自动电位滴定法测定铝合金铬酸阳极化溶液中氯离子含量
|
摘要
移取铬酸阳极化溶液5.00 mL置于150 mL烧杯中,加入硝酸(1+1)溶液10 mL,100g·L~(-1)抗坏血酸溶液10.0mL,摇匀,使Cr~(6+)完全还原为Cr~(3+)以消除铬酸的干扰,加水至体积为60mL,在40~50r·min~(-1)的搅拌速率下,以0.010mol·L~(-1)硝酸银标准溶液作为滴定剂,采用自动电位滴定法测定溶液中的氯离子。采用该方法分析氯离子质量浓度为0.200,0.500,1.00g·L~(-1)的铬酸阳极化溶液以及3批生产线实际样品,测定值的相对标准偏差(n=6)在0.51%~3.0%之间。针对3批生产线实际样品进行加标回收试验,回收率在97.0%~102%之间。
The chromic acid anodizing solution(5.00 mL)was transferred into a beaker of 150 mL,then 10 mL of HNO_3(1+1)solution,10.0 mL of 100 g·L~(-1) ascorbic acid solution were added.The solution was mixed well to make Cr~(6+)completely reduced to Cr~(3+)to eliminate the interference of chromic acid.Water was added to make the volume of the solution up to 60 mL.Cl~- in the solution was determined by automatic potentiometric titration,using 0.010 mol·L~(-1) AgNO_3 standard solution as titrant at a stirring rate of 40-50 r·min~(-1).The proposed method was applied to analysis of chromic acid anodizing solution containing Cl~- of 0.200,0.500,1.00 g·L~(-1) and 3 batches of substantial samples from production lines,giving RSDs(n=6)ranged from 0.51%to 3.0%.Recovery tests of 3 batches of substantial samples from production lines were performed by standard addition method,and values of recovery were in the range of 97.0%-102%.
The chromic acid anodizing solution(5.00 mL)was transferred into a beaker of 150 mL,then 10 mL of HNO_3(1+1)solution,10.0 mL of 100 g·L~(-1) ascorbic acid solution were added.The solution was mixed well to make Cr~(6+)completely reduced to Cr~(3+)to eliminate the interference of chromic acid.Water was added to make the volume of the solution up to 60 mL.Cl~- in the solution was determined by automatic potentiometric titration,using 0.010 mol·L~(-1) AgNO_3 standard solution as titrant at a stirring rate of 40-50 r·min~(-1).The proposed method was applied to analysis of chromic acid anodizing solution containing Cl~- of 0.200,0.500,1.00 g·L~(-1) and 3 batches of substantial samples from production lines,giving RSDs(n=6)ranged from 0.51%to 3.0%.Recovery tests of 3 batches of substantial samples from production lines were performed by standard addition method,and values of recovery were in the range of 97.0%-102%.
引文
[1]曾台彪,李立清.铝及其铝合金阳极氧化及电解着色工艺的研究进展[J].电镀与精饰,2007,29(5):21-24.
[2]王邈.铝锂合金铬酸阳极化工艺适用性研究[J].上海涂料,2011,49(8):16-18.
[3]孙振起,黄明辉.航空用铝合金表面处理的研究现状与展望[J].材料导报A:综述篇,2011,25(12):146-151.
[4]孙擎擎,孙睿吉,陈送义,等.大气污染物对7B50铝合金电化学腐蚀性能的影响[J].中国有色金属学报,2015,25(3):575-581.
[5]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.
[6]唐维学,赖心.离子选择电极法测定镀铬液中氯的研究[J].冶金标准化与质量,2007,45(2):24-26.
[7]白华,黄旭,施先义.氯离子选择电极法测定锌铟电解液中氯含量[J].理化检验-化学分册,2011,47(9):1117-1118.
[8]卢振国,黄文娴,彭速标,等.自动电位滴定法测定铁矿中水溶性氯化物[J].理化检验-化学分册,2007,43(9):732-734.
[9]宋晓红,高姗,杨杰,等.自动电位滴定法测定脱硫系统中氯化物[J].理化检验-化学分册,2011,47(6):684-686.
[10]胡清启,孙宁.自动电位滴定法测定工业铬酸酐中氯离子含量方法研究[J].浙江化工,2015,46(8):52-54.
[11]GB/T 3051-2000无机化工产品中氯化物含量测定的通用方法汞量法[S].
[12]夏玉宇.化验员实用手册[M].北京:化学工业出版社,2000:569-570.
[13]高俊伟,黄银波,陈妍.离子色谱测定铬酸钾中微量硫酸根和氯离子[J].化学试剂,2013,35(9):820-822.
[14]王少明.离子色谱法测定铬酸酐中的微量F-、SO42-、Cl-[J].化学分析计量,2002,11(1):18-20.
[15]GB/T 601-2002化学试剂标准滴定溶液的制备[S].
[16]戚淑芳,张杰,王莹,等.以抗坏血酸作还原滴定剂电位滴定法测定铁矿石中全铁[J].冶金分析,2011,31(5):63-66.
[2]王邈.铝锂合金铬酸阳极化工艺适用性研究[J].上海涂料,2011,49(8):16-18.
[3]孙振起,黄明辉.航空用铝合金表面处理的研究现状与展望[J].材料导报A:综述篇,2011,25(12):146-151.
[4]孙擎擎,孙睿吉,陈送义,等.大气污染物对7B50铝合金电化学腐蚀性能的影响[J].中国有色金属学报,2015,25(3):575-581.
[5]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.
[6]唐维学,赖心.离子选择电极法测定镀铬液中氯的研究[J].冶金标准化与质量,2007,45(2):24-26.
[7]白华,黄旭,施先义.氯离子选择电极法测定锌铟电解液中氯含量[J].理化检验-化学分册,2011,47(9):1117-1118.
[8]卢振国,黄文娴,彭速标,等.自动电位滴定法测定铁矿中水溶性氯化物[J].理化检验-化学分册,2007,43(9):732-734.
[9]宋晓红,高姗,杨杰,等.自动电位滴定法测定脱硫系统中氯化物[J].理化检验-化学分册,2011,47(6):684-686.
[10]胡清启,孙宁.自动电位滴定法测定工业铬酸酐中氯离子含量方法研究[J].浙江化工,2015,46(8):52-54.
[11]GB/T 3051-2000无机化工产品中氯化物含量测定的通用方法汞量法[S].
[12]夏玉宇.化验员实用手册[M].北京:化学工业出版社,2000:569-570.
[13]高俊伟,黄银波,陈妍.离子色谱测定铬酸钾中微量硫酸根和氯离子[J].化学试剂,2013,35(9):820-822.
[14]王少明.离子色谱法测定铬酸酐中的微量F-、SO42-、Cl-[J].化学分析计量,2002,11(1):18-20.
[15]GB/T 601-2002化学试剂标准滴定溶液的制备[S].
[16]戚淑芳,张杰,王莹,等.以抗坏血酸作还原滴定剂电位滴定法测定铁矿石中全铁[J].冶金分析,2011,31(5):63-66.