电位滴定法测定齿轮酸蚀检测用酸蚀液、漂白液总酸度
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摘要
准确测定使用过程中的齿轮酸蚀检测用酸蚀液、漂白液的总酸度,对于判定齿轮酸蚀检测用酸蚀液、漂白液能否继续使用具有重要意义。实验通过加入10mL草酸钠饱和溶液以有效掩蔽溶液中的Fe2+和Fe3+,采用0.5mol/L氢氧化钠标准滴定溶液进行滴定,选取滴定过程中第1个等当点EP1为滴定终点,实现了电位滴定法对齿轮酸蚀检测用酸蚀液、漂白液总酸度的测定。采用实验方法对未使用的、使用7d的、使用14d的齿轮酸蚀检测用酸蚀液、漂白液总酸度进行测定,并进行加标回收试验,结果表明,这3种样品测定结果的相对标准偏差(RSD,n=6)均小于1.0%,加标回收率分别在99%~102%、98%~102%之间。分别采用实验方法和手动酸碱滴定法对使用14d的齿轮酸蚀检测用酸蚀液和漂白液总酸度进行测定,测定结果基本一致。
The accurate determination of total acidity of acid etching solution and bleaching solution for acid etching detection of gear has important significance to decide that whether the acid etching solution and bleaching solution for acid etching detection of gear can be further used or not.10 mL of saturated sodium oxalate solution was added to effectively mask the Fe2+and Fe3+.The sample solution was titrated with0.5 mol/L sodium hydroxide standard titration solution.The first equivalent point(EP1)in titration process was selected as the titration endpoint,realizing the determination of total acidity of acid etching solution and bleaching solution for acid etching detection of gear by potentiometric titration.The total acidity of acid etching solution and bleaching solution(unused,used for 7 dand used for 14 d)was determined according to the experimental method.The recovery tests were also performed.The results showed that the relative standard deviations(RSD,n=6)of three samples were all less than 1.0%.The recoveries were99%-102% and 98%-102%,respectively.The total acidity of acid etching solution and bleaching solution for acid etching detection of gear(used for 14 d)was determined by the experimental method and manual acid-base titration,and the found results were basically consistent.
The accurate determination of total acidity of acid etching solution and bleaching solution for acid etching detection of gear has important significance to decide that whether the acid etching solution and bleaching solution for acid etching detection of gear can be further used or not.10 mL of saturated sodium oxalate solution was added to effectively mask the Fe2+and Fe3+.The sample solution was titrated with0.5 mol/L sodium hydroxide standard titration solution.The first equivalent point(EP1)in titration process was selected as the titration endpoint,realizing the determination of total acidity of acid etching solution and bleaching solution for acid etching detection of gear by potentiometric titration.The total acidity of acid etching solution and bleaching solution(unused,used for 7 dand used for 14 d)was determined according to the experimental method.The recovery tests were also performed.The results showed that the relative standard deviations(RSD,n=6)of three samples were all less than 1.0%.The recoveries were99%-102% and 98%-102%,respectively.The total acidity of acid etching solution and bleaching solution for acid etching detection of gear(used for 14 d)was determined by the experimental method and manual acid-base titration,and the found results were basically consistent.
引文
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[10]李超群,田宗平,曹健,等.游离酸测定过程中金属离子水解干扰和配位剂掩蔽的探讨[J].冶金分析,2016,36(5):69-75.LI Chao-qun,TIAN Zong-ping,CAO Jian,et al.Discussion on the hydrolysis interference of metallic ion and masking of coordination agent in measurement of free acid[J].Metallurgical Analysis,2016,36(5):69-75.
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[12]詹柏熙.硝酸铁溶液中游离酸的测定[J].四川化工与腐蚀控制(Sichuan Chemical Industry),1998,1(1):25-26.
[2]宋亚虎,孙胜伟,刘铁山,等.磁弹法在线监测渗碳齿轮的磨削烧伤[J].理化检验:物理分册,2015,51(12):853-857.SONG Ya-hu,SUN Sheng-wei,LIU Tie-shan,et al.Online detecting carburized gear grinding burn by magnetoelastic method[J].Physical Testing and Chemical Analysis Part A:Physical Testing,2015,51(12):853-857.
[3]孔德群,孔新建.18CrNiMo7-6钢齿轮磨削烧伤裂纹分析[J].金属加工:热加工(MV Metal Form),2016(19):20-24.
[4]朱正德.零部件的磨削烧伤检测及应用分析[J].现代零部件(Modern Components),2013(11):46-48.
[5]宋秀琴,苏磊,石磊.凸轮磨削烧伤的产生原因与解决措施[J].机械制造(Machinery),2017,55(3):75-76.
[6]鞍钢钢铁研究所,沈阳钢铁研究所.实用冶金分析方法与基础[M].沈阳:辽宁科学技术出版社,1990:782.
[7]郭志英,萧仙梅.电位滴定中和法连续测定电解液中酸、铁和铜[J].冶金分析(Metallurgical Analysis),1995,15(1):51-52.
[8]蔡璐,胡正阳,李海栋,等.自动电位滴定法测定冷轧薄板酸洗液中总酸度[J].中国无机分析化学,2013,3(1):44-46.CAI Lu,HU Zheng-yang,LI Hai-dong,et al.Determination of total acidity of acidic washing solution for cold-rolled thin sheet by automatic potentiometric titration method[J].Chinese Jorunal of Inorganic Analytical Chemistry,2013,3(1):44-46.
[9]李艳霞,谢东坡,任凯.自动电位滴定法在果蔬汁饮料总酸度测定中的应用[J].安徽农业科学,2009,37(36):18155-18156,18261.LI Yan-xia,XIE Dong-po,REN Kai.Application of automatic porentionmetric titration determination of total acidity in fruit and vegetable juices[J].Journal of Anhui Agricultural Sciences,2009,37(36):18155-18156,18261.
[10]李超群,田宗平,曹健,等.游离酸测定过程中金属离子水解干扰和配位剂掩蔽的探讨[J].冶金分析,2016,36(5):69-75.LI Chao-qun,TIAN Zong-ping,CAO Jian,et al.Discussion on the hydrolysis interference of metallic ion and masking of coordination agent in measurement of free acid[J].Metallurgical Analysis,2016,36(5):69-75.
[11]Graham T T Gibson,Mark F Mohamed,Alexei A,et al.Potentiometric titration of metal ions in ethanol[J].Inorganic Chemistry,2006,45(19):7891-7902.
[12]詹柏熙.硝酸铁溶液中游离酸的测定[J].四川化工与腐蚀控制(Sichuan Chemical Industry),1998,1(1):25-26.