五酸和硝酸微波消解法结合ICP-OES技术测定多金属矿中多种元素的对比研究

夏辉; 王小强; 杜天军; 赵亚男; 王书勤; 杨惠玲

doi:10.15898/j.cnki.11-2131/td.2015.03.006

五酸和硝酸微波消解法结合ICP-OES技术测定多金属矿中多种元素的对比研究

1.
河南省有色金属地质勘查总院, 河南郑州 450052

2.
河南省有色金属深部找矿勘查技术研究重点实验室, 河南郑州 450052

基金项目: 河南省国土资源厅2013年度地质科研项目(2013-12)——多金属矿中多元素连续测定方法研究

详细信息

作者简介: 夏辉, 工程师, 环境科学专业, 主要从事光谱、质谱分析应用工作. E-mail: xiahui_21@126.com

中图分类号: O657.31;P575

收稿日期: 2015-01-04

修回日期: 2015-05-05

录用日期: 2015-05-18

刊出日期: 2015-03-25

Determination of Multi-elements in Polymetallic Ores by ICP-OES with Mixed Acids and Nitric Acid Microwave Digestion

1.
General Institute for Nonferrous Metals and Geological Exploration of Henan Province, Zhengzhou 450052, China

2.
Key Laboratory of Deep Ore-prospecting Technology Research for Non-ferrous Metals of Henan Province, Zhengzhou 450052, China

Received Date: 04 January 2015

Revised Date: 05 May 2015

Accepted Date: 18 May 2015

Publish Date: 25 March 2015

摘要

摘要:
快速、准确测定多金属矿中的主次量元素需要根据多金属矿的具体类型选择不同的预处理方法。本文采集我国典型区域的铅锌、锡、钼、钒和铜镍等5种多金属矿, 对比了盐酸-硝酸-高氯酸-氢氟酸-硫酸五酸微波消解和硝酸微波消解的溶样效果, 应用电感耦合等离子体发射光谱法(ICP-OES)测定铜铅锌锡钨钼锰钛钒9种元素。通过国家标准物质分析验证, 五酸微波消解的溶样时间较长, 但一次可测定铜铅锌钼锰钒6种元素; 硝酸微波消解的溶样时间短, 但一次只能测定铜铅锌钼4种元素; 两种方法的准确度和精密度高(RSD < 5%), 检出限低(5.3~30 mg/kg), 均适合在地质行业推广应用。而由于锡钨钛3种元素不能完全被酸溶解, 上述两种消解方法均不适合。
- 多金属矿 /
- 主次量元素 /
- 盐酸-硝酸-高氯酸-氢氟酸-硫酸微波消解 /
- 硝酸微波消解 /
- 电感耦合等离子体发射光谱法
Abstract:
Different pretreatment methods should be used for quick and accurate determination of major and minor elements in different types of polymetallic ores. In this study, five types of polymetallic ores including Pb-Zn, Sn, Mo, V, and Cu-Ni polymetallic ores were collected from typical metallogenic areas of China. Comparison of microwave digestion using mixed acids of hydrochloric-nitric-perchloric-hydrofluoric-sulphuric acids with digestion using nitric acid only was performed. Nine elements, Cu, Pb, Zn, Sn, W, Mo, Mn, Ti, and V were determined by the Inductively Coupled Plasma-Optical Emission Spectrometry technique. Analytical results of National Standards Reference indicate that digestion with a mixture of five acids has a long digestion time and can simultaneously determine the 6 elements of Cu, Pb, Zn, Mo, Mn, and V. Digestion with nitric acid needs only 1 h and can determine 4 elements, Cu, Pb, Zn, and Mo. Two methods have good accuracy and precision (RSD < 5%) and low detection limits of 5.3-30 mg/kg, which are suitable for application in geological analyses. However, neither of these two methods are suitable for analyzing Sn, W, and Ti, because these elements cannot be digested completely by acids.

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图 1 五酸(a)和硝酸(b)微波溶样法分析结果

Figure 1.

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表 1 微波消解仪工作参数

Table 1. Working parameters of microwave digestion equipment

步骤	升温时间 (min)	保持时间 (min)	温度 (℃)	功率 (W)	压力 (kPa)
1	5	0	140	1000	自动
2	10	0	220	1000	自动
3	0	20	220	1000	自动

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表 2 元素谱线扣背景模式

Table 2. Background deduction model for analyzing spectrum line

元素	分析谱线 (nm)	扣背景模式	元素	分析谱线 (nm)	扣背景模式
Cu	324.754	右	Ti	336.121	左，右
Mn	257.610	左，右	V	309.311	右
Mo	202.030	左，右	W	239.709	左
Pb	220.353	左，右	Zn	213.856	左，右
Sn	189.989	左，右	Eu	381.967	左，右

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五酸和硝酸微波消解法结合ICP-OES技术测定多金属矿中多种元素的对比研究

1. 河南省有色金属地质勘查总院, 河南 郑州 450052 2. 河南省有色金属深部找矿勘查技术研究重点实验室, 河南 郑州 450052

作者简介: 夏辉, 工程师, 环境科学专业, 主要从事光谱、质谱分析应用工作. E-mail: xiahui_21@126.com

Determination of Multi-elements in Polymetallic Ores by ICP-OES with Mixed Acids and Nitric Acid Microwave Digestion

1. General Institute for Nonferrous Metals and Geological Exploration of Henan Province, Zhengzhou 450052, China 2. Key Laboratory of Deep Ore-prospecting Technology Research for Non-ferrous Metals of Henan Province, Zhengzhou 450052, China

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1.
河南省有色金属地质勘查总院, 河南郑州 450052

2.
河南省有色金属深部找矿勘查技术研究重点实验室, 河南郑州 450052

1.
General Institute for Nonferrous Metals and Geological Exploration of Henan Province, Zhengzhou 450052, China

2.
Key Laboratory of Deep Ore-prospecting Technology Research for Non-ferrous Metals of Henan Province, Zhengzhou 450052, China