1. Jiangxi Province Mass Spectrometry Science and Instrumentation Key Laboratory, Nanchang 330013, China; 2. Donghua University of Technology, Nanchang 330013, China
Abstract：During the determination of chlorine ion in rock ore sample by mercury nitrate titration method, the pretreatment usually includes many steps such as deionized water soaking, oscillation extraction and filtration. The operation procedures are long, and the samples are easily polluted and hardly filtrated. The determination of chlorine ion in quartz sandstone by ultrasonic extraction-mercury nitrate titration method was studied. The national standard rock sample GBW07106 was treated by ultrasonic extraction, standing and centrifugal separation. The content of chlorine ion in centrifugate was determined by mercury nitrate titration. Then the content of chlorine in quartz sandstone could be calculated. The following pretreatment conditions were obtained by experiments: the sample was treated by ultrasonic extraction for 2h; aluminum potassium sulfate was employed as the extraction agent; the extraction time was 30min; the centrifugal separation time was 10min. The interference of chromate (＞10mg/L) and Fe3+ (＞140mg/L) could be eliminated by adding 2mL of 100g/L hydroquinone solution. For the interference of sulfide and sulfite (＞10mg/L), the solution was firstly adjusted to alkalescence using sodium hydroxide followed by adding 1mL of 30% hydrogen peroxide. After shaking, the residual hydrogen peroxide was removed by heating to eliminate its interference to the determination of Cl-. The proposed method was applied for the determination of quartz sandstone. The relative standard deviation (RSD, n=5) of results was 5.5% and 6.2%, respectively. The recoveries were between 97% and 103%.
聂全新,陶文靖,胡兰.土壤中氯的比色测定[J].安徽地质,2014,24(3):215-216.NEI Quan-xin,TAO Wen-jing,HU Lan.Colorimetric determination of chlorine in huran soil[J].Anhui Geology,2014,24(3):215-216.
[2]
尹台芳,李多容,宗杰.离子选择电极法测定镁粉中氯离子[J].冶金分析,2017,37(10):70-73.YIN Tai-fang,LI Duo-rong,ZONG Jie.Determination of chloride ions in magnesium powder by ion selective electrode method[J].Metallurgical Analysis,2017,37(10):70-73.
[3]
古映莹,苏莎,杨天足,等.离子选择电极法测定电铅灰中氟与氯[J].冶金分析,2012,32(8):55-58.GU Ying-ying,SU Sha,YANG Tian-zu,et al.Determination of fluorine and chlorine in electric lead ash by ion selective electrode method[J].Metallurgical Analysis,2012,32(8):55-58.
[4]
钱庆长,史静,周颖,等.硝酸银自动电位滴定法测定铜电解液中氯离子时稳定剂的影响[J].冶金分析,2016,36(3):35-38.QIAN Qing-chang,SHI Jing,ZHOU Ying,et al.Effects of silver nitrate automatic potentiometric titration on the determination of chlorine ion stabilizer in copper electrolyte[J].Metallurgical Analysis,2016,36(3):35-38.
[5]
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.Chlorine ion selective electrode-standard addition method in the determination of rare earth carbonate chloride[J].Metallurgical Analysis,2017,37(4):22-26.
[6]
胡一航,王海北,王玉芳.水蒸气蒸馏-离子色谱法测定湿法炼锌溶液中氟和氯[J].冶金分析,2015,35(5):59-62.HU Yi-hang,WANG Hai-bei,WANG Yu-fang.Determination of fluorine and chlorine metallurgy in zinc hydrometallurgical zinc solution by steam distillation-ion chromatography[J].Metallurgical Analysis,2015,35(5):59-62.
[7]
姜傲璐,安秀菊.氯离子测定方法研究[J].现代工业经济和信息化,2017,7(4):78-79.JIANG Ao-lu,AN Xiu-ju.Research on determination methods of chlorine ions[J].Modern Industrial Economy and Information Technology,2017,7(4):78-79.
[8]
郝志宁.水中氯离子的测定方法及其研究进展[J].环境科学与管理,2016,41(5):162-164.HAO Zhi-ning.Determination methods and research progress of chlorine ions in water[J]. Environmental Science and Management,2016,41(5):162-164.
[9]
安泰莹,文庆珍,朱金华.氯离子测定方法研究进展[J].河南化工,2013,30(3-4):8-11.AN Tai-ying,WEN Qing-zhen,ZHU Jin-hua.Research progress of chloride ion determination methods[J].Henan Chemical Industry,2013,30(3-4):8-11.
[10]
苏金飞.硫氰酸汞-硫酸高铁铵分光光度法测定混凝土减水剂中氯离子含量的方法研究[J].中国建材科技,2018,27(2):1-4.SU Jin-fei.Determination of chloride ion in concrete water reducing agent by mercuric thiocyanate-ammonium ferrium sulfate spectrophotometry[J].China Building Materials Technology,2018,27(2):1-4.
[11]
刘玮,刘英,阳兆鸿.碱熔-离子色谱法测定次氧化锌中的氯离子[J].矿冶,2015,24(2):78-80.LIU Wei,LIU Ying,YANG Zhao-hong.Determination of chloride ions in zinc oxide by alkali fusion ion chromatography[J].Mineral Smelting,2015,24(2):78-80.
