碱熔-离子选择性电极法测定萤石中氟化钙

doi:10.13228/j.boyuan.issn1000-7571.011334

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摘要氟化钙含量是评定萤石质量等级的重要指标。先采用氢氧化钠、过氧化钠于700 ℃熔融分解样品,再用盐酸(1+4)进行溶解配制成溶液,以柠檬酸钠和硝酸钾为总离子强度调节剂,以茜红素S为指示剂,建立了以离子选择性电极法测定氟离子含量来推算萤石中氟化钙含量的方法。用高温、氢氧化钠熔融样品、氢氧化钠-过氧化钠熔融样品3种分解方法对萤石样品进行处理,并对处理后的样品分别进行扫描电子显微镜(SEM)、X射线能谱(EDS)和X射线衍射(XRD)表征,结果表明高温碱熔条件下氢氧化钠能使氟化钙完全分解从而促进样品被分解完全,过氧化钠将萤石中的硫元素完全氧化成硫酸根以消除硫对测定的影响。按照实验方法测定萤石标准样品和生产样品,结果的标准偏差为0.26%~0.40%,相对标准偏差为(RSD)0.28%~0.74%,标准样品和实际样品中氟化钙的含量与认定值或参考值相符。

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	蒋政
	罗旻延
	李玲
	梁振
	罗玉华
	钟宇斌

关键词 ：萤石, 氟化钙, 碱熔法, 氟离子选择电极

Abstract：The content of calcium fluoride is an important index to evaluate the quality grade of fluorite. The sample was fused and decomposed at 700 ℃ with sodium hydroxide and sodium peroxide followed by dissolution with hydrochloric acid (1+4) to prepare the solution. Sodium citrate and potassium nitrate were selected as the total ion strength adjustment buffer, and alizarin red S was used as indictor. The fluoride content was determined by ion selective electrode method, which could be used to calculate the content of calcium fluoride in fluorite. The fluorite sample was treated by three decomposition methods, i.e., high temperature, sodium hydroxide fusion, and sodium hydroxide-sodium peroxide fusion. The treated samples were characterized by scanning electron microscope (SEM), energy dispersive X-ray spectrometry (EDS) and X-ray diffraction (XRD). The results showed that the calcium fluoride could be completely decomposed by sodium hydroxide under high temperature alkali fusion conditions, thus accelerating the complete decomposition of sample. The sulfur in fluorite was fully oxidized to sulfate by sodium peroxide to eliminate the influence of sulfur on the determination. The standard samples and production samples of fluorite were determined according to the experimental method. The standard deviations of results were between 0.26% and 0.40%, and the relative standard deviations (RSD) were between 0.28% and 0.74%. The found results of calcium fluoride content in fluorite CRMs and samples were consistent with the certified or reference values.

Key words： fluorite calcium fluoride alkali fusion fluoride ion selective electrode

收稿日期: 2020-11-09

ZTFLH:	O657.1
	TF702+.5

作者简介: 蒋政(1989—),男,工程师,硕士,主要从事化学分析工作;E-mail:iamjiangzheng09@163.com

引用本文:

蒋政, 罗旻延, 李玲, 梁振, 罗玉华, 钟宇斌. 碱熔-离子选择性电极法测定萤石中氟化钙[J]. 冶金分析, 2021, 41(10): 91-97. JIANG Zheng, LUO Minyan, LI Ling, LIANG Zhen, LUO Yuhua, ZHONG Yubin. Determination of calcium fluoride in fluorite by ion selective electrode method after alkali fusion. , 2021, 41(10): 91-97.

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http://yjfx.chinamet.cn/CN/10.13228/j.boyuan.issn1000-7571.011334 或 http://yjfx.chinamet.cn/CN/Y2021/V41/I10/91

[1] 王利杰,杨志强.EDTA滴定法测定萤石中氟化钙[J].冶金分析,2018,38(12):69-74.
WANG Lijie,YANG Zhiqiang.Determination of calcium fluoride in fluorite by EDTA titration[J].Metallurgical Analysis,2018,38(12):69-74.
[2] 张越.EDTA滴定法测定萤石中氟化钙含量的方法改进[J].中国无机分析化学,2019,9(4):36-39.
ZHANG Yue.An improved method for determination of calcium fluoride in fluorite by EDTA titration[J].Chinese Journal of Inorganic Analytical Chemistry,2019,9(4):36-39.
[3] 杨笑,何冰.萤石中氟化钙含量的快速测定[J].南方金属,2013(3):24-25,32.
YANG Xiao,HE Bing.Fluorspar-quick determination of calcium fluoride content[J].Southern Metals,2013(3):24-25,32.
[4] 杨珍,孙银生,贺攀红,等.电感耦合等离子体原子发射光谱法快速测定萤石矿中氟化钙[J].冶金分析,2013,33(11):71-73.
YANG Zhen,SUN Yinsheng,HE Panhong,et al.Rapid determination of calcium fluoride in fluorite by inductivetly coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2013,33(11):71-73.
[5] 苏峥,马建平.X-射线荧光光谱法与红外吸收法联合测定萤石中氟化钙[J].冶金分析,2008,28(8):73-75.
SU Zheng,MA Jianping.Determination of calcium fluoride in fluorite with X-ray fluorescence spectrometry and infrared absorption[J].Metallurgical Analysis,2008,28(8):73-75.
[6] 佡云.粉末压片-X射线荧光光谱法与红外吸收光谱法联合测定萤石中各组分[J].中国无机分析化学,2014,4(1):50-52.
XIAN Yun.Analysis of component in fluorite using pressed powder pellet X-ray fluorescence spectrometry combined with infrared spectroscopy[J].Chinese Journal of Inorganic Analytical Chemistry,2014,4(1):50-52.
[7] B R, D N.Determination of fluoride content in drinking water and tea infusions using fluoride ion selective electrode[J].Journal of Agricultural Sciences,2007,52(2):155-168.
[8] Mccann H G.The solubility of fluorapatite and its relationship to that of calcium fluoride[J].Archives of Oral Biology,1968,13(8):987-1001.
[9] 刘玉城,林如丹,梁勇,等.氢氧化钠分解氟化钙的热力学分析[J].湿法冶金,2016,35(2):97-100.
LIU Yucheng,LIN Rudan,LIANG Yong,et al.Thermodynamic analysis for decomposition of calcium fluoride by sodium hydroxide[J].Hydrometallurgy of China,2016,35(2):97-100.
[10] 杨占菊,杜国栋,李建华,等.高温燃烧碘量法测定萤石中的总硫[J].化学分析计量,2019,28(5):81-85.
YANG Zhanju,DU Guodong,LI Jianhua,et al.Determination of total sulfur in fluorite by iodimetry with high temperature combustion[J].Chemical Analysis and Meterage,2019,28(5):81-85.
[11] 吴虹霞,龙如成.重量法测定萤石中硫的含量[J].化学分析计量,2007(3):64-65.
WU Hongxia,LONG Rucheng.Gravimetric determination of sulfur content in fluorite[J].Chemical Analysis and Meterage,2007(3):64-65.
[12] 刘毅,梁唐敏.pH值对氟化物离子选择电极法测定氟的影响[J].化工技术与开发,2014(1):45-46,19.
LIU Yi,LIANG Tangmin.Effect of pH on determination of fluorine by fluoride ion choosing electrode method[J].Technology & Development of Chemical Industry,2014(1):45-46,19.