Determination of chromium(Ⅵ) in soil by flame atomic absorption spectrometry with constant temperature shaking extraction
YANG Jianbo1,2, MENG Jianwei1,2, QIU Hongxu*1,2, LIU Xian1,2 LI Xiaojing1,2, YAO Ran1,2
1. Hebei Research Center for Geoanalysis,Baoding 071001,China; 2. Hebei Key Laboratory of Mineral Resources and Ecological Environment Monitoring,Baoding 071001,China
Abstract：The amount of Cr(Ⅵ) is an important index for the monitoring of soil environment. The leaching and accurate determination of Cr(Ⅵ) content is crucial to the soil pollution monitoring and remediation.Cr(Ⅵ) in soil was extracted with Na2CO3-NaOH alkaline extraction solution, phosphate buffer solution-MgCl2 system by shaking in constant temperature water bath shaking at 92.5 ℃. After centrifugation at 4 000 r/min for 10 min, the extracting solution was filtered by syringe combined with pinhole filter membrane. Phenolphthalein was used as the indicator. The pH of testing solution was adjusted to 7.0-8.0 with 50%(volume fraction) HNO3 for the secondary separation of Cr(Ⅲ) and Cr(Ⅵ). Consequently, the determination method of Cr(Ⅵ) in soil by flame atomic absorption spectrometry(FAAS) was established.Under the selection conditions,the mass concentration of Cr(Ⅵ) in range of 0.10-2.00 μg/mL was directly proportional to the corresponding absorption intensity. The correlation coefficient was 0.999 3. The limit of detection and limit of quantification was 0.43 μg/g and 1.51 μg/g, respectively.In the detection process,too high salt content in testing solution or the increase of flow rate would cause the rapid accumulation of salt in the combustion head, thus affecting the measurement results. The experimental results showed that the cleaning of combustion head with 20% HNO3 (volume fraction) for 5 s after each determination could eliminate such physical interference.Three certified reference materials of soil for composition analysis of chromium(Ⅵ)[GBW(E)070252, GBW(E)070254 and GBW(E)070255] with different content level and four soil samples from industrial land were determined for 12 times according to the experimental method. The determination results of certified reference materials were basically consistent with the certified values. The relative standard deviation (RSD, n=12) of determination results of samples were all not more than 5.6%. The proposed method was applied for the determination of certified reference materials of soil for composition analysis of chromium(Ⅵ). Meanwhile,different amounts of soluble K2Cr2O7 and insoluble PbCrO4 were used for standard addition recovery tests. The recoveries were between 94% and 106%.
杨建博, 孟建卫, 邱红绪, 刘显, 李晓敬, 姚然. 恒温振荡浸提-火焰原子吸收光谱法测定土壤中铬(Ⅵ)[J]. 冶金分析, 2022, 42(4): 45-52.
YANG Jianbo, MENG Jianwei, QIU Hongxu, LIU Xian LI Xiaojing, YAO Ran. Determination of chromium(Ⅵ) in soil by flame atomic absorption spectrometry with constant temperature shaking extraction. , 2022, 42(4): 45-52.
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