【摘要】：采用丙酮作為萃取溶劑,對(duì)電子電氣產(chǎn)品聚合物材料中的鹵代磷酸酯阻燃劑超聲萃取1.5h后,濃縮、定容、上機(jī)。為提高儀器分析方法的選擇性,減少前處理流程,選取負(fù)化學(xué)電離(NCI)模式,在離子源溫度210℃、甲烷氣流量2.5mL/min條件下對(duì)目標(biāo)分析物進(jìn)行定性定量分析。結(jié)果表明,磷酸三(2-氯乙基)酯(TCEP)和磷酸三(1-氯-2丙基)酯(TCPP)在0.1~10mg/L濃度范圍內(nèi),磷酸三(1,3-二氯異丙基)酯(TDCP)和磷酸三(2,3-二溴丙基)酯(TDBP)在0.010~10mg/L濃度范圍內(nèi),均有良好的線性關(guān)系,相關(guān)系數(shù)(R2)大于0.999。TCEP和TCPP的檢出限和定量限分別為0.010mg/kg(S/N=3)和0.10mg/kg(S/N=10);TDCP和TDBP的檢出限和定量限分別為0.001mg/kg(S/N=3)和0.010mg/kg(S/N=10)。本方法對(duì)空白樣品中目標(biāo)分析物的加標(biāo)回收率為85.6%~108.9%,相對(duì)標(biāo)準(zhǔn)偏差為8.5%。分析了30批次實(shí)際樣品,包括丙烯腈-丁二烯-苯乙烯共聚物(ABS)、聚氯乙烯(PVC)、印刷電路板(環(huán)氧樹脂為主要成分)和聚丙烯(PP)等電子電氣產(chǎn)品聚合物材料,有2批次檢出TCPP,其含量分別為367.5mg/kg、695.2mg/kg�？梢�,電子電氣產(chǎn)品聚合物材料中存在一定的鹵代磷酸酯阻燃劑污染風(fēng)險(xiǎn)。
[Abstract]:Ultrasonic extraction of halophosphate flame retardants from polymer materials of electrical and electronic products was carried out by ultrasonic extraction with acetone as extraction solvent for 1.5 h, then concentrated, constant volume and put on the machine. In order to improve the selectivity of instrumental analysis method and reduce the pretreatment process, a negative chemical ionization (NCI) model was selected to carry out qualitative and quantitative analysis of the target analyte under the condition of ion source temperature of 210C and methane gas flow rate of 2.5mL/min. The results showed that tris (2-chloroethyl) phosphate (TCEP) and tris (1-chloro-2-propyl) phosphate (TCPP) were in the range of 0.1~10mg/L concentration. Tris (1,3-dichloroisopropyl) phosphate (TDCP) and tris (2,3-dibromopropyl) phosphate (TDBP) showed good linear relationship in the concentration range of 0.010~10mg/L. The correlation coefficient (R2) was greater than the detection limit and quantitative limit of 0.999.TCEP and TCPP were 0.010mg/kg (S/N=3) and 0.10mg/kg (S/N=10), respectively. The detection limits and quantitative limits of TDCP and TDBP were 0.001mg/kg (S/N=3) and 0.010mg/kg (S/N=10), respectively. The recoveries of target analytes in blank samples were 85.6% ~ 108.9% and the relative standard deviation (RSD) was 8.5%. Thirty batches of practical samples, including acrylonitrile-butadiene-styrene copolymer (ABS), PVC (PVC), printed circuit board (epoxy resin as the main component) and polypropylene (PP) and other electronic and electrical products polymer materials, were analyzed. The content of TCPP, was 367.5 mg 路kg ~ (- 1) and 695.2 mg 路kg ~ (- 1) respectively in two batches. It can be seen that there is a certain risk of halogenated phosphate flame retardants pollution in the polymer materials of electronic and electrical products.
【作者單位】： 深圳市計(jì)量質(zhì)量檢測(cè)研究院;
【基金】：廣東省質(zhì)量技術(shù)監(jiān)督局科技項(xiàng)目基金(2014PJ03)資助
【分類號(hào)】：O657.63;TQ317

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