悬浮液进样石墨炉原子吸收光谱法测定环境样品中痕量铅

基金项目:

国土资源部“九五”科技项目 9505601- 2

DETERMINATION OF TRACE LEAD IN ENVIRONMENTAL SAMPLES BY SLURRY SAMPLING WITH GRAPHITE FURNACE ATOMIC ABSORPTION SPECTROMETRY

1.
Department of City Building and Environmental Protection, Jianghan University, Wuhan 430010, China
2.
Faculty of Material Science and Chemical Engineering, China University of Geosciences, Wuhan 430074, China

摘要: 提出了悬浮液进样石墨炉原子吸收光谱法测定环境样品中痕量铅的分析方法.讨论了悬浮颗粒粒径、悬浮液浓度、悬浮稳定剂、基体改进剂等因素对测定结果的影响.实验结果表明: 样品粒径 < 38μm, 以0.2g/L的Triton - 100为悬浮剂, 3g/L的(NH₄)₂HPO₄为基体改进剂, 电磁搅拌进样可简便快速地测定地质样品中的痕量铅, 方法的检出限为0.10ng/g, 精密度为3.31% (n =10).43GSD标样测定结果与推荐值一致
- 悬浮液进样 /
- 石墨炉原子吸收法 /
- 环境样品 /
- 铅
Abstract: A method has been developed for the determination of trace lead in the environmental samples by slurry sampling with graphite furnace atomic absorption spectrometry (GFAAS). The effects of particle size, slurry concentration, modifiers and slurry stability agents on the accurate determination are dealt with in this paper. The research shows that the particle size < 38 μm, the magnetic agitation with 0.2 g/L Triton-100 as stability agent, and the 3 g/L (NH₄)₂HPO₄ as a modifier are of practical use. The detection limit is 0.10ng/g, and the precision (RSD, n=10) is 3.31%. The analytical results of the standard reference samples are consistent with the certified values.
- slurry sampling /
- graphite furnace atomic absorption spectrometry /
- environmental sample /
- lead

图 1 样品悬浮液原子化曲线

1.样品; 2.样品+基体改进剂

Fig. 1. Atomization curve of sample slurry

下载: 全尺寸图片幻灯片

图 2 酸介质质量分数对吸光度的影响

1.HNO₃; 2.HCl; 3.H₂SO₄

Fig. 2. Effect of mass fraction of acidic medium on singal

下载: 全尺寸图片幻灯片

表 1 Pb的测定条件

Table 1. Instrumental conditions for the determination of Pb

表 2 样品粒度试验

Table 2. Sample particle size experiment

表 3 样品分析结果

Table 3. Comparison of Pb mass fraction in reference materials as determined by slurry technique

[1]	邓世林, 李新凤, 周平. 固体进样平台GFAAS直接测定土壤中铅和镉[J]. 光谱学与光谱分析, 1996, 16 (3): 106. https://www.cnki.com.cn/Article/CJFDTOTAL-GUAN603.020.htm
[2]	Brady D V, Montalvo J G, Glowacki G, et al. Direct determination of lead in plant leaves via GFAAS[J]. At Absorpt Newsl, 1974, 13(5): 118.
[3]	傅学起, 杨树. 电热原子吸收悬浊液进样测定煤飞灰中的铅[J]. 光谱学与光谱分析, 1997, 17 (5): 98. https://www.cnki.com.cn/Article/CJFDTOTAL-GUAN705.019.htm
[4]	林潮平. 石墨炉原子吸收测定铅时锂、钠、钙、镁的化学干扰[J]. 暨南大学学报, 1995, 16 (1): 80. https://www.cnki.com.cn/Article/CJFDTOTAL-JNDX501.012.htm
[5]	邬家祥. 快速塞曼石墨炉原子吸收法测定饮用水中的痕量铅和镉[J]. 光谱学与光谱分析, 1994, 16 (3): 41. https://www.cnki.com.cn/Article/CJFDTOTAL-GUAN801.021.htm