Abstract:
Halogenated phosphate ester flame retardants in polymer material of electrical and electronic products were extracted by ultrasound with acetone solvent for 1.5 h, then the extract was evaporated to almost dryness and dissolved with 1.0 mL
n-hexane, and detected by instrument. In order to improve method selectivity and reduce sample preparation procedure, negative chemical ionization (NCI) model was selected. Taget analytes were determined qualitatively and quantitatively at 210 ℃ of ion source temperature with 2.5 mL/min of methane gas flow. The linear range of tris-(2-chloroethyl) phosphate (TCEP) and tris-(1-chloro-2-propyl) phosphate (TCPP) are 0.10-10 mg/L with
R2≥0.999, while tris-(1,3-dichloro-2-propanol) phosphate (TDCP) and tris-(2,3-dibromo-1-propanol) phosphate (TDBP) are 0.010-10 mg/L with
R2≥0.999. The limit of detection (S/N=3) is 0.010 mg/kg for TCEP and TCPP, and 0.001 mg/kg for TDCP and TDBP. The limit of quantitative (S/N=10) is 0.10 mg/kg for TCEP and TCPP, and 0.010 mg/kg for TDCP and TDBP. The feasibility of this method was demonstrated by determination of halogenated phosphate ester fire retardants in electrical and electronic products with spiked recoveries, which is in the range of 85.6%-108.9%, the relative standard deviation (RSD) is less than 8.5%. 30 actual samples were analyzed, including acrylonitrile-butadiene-styrene (ABS), polyvinyl chloride (PVC), printed circuit board which was mainly made from epoxy resin and polypropylene (PP). Only two samples are detected with TCPP concentration of 367.5 mg/kg and 695.2 mg/kg. Therefore, there is a certain risk of halogenated phosphate ester flame retardants for polymer material of electrical and electronic products.