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Study of interferences and procedures for their removal in the spectrophotometric determination of ammonium and selected anions in coloured wastewater samples.
Analytical Methods ( IF 2.7 ) Pub Date : 2020-08-31 , DOI: 10.1039/d0ay01361g Andreea Oarga Mulec 1 , Ana Mladenovič , Alenka Mauko Pranjić , PrimoŽ Oprčkal , Janez Ščančar , Radmila Milačič
Analytical Methods ( IF 2.7 ) Pub Date : 2020-08-31 , DOI: 10.1039/d0ay01361g Andreea Oarga Mulec 1 , Ana Mladenovič , Alenka Mauko Pranjić , PrimoŽ Oprčkal , Janez Ščančar , Radmila Milačič
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Ammonium and selected anions were determined in wastewater samples with highly complex matrices by spectrophotometry using the reagent-kit method. For this purpose, the interferents of coloured compounds and S2−, SO32−, CO32− and Cl−, which are often present in wastewater samples, were systematically investigated in the spectrophotometric determination of ammonium, nitrate, chloride, sulphate, fluoride and phosphate. After this, innovative procedures for their removal were proposed. For sample decolourization, a DEAE column was used to determine ammonium, while a Florisil column was used for the colour removal and anions' determination. S2− and CO32− were eliminated from the samples by adding HCl or HNO3, which transformed them into gases H2S and CO2. The stepwise addition of CaCl2 to the sample, adjusted to pH 8, initiated the formation of CaSO3, which was removed by filtration. Cl− was removed by the addition of Ag2O, which formed a AgCl precipitate that was removed from the solution by filtration. The accuracy of the determination was tested with spike-recovery tests, which showed recoveries for the analytes in the spiked samples ranging from 95 to 105%. The repeatability of the measurements of nitrate, chloride, sulphate and phosphate in the wastewater samples was better than ±1%, while that for the ammonium and fluoride samples was ±2 and ±5%, respectively. The data from the present investigation revealed that the developed procedures for the decolourization and stepwise removal of interferents enabled accurate spectrophotometric determination of ammonium, nitrate, chloride, sulphate, fluoride and phosphate by using cuvette tests in complex wastewater and environmental water samples.
中文翻译：
在分光光度法测定有色废水样品中的铵和选定的阴离子中，研究干扰物和消除干扰物的方法。
使用试剂盒法通过分光光度法测定具有高度复杂基质的废水样品中的铵和选定的阴离子。为了这个目的，有色化合物和S的干扰2-，SO 3 2-，CO 3 2-和Cl - ，这往往存在于废水样品中，在分光光度法测定铵，硝酸盐，氯化物，硫酸盐进行了系统的研究，氟化物和磷酸盐。此后，提出了创新的清除程序。对于样品脱色，DEAE柱用于测定铵，而Florisil柱用于除色和阴离子的测定。S 2−和CO 3 2−通过添加HCl或HNO 3去除样品中的H2O，将其转化为气体H 2 S和CO 2。将CaCl 2逐步添加到样品中，调节至pH 8，开始形成CaSO 3，通过过滤将其除去。氯-通过Ag的添加除去2O，形成AgCl沉淀，将其通过过滤从溶液中除去。测定的准确性通过加标回收测试进行测试，加标回收测试显示加标样品中分析物的回收率在95％到105％之间。废水样品中硝酸盐，氯化物，硫酸盐和磷酸盐的测量重复性优于±1％，而铵和氟化物样品的重复性分别为±2和±5％。来自本次调查的数据表明，已开发出的用于脱色和逐步去除干扰物的程序，可以通过使用比色杯测试对复杂的废水和环境水样品进行准确的分光光度法测定铵，硝酸盐，氯化物，硫酸盐，氟化物和磷酸盐。
更新日期：2020-10-15
中文翻译：
在分光光度法测定有色废水样品中的铵和选定的阴离子中，研究干扰物和消除干扰物的方法。
使用试剂盒法通过分光光度法测定具有高度复杂基质的废水样品中的铵和选定的阴离子。为了这个目的，有色化合物和S的干扰2-，SO 3 2-，CO 3 2-和Cl - ，这往往存在于废水样品中，在分光光度法测定铵，硝酸盐，氯化物，硫酸盐进行了系统的研究，氟化物和磷酸盐。此后，提出了创新的清除程序。对于样品脱色，DEAE柱用于测定铵，而Florisil柱用于除色和阴离子的测定。S 2−和CO 3 2−通过添加HCl或HNO 3去除样品中的H2O，将其转化为气体H 2 S和CO 2。将CaCl 2逐步添加到样品中，调节至pH 8，开始形成CaSO 3，通过过滤将其除去。氯-通过Ag的添加除去2O，形成AgCl沉淀，将其通过过滤从溶液中除去。测定的准确性通过加标回收测试进行测试，加标回收测试显示加标样品中分析物的回收率在95％到105％之间。废水样品中硝酸盐，氯化物，硫酸盐和磷酸盐的测量重复性优于±1％，而铵和氟化物样品的重复性分别为±2和±5％。来自本次调查的数据表明，已开发出的用于脱色和逐步去除干扰物的程序，可以通过使用比色杯测试对复杂的废水和环境水样品进行准确的分光光度法测定铵，硝酸盐，氯化物，硫酸盐，氟化物和磷酸盐。
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