超声浸取-离子选择电极法测定银精矿中水溶性氯
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摘要
以水为溶剂超声浸取样品,加入适量0.25mol/L柠檬酸三钠-1mol/L硝酸钾溶液作为总离子强度调节剂,控制响应时间为5min,建立了离子选择电极法测定银精矿中水溶性氯的测定方法。对超声浸取的条件进行了优化,确定浸取条件如下:采用20mL水在水浴温度为50℃时对0.5g样品超声浸取15min。对测定条件进行了考察,结果表明,为减少电位的波动,保证测定结果的准确性,电极响应斜率S值的测定与样品测试均应在同一恒温体系下进行。在优化的实验条件下,氯离子在2～12μg/mL范围内其质量浓度的自然对数与电位值呈良好的线性关系,相关系数为0.9998,检出限为0.863μg/mL。选取两个银精矿样品,按实验方法分别平行测定6次,测定值与离子色谱法的测定值基本一致,相对标准偏差(RSD)为2.1%～2.8%。
The sample was leached by ultrasonic extraction using water as solvent.Proper amount of0.25 mol/L trisodium citrate-1 mol/L potassium nitrate solution was added as the total ion strength adjustment buffer.The time was controlled at 5 min.The determination method of water-soluble chloride in silver concentrate by ultrasonic extraction-ion selective electrode was established.The ultrasonic extraction con-ditions were optimized as follows:0.5 g of sample was treated by ultrasonic extraction for 15 min in 20 mL of water at bath temperature of 50℃.The determination conditions were also investigated.The results showed that the determination of S value(electrode response slope)and sample should be conducted in same constant temperature system in order to reduce the potential fluctuation and guarantee the accuracy of measurement results.Under optimized experimental conditions,the natural logarithm of mass concentration of chloride ion in range of 2-12μg/mL was in good linearity with the potential value.The correlation coefficient was 0.999 8 and the detection limit was 0.863μg/mL.Two silver concentrate samples were determined in parallel according to the experimental method.The found results were basically consistent with those obtained by the ion chromatography.The relative standard deviations(RSD,n=6)were between2.1%and 2.8%.
The sample was leached by ultrasonic extraction using water as solvent.Proper amount of0.25 mol/L trisodium citrate-1 mol/L potassium nitrate solution was added as the total ion strength adjustment buffer.The time was controlled at 5 min.The determination method of water-soluble chloride in silver concentrate by ultrasonic extraction-ion selective electrode was established.The ultrasonic extraction con-ditions were optimized as follows:0.5 g of sample was treated by ultrasonic extraction for 15 min in 20 mL of water at bath temperature of 50℃.The determination conditions were also investigated.The results showed that the determination of S value(electrode response slope)and sample should be conducted in same constant temperature system in order to reduce the potential fluctuation and guarantee the accuracy of measurement results.Under optimized experimental conditions,the natural logarithm of mass concentration of chloride ion in range of 2-12μg/mL was in good linearity with the potential value.The correlation coefficient was 0.999 8 and the detection limit was 0.863μg/mL.Two silver concentrate samples were determined in parallel according to the experimental method.The found results were basically consistent with those obtained by the ion chromatography.The relative standard deviations(RSD,n=6)were between2.1%and 2.8%.
引文
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[11]ASTM International.ASTMUOP991-2017Trace chloride,fluoride,and bromide in liquid organics by combustion ion chromatography(CIC)[S].West Conshohocken:UOP LLC,2017.
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[13]甘志勇,农耀京,彭靖茹,等.超声提取-石墨炉原子吸收光谱法测定土壤中有效态镉[J].理化检验:化学分册,2013,49(11):1315-1317.GAN Zhi-yong,NONG Yao-jing,PENG Jing-ru,et al.Ultrosonic extration-GF-AAS determination of available cadmium in soil[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2013,49(11):1315-1317.
[14]王恒,徐师,陈少亭,等.离子色谱法测定银精矿中氟和氯[J].铁合金,2018,49(2):41-44.WANG Heng,XU Shi,CHEN Shao-ting,et al.Determination of fluorine and chlorine concents in silver concentrates by ion chromatography[J].Ferro-alloys,2018,49(2):41-44.
[2]中华人民共和国国家质量监督检验检疫总局.SN/T2261-2009铁矿中水溶性氯化物的测定电位滴定法[S].北京:中国标准出版社,2009.
[3]中华人民共和国国家质量监督检验检疫总局.SN/T3919-2014铁矿石中水溶性氯化物含量的测定方法离子色谱法[S].北京:中国标准出版社,2014.
[4]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 6730.64-2007铁矿石水溶性氯化物含量的测定离子选择电极法[S].北京:中国标准出版社,2007.
[5]中华人民共和国国家质量监督检验检疫总局.SN/T3014-2011进出口铬矿石中氟和氯的测定离子选择电极法[S].北京:中国标准出版社,2011.
[6]张积锴,陈东英,邱小英,等.氯离子选择性电极-标准加入法测定碳酸稀土中氯[J].冶金分析,2017,37(4):22-26.ZHANG Ji-kai,CHEN Dong-ying,QIU Xiao-ying,et al.Determination of chlorine in rare earth carbonate by chloride ion selective electrode with standard addition method[J].Metallurgical Analysis,2017,37(4):22-26.
[7]Hirokazu Hara,Yoshiki Wakizaka,Satoshi Okazaki.Silver chloride pro-treatment for the direct potentionmetric determination of chloride in stream waters using a solidstate chloride ion-selective electrode[J].The Analyst,1985,110(9):1087-1090.
[8]黎香荣,黄园,赖天成.高温水解-离子色谱法测定有色金属矿中氟和氯[J].冶金分析,2018,38(2):53-58.LI Xiang-rong,HUANG Yuan,LAI Tian-cheng.Determination of fluoride and chloride in nonferrous metal ore by pyrohydrolysis-ion chromatography[J].Metallurgical Analysis,2018,38(2):53-58.
[9]Wang Qiaoyun,Makishima Akio,Nakamura Eizo.Determination of fluorine and chlorine by pyrohydrolysis and ion chromatography:Comparison with alkaline fusion digestion and ion chromatography[J].Geostandards and Geoanalytical Research,2010,34(2):175-183.
[10]ZHANG Shuai,ZHAO Tian-bo,WANG Jia,et al.Determination of fluorine,chlorine and bromine in household products by means of oxygen bomb combustion and ion chromatography[J].Journal of Chromatographic Science,2013,51(1):65-69.
[11]ASTM International.ASTMUOP991-2017Trace chloride,fluoride,and bromide in liquid organics by combustion ion chromatography(CIC)[S].West Conshohocken:UOP LLC,2017.
[12]史静,孟萌萌,路遥,等.电位滴定法测定铜精矿中氯[J].冶金分析,2016,36(10):52-56.SHI Jing,MENG Meng-meng,LU Yao,et al.Determination of chloride in copper concentrate by potentiometric titration[J].Metallurgical Analysis,2016,36(10):52-56.
[13]甘志勇,农耀京,彭靖茹,等.超声提取-石墨炉原子吸收光谱法测定土壤中有效态镉[J].理化检验:化学分册,2013,49(11):1315-1317.GAN Zhi-yong,NONG Yao-jing,PENG Jing-ru,et al.Ultrosonic extration-GF-AAS determination of available cadmium in soil[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2013,49(11):1315-1317.
[14]王恒,徐师,陈少亭,等.离子色谱法测定银精矿中氟和氯[J].铁合金,2018,49(2):41-44.WANG Heng,XU Shi,CHEN Shao-ting,et al.Determination of fluorine and chlorine concents in silver concentrates by ion chromatography[J].Ferro-alloys,2018,49(2):41-44.