离子色谱法测定固体废弃物中氨氮、亚硝酸盐氮和硝酸盐氮

Determination of ammonia nitrogen,nitrite nitrogen and nitrate nitrogen in solid waste by ion chromatography

建立离子色谱法测定固体废弃物中氨氮、亚硝酸盐氮和硝酸盐氮的方法。优化了前处理方法,取固体废弃物样品50.0 g,加入0.01 mol/L CaCl2溶液250 mL,振荡浸提60 min,静置10 min,取上层清液30 mL,以3000 r/min离心10 min,取上层清液经0.22μm滤膜过滤,采用Ion Pac CS12A型阳离子和Ion Pac AS19型阴离子色谱柱进行分析。待测物的质量浓度在0.0~5.0μg/mL的范围内与色谱峰面积线性关系良好,线性相关系数不小于0.9994,方法检出限为0.004~0.007 mg/kg。样品加标回收率为95.0%~100.1%,测定结果的相对标准偏差为0.80%~4.78%(n=6)。该方法灵敏度高,重复性良好,优化了标准检测方法,为快速、准确、高效检测固体废弃物样品提供了可靠的技术支撑。

A method for the determination of ammonia nitrogen,nitrite nitrogen and nitrate nitrogen in solid waste by ion chromatography was established.The pretreatment method was optimized,50.0 g of solid waste sample was added with 250 mL of 0.01 mol/L CaCl2 solution,then shaken and leached for 60 min,and allowed to stand for 10 min.The supernatant was taken at 30 mL and centrifuged at 3000 r/min for 10 min.The supernatant was filtered with 0.22μm filter and analyze by using Ion Pac CS12A cation and Ion Pac AS19 anion chromatography column.The mass concentration of ammonia nitrogen,nitrite nitrogen and nitrate nitrogen had a good linear relationship with chromatographic peak area in the range of 0.0-5.0μg/mL,the linear correlation coefficient was not less than 0.9994,and the detection limit of the method was 0.004-0.007 mg/kg.The recovery rate was 95.0%-100.1%,and the coefficient of variation was 0.80%-4.78%(n=6).The method has high sensitivity,good repeatability,optimized the standard detection method,and provide a reliable technical support for rapid,accurate and efficient detection of solid waste samples.