Citation: XU Gui-Ru, QU Jian-Guo, CHANG Yan, TANG Ai-Ling. Accurate Determination of Sulfur Content in Sediments by Double Focusing Inductively Coupled Plasma Mass Spectrometry Combined with Microwave Digestion and Studies on Related Matrix Effect[J]. Chinese Journal of Analytical Chemistry, ;2016, 44(2): 273-280. doi: 10.11895/j.issn.0253-3820.150735 shu

Accurate Determination of Sulfur Content in Sediments by Double Focusing Inductively Coupled Plasma Mass Spectrometry Combined with Microwave Digestion and Studies on Related Matrix Effect

1.
¹ State Key Laboratory of Estuarine and Coastal Research, East China Normal University, Shanghai 200062, China;
2.
² School of Ecological and Environment Science, East China Normal University, Shanghai 200241, China;
3.
³ Shanghai Environmental Monitoring Center, Shanghai 200235, China

Corresponding author: QU Jian-Guo,
Received Date: 16 September 2015
Available Online: 25 November 2015
Fund Project: 本文系河口海岸学国家重点实验室基本科研业务费项目(No. 2013JSKF01)资助 (No. 2013JSKF01)

A robust method for measuring sulfur content in sediments was established using double focusing inductively coupled plasma mass spectrometry at medium resolution combined with microwave digestion technique. The capability of standard curve method (SCM) and standard addition method (SAM) using Rh as internal standard was compared in correction of the matrix effect. The results showed the matrix effect was not suppressed by SCM, but was effectively eliminated by SAM with drawback of low sample throughout. Therefore, the standard addition calibration method (SACM) was creatively proposed in this study, which can simply and easily correct the matrix effect as the matrix content of sample and standard solution was matched within ±50%. The detection limit and liner range of this method were proved to be 0.5 mg/kg and 3.0-1000 μg/L, respectively, with the spiked recovery of 95.8%-99.2%. Four sediment standard reference materials GBW07306, GBW07309, GBW07313 and SRM1646a were analyzed repetitively with the obtained sulfur contents of (853±14) μg/g (2σ, n=12), (181±7) μg/g (2σ, n=9), (3131±52) μg/g (2σ, n=12) and (3543±70) μg/g (2σ, n=9), respectively. The relative error of the four reference materials was +8.8%, +13.3%, +1.0% and +0.7%, respectively, with precision (RSD) less than 2%. This method was applied to determine the sulfur content in the sediment cores collected in the Yangtze Estuary and Hangzhou Bay. This proposed method was demonstrated as an accurate and rapid way of determining sulfur content in great batch of sediments samples, and has a broad application range including soil samples.
- Microwave digestion,
- Inductively coupled plasma mass spectrometry,
- Sediment,
- Sulfur,
- Matrix interference,
- Standard addition calibration method
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