Determination of Chlorine in Marine Sediment by Inductively Coupled Plasma-Atomic Emission Spectrometry with Ammonia Extraction
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摘要: 氯的电离能高，在等离子体中难于解离，通常的电感耦合等离子体发射光谱(ICP-AES)光路不能彻底地将空气排出，使得氯的光波被强烈吸收，很难找出相应的特征谱线因而无法准确测定地质样品中的氯。本文对海洋沉积物样品用10%的氨水在超声振荡器中振荡30 min，即可完全提取其中的氯，用ICP-AES测定，选择分析谱线为725.670 nm，方法检出限为50 μg/g(10σ，稀释因子=100)。用海洋沉积物标准物质GBW 07313、GBW 07315、GBW 07316验证，方法精密度(RSD，n=7)为4.3%～8.6%，测定值与标准值的相对误差为2.9%～4.9%。方法简单快速，准确度高，实现了地质样品中氯的准确测定，能够满足海洋地球化学研究的需要。
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关键词:
- 海洋沉积物 /
- 氯 /
- 氨水提取 /
- 电感耦合等离子体发射光谱法
Abstract: It is difficult to dissociate Cl by plasma because of the high ionization energy. Since the optical path of Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) cannot produce a low enough vacuum, the light wave of Cl is absorbed intensively causing difficulty in identifying the characteristic spectrum and subsequently in obtaining an accurate measurement of Cl in geology samples. In this article, a method is described here for completely extracting Cl in marine sediment samples by 10% ammonia with 30 minutes ultrasound bath. The Cl was measured by ICP-AES with an analysis spectrum of 725.670 nm. The detection limit of this method, which was based on ten standard deviations of the blank (10σ, dilution factor=100), was 50 μg/g for Cl. The accuracy and precision of the method were verified by analyzing different geological certified reference materials GBW 07313, GBW 07315 and GBW 07316. The relative standard deviations (RSD, n=7) of the results of independent determination GBW 07316 were 4.3%-8.6%, and relative error (n=7) were 2.9%-7.5%. Compared with traditional methods, this method is simple, fast, easy to perform, and its precision and accuracy are suitable for marine geochemistry. -
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表 1 称样量对Cl溶出效果的影响
Table 1. The effect of sample quantity on Cl dissolution
标准物质编号 w(Cl)/% 称样量0.5000 g
(DF=20)称样量0.1000 g
(DF=100)标准值 GBW 07313 3.96 4.12 4.07±0.07 GBW 07315 3.91 4.07 3.9±0.3 GBW 07316 3.54 3.67 3.5±0.2 
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表 2 溶样时间对Cl溶出效果的影响
Table 2. The effect of dissolving time for samples on Cl dissolution
标准物质编号 w(Cl)/% 10 min 30 min 60 min 90 min 标准值 GBW 07313 2.90 4.21 3.91 4.15 4.07±0.07 GBW 07315 2.78 4.12 3.96 4.07 3.9±0.3 GBW 07316 2.70 3.87 3.54 3.51 3.5±0.2
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表 3 氨水浓度对测定结果的影响
Table 3. The effect of ammonia solution concentration on Cl dissolution
氨水浓度 w(Cl)/% RSD/% 相对误差RE/% 标准值 11次测定值 平均值 10% 3.5±0.2 3.62 3.55 3.73 3.57 3.68 2.44 5.30 3.71 3.82 3.68 3.82 3.74 3.67 3.63 20% 3.5±0.2 4.24 3.85 3.95 3.79 4.02 3.34 14.8 4.11 4.00 3.94 4.12 4.14 3.97 4.08
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表 4 方法精密度和准确度
Table 4. Precision and accuracy tests of the method
标准物质编号 w(Cl)/% RSD/% 相对误差RE/% 标准值 7次测定值 平均值 GBW 07313 4.07±0.07 3.91 4.39 3.97 4.19 4.7 2.9 4.18 4.32 4.41 4.14 GBW 07315 3.9±0.3 3.91 4.38 3.69 4.09 4.3 4.9 4.43 4.12 3.95 4.17 GBW 07316 3.5±0.2 3.94 3.46 3.15 3.64 8.6 4.0 4.01 3.87 3.53 3.51
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