CAJ | 학술논문

采用ICP-AES法同时测定工业铬酸钠溶液中微量Al，Ca，Fe，Mg，Si杂质元素。针对测定过程中存在的基体干扰、谱线干扰等问题，通过实验确定了铬酸钠中微量的Al，Ca，Fe，Mg，Si 的分析测试谱线：Al 167．079 nm，Ca 393．366 nm，Fe 259．940 nm，Mg 279．533 nm，Si 251．61 nm。实验用优级纯 HCl 将待测溶液调为酸性，消除工业铬酸钠溶液酸度不稳定引起的测定误差，采用标准加入法消除基体干扰，探讨了Al，Ca，Fe，Mg，Si等五种微量组分检测方法标准曲线线性相关性、检出限、精密度以及回收率等分析指标，详细研究了在选定分析谱线下，标准加入法对铬酸钠溶液中Al，Ca，Fe，Mg，Si等微量杂质含量测定结果的准确性的影响。结果表明标准曲线呈线性关系（R2＝0．9988～0．9996之间），五种元素检出限在（0．0134～0．0280）mg·L－1之间，11次测量标准偏差小于5．86％，回收率在97．30％～107．50％之间。实验建立的分析方法的检出限、精密度、准确度均能满足分析测试要求；方法实用性强，已经成功用于离子膜电解法中铬酸钠原料液微量离子检测；利用铬酸钠、重铬酸钠和重铬酸酐与溶液酸度的关系，实验建立的分析方法还可拓展于重铬酸钠及铬酐甚至其他六价铬产品中Al，Ca，Fe，Mg，Si 杂质离子的检测，同时也可以扩展到上述样品中其他杂质元素的测定。
채용ICP-AES법동시측정공업락산납용액중미량Al，Ca，Fe，Mg，Si잡질원소。침대측정과정중존재적기체간우、보선간우등문제，통과실험학정료락산납중미량적Al，Ca，Fe，Mg，Si 적분석측시보선：Al 167．079 nm，Ca 393．366 nm，Fe 259．940 nm，Mg 279．533 nm，Si 251．61 nm。실험용우급순 HCl 장대측용액조위산성，소제공업락산납용액산도불은정인기적측정오차，채용표준가입법소제기체간우，탐토료Al，Ca，Fe，Mg，Si등오충미량조분검측방법표준곡선선성상관성、검출한、정밀도이급회수솔등분석지표，상세연구료재선정분석보선하，표준가입법대락산납용액중Al，Ca，Fe，Mg，Si등미량잡질함량측정결과적준학성적영향。결과표명표준곡선정선성관계（R2＝0．9988～0．9996지간），오충원소검출한재（0．0134～0．0280）mg·L－1지간，11차측량표준편차소우5．86％，회수솔재97．30％～107．50％지간。실험건립적분석방법적검출한、정밀도、준학도균능만족분석측시요구；방법실용성강，이경성공용우리자막전해법중락산납원료액미량리자검측；이용락산납、중락산납화중락산항여용액산도적관계，실험건립적분석방법환가탁전우중락산납급락항심지기타륙개락산품중Al，Ca，Fe，Mg，Si 잡질리자적검측，동시야가이확전도상술양품중기타잡질원소적측정。
Coupled plasma atomic emission spectrometry (ICP-AES)was used to determine the trace impurities of Ca,Mg,Al, Fe and Si in industrial sodium chromate.Wavelengths of 167. 079,393. 366,259. 940,279. 533 and 251. 611 nm were selected as analytical lines for the determination of Al,Ca,Fe,Mg and Si,respectively.The analytical errors can be eliminated by adjus-ting the determined solution with high pure hydrochloric acid.Standard addition method was used to eliminate matrix effects. The linear correlation,detection limit,precision and recovery for the concerned trace impurities have been examined.The effect of standard addition method on the accuracy for the determination under the selected analytical lines has been studied in detail. The results show that the linear correlations of standard curves were very good (R2= 0. 998 8 to 0. 999 6)under the determined conditions.Detection limits of these trace impurities were in the range of 0. 013 4 to 0. 028 0 mg·L-1 .Sample recoveries were within 97. 30% to 107. 50%,and relative standard deviations were lower than 5. 86% for eleven repeated determinations.The detection limits and accuracies established by the experiment can meet the analytical requirements and the analytic procedure was used to determine trace impurities in sodium chromate by ion membrane electrolysis technique successfully.Due to sodium chro-mate can be changed into sodium dichromate and chromic acid by adding acids,the established method can be further used to mo-nitor trace impurities in these compounds or other hexavalent chromium compounds.