土壤中砷形态提取和分析的条件改进
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摘要
指出了通过改进砷的提取条件,以尽可能高的提取率来分析土壤和沉积物中的无机砷形态,同时可以最小化As(Ⅲ)和As(Ⅴ)之间的形态转化。选取磷酸混合盐酸作为提取剂,比较并优化了不同配比、不同的辅助提取手段、不同的预还原剂用量对提取土壤中不同形态砷的效率,并测定了土壤标准物质(GSS-32、GSS-33、GSS-35)和莲花山矿区周围农田土壤中各形态的砷含量以供参考。结果表明:使用1.5 mol/L的磷酸混合盐酸(4∶1)对土壤进行98℃水浴提取3次,每次1 h,浸取率最佳,可达91.34%。土壤标准物质和农田土壤中以As(Ⅴ)为主,占95.9%以上。精密度实验表明,相对误差小于3%(n=6,RSD,0.695～2.176%),该方法的加标回收率为94.87%～100.25%,可作为砷形态分析的理想方法。
The extraction conditions of arsenic were improved, and the inorganic arsenic species in soils and sediments were analyzed with the highest possible extraction rate, while the morphological transformation between As(III) and As(V) was minimized. Phosphoric acid and hydrochloric acid were used as extractant to compare and optimize the effects of different ratios, different auxiliary extraction methods and different pre-reducing agents on the extraction of species of arsenic in soil, and the arsenic content of various forms in the soil standard materials(GSS-32、GSS-33、GSS-35) and the soil around Lianhua Mountain mining area were determined for reference. The results showed that the soil subjected to 98 ℃ water bath heating extraction with 1.5 mol/L of phosphoric acid and hydrochloric acid(4:1) 3 times for 60 min each time can get the best extraction rate, up to 91.34%. As(V) is the main component of soil standard materials and farmland soil, accounting for more than 95.9%. The measurement accuracy experiments show that the relative error was less than 3%(n=6, RSD, 0.695～2.176%). Recovery studies were carried out and the obtained values were 94.87～100.25%, which could be an ideal method for arsenic speciation analysis.
The extraction conditions of arsenic were improved, and the inorganic arsenic species in soils and sediments were analyzed with the highest possible extraction rate, while the morphological transformation between As(III) and As(V) was minimized. Phosphoric acid and hydrochloric acid were used as extractant to compare and optimize the effects of different ratios, different auxiliary extraction methods and different pre-reducing agents on the extraction of species of arsenic in soil, and the arsenic content of various forms in the soil standard materials(GSS-32、GSS-33、GSS-35) and the soil around Lianhua Mountain mining area were determined for reference. The results showed that the soil subjected to 98 ℃ water bath heating extraction with 1.5 mol/L of phosphoric acid and hydrochloric acid(4:1) 3 times for 60 min each time can get the best extraction rate, up to 91.34%. As(V) is the main component of soil standard materials and farmland soil, accounting for more than 95.9%. The measurement accuracy experiments show that the relative error was less than 3%(n=6, RSD, 0.695～2.176%). Recovery studies were carried out and the obtained values were 94.87～100.25%, which could be an ideal method for arsenic speciation analysis.
引文
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[24]Zhao Y,Yang C Y,Qiu W.On the Determination of Arsenic in Desulfurization Waste Water by Hydride Generation Atomic Fluorescence Spectrometry [J].Journal of Tangshan University,2016.
[25]蔡保松,陈同斌,廖晓勇,等.土壤砷污染对蔬菜砷含量及食用安全性的影响[J].生态学报,2004,24(4):711～717.
[2]Rao Q,Sun Z,Tian L,et al.Assessment of arsenic and heavy metal pollution and ecological risk in inshore sediments of the Yellow River estuary,China [J].Stochastic Environmental Research and Risk Assessment,2018,32(10):2889～2902.
[3] Rahman M A,Rahman A,Mzk K,et al.Human health risks and socio-economic perspectives of arsenic exposure in Bangladesh:A scoping review[J].Ecotoxicology & Environmental Safety,2018(150):335～343.
[4]Madhukar M,Murthy B M S,Udayashankara T H.Sources of Arsenic in Groundwater and its health significance- a review [J].Nature Environment & Pollution Technology,2016,15(3):971～979.
[5]Lin H T,Wang M C,Seshaiah K.Mobility of adsorbed arsenic in two calcareous soils as influenced by water extract of compost [J].Chemosphere,2008,71(4):742～749.
[6]Wang Y,Ma F,Zhang Q,et al.An evaluation of different soil washing solutions for remediating arsenic-contaminated soils [J].Chemosphere,2017,173(3):68～72.
[7]Lock A,Wallschl?ger D,Mcmurdo C,et al.Validation of an updated fractionation and indirect speciation procedure for inorganic arsenic in oxic and suboxic soils and sediments [J].Environmental Pollution,2016(219).
[8]Zeng M,Liao B H,Zhang Y,et al.Study on the remediation effect of alkali solution on the arsenic-contaminated soil [J].Journal of Safety & Environment,2010,10(3):39～41.
[9]Saha S,Ghosh K,Das I,et al.Distribution of different inorganic forms of arsenic in selected arsenic affected soils of the Bengal Delta Basin [J].Journal- Indian Chemical Society,2005,8(2):364～367.
[10]Schmidt L,Landero J A,Santos R F,et al.Arsenic speciation in seafood by LC-ICP-MS/MS:method development and influence of culinary treatment[J].Journal of Analytical Atomic Spectrometry,2017,32(8).
[11]Tyruvola K,Nikolaidis N P,Veranis N,et al.Arsenic removal from geothermal waters with zero-valent iron--effect of temperature,phosphate and nitrate [J].Water Research,2006,40(12):2375～2386.
[12]赵秋香,李海萍,赵文海,等.土壤中毒性元素As的形态分析及其测定 [J].分析试验室,2007,26(2):56～59.
[13]刘伟鹏.砷在土壤—作物体系中的形态测定及累积规律研究[D].沈阳:沈阳农业大学,2017,15～16.
[14]Pumure I,Renton J J,Smart R B.Ultrasonic extraction of arsenic and selenium from rocks associated with mountaintop removal/valley fills coal mining:estimation of bioaccessible concentrations [J].Chemosphere,2010,78(11):1295～1300.
[15]白云飞.土壤底泥中砷形态提取与水样中砷形态保存实验研究[D].北京:中国地质大学,2007,17～21.
[16]Zhang J.Speciation Analysis of Arsenic in Soil Samples [J].Rock & Mineral Analysis,2008.
[17]Анатольевич В А.Экстракционная очистка медного электролита от мышьяка [J].2017,21(10(129)).
[18]马名扬,孙翠香,张朝阳,等.土壤中无机砷测定的三种前处理方法比较 [J].光谱实验室,2007,24(2):239～243.
[19]Chen S Z,Liu L P,Du H J,et al.Arsenic Species in Rat Serum after Oral Administration of Niuhuang Jiedu Tablet by HPLC-ICP-MS [J].Journal of Chinese Mass Spectrometry Society,2017,38(2):177～186.
[20]Phongsirirux S,Sricharoen P,Limchoowong N,et al.Mild Acid Ultrasonic Assisted Extraction of Arsenic Residues in Different Parts of Hot Chilli Prior to Ultra-Trace Determination by Flow Injection-Hydride Generation Atomic Absorption Spectrometry [J].Oriental Journal of Chemistry,2017,33(5):2347～2355.
[21]Wei M Q,Liu H C,Yan H M,et al.Determination of 4 kinds of arsenic species in rice by liquid chromatographyatomic fluorescence spectrometry [J].Journal of Food Safety & Quality,2016,7(9):3673～3677.
[22]Huber C S,Mgr V,Dessuy M B,et al.Sample preparation for arsenic speciation analysis in baby food by generation of substituted arsines with atomic absorption spectrometry detection [J].Talanta,2017(175):406～412.
[23]Santos G M D,Pozebon D,Cerveira C,et al.Inorganic arsenic speciation in rice products using selective hydride generation and atomic absorption spectrometry (AAS) [J].Microchemical Journal,2017(133):265.
[24]Zhao Y,Yang C Y,Qiu W.On the Determination of Arsenic in Desulfurization Waste Water by Hydride Generation Atomic Fluorescence Spectrometry [J].Journal of Tangshan University,2016.
[25]蔡保松,陈同斌,廖晓勇,等.土壤砷污染对蔬菜砷含量及食用安全性的影响[J].生态学报,2004,24(4):711～717.
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