自制氢化物发生系统与电感耦合等离子体发射光谱法联用测定土壤和水系沉积物中的砷锑铋

吴峥; 熊英; 王龙山

doi:10.15898/j.cnki.11-2131/td.2015.05.006

自制氢化物发生系统与电感耦合等离子体发射光谱法联用测定土壤和水系沉积物中的砷锑铋

陕西省地质矿产实验研究所, 陕西西安 710054

详细信息

作者简介: 吴峥, 硕士, 工程师, 分析化学专业, 主要从事岩石矿物分析测试工作. E-mail: yswz007@163.com

中图分类号: S151.93;O657.31

收稿日期: 2014-01-18

修回日期: 2015-08-25

录用日期: 2015-09-05

刊出日期: 2015-05-25

Determination of As, Sb and Bi in Soil and Stream Sediment by a Self-developed Hydride Generation System Coupled with Inductively Coupled Plasma-Optical Emission Spectrometry

Experimental Institute of Geology and Mineral Resources of Shaanxi Province, Xi'an 710054, China

Received Date: 18 January 2014

Revised Date: 25 August 2015

Accepted Date: 05 September 2015

Publish Date: 25 May 2015

摘要

摘要:
氢化物发生法-电感耦合等离子体发射光谱(ICP-OES)联用可以提高仪器测定的灵敏度, 但氢化物发生的化学反应过程不稳定, 导致检测精密度变差。本文设计了一套简易氢化物发生系统, 将样品进样管内径由0.32 mm扩大为0.76 mm, 与还原剂(硼氢化钾)管路通过三通混合, 混合后反应管路内径由0.76 mm扩大为1.14 mm, 反应管长度由30 cm延长至50 cm, 显著增加了待测元素氢化反应的空间和时间, 使氢化反应达到平衡态从而提高了氢化物的稳定性。土壤和水系沉积物样品用盐酸-硝酸水浴浸提、硫脲-抗坏血酸预还原后利用此套系统与ICP-OES联用测定了砷锑铋的含量。砷锑铋的检出限分别为0.35 μg/g、0.33 μg/g、0.25 μg/g, 测定范围分别为1.1~300 μg/g、1.0~100 μg/g、0.75~100 μg/g, 均满足了相关分析要求。
- 土壤 /
- 水系沉积物 /
- 砷 /
- 锑 /
- 铋 /
- 氢化物发生 /
- 电感耦合等离子体发射光谱法
Abstract:
Hydride Generation (HG) combined with Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES) has excellent analytical sensitivity. However, the instable chemical reactions of HG may cause unsatisfactory analytical precision. In this study, a novel and self-made HG system coupled with ICP-OES was developed for measurement of As, Sb and Bi in geological samples. Inner diameter (i.d.) of introduction tubing changed from 0.32 mm to 0.76 mm. Reaction tubing i.d. changed from 0.76 mm to 1.14 mm and length increased from 30 cm to 50 cm. These changes significantly improve the stability of HG reaction by increasing space and time of chemical reactions to reach reaction equilibrium. Arsenic, Sb and Bi were firstly leached from soil and stream sediment using HCl-HNO₃ water bath, pre-reduced by thiocarbamide-ascorbic acid mixture, and were finally determined by the modified HG-ICP-OES. The detection limits of this method are 0.35 μg/g, 0.33 μg/g and 0.25 μg/g for As, Sb and Bi, respectively. The linear ranges are 1.1-300 μg/g for As, 1.0-100 μg/g for Sb and 0.75-100 μg/g for Bi, which is sufficient for the measurement of As, Sb and Bi in geological samples.
- soil /
- stream sediment /
- As /
- Sb /
- Bi /
- Hydride Generation /
- Inductively Coupled Plasma-Optical Emission Spectrometry

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图 1 氢化物发生-ICP-OES系统示意图

Figure 1.

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图 2 硼氢化钠浓度对砷、锑、铋信号强度影响

Figure 2.

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表 1 样品处理方式的对比

Table 1. omparison of analytical results of As, Sb and Bi with differents pretreatment methods

元素	GBW07406(土壤)			GBW07430(土壤)			GBW07312(水系沉积物)
元素	四酸溶矿测定值 (μg/g)	水浴浸提测定值 (μg/g)	标准值 (μg/g)	四酸溶矿测定值 (μg/g)	水浴浸提测定值 (μg/g)	标准值 (μg/g)	四酸溶矿测定值 (μg/g)	水浴浸提测定值 (μg/g)	标准值 (μg/g)
As	198	218	220	16.8	19.3	18	105	116	115
Sb	53.4	58.9	60	1.55	1.85	1.9	20.4	25.3	24.5
Bi	45.1	51.4	49	1.23	1.51	1.44	8.34	11.1	10.9

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表 2 方法精密度和准确度

Table 2. Precision and accuracy tests of the method

标准物质编号	元素	含量(μg/g)		RSD (%)	相对误差 (%)
标准物质编号	元素	平均值	标准值	RSD (%)	相对误差 (%)
GBW07404 (土壤)	As	55.4	58.0	6.7	4.4
	Sb	6.02	6.30	7.3	4.4
	Bi	0.99	1.04	9.6	4.8
GBW07429 (土壤)	As	20.6	21.7	5.4	5.0
	Sb	2.00	1.90	7.7	5.5
	Bi	1.08	1.16	3.9	6.8
GBW07306 (水系沉积物)	As	13.5	13.6	4.3	0.7
	Sb	1.27	1.25	5.9	1.6
	Bi	5.14	5.00	4.6	2.8
GBW07311 (水系沉积物)	As	183	188	5.4	2.9
	Sb	14.7	14.9	9.3	1.3
	Bi	50.3	50.0	4.8	0.6
GBW07312 (水系沉积物)	As	115	115	3.3	0.1
	Sb	24.5	24.0	6.6	2.0
	Bi	10.8	10.9	8.7	0.8

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表 3 不同方法测定结果的比较

Table 3. A comparison of analytical results between HG-ICP-OES and HG-AFS

样品编号	元素	测定值(μg/g)
样品编号	元素	HG-ICP-OES(本法)	HG-AFS
土壤样品1	As	5.25	5.43
	Sb	10.4	10.9
	Bi	2.66	2.98
土壤样品2	As	23.5	24.4
	Sb	6.12	5.85
	Bi	6.84	6.53
水系沉积物样品1	As	0.68	0.61
	Sb	1.08	0.98
	Bi	3.21	3.42
GBW07306 (水系沉积物)	As	13.1	14.2
	Sb	1.15	1.11
	Bi	4.87	5.11

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自制氢化物发生系统与电感耦合等离子体发射光谱法联用测定土壤和水系沉积物中的砷锑铋

陕西省地质矿产实验研究所, 陕西 西安 710054

作者简介: 吴峥, 硕士, 工程师, 分析化学专业, 主要从事岩石矿物分析测试工作. E-mail: yswz007@163.com

Determination of As, Sb and Bi in Soil and Stream Sediment by a Self-developed Hydride Generation System Coupled with Inductively Coupled Plasma-Optical Emission Spectrometry

Experimental Institute of Geology and Mineral Resources of Shaanxi Province, Xi'an 710054, China

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陕西省地质矿产实验研究所, 陕西西安 710054