【引用本文】 任冬, 陈宇豪, 张廷忠, . 高压密闭消解技术在土壤有效态样品前处理中的应用[J]. 岩矿测试, 2020, 39(1): 143-149. doi: 10.15898/j.cnki.11-2131/td.201902270027
REN Dong , CHEN Yu-hao , ZHANG Ting-zhong . Application of High Pressure Closed Digestion in Pretreatment of Effective Soil Samples[J]. Rock and Mineral Analysis, 2020, 39(1): 143-149. doi: 10.15898/j.cnki.11-2131/td.201902270027

高压密闭消解技术在土壤有效态样品前处理中的应用

甘肃省有色金属地质勘查局张掖矿产勘查院, 甘肃 张掖 734000

收稿日期: 2019-02-27  修回日期: 2019-04-07 

基金项目: 甘肃省自然科学基金项目(2008BADA4B09)

作者简介: 任冬,工程师,主要从事土壤分析检测工作。E-mail:296536872@qq.com。。

Application of High Pressure Closed Digestion in Pretreatment of Effective Soil Samples

Zhangye Mineral Exploration Institute, Gansu Province Non-ferrous Metal Geological Exploration Bureau, Zhangye 734000, China

Received Date: 2019-02-27
Revised Date: 2019-04-07

摘要:土壤样品经有机酸浸提后,浸提出的溶液中存在大量有机酸及有机质,如未进行破坏处理,进入电感耦合等离子体发射光谱仪(ICP-OES)进样系统后容易堵塞雾化器、中心管、矩管等,或有颗粒黏附于中心管壁和矩管壁上,造成测定结果精密度和准确度差、空白高等问题,进而影响土壤有效态的综合评价。本文将土壤样品用有机酸(DTPA、草酸-草酸铵、柠檬酸等)浸提后,过滤或离心,吸取上清液加入高压密闭消解罐中,经电热板上处理,再加2mL浓硝酸,于180℃烘箱中保温至少3h,采用ICP-OES测定有效态元素铜锌铁锰镉铅镍铬钼硅的含量。本方法采用高压密闭消解技术处理土壤样品,各元素测定结果的相对标准偏差(RSD)为2.5%~9.8%,相对误差为-2.1%~5.2%,回收率为90.1%~103.2%,方法检出限为0.32μg/kg~0.038mg/kg;而采用以往高温炉中灼烧法、硝酸-高氯酸(硫酸)敞开消解法等技术手段,回收率为89.2%~100.5%,方法检出限为0.50μg/kg~0.050mg/kg,两者相比,本方法的测定结果稳定、空白低,分析周期短,适合批量样品的连续分析。

关键词: 土壤, 高压密闭消解, 有机酸, 有机质, 有效态, 电感耦合等离子体发射光谱法

Application of High Pressure Closed Digestion in Pretreatment of Effective Soil Samples

KEY WORDS: soil, high pressure closed digestion, organic acid, organic matter, effective state, inductively coupled plasma-optical emission spectrometry

本文参考文献

[1]

鲍士旦.土壤农化分析[M].北京:中国农业出版社,2000. Bao S T.Soil Agricultural Chemistry Analysis[M].Beijing:China Agricultural Publishing House,2000.

[2]

周卫红,张静静,邹萌萌,等.土壤重金属有效态含量检测与监测现状、问题及展望[J].中国生态农业学报,2017,25(4):605-615.

Zhou W H,Zhang J J,Zou M M,et al.The detection and monitoring of available heavy metal content in soil:A review[J].Chinese Journal of Eco-Agriculture,2017,25(4):605-615.

[3]

Khan A,Khan S,Khan M A,et al.The uptake and bio-accumulation of heavy metals by food plants,their effects on plants nutrients,and associated health risk:A review[J].Environmental Science and Pollution Research,2015,22(18):13772-13799.

[4]

Stasinos S,Zabetakis I.The uptake of nickel and chro-mium from irrigation water by potatoes,carrots and onions[J].Ecotoxicology and Environmental Safety,2013,91:122-128.

[5]

李锡坤,李鉴伦,洪翊,等.土壤中元素有效态分析质量管理实践[J].岩矿测试,2001,20(4):294-296.

Li X K,Li J L,Hong Y,et al.Quality management practice of effective state analysis of elements in soil[J].Rock and Mineral Analysis,2001,20(4):294-296.

[6]

李锡坤,李鉴伦,洪翊,等.酸性土壤中20种元素有效态浸提体系浅析[J].岩矿测试,2001,20(3):167-173.

Li X K,Li J L,Hong Y,et al.Preliminary analysis of 20 elements available extraction systems in acid soils[J].Rock and Mineral Analysis,2001,20(3):167-173.

[7]

岩石矿物分析编委会.岩石矿物分析(第四版第四分册)[M].北京:地质出版社,2011:891-892. The Editorial Committee of Rock and Mineral Analysis.Rock and Mineral Analysis (The Fourth Edition:Vol.Ⅳ)[M].Beijing:Geological Publishing House,2011:891

-892.

[8]

刘妹,顾铁新,程志中,等.10个土壤有效态成分分析标准物质研制[J].岩矿测试,2011,30(5):536-544.

Liu M,Gu T X,Cheng Z Z,et al.Ten reference materials for available nutrients of agricultural soils[J].Rock and Mineral Analysis,2011,30(5):536-544.

[9]

季海冰,潘荷芳,李震宇,等.电感耦合等离子体质谱法测定土壤中重金属有效态浓度[J].环境污染与防治,2008,30(12):60-62.

Ji H B,Pan H F,Li Z Y,et al.Determination of available concentrations of heavy metals in soil by inductively coupled plasma mass spectrometry[J].Environmental Pollution and Prevention,2008,30(12):60-62.

[10]

刘永林,邱祖民,周萍,等.电感耦合等离子体质谱法测定土壤中有效态微量元素[J].分析科学学报,2012,28(6):862-864.

Liu Y L,Qiu Z M,Zhou P,et al.Determination of available trace elements in soil by inductively coupled plasma mass spectrometry[J].Journal of Analytical Sciences,2012,28(6):862-864.

[11]

郭继斌,王莉,韩娇,等.联合浸提法测定土壤有效态镉[J].江苏农业科学,2016,44(3):369-372.

Guo J B,Wang L,Han J,et al.Combined extraction method for the determination of available cadmium in soil[J].Jiangsu Agricultural Science,2016,44(3):369-372.

[12]

杨俐苹,金继运,梁鸣早,等.ASI法测定土壤有效P、K、Zn、Cu、Mn与我国常规化学方法的相关性研究[J].土壤通报,2000,31(6):277-279.

Yang L P,Jin J Y,Liang M Z,et al.Study on the correlation between ASI determination of available P,K,Zn,Cu,Mn in soil and conventional chemical methods in China[J].Chinese Journal of Soil Science,2000,31(6):277-279.

[13]

仝淑慧,王莉,赵娟,等.M3法与DTPA法测定我国北方土壤微量元素的相关性及其浸提特征的研究[J].土壤通报,2016,44(2):420-424.

Tong S H,Wang L,Zhao J,et al.Study on the correlation and extraction characteristics of trace elements in soil of Northern China by DTPA and M3 method[J].Chinese Journal of Soil Science,2016,44(2):420-424.

[14]

韩张雄,熊英,王龙山,等.DTPA浸提-电感耦合等离子体质谱法测定石灰性土壤中的有效态钴和有效态铅[J].岩矿测试,2012,31(6):950-953.

Han Z X,Xiong Y,Wang L S,et al.Rapid determination of available cobalt & lead in calcareous soils by inductively coupled plasma-mass spectrometry with DTPA extraction[J].Rock and Mineral Analysis,2012,31(6):950-953.

[15]

盖荣银,孙友宝,马晓玲,等.二乙烯三胺五乙酸提取结合火焰原子吸收光谱法测定土壤中的有效态元素[J].环境化学,2016,35(5):1096-1097.

Gai R Y,Sun Y B,Ma X L,et al.diethylenetriamine pentaacetic acid and determination of available elements in soil by flame atomic absorption spectrometry[J].Environmental Chemistry,2016,35(5):1096-1097.

[16]

Li J,He P,Yu C.DPTA-catalyzed one-pot regioselective synthesis of polysubstituted pyridines and 1,4-dihydropyridines[J].Tetrahedron,2012,68(22):4138-4144.

[17]

胡德新,武素茹,刘跃勇,等.改进BCR法-电感耦合等离子体发射光谱法测定矿产品堆场土壤中镉砷铅的化学形态[J].岩矿测试,2014,33(3):374-378.

Hu D X,Wu S R,Liu Y Y,et al.Determination of chemical species of cadmium,arsenic and lead in mineral yard soil by modified BCR and ICP-AES method[J].Rock and Mineral Analysis,2014,33(3):374-378.

[18]

孙媛媛,孙友宝,盖荣银,等.二乙烯三胺五乙酸(DTPA)提取ICP-AES法测定土壤中有效态元素[J].环境化学,2015,34(8):1578-1579.

Sun Y Y,Sun Y B,Gai R Y,et al.Extraction of diethylenetriamine pentaacetic acid (DTPA) and determination of available elements in soil by ICP-AES[J].Environmental Chemistry,2015,34(8):1578-1579.

[19]

孙朝阳,贺颖婷,王雯妮.端视电感耦合等离子体发射光谱法测定土壤中有效钼[J].岩矿试,2010,29(3):267-270.

Sun C Y,He Y T,Wang W N.End-view ICP-OES determination of available molybdenum in soil[J].Rock and Mineral Analysis,2010,29(3):267-270.

[20]

陈志慧,孙洛新,钟莅湘,等.快速催化极谱法测定土壤中的有效态钼[J].岩矿测试,2014,33(4):584-588.

Chen Z H,Sun L X,Zhong L X,et al.Rapid catalytic polarographic determination of available molybdenum in soil[J].Rock and Mineral Analysis,2014,33(4):584-588.

[21]
[22]

孙鸣镝,方海兰,郝冠军,等.AB-DTPA,CaCl2-DTPA两种方法分析土壤8种元素的有效态含量[J].土壤与作物,2014,3(2):50-55.

Sun M D,Fang H L,Hao G J,et al.Analysing the available content of eight elements in soil from Shanghai by AB-DTPA and CaCl2-DTPA method[J].Soil and Crop,2014,3(2):50-55.

[23]

周春燕,张玉龙,石岩,等.不同浸提剂对保护地土壤有效硅测定结果的影响[J].中国农学通报,2006,22(2):226-230.

Zhou C Y,Zhang Y L,Shi Y,et al.Effects of different extractants on the determination results of available silicon in protected soil[J].China Agricultural Bulletin,2006,22(2):226-230.

[24]

吴磊,刘义博,王家松,等.高压密闭消解-电感耦合等离子体质谱法测定锰矿石中的稀土元素前处理方法研究[J].岩矿测试,2018,37(6):637-643.

Wu L,Liu Y B,Wang J S,et al.Study on the pretreatment method for determination of rare earth elements in manganese ores by high pressure sealed digestion-inductively coupled plasma-mass spectrometry[J].Rock and Mineral Analysis,2018,37(6):637-643.

[25]

鲁照玲,胡红云,姚洪.土壤中重金属元素电感耦合等离子体质谱定量分析方法的研究[J].岩矿测试,2012,31(2):241-246.

Lu Z L,Hu H Y,Yao H.Quantitative analysis of heavy metal elements in soil by inductively coupled plasma mass spectrometry[J].Rock and Mineral Analysis,2012,31(2):241-246.

[26]

冯婧.重金属元素分析消解技术在镉、砷检测中的应用比较[J].食品研究与开发,2017,38(16):153-158.

Feng J.Comparison of the application of heavy metal element analysis and digestion technology in the detection of cadmium and arsenic[J].Food Research and Development,2017,38(16):153-158.

[27]

贾双琳,赵平,杨刚,等.混合酸敞开或高压密闭溶样-ICP-MS测定地质样品中稀土元素[J].岩矿测试,2014,33(2):186-191.

Jia S L,Zhao P,Yang G,et al.Determination of rare earth elements in geological samples by ICP-MS with mixed acid open or high pressure closed solution samples[J].Rock and Mineral Analysis,2014,33(2):186-191.

[28]

田娟娟,杜慧娟,潘秋红,等.电热板消解与密闭罐消解对土壤中49种矿质元素ICP-MS法检测的影响[J].分析测试学报,2009,28(3):319-325.

Tian J J,Du H J,Pan Q H,et al.Effects of electrothermal plate digestion and closed tank digestion on the determination of 49 mineral elements in soil by ICP-MS[J].Journal of Instrumental Analysis,2009,28(3):319-325.

[29]

褚卓栋,肖亚兵,刘文菊,等.高压密闭消解土壤砷、汞、铅、镉酸体系比较[J].中国环境监测,2009,25(5):57-61.

Zhu Z D,Xiao Y B,Liu W J,et al.Comparisons of soil arsenic,mercury,lead and cadmium digestion systems by high pressure closed digestion[J].China Environmental Monitoring,2009,25(5):57-61.

[30]

任冬,刘彤彤,刘安安,等.高压密闭消解处理草酸-草酸铵浸提剂方法的改进[J].中国土壤与肥料,2019(3):198-201. Ren D,Liu T T,Liu A A,et al.Improvement of high pressure sealed digestion method for treating oxalic acid-ammonium oxalate extractant[J].Soil and Fertilizer Sciences in China,2019

(3):198-201.

[31]

EN 13656:2002.Characterization of Waste-microwave Assisted Digestion with Hydrofluoric (HF),Nitric (HNO3),and Hydrochloric (HCl) Acid Mixture for Subsequent Determination of Elements[S].

[32]

Link D D,Kingston H M S,Harrilla G J,et al.Development of microwave-assisted drying methods for sample preparation for dried spot micro-X-ray fluorescence analysis[J].Analytical Chemistry,2002,74(5):1165-1170.

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高压密闭消解技术在土壤有效态样品前处理中的应用

任冬, 陈宇豪, 张廷忠