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

REN Dong; ZHOU Xiao-lin; ZONG You-yin; ZHANG Ting-zhong

doi:10.15898/j.cnki.11-2131/td.201901170009

Rock and Mineral Analysis > 2019 > 38(6): 734-740. > DOI: 10.15898/j.cnki.11-2131/td.201901170009

REN Dong, ZHOU Xiao-lin, ZONG You-yin, ZHANG Ting-zhong. 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

Citation:

PDF (3181 KB)

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

More Information

Received Date: January 16, 2019
Revised Date: June 24, 2019
Accepted Date: July 15, 2019
Published Date: October 31, 2019

Abstract

HIGHLIGHTS
(1) The application of high-pressure sealed digestion technology to sample treatment improved the decomposition efficiency, and iodine was not easy to volatilize.

(2) The decomposition conditions of the sample were determined.

(3) This method could be used as a supplementary method for the determination of iodine.

ABSTRACT

BACKGROUNDIodine is an active element with many valences. It is easy to transform each other between valence states and its chemical properties are unstable. In terms of determination of trace iodine in soil, sediment and rock samples by inductively coupled plasma-mass spectrometry (ICP-MS), sample pretreatment and result stability are the main problems.
OBJECTIVESTo obtain stable results, low blank, a short analysis period and complete extraction.
METHODSThe sample was digested by phosphoric acid-perchloric acid under high-pressure sealed conditions. The decomposition efficiency of the sample was improved and the volatilization loss of iodine was avoided. The stability of iodine was improved by adding 0.5mL 20g/L hydroxylamine hydrochloride solution to reduce iodine to I^-. The iodine was kept in an oven at 10℃ for at least 20 minutes, and the memory effect during ICP-MS analysis was reduced by using dilute ammonia water as the medium.
RESULTSThe relative standard deviations of the method were 4.88%-9.19%, the relative errors were -6.90%-8.33%, the recoveries were 92.5%-109.6% and the detection limit (3s) was 0.012μg/g.
CONCLUSIONSThe data obtained by this method are in good agreement with those obtained by the semi-melting method. It solves the problems of long analysis process, high blank, incomplete extraction of rock samples and various extraction devices. It can be used as a supplement to the determination of trace iodine in soil, sediment and rock, and is suitable for batch sample analysis.
- soils,
- sediments,
- rocks,
- pressurized acid digestion,
- hydroxylamine hydrochloride,
- inductively coupled plasma-mass spectrometry,
- iodine

FullText(HTML)

References (27)

References

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. doi: 10.3969/j.issn.0254-5357.2001.03.001

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. doi: 10.3969/j.issn.0254-5357.2001.03.001

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. doi: 10.3969/j.issn.0254-5357.2001.04.001

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. doi: 10.3969/j.issn.0254-5357.2001.04.001

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. doi: 10.1039/an9931801015

Larsen E H, 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. http://www.wanfangdata.com.cn/details/detail.do?_type=perio&id=c01c01da0ead18e6e2bbc23e1737378e

Pieoloto R S, Cruz S M, Mello P A, et al.Combining pyrohydrolysis and ICP-MS for bromine and iodine determination in airborne particulate matter[J].Microchemical Journal, 2014, 116:225-229. doi: 10.1016/j.microc.2014.05.002

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. http://www.wanfangdata.com.cn/details/detail.do?_type=perio&id=dbaba7eba761eea50c8f38ea7f4ff288

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. doi: 10.1111/j.1751-908X.2003.tb00643.x

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. doi: 10.3969/j.issn.0254-5357.2010.04.026

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. doi: 10.3969/j.issn.0254-5357.2010.04.026

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. doi: 10.3969/j.issn.2095-1035.2015.04.009

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. doi: 10.3969/j.issn.2095-1035.2015.04.009

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. doi: 10.15898/j.cnki.11-2131/td.201805070055

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. doi: 10.15898/j.cnki.11-2131/td.201805070055

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. http://www.ykcs.ac.cn/article/id/ykcs_19930103

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. http://www.ykcs.ac.cn/article/id/ykcs_19930103

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. doi: 10.3969/j.issn.0254-5357.2005.01.008

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. doi: 10.3969/j.issn.0254-5357.2005.01.008

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. doi: 10.3969/j.issn.2095-1035.2017.04.012

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. doi: 10.3969/j.issn.2095-1035.2017.04.012

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. doi: 10.3969/j.issn.1001-9677.2018.04.032

Dong W.Catalytic kinetic spectrophotometric determination of iodine in regional geochemical samples[J].Guangzhou Chemical Industry, 2018, 46(4):99-100. doi: 10.3969/j.issn.1001-9677.2018.04.032

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. doi: 10.3969/j.issn.0254-5357.2007.05.011

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. doi: 10.3969/j.issn.0254-5357.2007.05.011

安华娟, 张明杰, 戴雪峰, 等.电感耦合等离子体质谱法测定地质样品中痕量碘[J].理化检验(化学分册), 2010, 46(6):692-693. http://d.old.wanfangdata.com.cn/Periodical/ykcs200103001

An H J, Zhang M J, Dai X F, et al.Inductively coupled plasma mass spectrometry for the determination of trace iodine in geological samples[J].Physical Testing and Chemical Analysis (Part B:Chemical Analysis), 2010, 46(6):692-693. http://d.old.wanfangdata.com.cn/Periodical/ykcs200103001

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. doi: 10.3969/j.issn.0254-5357.2003.03.004

Ma X R, Li B, Han 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. doi: 10.3969/j.issn.0254-5357.2003.03.004

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. doi: 10.15898/j.cnki.11-2131/td.2016.04.008

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. doi: 10.15898/j.cnki.11-2131/td.2016.04.008

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. doi: 10.15898/j.cnki.11-2131/td.201712060189

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. doi: 10.15898/j.cnki.11-2131/td.201712060189

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. doi: 10.3969/j.issn.0254-5357.2014.02.005

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. doi: 10.3969/j.issn.0254-5357.2014.02.005

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. http://www.wanfangdata.com.cn/details/detail.do?_type=perio&id=QKC20172017051900161919

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. http://www.wanfangdata.com.cn/details/detail.do?_type=perio&id=QKC20172017051900161919

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. doi: 10.15898/j.cnki.11-2131/td.201803290033

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. doi: 10.15898/j.cnki.11-2131/td.201803290033

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. http://d.old.wanfangdata.com.cn/Periodical/trfl201903030

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. http://d.old.wanfangdata.com.cn/Periodical/trfl201903030

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. doi: 10.3969/j.issn.1004-4957.2009.03.014

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. doi: 10.3969/j.issn.1004-4957.2009.03.014

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].

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. doi: 10.1021/ac010726t

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. doi: 10.3969/j.issn.0254-5357.2009.05.005

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. doi: 10.3969/j.issn.0254-5357.2009.05.005

Supplements (0)

Cited By