【引用本文】 黄海波, 沈加林, 陈宇, 等. 全谱发射光谱仪应用于分析地质样品中的银锡硼钼铅[J]. 岩矿测试, 2020, 39(4): 555-565. doi: 10.15898/j.cnki.11-2131/td.201909230137
HUANG Hai-bo, SHEN Jia-lin, CHEN Yu, et al. Simultaneous Determination of Silver, Boron, Tin, Molybdenum and Lead in Geological Samples by Atomic Emission Spectrometer with Full Spectrum[J]. Rock and Mineral Analysis, 2020, 39(4): 555-565. doi: 10.15898/j.cnki.11-2131/td.201909230137

全谱发射光谱仪应用于分析地质样品中的银锡硼钼铅

中国地质调查局南京地质调查中心, 江苏 南京 210016

收稿日期: 2019-09-23  修回日期: 2020-01-18  接受日期: 2020-04-24

基金项目: 国家重点研发计划项目“土地生态恢复评价检验检测及质量控制标准研究”(2017YFF0206804)

作者简介: 黄海波, 工程师, 主要从事光谱、ICP-OES/MS等分析方法的应用与研究。E-mail:huanxinxing@163.com; 。沈加林, 硕士, 高级工程师, 主要从事分析测试、物相分析、地质矿产的研究。E-mail:sjlilu@163.com

Simultaneous Determination of Silver, Boron, Tin, Molybdenum and Lead in Geological Samples by Atomic Emission Spectrometer with Full Spectrum

Nanjing Center of Geological Survey, China Geological Survey, Nanjing 210016, China

Received Date: 2019-09-23
Revised Date: 2020-01-18
Accepted Date: 2020-04-24

摘要:掌握地质样品中银锡硼钼铅的含量对于研究成矿规律和地球化学找矿极其重要,目前的分析方法很少能一次性准确高效检出银锡硼钼铅。本文在前人研究基础上建立了应用全谱发射光谱仪固体粉末进样,一次性高效、准确地分析检测地质样品中银锡硼钼铅的方法。采用国家一级标准物质(岩石、土壤和水系沉积物)对合成硅酸盐标准曲线进行第二次拟合以降低基体的干扰;设置元素分析谱线转换值实现元素分析谱线的简单切换,不同的样品含量使用不同的分析谱线,达到分析结果更加接近样品真值的效果,同时扩大了标准曲线线性范围。结果表明:银锡硼钼铅的检出限分别为0.0077μg/g、0.19μg/g、0.68μg/g、0.058μg/g、0.49μg/g,方法精密度在3.23%~9.39%之间。应用本方法分析土壤、水系沉积物、岩石国家一级标准物质的测定值与其认定值相符,△logC值的绝对值均小于0.10;实际样品和外控样的一次测试结果合格率分别为92%~98%、100%。本方法简单,分析速度快,避免了样品稀释带来的污染,使用多条分析谱线测定国家标准物质,相比传统发射光谱法使用单分析谱线的测定值更加接近认定值,检出限优于《地质矿产实验室测试质量管理规范》的规定值。

关键词: 地质样品, 金属和非金属元素, 全谱, 发射光谱仪, 二次拟合, 分析谱线转换值

要点

(1) 建立了全谱发射光谱仪一次性分析检测地质样品中银锡硼钼铅含量的方法。

Simultaneous Determination of Silver, Boron, Tin, Molybdenum and Lead in Geological Samples by Atomic Emission Spectrometer with Full Spectrum

ABSTRACT

BACKGROUND:

The contents of silver, tin, boron, molybdenum, and lead in geological samples are extremely important for studying the metallogenic regularity and for geochemical prospecting. Current analytical methods rarely determine silver, tin, boron, molybdenum, and lead simultaneously.

OBJECTIVES:

To establish a method to simultaneously determine silver, tin, boron, molybdenum and lead in geological samples.

METHODS:

To eliminate the matrix interference, first-class standard materials (rock, soil and water sediments) were used for linear fitting of the synthetic silicate standard materials curve. By setting analytical line conversion values, different analytical line can be used for samples with different contents.

RESULTS:

The detection limits of silver, tin, boron, molybdenum, and lead were 0.0077μg/g, 0.19μg/g, 0.68μg/g, 0.058μg/g, 0.49μg/g, respectively. The precisions of the method were 3.23%-9.39%. The measured value of national first class standard materials including soil, water sediments and rock by this method was in accordance with standard values, with an absolute value of △logC < 0.10. The qualified rates of actual sample were 92%-98%, and the qualified rate of the inspection sample was 100%.

CONCLUSIONS:

This method is easy to apply and can be used to analyze samples rapidly. It can also be used to avoid contamination during sample dilution. Compared with traditional atomic emission spectrometry that uses a single analytical spectrum line, this method can be used to obtain a value which is closer to the standard value of national standard materials. The detection limit of this method is much lower than the standard value of the specification of testing quality management for geological laboratories.

KEY WORDS: geological sample, metal and non-metal elements, full spectrum, atomic emission spectrometry, second fitting, analytical line conversion values

HIGHLIGHTS

(1) A method was established to detect the contents of silver, boron, tin, molybdenum and lead in geological sample with a full spectrum atomic emission spectrometer.

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全谱发射光谱仪应用于分析地质样品中的银锡硼钼铅

黄海波, 沈加林, 陈宇, 刘建坤