微波消解-石墨炉原子吸收光谱法测定火山灰中的痕量铅铬铜

侯广顺; 李英杰; 刘瑞恒; 谭路路

doi:10.15898/j.cnki.11-2131/td.2015.05.007

微波消解-石墨炉原子吸收光谱法测定火山灰中的痕量铅铬铜

1.
河南理工大学资源环境学院, 河南焦作 454000

2.
河南理工大学物理化学学院, 河南焦作 454000

基金项目: 国家自然科学基金资助项目(41003015);河南省教育厅自然科学研究计划项目(2011B150010)

详细信息

作者简介: 侯广顺, 副教授, 地球化学专业. E-mail: houguangshun@163.com

通讯作者: 李英杰, 副教授, 主要从事光谱分析、样品前处理技术研究. E-mail: liyingjie@hpu.edu.cn

中图分类号: O614.433;O614.242;O614.121;O657.31

收稿日期: 2014-12-09

修回日期: 2015-07-15

录用日期: 2015-09-05

刊出日期: 2015-05-25

Determination of Trace Lead, Chromium and Copper in Volcanic Ash from Shinmoe-Dake Volcano by Microwave Digestion-Graphite Furnace Atomic Absorption Spectrometry

1.
School of Resources and Environment Engineering, Henan Polytechnic University, Jiaozuo 454000, China

2.
Department of Physics and Chemistry, Henan Polytechnic University, Jiaozuo 454000, China

More Information

Corresponding author: LI Ying-jie, liyingjie@hpu.edu.cn

Received Date: 09 December 2014

Revised Date: 15 July 2015

Accepted Date: 05 September 2015

Publish Date: 25 May 2015

摘要

摘要:
火山灰是重要的土壤母质且易风化, 铅、铬和铜是其中主要的重金属元素, 样品风化后不可避免地进入环境中对人体健康造成危害。本研究针对火山灰样品的特点, 建立了采用硝酸-氢氟酸微波消解, 石墨炉原子吸收光谱法测定火山灰中痕量铅、铬、铜的分析方法。通过实验确定了灰化温度为600℃(Pb)、1000℃(Cr)和800℃(Cu), 原子化温度为1800℃(Pb和Cu)、2200℃(Cr)。在优化实验条件下, 测定Pb、Cr和Cu的检出限分别为3.50 ng/mL、0.92 ng/mL和1.22 ng/mL, 相对标准偏差(RSD)均低于4%, 加标回收率为92.8%~107.0%。本方法快速简便、准确度高、成本低。
- 火山灰 /
- 重金属 /
- 硝酸-氢氟酸 /
- 微波消解 /
- 石墨炉原子吸收光谱法
Abstract:
Volcanic ash is an important parent material for soil and is easily weathered. Pb, Cr and Cu are the main heavy metals in weathered volcanic ash and are inevitably discharged into the environment and finally harmful to human health. A simple and reliable method for the determination of Pb, Cr and Cu in volcanic ash by microwave digestion combined with Graphite Furnace Atomic Absorption Spectrometry (GFAAS) has been proposed. The ashing temperatures are 600℃ for Pb, 1000℃ for Cr and 800℃ for Cu. The atomization temperatures are 1800℃ for Pb and Cu, and 2200℃ for Cr. The detection limits of the proposed method are 3.50, 0.92 and 1.22 ng/mL for Pb, Cr and Cu, respectively. The relative standard deviations (RSDs) for eleven replicate analyses (50 ng/mL) of the above three metals are less than 4%, and the recoveries by standard addition are 92.8%-107.0%. The proposed method is rapid and convenient with high accuracy and low cost.
- volcanic ash /
- heavy metals /
- microwave digestion /
- Graphite Furnace Atomic Absorption Spectrometry /

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图 1 灰化温度(a)和原子化温度(b)的影响

Figure 1.

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表 1 GFAAS仪器工作条件和石墨炉升温程序

Table 1. Operating parameters of the GFAAS instrument and temperature programs of graphite furnace

待测元素	GFAAS仪器工作条件				石墨炉升温程序
待测元素	分析波长 (nm)	灯电流 (mA)	光谱带宽 (nm)	背景校正	干燥条件	灰化条件	原子化条件	净化条件
Pb	283.3	2.0	0.4	氘灯校正	100℃, 10/15s	600℃, 10/15s	1800℃, 0/3s	2100℃, 0/2s
Cr	357.9	4.0	0.4	氘灯校正	100℃, 10/15s	1000℃, 10/15s	2200℃, 0/4s	2400℃, 0/2s
Cu	324.8	3.0	0.4	氘灯校正	100℃, 10/15s	800℃, 10/15s	1800℃, 0/4s	2100℃, 0/2s

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表 2 方法的分析性能

Table 2. Analytical performance of the method

待测元素	线性方程	线性范围 (ng/mL)	相关系数	检出限 (ng/mL)	RSD (%)
Pb	y=0.0025ρ+0.0508	0~200	0.9937	3.50	2.1
Cr	y=0.0061ρ+0.0403	0~100	0.9968	0.92	3.6
Cu	y=0.0051ρ+0.0026	0~100	0.9991	1.22	2.8

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表 3 火山灰样品待测元素含量及加标回收率

Table 3. Analytical results of three heavy metals in volcanic ash samples and spiked recovery of the method

待测元素	样品测定值 (μg/g)	加标值 (μg/g)	加标后测定值 (μg/g)	回收率 (%)
Pb	8.82±0.44	4	11.9±0.61	92.8
Pb	8.82±0.44	8	17.5±0.95	104.0
Cr	12.0±0.32	6	16.8±0.52	93.3
Cr	12.0±0.32	12	22.9±1.21	95.4
Cu	21.3±0.13	10	33.6±2.43	107.0
Cu	21.3±0.13	20	39.2±2.13	94.9

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