (SCCPs) with five to ten chlorine substitutions in soil. This document is applicable to the determination of the total mass of short-chain chlorinated paraffins (SCCPs) with five to ten chlorine substitutions in soil. When the soil sample quantity is 10 g and the volumetric capacity is 20 μl, the detection limit of the short-chain chlorinated paraffins determined by this document is 4 μg/kg, and the lower limit of determination is 16 μg/kg. Main technical content: Method principle: After extraction, concentration, purification, and volumetric capacity of SCCPs in soil, they are separated and detected by gas chromatography-mass spectrometry, and their qualitative identification is based on retention time, mass-to-charge ratio, and characteristic ion abundance ratio. Quantitative determination is performed using internal standard method. Precision: Four laboratories respectively measured SCCP samples with added concentrations of 20 μg/kg, 40 μg/kg, and 100 μg/kg. The relative standard deviations within laboratories were 2.8%~18.8%, 1.5%~17.6%, and 7.2%~24.5%, respectively; the relative standard deviations between laboratories were 47%, 61%, and 40%, respectively; the repeatability limits were 41.7 μg/kg, 65.9 μg/kg, and 250.9 μg/kg, respectively; and the reproducibility limits were 50.6 μg/kg, 81.4 μg/kg, and 247.3 μg/kg, respectively. Accuracy: Four laboratories respectively performed six parallel measurements on soil samples with added SCCP concentrations of 20 μg/kg, 40 μg/kg, and 100 μg/kg. The recovery rates of the added SCCPs ranged from 72% to 130%, 74% to 129%, and 69% to 127%, respectively.