过氧化钠碱熔-电感耦合等离子体原子发射光谱法测定富锡渣中锑

doi:10.13228/j.boyuan.issn1000-7571.011815

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摘要富锡渣是锡一次还原熔炼后的含锡中间产品,一般含有难溶锡氧化物,普通酸溶法和微波消解法无法将样品完全分解,而采用酸溶-碱熔法虽能将样品完全分解,但其操作流程长且易造成待测元素的损失。采用过氧化钠为熔剂碱熔样品,再使用盐酸(1+1)提取,将溶液稀释后使用钠盐匹配的标准溶液系列绘制校准曲线,建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定富锡渣中锑的方法。结果表明:锑的质量浓度为0.50~10.00 μg/mL时,校准曲线的线性相关系数r为0.999 8;方法检出限为0.002%。锡基体及样品中共存元素对锑的测定结果无影响。按照实验方法测定4个富锡渣中锑,测定结果的相对标准偏差(RSD,n=6)均小于2.0%;回收率为95%～101%。

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	杨赟金
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关键词 ：电感耦合等离子体原子发射光谱法(ICP-AES), 富锡渣, 过氧化钠, 碱熔, 锑

Abstract：Tin-riched slag is a tin-containing intermediate product by one-time retailoring of tin. It generally contains insoluble tin oxides, which cannot be fully decomposed by ordinary acid dissolution and microwave digestion. Although the acid solution-alkali fusion method can completely decompose the sample, its operation process is long and easy to cause the loss of elements to be measured. Sodium peroxide was used as the flux for the alkali fusion of sample. After leaching with hydrochloric acid(1+1), the solution was diluted. The standard solution series after matching with sodium salt were used to prepare the calibration curve. Thus, a method for determination of antimony in tin-riched slag was established by inductively coupled plasma atomic emission spectrometry (ICP-AES). The results showed that the linear correlation coefficient (r) of calibration curve was 0.999 8 when the mass concentration of antimony was in range of 0.50-10.00 μg/mL. The limit of detection was 0.002%. The tin matrix and coexisting elements in sample had no influence on the determination results of antimony. The content of antimony in four tin-riched slag samples was determined according to the experimental method. The relative standard deviations (RSD, n=6) of determination results were all less than 2.0%. The recoveries were between 95% and 101%.

Key words： inductively coupled plasma atomic emission spectrometry(ICP-AES) tin-riched slag sodium peroxide alkali fusion antimony

收稿日期: 2022-03-28

ZTFLH:	O657.31
	TF03+1

基金资助:昆明市“春城计划”高层次人才培养工程“首席技师”专项

作者简介: 杨赟金(1985—),男,高级工程师,硕士,主要研究方向为ICP-AES、AAS、ICP-MS分析方法的研究及应用;E-mail:280218912@qq.com

引用本文:

杨赟金, 程婧娴, 余波, 余晓. 过氧化钠碱熔-电感耦合等离子体原子发射光谱法测定富锡渣中锑[J]. 冶金分析, 2023, 43(1): 49-53. YANG Yunjin, CHENG Jingxian, YU Bo, YU Xiao. Determination of antimony in tin-riched slag by inductively coupled plasma atomic emission spectrometry with sodium peroxide alkali fusion. , 2023, 43(1): 49-53.

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[1] 陈丽珠,曹胜.电感耦合等离子体发射光谱(ICP-OES)法测定矿石中锑[J].中国无机分析化学,2017,7(4):60-63.
CHEN Lizhu,CAO Sheng.Determination of antimony in ores by inductively coupled plasma optical emission spectrometry (ICP-OES)[J].Chinese Journal of Inorganic Analytical Chemistry,2017,7(4):60-63.
[2] 范兢克,许蕃,吕超飞,等.电感耦合等离子体原子发射光谱法测定铜熔炼渣中铅锌镍锑铋砷[J].黄金,2021,42(3):87-91.
FAN Jingke,XU Fan,L Chaofei,et al.Determination of Pb,Zn,Ni,Sb,Bi and As in copper smelting slag by inductive coupled plasma-atomic emission spectrometry[J].Gold,2021,42(3):87-91.
[3] 刘芳美,赖秋祥,廖彬玲,等.电感耦合等离子体原子发射光谱(ICP-AES)法测定粗二氧化碲中铜、铅、锑、铋、砷和硒[J].中国无机分析化学,2022,12(2):56-60.
LIU Fangmei,LAI Qiuxiang,LIAO Binling,et al.Determination of copper,lead,antimony,bismuth,arsenic and selenium in crude tellurium dioxide by inductively coupled plasma atomic emission spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2022,12(2):56-60.
[4] 杨斌,胡向平,何蓉,等.电感耦合等离子体原子发射光谱(ICP-AES)法测定H-ZF类光学玻璃中锑含量[J].中国无机分析化学,2022,8(6):21-24.
YANG Bin,HU Xiangping,HE Rong,et al.Determination of stibium in H-ZF types optical glasses by ICP-AES[J].Chinese Journal of Inorganic Analytical Chemistry,2022,8(6):21-24.
[5] 郑智慷,曾江萍,王家松,等.常压密闭微波消解-电感耦合等离子体发射光谱法测定锑矿石中的锑[J].岩矿测试,2020,39(2):208-215.
ZHENG Zhikang,ZENG Jiangping,WANG Jiasong,et al.Determination of antimony in antimony ores by inductively coupled plasma-optical emission spectrometry with microwave digestion[J].Rock and Mineral Analysis,2020,39(2):208-215.
[6] 李海.微波消解-电感耦合等离子体原子发射光谱法测定锌精矿中锑[J].冶金分析,2019,39(6):29-33.
LI Hai.Determination of antimony in zinc concentrate by inductively coupled plasma atomic emission spectrometry with microwave digestion[J].Metallurgical Analysis,2019,39(6):29-33.
[7] 李皓,张尼,马熠罡.碱熔样电感耦合等离子体发射光谱法测定锑矿石中锑[J].化学分析计量,2016,25(2):69-71.
LI Hao,ZHANG Ni,MA Yigang.Determination of antimony in antimony ore by inductively coupled plasma emission spectrometry combined with alkali fusion pretreatment[J].Chemical Analysis and Meterage,2016,25(2):69-71.
[8] 成勇,刘力维,袁金红,等.碱熔-电感耦合等离子体原子发射光谱法测定钒渣中钒、硅、钙、镁、铝、锰、铬、钛、磷[J].冶金分析,2021,41(4):59-67.
CHENG Yong,LIU Liwei,YUAN Jinhong,et al.Determination of vanadium,silicon,calcium,magnesium,aluminum,manganese,chromium,titanium and phosphorus in vanadium slag by inductively coupled plasma atomic emission spectrometry after alkali fusion[J].Metallurgical Analysis,2021,41(4):59-67.
[9] 肖红新,庄艾春,张永进,等.电感耦合等离子体发射光谱法测定锡精矿中10种元素[J].化学分析计量,2018,27(6):30-33.
XIAO Hongxin,ZHUANG Aichun,ZHANG Yongjin,et al.Determination of 10 elements in tin concentrate by inductively coupled plasma atomic emission spectrometry[J].Chemical Analysis and Meterage,2018,27(6):30-33.
[10] 曾玲玲,王荟蓉,苏晓梅,等.ICP-AES法测定黑铜泥中的铅、砷、铋、锑的含量[J].现代制造技术与装备,2015(5):44-45.
ZENG Lingling,WANG Huirong,SU Xiaomei,et al.Determination of black copper mud of lead,arsenic,bismuth and antimony by ICP-AES[J].Modern Manufacturing Technology and Equipment,2015(5):44-45.