磷酸三(2-氯乙基)酯标准物质的研制

研制了有机磷阻燃剂磷酸三(2-氯乙基)酯(TCEP)标准物质。采用硅胶柱层析法对TCEP原料进行纯化,得到纯度大于99%的TCEP纯品。通过红外光谱和气相色谱–质谱准确定性分析后,利用气相色谱法和气相色谱–质谱法结合热重分析法分别对TCEP纯物质进行纯度定值。将制备的50 g TCEP纯品分装到100个小瓶中,每瓶0.5g,从中随机选取10瓶,进行均匀性和稳定性实验,结果表明,研制的TCEP标准物质均匀性良好,在半年内是稳定的。研制的有机磷阻燃剂磷酸三(2-氯乙基)酯标准物质的纯度定值为99.56%,扩展不确定度为1.18%(k=2)。研制的磷酸三(2-氯乙基)酯标准物质满足国家二级标准物质标准的要求。

Preparation of Certified Reference Material of Tris(2-Chloroethyl) Phosphate

The reference material of tris(2-chloroethyl) phosphate(TCEP) was developed. The commercially available materials were purified by silica gel column chromatography to obtain TCEP pure products with purity of more than 99％. After the qualitative analysis on pure substance by infrared spectroscopy and gas chromatography-mass spectrometry. The purity of TCEP was certified by gas chromatography and gas chromatography-mass spectrometry combined with thermogravimetric analysis. The 50 g TCEP pure substance prepared was divided into 100 vials with 0.5 g in each bottle, and 10 bottles were randomly selected to test the uniformity and stability. The reference materials of TCEP has a good homogeneity and validity within half a year period. The purity value of TCEP standard material of organophosphorous fire retardants was 99.56％ with the expand uncertainty of 1.18％(k=2). Tris(2-chloroethyl) phosphate standard material developed can meet the requirements of the national secondary standard material.