自动电位滴定法测定工业氢氧化铝产品的纯度

doi:10.13228/j.boyuan.issn1000-7571.011893

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摘要氢氧化铝的纯度是工业氢氧化铝质量标准中重要的检测指标,建立一种准确的测定方法对工业氢氧化铝的质量控制具有重要意义。采用滴定法测定工业氢氧化铝产品的纯度时,Al³⁺易水解造成了Al³⁺的损失,且目视判断终点存在误差相对较大的问题,影响测定结果的准确度。通过控制前处理过程中溶液pH≤3,在pH≈3.0的乙酸-乙酸钠缓冲体系中,以EDTA络合Al³⁺,解决了Al³⁺水解易损失的问题;过量的EDTA以二甲酚橙为指示剂、用光度电极为指示电极,用氯化锌标准滴定溶液在590 nm波长下采用等步长滴定模式(MET)返滴定,建立了自动电位滴定法测定工业氢氧化铝产品纯度的方法。按照实验方法测定了阻燃剂氢氧化铝和水处理剂用氢氧化铝样品的纯度,测定结果的相对标准偏差(RSD,n=7)分别为0.06%和0.07%,结果与标准方法GB/T 4294—2010基本一致;测定阻燃剂氢氧化铝样品的加标回收率为99.66%～100.20%。

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	王瑞菲
	高爱红
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	王艳
	岳涛

关键词 ：自动电位滴定法, 光度电极, 氢氧化铝, 返滴定, EDTA, 氯化锌标准滴定溶液, 纯度

Abstract：The purity of aluminum hydroxide is an important detection index in the quality standards of industrial aluminum hydroxide products. It is of great significance to establish an accurate determination method for the quality control of industrial aluminum hydroxide. During the determination of industrial aluminum hydroxide product purity by titration, the easy hydrolysis of Al³⁺ will cause its loss. Moreover, there is a relatively large error in visual judgment of the endpoint, which also affects the accuracy of determination results. The pH of solution in pretreatment was controlled to not more than 3. Al³⁺ were complexed with EDTA in acetic acid-sodium acetate buffer solution at pH≈3.0, which solved the loss problem of Al³⁺ due to hydrolysis. Excessive EDTA was back-titrated with zinc chloride standard titration solution at 590 nm by monotonic titration (MET) mode using xylenol orange as indicator and photometric electrode as indicating electrode. The method for the determination of industrial aluminum hydroxide product purity by automatic potentiometric titration was established. The purity of flame-retardant and water treatment agent samples of aluminum hydroxide were determined according to the experimental method. The relative standard deviations (RSD, n=7) of determination results were 0.06% and 0.07%, respectively. The found results were basically consistent with those obtained by national standard method of GB/T 4294-2010. The recoveries of flame-retardant sample of aluminum hydroxide were between 99.66% and 100.20%.

Key words： automatic potentiometric titration photometric electrode aluminum hydroxide back titration EDTA zinc chloride standard titration solution purity

收稿日期: 2022-05-30

ZTFLH:	O655.2
	TF03+1

基金资助:山东省政府“泰山学者”建设工程(08190201)

通讯作者: 岳涛(1982—),男,研究员,博士,研究方向为化工产品研发与检测;E-mail:yuetao@iccas.ac.cn

作者简介: 王瑞菲(1986—),女,工程师,硕士,研究方向为化工产品研发与检测;E-mail:hg076@qust.edu.cn

引用本文:

王瑞菲, 高爱红, 刘友彬, 王艳, 岳涛. 自动电位滴定法测定工业氢氧化铝产品的纯度[J]. 冶金分析, 2023, 43(1): 82-87. WANG Ruifei, GAO Aihong, LIU Youbin, WANG Yan, YUE Tao. Determination of industrial aluminum hydroxide purity by automatic potentiometric titration. , 2023, 43(1): 82-87.

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http://yjfx.chinamet.cn/CN/10.13228/j.boyuan.issn1000-7571.011893 或 http://yjfx.chinamet.cn/CN/Y2023/V43/I1/82

[1] 汪世侯.工业氢氧化铝中三氧化二铝的直接测定[J].铀矿冶,1996,15(2):136-139.
WANG Shihou.Determining directly aluminium oxide in technical purity aluminium hydroxide[J].Uranium Mining and Metallurgy,1996,15(2):136-139.
[2] 张晓霞,王瑞菲,唐晓婵,等.氢氧化铝反应液中铝离子含量的测定[J].轻金属,2020(4):56-58.
ZHANG Xiaoxia,WANG Ruifei,TANG Xiaochan,et al.Determination of aluminum ion content in aluminum hydroxide reaction solution[J].Light Metals,2020(4):56-58.
[3] 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 4294—2010氢氧化铝[S].北京:中国标准出版社,2011.
[4] 中华人民共和国国家质量监督检验检疫总局,中华人民共和国工业和信息化部.HG/T 4530—2013氢氧化铝阻燃剂[S].北京:中国标准出版社,2013.
[5] 中华人民共和国国家质量监督检验检疫总局,中华人民共和国工业和信息化部.HG/T 5567—2019水处理剂用氢氧化铝[S].北京:中国标准出版社,2019.
[6] 曾莉,黄定芳,古星,等.氢氧化铝中氧化铝含量测定的几种方法比较[J].四川理工学院学报(自然科学版),2010,23(5):583-585.
ZENG Li,HUANG Dingfang,GU Xing,et al.Comparison between the three methods of determining for the amount of aluminum oxide in aluminum hydroxide[J].Journal of Sichuan University of Science ＆ Engineering (Natural Science Edition),2010,23(5):583-585.
[7] 刘向阳,金斌.一种快速测定无机包膜钛白粉用氢氧化铝中氧化铝含量的方法[J].中国涂料,2017,32(4):71-73.
LIU Xiangyang,JIN Bin.A method for rapid determination of alumina content in aluminum hydroxide for inorganic coated titanium dioxide[J].China Coatings,2017,32(4):71-73.
[8] 杨燕强,张鑫鑫,赵发宝.棕刚玉中氧化铝含量的快速测定[J].检验检疫学刊,2009,19(2):31-32.
YANG Yanqiang,ZHANG Xinxin,ZHAO Fabao.The rapid determination of aluminum oxide in brown corundum[J].Journal of Inspection and Quarantine,2009,19(2):31-32.
[9] 贺晓唯,毕诗文,周金海.铝酸钠溶液中苛性碱、碳酸碱和氧化铝含量的连续测定[J].吉林大学学报(理学版),2006,44(5):821-823.
HE Xiaowei,BI Shiwen,ZHOU Jinhai.Determination of caustic hydroxide sodium carbonate and alumna in sodium aluminate solutions[J].Journal of Jilin University(Science Edition),2006,44(5):821-823.
[10] 黎香荣,罗明贵,黄园,等.光度滴定法测定铜精矿中铜[J].冶金分析,2020,40(5):31-36.
LI Xiangrong,LUO Minggui,HUANG Yuan,et al.Determination of copper in copper concentrate by photometric titration[J].Metallurgical Analysis,2020,40(5):31-36.
[11] 黎香荣,罗明贵,黄园,等.自动光度滴定法测定铅精矿中铅含量[J].化工设计通讯,2020,46(1):73-74.
LI Xiangrong,LUO Minggui,HUANG Yuan,et al.Determination of lead content in lead concentrate by automatic photometric titration[J].Chemical Engineering Design Communications,2020,46(1):73-74.
[12] Ziółkowska D,Lamkiewicz J,Shyichuk A.Determination of sodium dodecyl sulfate by means of photometric titration with o-toluidine blue dye[J].J.Surfact.Deterg.,2018,21(5):751-756.
[13] 董绍楠.水溶液中铝离子水解-络合反应和铝矿物溶解机制的密度泛函理论研究[D].南京:南京大学,2019.
[14] 中华人民共和国国家质量监督检验检疫总局,中华人民共和国工业和信息化部.GB/T 601—2016化学试剂标准滴定溶液的制备[S].北京:中国标准出版社,2016.
[15] 朱志平.铝盐(铁盐)混凝过程行为分析与最佳pH值预测[J].水处理技术,1993,19(2):51-58.
ZHU Zhiping.The process analyzing and the optimum pH predicting of the coagulation of aluminum (and ferric) salts[J].Technology of Water Treatment,1993,19(2):51-58.