食品中天然铀、钍的三正辛胺萃取—分光光度法联合测定研究
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摘要
目的建立食品中天然铀、钍联合测定的方法。方法基于N235萃取-分光光度法和三正辛胺(TOA)与N235的化学类似性,通过以TOA代替N235完成了必要的条件实验研究并获得了主要分析步骤的最佳条件。集合所获各项最佳条件,建立了本法的实验程序的方法学依据并对所建方法进行了验证。结果方法最低探测限为3.47×10-8gTh／g灰和9.47×10-8g U／g灰。Th、U的加标回收率分别为98.7%、96.7%,相对标准偏差分别为±5.95%、±6.31%。对主要种类食品样品(牛奶、红薯、面粉、绿豆、海产、茶叶、菠菜)的铀、钍含量进行了测定,其化学回收率均在70%-90%。结论首次建立了食品中三正辛胺萃取-分光光度法作为天然铀、钍联合测定的方法。本法简便快速、准确度和精密度好。
Objective This study aimed to establish a method which can determine the natural uranium and thorium in food simultaneously. Methods Based on the N-235 extraction-spectrophotometry and the chemical similarity of TOA and N235, necessary condition experiments were finished by substituting TOA for N235, the best conditions for the main analytical steps were obtained. By adopting these best conditions, methodological bases of the new analytical procedures were established. The new analytical method has been tested and verified. Results The lowest detectable limits of the method were 3.47x 10-8g Th/g ash and 9.47×10-8g U/g ash. The recovery of standard addition of Th and U are 98.7%and 96.7%respectively. The relative standard deviation of Th and U are±5.95%and±6.31%respectively. The uranium and thorium contents in main types of food ash samples were determined, the chemical recoveries were all between 70%and 90%. Conclusions The Tri-n-octylamine extraction spectrophotometric method of simultaneous determination for natural uranium, thorium in food was established for the first time. This method is simple, quick and has good accuracy and precision.
Objective This study aimed to establish a method which can determine the natural uranium and thorium in food simultaneously. Methods Based on the N-235 extraction-spectrophotometry and the chemical similarity of TOA and N235, necessary condition experiments were finished by substituting TOA for N235, the best conditions for the main analytical steps were obtained. By adopting these best conditions, methodological bases of the new analytical procedures were established. The new analytical method has been tested and verified. Results The lowest detectable limits of the method were 3.47x 10-8g Th/g ash and 9.47×10-8g U/g ash. The recovery of standard addition of Th and U are 98.7%and 96.7%respectively. The relative standard deviation of Th and U are±5.95%and±6.31%respectively. The uranium and thorium contents in main types of food ash samples were determined, the chemical recoveries were all between 70%and 90%. Conclusions The Tri-n-octylamine extraction spectrophotometric method of simultaneous determination for natural uranium, thorium in food was established for the first time. This method is simple, quick and has good accuracy and precision.
引文
[1]GB／T14883.7-1994.食品中放射性物质检验[S]．北京：中国标准出版社,1994.
[2]GB 18871-2002.电离辐射防护与辐射源安全基本标准[S]．北京：中国标准出版社,2002.
[3]杨天林,杨永会,孙思修.TOA萃取硫酸铀酰的动力学研究[J].核化学与放射化学,1999,21(4)：207-212.
[4]杨天林,杨永会,孙思修.三正辛胺和三正辛基氧膦协同萃取硫酸铀酰的动力学研究[J].核化学与放射化学2001,23(4)：241-245.
[5]周治发.铀、钍和226Ra的分析.海产食品放射性调查[M]．北京：原子能出版社,1981：231-253.
[6]GB/T16126-1995.生物监测质量保证规范[S].北京：中国标准出版社,1995.
[7]诸洪达等.中国人镧系元素膳食摄入量和主要器官或组织负荷量研究[J].中华放射医学与防护杂志,2004,24(1)：1-5.
[8].刘英,白石久二雄.ICP-MS在核事故应急监测中的应用[J]_中华放射医学与防护杂志,2001,21(4)：238-239.
[9]覃家光,冯兰英,杨刚.N235萃取-分光光度法测定建材中的钍[J].中国辐射卫生,2006,15(4)：504-505.
[10]罗道成,郑李辉.萃取分光光度法测定痕量六价铬的研究[J].无机盐工业,2009,41(6)：60-62.
[11]陈文君,吴政宙,卢志琴.液液萃取-分光光度法测定三溴苯酚中铁[J].理化检验-化学分册,2006,(42)：859.
[1]高艳辉,诸洪达,樊体强,刘庆芬等.食品中天然铀、钍的三正辛胺萃取-分光光度法联合测定研究[J].中华放射医学与防护杂志,2010,30(2),218-221.
[2]J. Sabine Becker, Hans-Joachim Dietze.precise isotope ratio measurements for uranium, thorium and plutonium by quadrupole-based inductively coupled plasma mass spectrometry[J]. Fresenius'Journal of Analytical Chemistry,1999,364(5):1999.
[3]杨海友,邹晓颖,刘丽萍等.ICP-MS技术测定贫铀在土壤中的含量及分布[J]．辐射防护,2008,28(5)：292-295.
[4]程天民,李蓉,粟永萍.贫铀弹伤害及其医学防护[j]．解放军医学杂志,2005,30(7)：549-551.
[5]于水,赵法.贫铀武器对人员和环境的影响评价[M]．北京：中国环境科学出版社,2002.
[1]葛鹏.贫铀材料的工业应用[J].稀有金属快报,2004,23(2)：36-37.
[2]Rita Hindin, Doug Brugge and Bindu Panikkar.Teratogenicity of depleted uranium aerosols:A review from an epidemiological perspective[J].Environmental Health:A Global Access Science Source,2005,4:17.
[3]刘琼,王海军(综述),范正平(审校).贫铀弹的危害及其防护[J].海军医学杂志,2004,25(2)：170-173.
[4]樊飞跃.贫铀武器应用及其危害[J].中华放射医学与防护杂志,2000,20(1)：27-28.
[5]潘本兴,叶锦韶.核弹和贫铀弹的环境污染[J].暨南大学学报(自然科学版),2003,24(1)：31-35.
[6]P Gustavsson,M Talba"ck,A Lundin,B Lagercrantz,P-E Gyllestad,L Fornell.Incidence of cancer among Swedish military and civil personnel involved in UN mission in the Balkans1989-99[J]. SHORT REPORT Occup Environ Med,2004,61:171-173.
[7]朱茂祥,周平坤.贫铀的健康影响研究进展[J].辐射防通,2009,29(5)：25-29.
[8]于水,叶常青.贫铀武器对科索沃环境的影响评价[J].中华放射医学与防护杂志2002,22(3)：227-230.
[9]郭志英,于水,郑永红等.贫铀气溶胶在土壤中迁移深度的研究[J].中华放射医学与防护杂志,2007,27(4)：314-317.
[10]李蓉,艾国平,徐辉等。吸入贫铀粉尘和／或嵌入贫铀片大鼠体内铀的分布[J].第四军医大学学报,2004,25(6)：503-506.
[11]Dang H S,Pullat V R,Sharma R C.Distribution of uranium in human organs of an urban Indium population and its relationship with clearance half-lives[J]. Health Phys,1995,68(3):328-331.
[12]冷言冰,李蓉,艾国平等。长期接触贫铀对大鼠遗传毒性的初步研究[J].第三军医大学学报,2006,28(9)：869-871.
[13]Stradling G N. Decorporation of actinides:a review of recent research [J]. J Alloys Compd,1998,271-273:72-77.
[14]潘秀颉,杨陟华,曹珍山等。DMSO对大鼠吸入贫铀气溶胶后体内铀的促排作用[J]．毒理学杂志,2005年,19(3增刊)：248-249.
[15]刘实晶,罗梅初,陈桂宝等。小剂量8102对大鼠急性铀中毒血象与肝肾功能的影响。第三军医大学学报,2004,25(6)：1643-1646.
[16]李蓉,任炯,杨峥嵘等.含邻苯二酚基团的黄酮化合物促排急性贫铀中毒效果的研究[J].第三军医大学学报,2008,30(24)：2251-2253.
[17]John W. Ejnik,Todor I. Todorov,Florabel G. Mullick,et al.Uranium analysis in urine by inductively coupled plasma dynamic reaction cell mass spectrometry[J]. Analytical and Bioanalytical Chemistry,2005,382(1):73-79.
[18]吉艳琴,李金英,罗上庚.TOPO萃取色层分离-ICP-MS法测定土壤中痕量铀的同位素丰度比[J].核化学与放射化学,2004,26(2)：88-93.
[19]诸洪达等.中国人镧系元素膳食摄入量和主要器官或组织负荷量研究[J].中华放射医学与防护杂志,2004,24(1)：1-5.
[20].刘英,白石久二雄.ICP-MS在核事故应急监测中的应用[J].中华放射医学与防护杂志,2001,21(4)：238-239.
[21]K.Shiraishi, Y.lgarashi.Concentrations of thorium and uranium in freshwater samples collected in the former USSR[J]. Journal of Radioanalytical and Nuclear Chemistry, Articles,1994,185(1):157-165.
[22].Chang-Kyu, Riki Siki.Application of a high Resolution Inductively Coupled Plasma Mass Spectrometer to the Measurement of Long-lived Radionuclides[J]. Journal of Analytical Atomic Spectrometry,1991, Vol.6,205-209.
[23].K.Shiraishi,Y.lgarashi. Daily Intakes of 232Th and 238U in Japanese Males[J]. Health Phys,1992,63(2):187-191.
[24].L.Holmes. Determination of Thorium by ICP-MS and ICP-OES[J]. Radiation Protection Dosimetry,2001,97(2):117-122.
[25]. K.Shiraishi and James F.Mclnroy. Simultaneous Multielement Analysis of Human Tissues by Inductively Coupled Plasma Mass Spectrometer[J]. The Journal of Trace Elements in Experimental Medicine,1991,4:191-202.
[26]梁志荣,陈琦,刘学军.α能谱法测定土壤样品中的235U、238U[J].核化学与放射化学,2007,29(1)：57-59.
[27]侯庆梅 李文元 吕慧敏 魏宗源.环境样品和生物样品中钍同位素联合分析方法的研究[J].中华放射医学与防护杂志,1990,10(4)：243-247.
[28]Bleise P R, Burkart D W. Properties, Use and Health Effects of Depleted Uranium (DU):a General Overview[J]. Journal of Environmental,2003,64:93.
[29]Mo D. Report of a visit to develop an enhanced environmental monitoring programme in the Britis Med Sector in Kosovo[M] UK:Minis of Defence,2001.
[2]GB 18871-2002.电离辐射防护与辐射源安全基本标准[S]．北京：中国标准出版社,2002.
[3]杨天林,杨永会,孙思修.TOA萃取硫酸铀酰的动力学研究[J].核化学与放射化学,1999,21(4)：207-212.
[4]杨天林,杨永会,孙思修.三正辛胺和三正辛基氧膦协同萃取硫酸铀酰的动力学研究[J].核化学与放射化学2001,23(4)：241-245.
[5]周治发.铀、钍和226Ra的分析.海产食品放射性调查[M]．北京：原子能出版社,1981：231-253.
[6]GB/T16126-1995.生物监测质量保证规范[S].北京：中国标准出版社,1995.
[7]诸洪达等.中国人镧系元素膳食摄入量和主要器官或组织负荷量研究[J].中华放射医学与防护杂志,2004,24(1)：1-5.
[8].刘英,白石久二雄.ICP-MS在核事故应急监测中的应用[J]_中华放射医学与防护杂志,2001,21(4)：238-239.
[9]覃家光,冯兰英,杨刚.N235萃取-分光光度法测定建材中的钍[J].中国辐射卫生,2006,15(4)：504-505.
[10]罗道成,郑李辉.萃取分光光度法测定痕量六价铬的研究[J].无机盐工业,2009,41(6)：60-62.
[11]陈文君,吴政宙,卢志琴.液液萃取-分光光度法测定三溴苯酚中铁[J].理化检验-化学分册,2006,(42)：859.
[1]高艳辉,诸洪达,樊体强,刘庆芬等.食品中天然铀、钍的三正辛胺萃取-分光光度法联合测定研究[J].中华放射医学与防护杂志,2010,30(2),218-221.
[2]J. Sabine Becker, Hans-Joachim Dietze.precise isotope ratio measurements for uranium, thorium and plutonium by quadrupole-based inductively coupled plasma mass spectrometry[J]. Fresenius'Journal of Analytical Chemistry,1999,364(5):1999.
[3]杨海友,邹晓颖,刘丽萍等.ICP-MS技术测定贫铀在土壤中的含量及分布[J]．辐射防护,2008,28(5)：292-295.
[4]程天民,李蓉,粟永萍.贫铀弹伤害及其医学防护[j]．解放军医学杂志,2005,30(7)：549-551.
[5]于水,赵法.贫铀武器对人员和环境的影响评价[M]．北京：中国环境科学出版社,2002.
[1]葛鹏.贫铀材料的工业应用[J].稀有金属快报,2004,23(2)：36-37.
[2]Rita Hindin, Doug Brugge and Bindu Panikkar.Teratogenicity of depleted uranium aerosols:A review from an epidemiological perspective[J].Environmental Health:A Global Access Science Source,2005,4:17.
[3]刘琼,王海军(综述),范正平(审校).贫铀弹的危害及其防护[J].海军医学杂志,2004,25(2)：170-173.
[4]樊飞跃.贫铀武器应用及其危害[J].中华放射医学与防护杂志,2000,20(1)：27-28.
[5]潘本兴,叶锦韶.核弹和贫铀弹的环境污染[J].暨南大学学报(自然科学版),2003,24(1)：31-35.
[6]P Gustavsson,M Talba"ck,A Lundin,B Lagercrantz,P-E Gyllestad,L Fornell.Incidence of cancer among Swedish military and civil personnel involved in UN mission in the Balkans1989-99[J]. SHORT REPORT Occup Environ Med,2004,61:171-173.
[7]朱茂祥,周平坤.贫铀的健康影响研究进展[J].辐射防通,2009,29(5)：25-29.
[8]于水,叶常青.贫铀武器对科索沃环境的影响评价[J].中华放射医学与防护杂志2002,22(3)：227-230.
[9]郭志英,于水,郑永红等.贫铀气溶胶在土壤中迁移深度的研究[J].中华放射医学与防护杂志,2007,27(4)：314-317.
[10]李蓉,艾国平,徐辉等。吸入贫铀粉尘和／或嵌入贫铀片大鼠体内铀的分布[J].第四军医大学学报,2004,25(6)：503-506.
[11]Dang H S,Pullat V R,Sharma R C.Distribution of uranium in human organs of an urban Indium population and its relationship with clearance half-lives[J]. Health Phys,1995,68(3):328-331.
[12]冷言冰,李蓉,艾国平等。长期接触贫铀对大鼠遗传毒性的初步研究[J].第三军医大学学报,2006,28(9)：869-871.
[13]Stradling G N. Decorporation of actinides:a review of recent research [J]. J Alloys Compd,1998,271-273:72-77.
[14]潘秀颉,杨陟华,曹珍山等。DMSO对大鼠吸入贫铀气溶胶后体内铀的促排作用[J]．毒理学杂志,2005年,19(3增刊)：248-249.
[15]刘实晶,罗梅初,陈桂宝等。小剂量8102对大鼠急性铀中毒血象与肝肾功能的影响。第三军医大学学报,2004,25(6)：1643-1646.
[16]李蓉,任炯,杨峥嵘等.含邻苯二酚基团的黄酮化合物促排急性贫铀中毒效果的研究[J].第三军医大学学报,2008,30(24)：2251-2253.
[17]John W. Ejnik,Todor I. Todorov,Florabel G. Mullick,et al.Uranium analysis in urine by inductively coupled plasma dynamic reaction cell mass spectrometry[J]. Analytical and Bioanalytical Chemistry,2005,382(1):73-79.
[18]吉艳琴,李金英,罗上庚.TOPO萃取色层分离-ICP-MS法测定土壤中痕量铀的同位素丰度比[J].核化学与放射化学,2004,26(2)：88-93.
[19]诸洪达等.中国人镧系元素膳食摄入量和主要器官或组织负荷量研究[J].中华放射医学与防护杂志,2004,24(1)：1-5.
[20].刘英,白石久二雄.ICP-MS在核事故应急监测中的应用[J].中华放射医学与防护杂志,2001,21(4)：238-239.
[21]K.Shiraishi, Y.lgarashi.Concentrations of thorium and uranium in freshwater samples collected in the former USSR[J]. Journal of Radioanalytical and Nuclear Chemistry, Articles,1994,185(1):157-165.
[22].Chang-Kyu, Riki Siki.Application of a high Resolution Inductively Coupled Plasma Mass Spectrometer to the Measurement of Long-lived Radionuclides[J]. Journal of Analytical Atomic Spectrometry,1991, Vol.6,205-209.
[23].K.Shiraishi,Y.lgarashi. Daily Intakes of 232Th and 238U in Japanese Males[J]. Health Phys,1992,63(2):187-191.
[24].L.Holmes. Determination of Thorium by ICP-MS and ICP-OES[J]. Radiation Protection Dosimetry,2001,97(2):117-122.
[25]. K.Shiraishi and James F.Mclnroy. Simultaneous Multielement Analysis of Human Tissues by Inductively Coupled Plasma Mass Spectrometer[J]. The Journal of Trace Elements in Experimental Medicine,1991,4:191-202.
[26]梁志荣,陈琦,刘学军.α能谱法测定土壤样品中的235U、238U[J].核化学与放射化学,2007,29(1)：57-59.
[27]侯庆梅 李文元 吕慧敏 魏宗源.环境样品和生物样品中钍同位素联合分析方法的研究[J].中华放射医学与防护杂志,1990,10(4)：243-247.
[28]Bleise P R, Burkart D W. Properties, Use and Health Effects of Depleted Uranium (DU):a General Overview[J]. Journal of Environmental,2003,64:93.
[29]Mo D. Report of a visit to develop an enhanced environmental monitoring programme in the Britis Med Sector in Kosovo[M] UK:Minis of Defence,2001.