【引用本文】 任冬, 周小琳, 宗有银, 等. 封闭酸溶-盐酸羟胺还原ICP-MS法测定土壤沉积物岩石中的痕量碘[J]. 岩矿测试, 2019, 38(6): 734-740. doi: 10.15898/j.cnki.11-2131/td.201901170009
REN Dong , ZHOU Xiao-lin , ZONG You-yin , et al. Determination of Trace Iodine in Soils, Sediments and Rocks by ICP-MS after Pressurized Acid Digestion-Hydroxylamine Hydrochloride Reduction[J]. Rock and Mineral Analysis, 2019, 38(6): 734-740. doi: 10.15898/j.cnki.11-2131/td.201901170009

封闭酸溶-盐酸羟胺还原ICP-MS法测定土壤沉积物岩石中的痕量碘

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: 2019-01-17  修回日期: 2019-06-25 

作者简介: 任冬,工程师,从事ICP-MS分析检测工作。E-mail:296536872@qq.com。。

Determination of Trace Iodine in Soils, Sediments and Rocks by ICP-MS after Pressurized Acid Digestion-Hydroxylamine Hydrochloride Reduction

Zhangye Mineral Exploration Institute, Gansu Nonferrous Metal Geological Exploration Bureau, Zhangye 734000, China

Received Date: 2019-01-17
Revised Date: 2019-06-25

摘要:碘是活跃元素,价态多,各价态间易相互转化,化学性质不稳定,使用ICP-MS测定土壤、沉积物和岩石样品中的痕量碘,样品前处理和测定结果的稳定性是主要问题。本文采用磷酸-高氯酸高压密闭消解处理样品,提高了样品分解效率,也避免了碘的挥发损失,通过加入0.5mL 20g/L盐酸羟胺溶液将碘还原为I-,提高了碘的稳定性,再于100℃烘箱中保温至少20min,以稀氨水作介质,降低了ICP-MS测定过程中的记忆效应。方法的相对标准偏差(RSD)为4.9%~9.2%,相对误差为-6.9%~8.3%,回收率为92.5%~109.6%,检出限(3s)为0.012μg/g。本方法的测定数据与半熔法吻合,解决了当前方法中存在的分析流程长、空白高、岩石样品提取不完全、提取装置繁多等问题,可以作为土壤、沉积物、岩石中痕量碘测定方法的一种补充,适合批量样品分析。

关键词: 土壤, 沉积物, 岩石, 封闭酸溶, 盐酸羟胺, 电感耦合等离子体质谱法,

Determination of Trace Iodine in Soils, Sediments and Rocks by ICP-MS after Pressurized Acid Digestion-Hydroxylamine Hydrochloride Reduction

KEY WORDS: soil, sediment, rocks, pressurized acid digestion, hydroxylamine hydrochloride, inductively coupled plasma-mass spectrometry, iodine

本文参考文献

[1]

李冰,何红蓼,史世云,等.电感耦合等离子体质谱同时测定地质样品中痕量碘溴砷硒的研究Ⅰ.不同阴离子形态及不同介质对分析信号的影响[J].岩矿测试,2001,20(3):161-166.

Li B,He H L,Shi S Y,et al.Determination of trace iodine,bromine,selenium and arsenic in geological samples by inductively coupled plasma mass spectrometry.Ⅰ.Signal response of different anion species in media[J].Rock and Mineral Analysis,2001,20(3):161-166.

[2]

李冰,史世云,何红蓼,等.电感耦合等离子体质谱同时测定地质样品中痕量碘溴砷硒的研究Ⅱ.土壤及沉积物标准物质分析[J].岩矿测试,2001,20(4):241-245.

Li B,Shi S Y,He H L,et al.Determination of trace iodine,bromine,selenium and arsenic in geological samples by inductively coupled plasma mass spectrometry.Ⅱ.Standard material analysis of soil and sediment[J].Rock and Mineral Analysis,2001,20(4):241-245.

[3]

Vanhoe H,Allemeersch F V,Versieck J,et al.Effect of solvent type on the determination of total iodine in milk powder and human serum by inductively coupled plasma mass spectrometry[J].Analyst,1993,118(8):1015-1019.

[4]

Larsen EH,Ludwigsen M B.Determination of iodine in food-related certified reference materials using wet ashing and determination by inductively coupled plasma mass spectrometry[J].Journal of Analytical Atomic Spectrometry,1997,12(6):435-439.

[5]

Pieoloto R S,Cruz S M,Mello P A,et a1.Combining pyrohydrolysis and ICP-MS for bromine and iodine determination in airborne particulate matter[J].Microchemical Journal,2014,116:225-229.

[6]

Tagami K,Uchida S.Sample storage conditions and holding times for the determination of total iodine in natural water samples by ICP-MS[J].Atomic Spectroscopy,2005,26(6):209-214.

[7]

Michel A,Villemant B.Determination of halogens (F,Cl,Br,I),sulfur and water in seventeen geological reference materials[J].Geostandards and Geoanalytical Research,2003,27(2):163-171.

[8]

赵庆令,李清彩,蒲军,等.电感耦合等离子体发射光谱法同时测定土壤样品中砷硼铈碘铌硫钪锶钍锆等31种元素[J].岩矿测试,2010,29(4):455-457.

Zhao Q L,Li Q C,Pu J,et al.Simultaneous determination of 31 elements such as arsenic,boron,cerium,iodine,niobium,sulfur,scandium,strontium,thorium and zirconium in soil samples[J].Rock and Mineral Analysis,2010,29(4):455-457.

[9]

程素敏,王娟,张岩,等.分光光度法测定土壤中碘的方法改进[J].中国无机分析化学,2015,5(4):41-43.

Cheng S M,Wang J,Zhang Y,et al.Improvement of spectrophotometric method for the determination of iodine in soil[J].China Inorganic Analytical Chemistry,2015,5(4):41-43.

[10]

阳国运,唐裴颖,张洁,等.电感耦合等离子体质谱法测定地球化学样品中的硼碘锡锗[J].岩矿测试,2019,38(2):154-159.

Yang G Y,Tang P Y,Zhang J,et al.Determination of boron,iodine,tin and germanium in geochemical samples by inductively coupled plasma-mass spectrometry[J].Rock and Mineral Analysis,2019,38(2):154-159.

[11]

李锦昕,邵一立,刘国均.流动注射G光度法测定地质样品中痕量碘[J\].岩矿测试,1993,12(1):11-13.

Li J X,Shao Y L,Liu G J.Flow injection G spectrophotometric determination of trace iodine in geological samples[J].Rock and Mineral Analysis,1993,12(1):11-13.

[12]

张培新,黄光明,董丽,等.电感耦合等离子体质谱法同时测定地质样品中锗碘[J].岩矿测试,2005,24(1):36-38.

Zhang P X,Huang G M,Dong L,et al.Simultaneous determination of germanium and iodine in geological samples by inductively coupled plasma mass spectrometry[J].Rock and Mineral Analysis,2005,24(1):36-38.

[13]

万兵,孙立欣,贾雨薇,等.电感耦合等离子体质谱(ICP-MS)法测定地球化学样品中的碘[J].中国无机分析化学,2017,7(4):57-59.

Wan B,Sun L X,Jia Y W,et al.Determination of iodine in geochemical samples by inductively coupled plasma mass spectrometry (ICP-MS)[J].China Inorganic Analytical Chemistry,2017,7(4):57-59.

[14]

董薇.催化动力学分光光度法测定区域地球化学样品中的碘[J].广州化工,2018,46(4):99-100.

Dong W.Catalytic kinetic spectrophotometric determination of iodine in regional geochemical samples[J].Guangzhou Chemical Industry,2018,46(4):99-100.

[15]

张学华,王君玉,韩敏.氯胺T-四碱催化分光光度法测定河南省黄淮平原农业地质调查样品中痕量碘[J].岩矿测试,2007,26(5):391-394.

Zhang X H,Wang J Y,Han M.Catalytic spectrophotometric determination of trace iodine in agricultural geological survey samples of Huanghuai Plain,Henan Province by chloramine T-tetraalkali[J].Rock and Mineral Analysis,2007,26(5):391-394.

[16]
[17]

马新荣,李冰,韩丽荣.稀氨水密封溶解-电感耦合等离子体质谱测定土壤沉积物及生物样品中的碘溴[J].岩矿测试,2003,22(3):174-178.

Ma X R,Li B,Hang L R.Determination of total iodine and bromine in soil,sediment and biological samples by inductively coupled plasma mass spectrometry with dilute ammonia pressurizing decomposition[J].Rock and Mineral Analysis,2003,22(3):174-178.

[18]

宋萍,温宏利.液氮冷凝吸收热解-电感耦合等离子体质谱法测定岩石土壤沉积物中的溴碘[J].岩矿测试,2016,35(4):384-388.

Song P,Wen H L.Determination of bromine and iodine in rock and soil sediments by liquid nitrogen condensation absorption pyrolysis-inductively coupled plasma mass spectrometry[J].Rock and Mineral Analysis,2016,35(4):384-388.

[19]

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.

[20]

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.

[21]

王祝,苏思强,邵蓓,等.高压密闭消解-电感耦合等离子体原子发射光谱/质谱法测定鸡蛋中16种元素的含量[J].理化检验(化学分册),2017,52(4

):108-112. Wang Z,Su S Q,Shao B,et al.Determination of 16 elements in eggs by high pressure closed digestion-inductively coupled plasma atomic emission spectrometry/mass spectrometry[J].Physical Testing and Chemical Analysis (Part B:Chemical Analysis),2017,52(4):108-112.

[22]

张兴超,刘超,黄艺,等.干法灰化处理对含有机质土壤样品铜同位素测量的影响[J].岩矿测试,2018,37(4):347-355.

Zhang X C,Liu C,Huang Y,et al.The effect of dry-ashing method on copper isotopic analysis of soil samples with organic matter[J].Rock and Mineral Analysis,2018,37(4):347-355.

[23]

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.

[24]

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.

[25]

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].

[26]

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

[27]

高孝礼,黄光明,张培新,等.电感耦合等离子体质谱法测定磷矿石中的碘[J].岩矿测试,2009,28(5):423-426.

Gao X L,Huang G M,Zhang P X,et al.Determination of iodine in phosphate ore by inductively coupled plasma mass spectrometry[J].Rock and Mineral Analysis,2009,28(5):423-426.

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封闭酸溶-盐酸羟胺还原ICP-MS法测定土壤沉积物岩石中的痕量碘

任冬, 周小琳, 宗有银, 张廷忠