Abstract：A method for development and certification of certified reference material of 2,3,4-trichloroanisoles is presented.According to analysis procedure of homogeneity, 11 bottles of sample are taken from 500 bottles at random, and the result is validated by F-test and T-test statistical methods. The stability inspection is carried on short-term(1 month) and long-term(12 months), the result indicated that the period for 2,3,4-trichloroanisoles of storage is 12 months at 20℃.The purity of 2,3,4-trichloroanisoles are determined by two methods of different principles, which are high performance liquid chromatography method and differential scanning calorimetry method.The qualitative analysis of main impurity is determined with standard addition by liquid chromatography with photo-diode array and the impurity is 2,3,6-trichloroanisoles; The content of water in 2,3,4-trichloroanisoles is measured by Karl-Fischer titrator with drying oven. The uncertainty of HPLC and DSC methods are respectively evaluated. The certified result is 99.56% and expanded uncertainty is 0.40%（k=2）.
［1］Salemia A, Lacorteb S, Bagheria H, et al. Automated trace determination of earthy-musty odorous compounds in water samples by on-line purge-and-trap-gas chromatograph-mass spectrometry［J］. Journal of Chromatography A, 2006, 1136（2）: 170-175.
［2］Zhang L F, Hu R K, Yang Z G. Simultaneous picogram determination of “earthy-musty” odorous compounds in water using solid-phase microextraction and gas chromatography-mass spectrometry coupled with initial cool programmable temperature vaporizer inlet［J］.Journal of Chromatography A,2005, 1098 (4): 7-13.
［3］Richardson S D. Disinfection by-products and other emerging contaminants in drinking water［J］. Trends in Analytical Chemistry, 2003, 22(10): 666-684.
［4］Insa S, Anticó E, Ferreira V. Highly selective solid-phase extraction and large volume injection for the robust gas chromatography-mass spectrometric analysis of TCA and TBA in wines ［J］. Journal of Chromatography A, 2005, 1089(1-2): 235-242.
［5］Jnsson S, Uusitalo T, Bavel B V, et al. Determination of 2,4,6-trichloroanisole and 2,4,6-tribromoanisole on ng/L to pg/L levels in wine by solid-phase microextraction and gas chromatography-high-resolution mass spectrometry［J］. Journal of Chromatography A, 2006, 1111(1): 71-75.
［6］邓晓军,郭德华,李波,等. 葡萄酒中痕量木塞污染物的顶空固相微萃取一气相色谱串联质谱法检测 ［J］. 分析测试学报,2008,27（12）:1375-1378.
［7］Bianchi F,Careri M,Mangia A. Optimization of headspace sampling using solid-phase microextraction for chloroisoles in cork stopper and gas chromatography-ion-trap tandem mass spectrometric analysis ［J］.J Sep Sci,2003,26(4):369-375.
［8］Díaz A, Ventura F, Galceran M T. Determination of odorous mixed chloro-bromoanisoles in water by solid-phase micro-extraction and gas chromatography-mass detection［J］. Journal of Chromatography A, 2005, 1064(1): 97-106.
［9］ISO Guide 31:2000,Reference materials—Contents of certificates and label［S］.
［10］ISO Guide 34:2000, General requirements for the competence of reference material producers［S］.
［11］ISO Guide 35, 1-7 (2000),Certification of reference materials-General and statistical principles［S］.
［12］Ma K,Wang H F,Zhao M,et al.Purity determination and uncertainty evaluation of therophylline by mass balance method,high performance liquid chromatography and differential scanning calorimetry ［J］.Analytica Chimica Acta,2009,650(2):227-233.
［13］ASTM E928-01,Standard Test Method for Determination of Purity by Differential Scanning Calorimetry ［S］.
2012, Vol. 33 
