Effect of Temperatures on Determination of Arsenic in Water by Atomic Fluorescence Spectrometry
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摘要: 氢化物发生-原子荧光光谱法受到仪器工作温度的影响主要来自于氢化物发生反应和仪器漂移，工作温度升高会增加仪器的背景值，而过低的工作温度又不利于氢化物发生反应进行。本文根据原子荧光光谱测定水体中砷的方法，在10℃、20℃和30℃的工作温度条件下，分别测试校准曲线、空白样品、自配质控样品和有证标准物质来确定最适宜的工作温度。结果表明：三个温度条件下的校准曲线均具有较好的线性相关性；仪器工作温度过高会引起空白荧光值变大、检出限升高，同时会造成仪器灵敏度的降低，增加了样品测试误差，测试结果不能满足准确度的要求。本文提出，利用原子荧光光谱法测定砷含量时，应控制仪器工作温度在10~20℃，并且保证温度变化相对稳定。Abstract:
BACKGROUNDThe influence of the operating temperature on Hydride Generation-Atomic Fluorescence Spectrometry comes mainly from the hydride reaction and the drift of the instrument. An increase in operating temperature increases the background value of the instrument, while a low operating temperature is not conducive to hydride reaction. OBJECTIVESTo investigate the effect of operating temperature on the determination of arsenic and to find the optimal temperature conditions. METHODSAccording to the standard method of Atomic Fluorescence Spectrometry for determination of arsenic in water, the calibration curves, the blank samples, the QC samples and the standard materials were analyzed at temperatures of 10℃, 20℃ and 30℃, respectively. RESULTSThe calibration curves in three temperature conditions had good linear correlation. However, when the operating temperature increased, the blank fluorescence value and detection limit increased accordingly, and the instrument sensitivity decreased. The analytical results cannot meet the accuracy requirement. CONCLUSIONSWhen the arsenic content is determined by Atomic Fluorescence Spectrometry, the working temperature of the instrument should be controlled at 10-20℃, where the temperature change is relatively stable. -
Key words:
- water /
- arsenic /
- Atomic Fluorescence Spectrometry /
- hydride generation /
- operating temperature /
- sensitivity
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表 1 不同室温条件下空白样品的荧光强度
Table 1. Intensity of blank samples in different room temperature
室温(℃) 连续11次空白荧光强度测量值 测量均值 标准偏差 检出限(μg/L) 31.73 28.86 34.15 26.28 10 30.24 30.52 31.09 30.27 30.39 2.56 0.02 26.05 33.53 31.56 35.73 35.99 30.07 32.04 20 32.40 25.80 27.10 22.78 28.73 4.92 0.04 28.58 22.21 23.78 44.75 46.10 50.32 41.61 30 42.09 41.38 36.10 43.51 42.91 4.57 0.04 34.72 44.03 47.44 
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表 2 不同工作温度条件下测定自配质控样品的浓度
Table 2. Concentration of QC samples at different working temperatures
室温(℃) 质控1# (μg/L) 相对误差(%) 质控2# (μg/L) 相对误差(%) 质控3# (μg/L) 相对误差(%) 10 2.06 3.0 10.3 3.0 15.2 1.3 20 1.90 4.5 10.4 4.0 15.4 2.7 30 1.85 7.7 9.63 3.7 15.8 5.6
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表 3 不同工作温度条件下测定标准样品的浓度
Table 3. Concentration of standard samples at different working temperatures
室温(℃) 标准样品9次测试值(μg/L) 平均值(μg/L) 相对标准偏差(%) 相对误差(%) 10 27.4 27.1 27.1 27.5 27.0 27.1 0.96 4.2 27.5 27.0 26.9 26.8 （合格） 20 25.9 26.0 25.9 25.8 25.6 25.7 0.86 1.2 25.6 25.5 25.5 25.3 （合格） 30 28.4 28.5 28.8 28.6 28.7 28.5 0.64 9.6 28.3 28.7 28.6 28.3 （不合格）
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