Simultaneous Determination of Copper, Lead, Zinc and Nickel in Geochemical Samples by Emission Spectrometry with Solid Sampling Technique

MA Jingzhi; QU Shaopeng; LI Guangyi; DONG Xuebing; WU Meng; WU Jun; LI Ce; DONG Xuelin

doi:10.15898/j.cnki.11-2131/td.202202230030

Rock and Mineral Analysis > 2022 > 41(6): 1007-1016. > DOI: 10.15898/j.cnki.11-2131/td.202202230030

MA Jingzhi, QU Shaopeng, LI Guangyi, DONG Xuebing, WU Meng, WU Jun, LI Ce, DONG Xuelin. Simultaneous Determination of Copper, Lead, Zinc and Nickel in Geochemical Samples by Emission Spectrometry with Solid Sampling Technique[J]. Rock and Mineral Analysis, 2022, 41(6): 1007-1016. DOI: 10.15898/j.cnki.11-2131/td.202202230030

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Simultaneous Determination of Copper, Lead, Zinc and Nickel in Geochemical Samples by Emission Spectrometry with Solid Sampling Technique

1.
Key Laboratory of Rare Mineral, Ministry of Natural Resources; Hubei Province Geological Experimental Testing Center, Wuhan 430034, China
2.
Hubei Huaxiang Geological Environment Detection Technology Co., Ltd., Wuhan 430034, China
3.
Hubei Key Laboratory of Resources and Eco-Environment Geology, Geological Bureau of Hubei Province, Wuhan 430034, China

More Information

Received Date: February 22, 2022
Revised Date: March 31, 2022
Accepted Date: April 29, 2022
Available Online: December 13, 2022

Abstract

HIGHLIGHTS
(1) Internal standard method and average value of two parallel analyses were used to improve analytical precision.

(2) The sensitive line and hyposensitive line were both selected to extend the determination range of elements so that samples with different contents were analyzed using a different analytical line.

(3) Direct solid sampling technique was applied because it can simplify sample preparation. The quality and efficiency of analysis has been improved by adopting the photoelectric direct reading system instead of photosensitive plate.

ABSTRACT

BACKGROUND
The fast detection of Cu, Pb, Zn and Ni in geochemical samples helps to determine the level of heavy metal pollution, thus assisting in the employment of efficient treatments.
OBJECTIVES
To establish a method for the simultaneous determination of Cu, Pb, Zn and Ni in geochemical samples by AC Arc direct reading atomic emission spectrometry with solid sampling technique.
METHODS
With sodium fluoride, alumina, silicon dioxide and carbon powder as buffer agents and germanium as the internal standard element, the element analysis line pairs were optimized, and the exposure time was also optimized at 25s. The standard curve of synthetic silicate was corrected using national first-class reference materials (soil, rock and sediment), so as to reduce the interference of the matrix. Sensitive line and hyposensitive line were selected to enhance the accuracy as well as expand the measurable linear range of elements. Average value of two parallel analyses was adopted for further improved analytical precision.
RESULTS
The detection limits of Cu, Pb, Zn and Ni were 0.45μg/g, 1.46μg/g, 2.40μg/g and 1.58μg/g, respectively. The precision ranges of the method were 1.36%-6.25% for Cu, 1.17%-8.06% for Pb, 1.64%-9.68% for Zn and 0.91%-5.31% for Ni. Measured values with this method for the national first-class reference materials of soil, sediment and rock were consistent with the certified values (|△logC| ≤ 0.05), qualification rates of the actual samples and external quality control samples were all above 90%.
CONCLUSIONS
With simple operation, direct solid sampling technique is applied. The method reported here is more environmentally friendly compared to the acid dissolving method, sample contamination caused by reagent blank and vessels used is avoided at the same time. The average results of twice spectral acquisitions are calculated, which is more accurate and precise than the single analysis reported in the literature. All indicators of this method are better than the requirements of regulation (1:250000) DZ/T 0130.5-2006.
- geochemical samples,
- heavy metal elements,
- solid sampling,
- emission spectrometry

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References (37)

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