基于水溶性探针法测镁的高纯碳酸锂快速质检

doi:10.19964/j.issn.1006-4990.2022-0276

无机盐工业 ›› 2023, Vol. 55 ›› Issue (1): 87-92.doi: 10.19964/j.issn.1006-4990.2022-0276

基于水溶性探针法测镁的高纯碳酸锂快速质检

李岩¹(),王岩松¹,成怀刚^1,³(),康锦^1,²,李恩泽¹,吕宏洲¹,刘倩⁴

1.山西大学资源与环境工程研究所, 山西太原 030006
2.晋中学院化学化工系, 山西晋中 030619
3.青海大学化工学院, 青海西宁 810016
4.山西大地生态环境技术研究院有限公司, 山西太原 030006

收稿日期:2022-05-20 出版日期:2023-01-10 发布日期:2023-01-17
作者简介:李岩（1996— ），女，硕士研究生，研究方向为无机盐资源循环工程；E-mail：18856123825@163.com。
基金资助:
国家自然科学基金区域创新发展联合基金(U20A20149);山西省研究生教育创新项目(2021Y139);国家自然科学基金青年项目(21908137);青海省昆仑英才·高端创新创业人才（2021）

Rapid quality inspection of high-purity lithium carbonate based on determination of magnesium by water-soluble probe method

LI Yan¹(),WANG Yansong¹,CHENG Huaigang^1,³(),KANG Jin^1,²,LI Enze¹,LÜ Hongzhou¹,LIU Qian⁴

1. Institute of Resources and Environmental Engineering，Shanxi University，Taiyuan 030006，China
2. College of Chemistry and Chemical Engineering，Jinzhong University，Jinzhong 030619，China
3. School of Chemical Engineering，Qinghai University，Xining 810016，China
4. Shanxi Dadi Ecological Environment Technology（Research Institute）Co. ，Ltd. ，Taiyuan 030006，China

Received:2022-05-20 Published:2023-01-10 Online:2023-01-17

摘要/Abstract

摘要：

碳酸锂生产过程及最终产品中，微量镁的掺杂会直接影响碳酸锂的产品品质及其下游产品的加工应用，而高纯碳酸锂中微量镁的快速检测仍是一个难点。研究提出利用水溶性荧光探针检测碳酸锂中微量镁的方法，以水溶性极强的三（羟甲基）氨基甲烷对2-（2-羟基苯基）苯并噁唑进行修饰，构建了具有高灵敏度和高选择性的水溶性Mg²⁺荧光探针A。该方法可实现对碳酸锂溶液中Mg²⁺的快速荧光检测，并确定了探针A被Mg²⁺所激发的荧光信号强度与Mg²⁺浓度之间的定量关系。结果表明在水溶条件下检测含镁杂质的碳酸锂时，该方法对微量镁的检出限为2.014 9 μmol/L，检测工作曲线相关系数达到0.991 5，检测灵敏度高，对高纯碳酸锂中微量镁的检测时间为3.666 s，可实现对Mg²⁺的快速质检。

关键词: 荧光探针, 高纯碳酸锂, 质检, 水溶性

Abstract:

In the production process of lithium carbonate and the final product，the doping of trace magnesium will directly affect the product quality of lithium carbonate and the processing and application of downstream products，and the rapid detection of trace magnesium in high-purity lithium carbonate is still a difficulty.In this study，a method for detecting trace amounts of magnesium in lithium carbonate using a water-soluble fluorescent probe was proposed.The highly water-soluble tris（hydroxy） methyl aminomethane was used to modify 2-（2-hydroxyphenyl） benzoxazole.Water-soluble Mg²⁺ fluorescent probe A with high sensitivity and selectivity was constructed.This method could realize the rapid fluorescence detection of Mg²⁺ in lithium carbonate solution，and determine the quantitative relationship between the fluorescence signal intensity of probe A excited by Mg²⁺ and the concentration of Mg²⁺.The results showed that the detection limit of this method for trace magnesium was 2.014 9 μmol/L when the lithium carbonate containing magnesium impurities was detected under water-soluble conditions，and the correlation coefficient of the detection working curve reached 0.991 5，and the detection sensitivity was high.The detection time of magnesium was 3.666 s，which could realize the rapid quality inspection of Mg²⁺.

Key words: fluorescence probe, high purity lithium carbonate, quality control, water-solubility

中图分类号:

TQ131.11

李岩,王岩松,成怀刚,康锦,李恩泽,吕宏洲,刘倩. 基于水溶性探针法测镁的高纯碳酸锂快速质检[J]. 无机盐工业, 2023, 55(1): 87-92.

LI Yan,WANG Yansong,CHENG Huaigang,KANG Jin,LI Enze,LÜ Hongzhou,LIU Qian. Rapid quality inspection of high-purity lithium carbonate based on determination of magnesium by water-soluble probe method[J]. Inorganic Chemicals Industry, 2023, 55(1): 87-92.

图/表 6

图1

图2

图3

图4

图5

图6

参考文献 18

1	戴江洪, 王宏岩, 李平. 高纯碳酸锂制备研究进展[J].中国有色冶金, 2020, 49（1）：49-53.
	DAI Jianghong, WANG Hongyan, LI Ping. Research development of preparation of high purity lithium carbonate[J].China Nonferrous Metallurgy, 2020, 49（1）：49-53.
2	南东东, 曾小毛, 刘剑叶, 等. 基于一步法对以锂云母为原料制备电池级碳酸锂的方法研究[J].冶金与材料, 2020, 40（5）：41-42.
3	王孟雪, 余晓平, 郭亚飞, 等. 卤水中镁的分离提取研究进展[J].盐科学与化工, 2017, 46（7）：4-8.
	WANG Mengxue, YU Xiaoping, GUO Yafei, et al. Progresses on the separation and extraction of magnesium from brine[J].Journal of Salt Science and Chemical Industry, 2017, 46（7）：4-8.
4	尹记帅, 孙文亮, 郝如斯, 等. 沉锂反应条件对碳酸锂纯度及杂质影响的研究[J].无机盐工业, 2019, 51（3）：29-33.
	YIN Jishuai, SUN Wenliang, HAO Rusi, et al. Study on the influence of lithium deposition reaction conditions on purity and impurities of lithium carbonate[J].Inorganic Chemicals Industry, 2019, 51（3）：29-33.
5	郭春平, 周有池, 文小强, 等. 磷酸锂渣制备电池级碳酸锂工艺研究[J].无机盐工业, 2022, 54（3）：82-86.
	GUO Chunping, ZHOU Youchi, WEN Xiaoqiang, et al. Study on preparation process of battery-grade lithium carbonate from slag containing lithium phosphate[J].Inorganic Chemicals Industry, 2022, 54（3）：82-86.
6	LI Liqin, YAN Zhenning, ZHANG Shuangyan. Development and application of a novel lead ion-selective electrode with the alkylamines modified molecular sieve as carrier[J].Journal of the Iranian Chemical Society, 2021, 18（11）：2853-2862.
7	TAYLOR A, BARLOW N, DAY M P, et al. Atomic spectrometry update：Review of advances in the analysis of clinical and biological materials，foods and beverages[J].Journal of Analytical Atomic Spectrometry, 2019, 34（3）：426-459.
8	PICONE G, CAPPADONE C, FARRUGGIA G, et al. The assessment of intracellular magnesium：Different strategies to answer different questions[J].Magnesium Research, 2020, 33（1）：1-11.
9	ZHONG Shenghui, CHENG Nannan, WU Jianqiong, et al. Determination of sodium，magnesium，potassium，calcium，iron，copper and zinc in methanol by inductively coupled plasma atomic emission spectrometry[J].Zhejiang Chemical Industry, 2018, 49（3）：14-17.
10	WU Qi, FENG Liheng, CHAO Jianbin, et al. Ratiometric sensing of Zn²⁺ with a new benzothiazole-based fluorescent sensor and living cell imaging[J].The Analyst, 2021, 146（13）：4348-4356.
11	ZHANG Qiang, MA Ruifang, LI Zhuying, et al. A multi-responsive crown ether-based colorimetric/fluorescent chemosensor for highly selective detection of Al³⁺，Cu²⁺ and Mg²⁺ [J].Spectrochimica Acta Part A：Molecular and Biomolecular Spectroscopy, 2020, 228.Doi：10.1016/j.saa.2019.117857.
12	付振海, 王敏, 李志伟, 等. 一种8-羟基喹啉衍生物的制备及其对Mg²⁺的检测[J].分析测试学报, 2021, 40（10）：1520-1525.
	FU Zhenhai, WANG Min, LI Zhiwei, et al. Synthesis of a fluorescence probe based on 8-hydroxyquinoline derivative and its application in Mg²⁺ ion detection[J].Journal of Instrumental Analysis, 2021, 40（10）：1520-1525.
13	WANG Zhen, CUI Shiqiang, QIU Shouyu, et al. A novel diarylethene-based fluorescent “turn-on” sensor for the selective detection of Mg²⁺ [J].RSC Advances, 2019, 9（11）：6021-6026.
14	阳清亮, 李浩榛, 刘刚, 等. 基于水杨醛荧光探针的营养液镁离子检测方法[J].农业机械学报, 2021, 52（S1）：344-350.
	YANG Qingliang, LI Haozhen, LIU Gang, et al. Salicylaldehyde fluorescent probe based on detection of magnesium ions in nutrient solutions[J].Transactions of the Chinese Society for Agricultural Machinery, 2021, 52（S1）：344-350.
15	张慧芳. 萘酰亚胺类钙镁离子荧光探针的设计及应用[D].太原：山西大学, 2018.
	ZHANG Huifang. The design of naphthalimide fluorescent probes for calcium and magnesium ion and their application[D].Taiyuan：Shanxi University, 2018.
16	YANG Wensheng, YANG Wan, MA Yajun. Synthesis of coumarin fluorescent probe based on schiff base structure and identification to Mg²⁺ [J].Chinese Journal of Luminescence, 2019, 40（7）：941-946.
17	张灯青. 镁离子荧光探针[J].化学进展, 2009, 21（4）：715-723.
	ZHANG Dengqing. Fluorescent probes for sensing magnesium ions[J].Progress in Chemistry, 2009, 21（4）：715-723.
18	杨文生, 杨菀, 师旺, 等. 荧光素类镁离子荧光增强型分子探针的制备及光谱性能研究[J].分析试验室, 2020, 39（6）：645-648.
	YANG Wensheng, YANG Wan, SHI Wang, et al. Preparation and spectral properties of fluoresce in magnesium ion fluorescent enhanced molecular probe[J].Chinese Journal of Analysis Laboratory, 2020, 39（6）：645-648.

[1]	杨红军, 王敏, 戈海文, 乔友民, 乔子洋. 铝酸钙飞灰中钾的回收利用工艺研究[J]. 无机盐工业, 2023, 55(10): 121-127.
[2]	陈红琼,马航. 水溶性磷酸一铵防结块剂的研究与应用[J]. 无机盐工业, 2022, 54(2): 78-80.
[3]	李婷婷,周贵云,母鸿. 二氧化硅制备水溶性硅钾肥的研究[J]. 无机盐工业, 2022, 54(12): 74-78.
[4]	王月香,邵兰燕,徐天男,蔡彩红,袁俊生,张英武. 垃圾焚烧飞灰中氯元素存在形态及深度脱氯的研究[J]. 无机盐工业, 2021, 53(5): 78-83.
[5]	凌浩瀚，王辛龙，许德华，梁文，谢汶级. 不同聚合度水溶性聚磷酸铵螯合镁离子的研究[J]. 无机盐工业, 2019, 51(12): 20-22.
[6]	彭雪峰1，2，于海斌2，宋国良2，张玉婷2，张尚强2，张景成2，孙彦民2，辛峰1. 器外预硫化型加氢催化剂的制备与性能研究[J]. 无机盐工业, 2019, 51(11): 78-81.
[7]	邓姝皓, 杨子萱, 杨佳逸, 杨曦, 尹翀, 韩江, 易丹青. 由扎布耶盐湖粗盐制备高纯碳酸锂新工艺研究[J]. 无机盐工业, 2016, 48(4): 26-.
[8]	汪发红, 李波. 铬铁渣水泥固化体水溶性Cr6+溶出规律及其水化产物[J]. 无机盐工业, 2015, 47(7): 52-.
[9]	余林春, 杜怀明, 叶宇玲, 黄斌, 周刚. 低水溶性聚磷酸铵的研制及晶体构型[J]. 无机盐工业, 2014, 46(2): 27-.
[10]	王树轩, 李宁, 李波, 李玉龙. 铬铁渣中水溶性六价铬浸取研究[J]. 无机盐工业, 2012, 44(7): 47-.
[11]	林茹, 梁宇. 纳米CeFeO³的制备及其光催化性能研究[J]. 无机盐工业, 2011, 43(9): 20-.
[12]	仪德启;杨荣杰. 水在制备结晶Ⅱ型聚磷酸铵中的作用研究[J]. 无机盐工业, 2010, 0(1): 0-0.
[13]	仪德启;杨荣杰. 结晶Ⅱ型聚磷酸铵制备过程中氨的作用研究[J]. 无机盐工业, 2008, 0(3): 0-0.

首页

全国无机盐信息中心

中国化工学会

无机酸碱盐专业委员会

基于水溶性探针法测镁的高纯碳酸锂快速质检

Rapid quality inspection of high-purity lithium carbonate based on determination of magnesium by water-soluble probe method

RichHTML

PDF (PC)

可视化

摘要/Abstract

引用本文

使用本文

图/表 6

参考文献 18

相关文章 13

Metrics

本文评价

推荐阅读 0

首 页

基于水溶性探针法测镁的高纯碳酸锂快速质检

Rapid quality inspection of high-purity lithium carbonate based on determination of magnesium by water-soluble probe method

RichHTML

PDF (PC)

可视化

引用本文

使用本文

首页