焦硫酸钾碱熔在EDTA滴定法测定铝灰渣中铝中的应用

doi:10.13228/j.boyuan.issn1000-7571.011609

摘要
图/表
参考文献
相关文章 (15)

全文: PDF (536 KB) HTML (1 KB)
输出: BibTeX | EndNote (RIS)

摘要近年来随着铝资源的逐渐紧缺,加紧对铝灰渣中铝资源的回收利用变得日益重要,所以准确测定铝灰渣中铝含量十分重要。由于铝灰渣中铝的存在形态多样而导致样品难以熔解,而且铝灰渣中氟含量高,目前已报道的采用氢氧化钾和氢氧化钠熔解样品后使用EDTA滴定法测定铝时,结果容易偏低。将铝灰渣样品置于铂坩埚中,加入8 g焦硫酸钾试剂,于725 ℃±25 ℃的马弗炉中保温熔融20~25 min至样品熔融完全。由于焦硫酸钾高温熔融样品时冒硫酸烟,从而可以完全驱除样品中F^—。再将样品溶解后加入EDTA,用锌标准滴定溶液滴定过量的EDTA,然后用F^—置换出与铝络合的EDTA,再用锌标准滴定溶液滴定置换出的EDTA,从而得出铝含量。按照实验方法测定两个铝灰渣样品中铝,测定结果的相对标准偏差(RSD,n=9)分别是0.16%和0.34%,加标回收率为98.7%~101%。实验有效解决了铝灰渣样品难以熔解和高含量氟的干扰使得EDTA滴定法测定铝含量时测定结果偏低的问题,适用于成分复杂且铝和氟含量均高的铝灰渣中铝含量测定。

	服务

	把本文推荐给朋友
	加入我的书架
	加入引用管理器
	E-mail Alert
	RSS
	作者相关文章
	黄葡英
	唐清
	李雨

关键词 ：焦硫酸钾, 碱熔, 铝灰渣, 铝, EDTA滴定法, 氟

Abstract：With the gradual shortage of aluminum resources in recent years,the recycling of aluminum resources in aluminum dross becomes increasingly important.Thus,it is of great significance for the determination of aluminum content in aluminum dross.Since there are various existing forms of aluminum,the aluminum dross is difficult to be dissolved.Moreover,the content of fluorine in aluminum dross is high,if the sample is dissolved with potassium hydroxide and sodium hydroxide for the determination of aluminum by EDTA titration,the results are usually lower. The aluminum dross sample was placed in platinum crucible.After adding 8 g of potassium pyrosulfate,the crucible was heated in a muffle furnace at 725 ℃±25 ℃ for 20-25 min to completely melt the sample.Since sulfuric acid smoke occurred during high temperature fusion of sample by pot assium pyrosulfate, F^- ions in sample could be fully removed.After dissolving the sample again,EDTA solution was added.The excessive EDTA was titrated by zinc standard titration solution.Then the EDTA complexed with aluminum was replaced with F^-,which was then titrated by zinc standard titration solution.Thus,the content of aluminum could be obtained.The contents of aluminum in two aluminum dross samples were determined according to the experimental method.The relative standard deviation (RSD, n=9) of the measured values was 0.16% and 0.34%,respectively.The spiked recoveries were between 98.7% and 101%.The proposed method effectively solved the problems that the aluminum dross samples were hardly dissolved and the interference of high fluoride content to cause lower determination results of aluminum.It was suitable for the determination of aluminum content in aluminum dross with complicated composition and high content of aluminum and fluorine.

Key words： potassium pyrosulfate alkali fusion aluminum dross aluminum EDTA titration fluorine

收稿日期: 2021-08-19

ZTFLH:	O655.2
	TF801+.3

基金资助:国家自然科学基金青年基金项目(52001074);2021年广东省省属科研机构改革创新领域稳定支持项目;广州市科技计划项目(202102020626);广东省科学院建设国内一流研究机构行动专项资金项目(2021GDASYL20210103086)

通讯作者: 李雨(1989—),男,高级工程师,博士,研究方向为材料化学分析;E-mail:yuli11s@alum.imr.ac.cn

作者简介: 黄葡英(1982—),女,高级工程师,大学本科,研究方向为矿物分析、冶金分析等;E-mail:254623348@qq.com

引用本文:

黄葡英, 唐清, 李雨. 焦硫酸钾碱熔在EDTA滴定法测定铝灰渣中铝中的应用[J]. 冶金分析, 2022, 42(5): 55-60. HUANG Puying, TANG Qing, LI Yu. Application of potassium pyrosulfate alkali fusion in determination of aluminum in aluminum dross by EDTA titration. , 2022, 42(5): 55-60.

链接本文:

http://yjfx.chinamet.cn/CN/10.13228/j.boyuan.issn1000-7571.011609 或 http://yjfx.chinamet.cn/CN/Y2022/V42/I5/55

[1] 石志平,姜澜,杨洪亮,等.铝灰的回收处理及资源化利用研究现状[J].无机盐工业,2020,52(9):21-25.
SHI Zhiping,JIANG Lan,YANG Hongliang,et al.Research status of recycling and resource utilization of aluminum dross[J].Inorganic Chemicals Industry, 2020,52(9):21-25.
[2] 梁诚,彭建平,狄跃忠,等.铝灰中铝及其氧化物回收方法现状[J].资产保护与利用,2019,39(3):37-41.
LIANG Cheng,PENG Jianping,DI Yuezhong,et al.Research status of recovery methods of aluminum and its oxide in aluminum ash[J].Conservation and Utilization of Mineral Resources,2019,39(3):37-41.
[3] Shen H,Liu B,Ekberg C,et al.Harmless disposal and resource utilization for secondary aluminum dross:A review[J].Science of The Total Environment,2020,760:143968.
[4] 张景超.微波消解-石墨炉原子吸收光谱法检测食品中的铝[J].食品界(Shi Pin Jie),2018(8):137.
[5] SUN M,WU Q.Determination of ultra-trace aluminum in human albumin by cloud point extraction and graphite fernace atomic absorption spectrometry[J].Journal of Hazardous Materials,2010,176(1):901-905.
[6] 邢书才,李风华,赵彦辉,等.分光光度法测定水中铝的比对分析及方法评价[J].应用化工,2018,47(1):199-202.
XING Shucai,LI Fenghua,ZHAO Yanhui,et al.The contrastive analysis and method evaluation of the determination of aluminum in water by spectrophotometry[J].Applied Chemical Industry,2018,47(1):199-202.
[7] 李帆,杨春晟,丁妍,等.称量定容-ICP-AES法测定纯铁中痕量铝、铬、铜、锰、镍和硅[J].分析试验室,2019(5):542-547.
LI Fan,YANG Chunsheng,DING Yan,et al.Determination of trace Al,Cr,Cu,Mn,Ni,Si in pure iron by ICP-AES with mass dilution method[J].Chinese Journal of Analysis Laboratory,2019(5):542-547.
[8] 赵广开.EDTA连续滴定法测定铝土矿、赤泥中氧化铝含量的改进方法研究[J].铝镁通讯(Lvmei Tongxun),2008(2):33-35.
[9] 程宏伟.铝灰中的三氧化二铝的测定[J].新疆有色金属(Xinjiang Youse Jinshu),2014,37(7):135-136.
[10] 杨忠梅,李静.EDTA滴定法测定铝灰中金属铝[J].冶金分析,2020,40(9):87-91.
YANG Zhongmei,LI Jing.Determination of metallic aluminum in aluminum ash by EDTA titrimetry[J].Metallurgical Analysis,2020,40(9):87-91.
[11] 国家发展和改革委员会,全国有色金属标准化技术委员会.YS/T 575.1—2007 铝土矿石化学分析方法第1部分氧化铝含量的测定 EDTA滴定法[S].北京:中国标准出版社,2008.
[12] 国家发展和改革委员会,全国有色金属标准化技术委员会.YS/T 581.4—2006 氟化铝化学分析方法和物理性能测定方法第4部分:EDTA容量法测定铝含量[S].北京:中国标准出版社,2006.
[13] 张晨.碱消解-电感耦合等离子体原子发射光谱(ICP-AES)法测定铝灰中铝[J].中国无机分析化学,2020,10(5):24-27.
ZHANG Chen.Determination of aluminum in aluminum ash by inductively coupled plasma atomic emission spectrometry with alkaline digestion[J].Chinese Journal of Inorganic Analytical Chemistry,2020,10(5):24-27.
[14] 丛琳琳,王凡,田小亭,等.电感耦合等离子体原子发射光谱法测定铝生产过程固体废弃物铝灰中金属铝和氧化铝[J].冶金分析,2018,38(11):43-47.
CONG Linlin,WANG Fan,TIAN Xiaoting,et al.Determination of metallic aluminum and aluminum oxide in solid waste aluminum as generated in aluminum production process by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2018,38(11):43-47.