干灰化-碳酸钠碱熔-电感耦合等离子体发射光谱法测定植物样品中硅含量

doi:10.16178/j.issn.0528-9017.20240515

摘要/Abstract

摘要：

该研究建立了一种通过干灰化-碳酸钠碱熔-电感耦合等离子体发射光谱法(ICP-OES)测定植物样品中硅(Si)含量的方法。即根据不同种类样品中的灰分含量,将适量样品经马弗炉灼在600 ℃条件下灰化,然后加入碳酸钠在950 ℃熔融,使用稀盐酸溶液提取熔块后,用ICP-OES测得Si含量。结果表明,该方法在最佳试验条件下,检出限为6 mg·kg^-1,测定下限为24 mg·kg^-1,精密度和准确度符合相关规范要求。将所建方法应用于实际植物样品中的Si含量测试,其测定结果与标准物质的相对误差在-16.4%~10.5%,满足《生态地球化学评价生物样品技术要求》(DD2005-03)中对分析准确度的要求,即分析平均值与标准物质推荐值的相对误差RE≤30%。

关键词: 干灰化, 碱熔, 植物样品, 硅含量

Abstract:

In this study, a method for determining silicon (Si) content in plant samples using sodium carbonate alkali fusion ash-inductively coupled plasma emission spectroscopy (ICP-OES) has been established. The method involves ashing a suitable amount of sample at 600 ℃ in a muffle furnace, fusing the ash with sodium carbonate at 950 ℃, and extracting the fusion residue with dilute hydrochloric acid before measuring the Si content using ICP-OES. The results indicated that under optimal conditions, the method has a detection limit of 6 mg·kg^-1 and a quantification limit of 24 mg·kg^-1, with precision and accuracy meeting relevant standards. When applied to actual plant samples, this method showed a relative error of -16.4% to 10.5% compared with the standard materials, meeting the accuracy requirements specified in the “Technical Requirements for Ecological Geochemical Evaluation of Biological Samples” (DD2005-03), which stipulates that the relative error (RE) between the analytical mean and the recommended value of the standard material should be≤30%.

Key words: dry ashing, alkali fusion, plant samples, silicon content

中图分类号:

Q94-33

许熔熔, 阮泽斌, 胡铁军, 周飞. 干灰化-碳酸钠碱熔-电感耦合等离子体发射光谱法测定植物样品中硅含量[J]. 浙江农业科学, 2025, 66(1): 163-167.

XU Rongrong, RUAN Zebin, HU Tiejun, ZHOU Fei. Determination of silicon content in plant samples by sodium carbonate alkali fusion ash-inductively coupled plasma emission spectroscopy[J]. Journal of Zhejiang Agricultural Sciences, 2025, 66(1): 163-167.

图/表 5

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参数	数值
高频功率	1 100 W
冷却气流量	18 L·min^-1
辅助气流量	0.2 L·min^-1
蠕动泵提升量	1.0 L·min^-1
积分时间	15 s
积分次数	2
背景校正	离峰左右两点

参数	数值
高频功率	1 100 W
冷却气流量	18 L·min^-1
辅助气流量	0.2 L·min^-1
蠕动泵提升量	1.0 L·min^-1
积分时间	15 s
积分次数	2
背景校正	离峰左右两点

类别	灰分含量/%	称样量/g
精粮(大米、小麦、玉米)	1	5
豆类	5	2
植物(根茎叶)	10~15	1
果实类	5	2

类别	灰分含量/%	称样量/g
精粮(大米、小麦、玉米)	1	5
豆类	5	2
植物(根茎叶)	10~15	1
果实类	5	2

样品	测定值/(mg·kg^-1)	平均值/ (mg·kg^-1)	相对标准偏差/%
GSB6(菠菜)	0.19,0.19,0.21,0.20,0.20,0.18,0.20,0.19,0.19,0.21,0.20,0.21	0.20	4.89
GSB11(柑橘叶)	0.42,0.44,0.41,0.45,0.38,0.42,0.39,0.43,0.45,0.39,0.43,0.41	0.42	5.57