改进BCR法-电感耦合等离子体发射光谱法测定矿产品堆场土壤中镉砷铅的化学形态

胡德新; 武素茹; 刘跃勇; 王虹; 王向东; 李权斌; 谷松海

改进BCR法-电感耦合等离子体发射光谱法测定矿产品堆场土壤中镉砷铅的化学形态

1.
天津出入境检验检疫局化矿金属材料检测中心, 天津 300456

2.
天津口岸检测分析开发服务有限公司, 天津 300457

基金项目: 天津市滨海新区塘沽科技发展专项资金项目（2012STHB04-04）

详细信息

作者简介: 胡德新, 工程师, 主要从事矿产品的检测工作. E-mail: hudx@tjciq.gov.cn

中图分类号: S151.93;O657.31

收稿日期: 2013-09-17

录用日期: 2013-11-13

刊出日期: 2014-03-25

Determination of Chemical Species of Cadmium, Arsenic and Lead in Mineral Yard Soil by Modified BCR and ICP-AES Method

1.
Minerals and Metallic Materials Inspection Center, Tianjin Entry-Exit Inspection and Quarantine Bureau, Tianjin 300456, China

2.
Tianjin Inspection and Test Development Service Co., Ltd, Tianjin 300457, China

Received Date: 17 September 2013

Accepted Date: 13 November 2013

Publish Date: 25 March 2014

摘要

摘要:
矿产品堆场土壤中重金属在环境中富集，随着元素的迁移、转化及地下水的循环，成为环境污染问题。本文将改进的顺序提取法（BCR）应用于矿产品堆场土壤中Cd、As、Pb的化学形态分析，结合这三种元素的性质，将堆场土壤中Cd、As、Pb分为可交换态、可还原态、可氧化态和残渣态，并利用电感耦合等离子体发射光谱法测定其含量。采用形态分析标准参考物质GBW 07436验证了三步提取态的准确性，并对6个矿产品堆场土壤中Cd、As、Pb形态含量进行了分析，三步提取态加上残渣态质量分数之和与重金属总量进行了比较，回收率在85%~103%之间。通过对矿产品堆场土壤实际样品分析，Cd、As、Pb三种元素非残渣态含量顺序为Cd（79.40%~94.94%）>Pb（24.27%~37.73%）>As（22.89%~31.51%），表明Cd元素较为容易进入生物圈。该方法解决了港口堆场土壤中重金属化学形态提取问题，对污染土壤的治理具有指导意义。
- 矿产品堆场土壤 /
- 镉 /
- 砷 /
- 铅 /
- 化学形态 /
- 改进BCR法 /
- 电感耦合等离子体发射光谱法
Abstract:
Heavy metal elementals can be enriched in soil at mineral products yard, which become a problem of environmental pollution caused by elemental migration, transformation and circulation in underground water. In this experimentation the modified BCR sequential extraction method was applied to the chemical species analysis of Cd, As and Pb. Based on the properties of these three elementals, the chemical species of Cd, As and Pb were divided into four fractions: exchangeable, reducible, oxidizable and residual, and Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) were used to measure the content of Cd, As and Pb. Morphological analysis standard reference material GBW 07436 was conducted to verify the accuracy of the three step extraction state. Contents of chemical species of Cd, As and Pb in soil from six mineral products yard were analyzed, including contents of three step extraction state plus the residual and the total contents of the desired metals elements. The recoveries were from 84.54% to 102.88%. The analysis results for actual samples demonstrated the contents of Cd, As and Pb in non-residual fraction were in order as Cd (79.40%-94.94%)>Pb(24.27%-37.73%)>As (22.89%-31.51%), which indicated Cd is easy to enter the biosphere. This method has resolved the problem to extract the chemical species of heavy metal elements in soil from port mineral products yard, and has profound significance to the treatment of contaminated soil.
- mineral yard soil /
- cadmium /
- arsenic /
- lead /
- chemical species /
- modified BCR method /
- Inductively Coupled Plasma-Atomic Emission

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表 1 标准工作曲线

Table 1. Calibration curves of elements

待测元素	线性范围 ρ/(mg·L^-1)	线性方程	相关系数
Cd	0~25.0	y=53578x-0.5997	0.99999
As	0~50.0	y=1531.7x+7.2654	0.99996
Pb	0~25.0	y=3125x+21.54	0.99998

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表 2 方法检出限

Table 2. Detection limits of the method

元素形态	检出限/(μg·g^-1)
元素形态	Cd	As	Pb
可交换态	0.023	0.015	0.017
可还原态	0.026	0.024	0.031
可氧化态	0.043	0.033	0.022
残渣态	0.147	0.219	0.108

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表 3 方法精密度

Table 3. Precision tests of the method

元素形态	样品编号	Cd		As		Pb
元素形态	样品编号	w/(μg·g^-1)	RSD/%	w/(μg·g^-1)	RSD/%	w/(μg·g^-1)	RSD/%
可交换态	1	2.1	2.9	5.2	1.0	1.4	2.7
	2	1.2	4.8	1.3	5.0	0.4	7.8
	3	18.1	0.4	16.2	0.4	0.7	4.5
可还原态	1	4.5	2.1	7.1	0.4	0.5	5.6
	2	0.9	3.7	1.6	3.7	0.3	9.3
	3	3.6	1.7	21.2	0.2	0.6	5.2
可氧化态	1	1.1	5.2	89.4	0.2	15.9	0.6
	2	4.7	0.8	15.7	0.6	1.9	3.7
	3	8.3	0.4	199.1	1.2	4.5	2.4
残渣态	1	0.6	7.2	221.2	1.7	28.1	0.8
	2	0.5	7.3	60.1	3.5	5.5	2.0
	3	5.6	0.5	679.8	2.3	13.4	0.6

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表 4 改进BCR法分析GBW 07436标准物质中Cd、As、Pb的测定值与标准值(n=5)

Table 4. Certified and determined contents of extractable contents of Cd, As and Pb in certified reference material of GBW 07436 (n=5)w/(μg·g^-1)

测试元素	可交换态		可还原态		可氧化态
测试元素	测试值	标准值	测试值	标准值	测试值	标准值
Cd	1.53±0.25	1.46±0.20	0.94±0.07	0.86±0.03	0.15±0.02	0.12±0.03
As	0.23±0.04	0.25±0.03	1.52±0.05	1.48±0.04	0.47±0.04	0.44±0.03
Pb	1.61±0.22	1.58±0.17	48.4±4.6	49.1±5.5	5.1±0.34	5.4±0.23

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表 5 土壤样品Cd、As、Pb形态分析

Table 5. Analytical results of Cd, As and Pb in soil samples

样品编号	测试元素	w/(μg·g^-1)						回收率 /%
样品编号	测试元素	可交换态	可还原态	可氧化态	残渣态	四形态之和	总量	回收率 /%
1	Cd	2.1	4.5	1.1	0.6	8.2	9.4	88.2
	As	5.2	7.1	89.4	221.2	322.8	333.6	96.8
	Pb	1.34	0.5	15.9	28.1	45.9	47.9	95.9
2	Cd	1.9	1.34	2.5	0.7	6.5	7.1	91.9
	As	7.9	10.2	116.8	428.4	563.4	600.5	93.8
	Pb	0.3	0.2	4.4	13.7	18.6	19.0	98.1
3	Cd	1.2	0.9	4.7	0.5	7.2	8.5	84.5
	As	1.3	1.6	15.7	60.1	78.7	79.8	98.6
	Pb	0.4	0.3	1.9	5.5	8.1	9.0	89.8
4	Cd	1.7	2.2	2.5	0.5	6.9	7.2	96.6
	As	1.3	1.6	19.0	69.9	91.7	95.5	96.1
	Pb	2.3	1.2	17.4	34.1	55.0	55.1	99.7
5	Cd	22.1	17.4	20.5	3.3	63.3	61.5	102.9
	As	16.9	18.9	300.7	687.4	1024.0	1077.0	95.1
	Pb	1.8	1.7	23.0	40.6	67.2	68.4	98.1
6	Cd	18.1	3.6	8.3	5.6	35.5	36.5	97.2
	As	16.12	21.2	199.1	679.8	916.4	954.1	96.1
	Pb	0.7	0.6	4.5	13.4	19.2	22.1	86.7

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表 6 堆场土壤中Cd、As、Pb各种化学形态所占比例

Table 6. Species distribution of Cd, As and Pb in soil samples

样品编号	测试元素	各形态含量的比例/%
样品编号	测试元素	可交换态	可还原态	可氧化态	残渣态
1	Cd	23.1	47.8	11.8	6.1
	As	1.6	2.1	27.5	67.9
	Pb	2.7	1.1	32.0	56.4
2	Cd	26.7	19.3	34.5	10.3
	As	1.5	1.7	20.6	75.6
	Pb	1.6	1.0	21.7	68.6
3	Cd	14.4	10.2	56.7	5.7
	As	1.6	2.0	19.4	74.0
	Pb	4.6	3.6	22.5	66.3
4	Cd	24.1	30.2	35.2	6.7
	As	1.4	1.6	20.1	73.8
	Pb	4.1	2.2	31.0	60.4
5	Cd	34.5	28.4	32.1	5.1
	As	1.6	1.8	28.2	64.4
	Pb	2.7	2.4	32.	57.5
6	Cd	47.8	9.7	21.9	14.9
	As	1.7	2.2	21.1	72.0
	Pb	3.3	2.6	22.1	64.9

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改进BCR法-电感耦合等离子体发射光谱法测定矿产品堆场土壤中镉砷铅的化学形态

1. 天津出入境检验检疫局化矿金属材料检测中心, 天津 300456 2. 天津口岸检测分析开发服务有限公司, 天津 300457

作者简介: 胡德新, 工程师, 主要从事矿产品的检测工作. E-mail: hudx@tjciq.gov.cn

Determination of Chemical Species of Cadmium, Arsenic and Lead in Mineral Yard Soil by Modified BCR and ICP-AES Method

1. Minerals and Metallic Materials Inspection Center, Tianjin Entry-Exit Inspection and Quarantine Bureau, Tianjin 300456, China 2. Tianjin Inspection and Test Development Service Co., Ltd, Tianjin 300457, China

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目录

1.
天津出入境检验检疫局化矿金属材料检测中心, 天津 300456

2.
天津口岸检测分析开发服务有限公司, 天津 300457

1.
Minerals and Metallic Materials Inspection Center, Tianjin Entry-Exit Inspection and Quarantine Bureau, Tianjin 300456, China

2.
Tianjin Inspection and Test Development Service Co., Ltd, Tianjin 300457, China