Eutrophication in water bodies has a close relationship with the phosphorus speciation in sediments.The European Union developed the first reference material for phosphorus speciation of sediments BCR 684 in 2000 in order to determine accurately the contents of phosphorus speciation in sediments.However,supplies of BCR 684 are now exhausted.Moreover,the reference material of BCR 684 was collected from a lake in Europe which does not match the type and conditions of pollution in sediments in China.To this end,two phosphorus speciation reference materials of lake sediments (serial numbers:GBW 07462 and GBW 07463)on the fundamental of BCR 684,which were collected from Tai Lake,Jiangsu province and Dongting Lake,Hunan province in China,have been developed. The reference material was prepared by being dried,ground,sterilized and aged.Homogeneity and stability tests were conducted according to the JJG 1 006—1 994 and ISO Guide 35 .For the homogeneity test,the variance test F value of 1 5 subsamples was less than the threshold value.During one year,four analysis results showed that there were no significant statistical changes in stability.The stability of the samples was checked twice in 201 2 and 201 3. The results show that the stability of the two reference materials is perfectly matched.Collaboration with 8 laboratories was adopted in order to obtain certified value and uncertainty calculations.Parameter for certified values includes total phosphorus,inorganic phosphorus,organic phosphorus,apatite phosphorus and non-apatite phosphorus.SMT was used as the extraction method and the determined methods are Sb-Mo-Sc Spectrophotometry and Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES).BCR 684 was used for the quality control.The certified values and uncertainty were obtained under the JJG 1 006—1 994 and ISO Guide 35 .These reference materials represent sediments in lakes with high eutrophication in China.The advantages of good representation of the sampling area,reasonable proxy selection and accurate certification values deem the reference materials suitable for quality monitoring of phosphorus speciation in sediments in the fields of environment,geology,agriculture and geochemistry.%水体富营养化与沉积物中磷元素的形态有密切关系。为了准确测定沉积物中不同形态磷的含量，欧盟在2000年研制了第一个湖泊沉积物中磷形态标准物质（BCR 684），但基本用尽已不能满足需求，而且该标准物质采集于欧洲某湖泊，沉积物类型及污染情况与我国湖泊不相匹配。本文结合我国沉积物的类型和湖泊污染状况，研制了我国首批2个湖泊沉积物中磷形态标准物质（批准编号为 GBW 07462和 GBW 07463）。候选物样品采集地点为江苏太湖和湖南洞庭湖，样品经过自然干燥、研磨、灭菌、陈化等加工处理，随机抽取15个子样采用单因素方差分析（F检验法）进行均匀性检验，检验的F实测值均小于临界值，表明样品均匀性良好。根据ISO导则35推荐方法对候选物样品在一年内进行4次稳定性检查，分析结果无方向性变化，再通过2次验证实验，样品稳定性良好。此批磷形态标准物质采用8家实验室联合定值，定值参数包括5种磷形态：总磷、无机磷、有机磷、磷灰石态磷、非磷灰石态磷；磷形态提取方法采用欧盟SMT法，测定方法采用钼锑钪光度法和电感耦合等离子体发射光谱法（实验过程中用欧盟BCR 684作为质量监控）；按照《一级标准物质研制规范》（JJG 1006—1994）和ISO导则35的要求给出了5种磷形态的标准值和不确定度。此批磷形态标准物质样品代表了我国典型富营养化湖泊的沉积物类型，采样点的区域代表性强，定值项目选择合理、量值准确，可应用于环境、地质、农业、地球化学等研究领域沉积物的磷形态样品质量监控。
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