摘要
采用二级水三次水洗抽滤的方法对三乙膦酸铝原药进行纯化。对制备的纯品采用碘量法、离子色谱法测定,质量分数均大于99.0%,能够满足离子色谱分析对标样的要求。同时采用AS 14、AS 9离子色谱柱明确了常见阴离子、淋洗液浓度对三乙膦酸铝分离的影响,最后采用Na2CO3溶液为淋洗液,AS 9离子色谱柱,电导检测器建立了三乙膦酸铝的离子色谱定量方法,并对该方法进行了评价。结果表明,常量分析方法的准确度(添加回收率99.6%~101.0%)和精密度(RSD 0.31%)均较好。
The fosetyl-Al whose impurities are mostly sulfate is purified with washing three times by redistilled water, and the purified fosetyl-Al could satisfy the demand of ion chromatography. The purified sample is further confirmed with iodimetry and ion chromatography, and its content is beyond 99.0%. The influences of common anions and the concentration of eluent on the separation of fosetyl-A1 are studied by using AS 14 and AS 9 analytical columns. The ion chromatography method to analyze fosetyl-Al isestablished with electronic conductivity detector, AS 9 column and Na2CO3 solution as eluent, and corresponding evaluate is also carried out. The results indicate that the accuracy(99. 6~100. 1%) and the precision with RSD of 0.31 % of the method are satisfying.
出处
《青岛科技大学学报(自然科学版)》
CAS
2008年第3期200-203,209,共5页
Journal of Qingdao University of Science and Technology:Natural Science Edition
关键词
三乙膦酸铝
纯化
离子色谱
定量分析
fosetyl-Al
purification
ion chromatography
quantitative analysis