磷酸酯萃取色层放置法分析土壤中锶-90的研究
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摘要
在环境放射性检测项目中,土壤中锶―90含量分析是较为繁琐和分析结果稳定性差的,通常通过测量与~(90)Sr处于平衡的子体~(90)Y的活度来推算~(90)Sr的活度。在~(90)Sr分离过程中,关键是锶与同族元素钙、钡及镭之间的分离,尤其是锶与钙的相互分离。其次就是从~(90)Sr和其他放射性核素中分离出放射性纯的~(90)Y,以便进行β活度的测定。本课题结合了国家标准GB/T6764~GB/T6766 1986和GB/T1222.1 1989水和生物灰中对放射性~(90)Sr化学分析方法,对江西省国家监控点位土壤样中~(90)Sr进行了二―(2―乙基己基)磷酸酯萃取放置法的测定,在前人的研究成果基础上提出了适合测定50g土壤样中~(90)Sr活度浓度测定的分析程序,并用一般较为常用的快速法从锶的化学回收率、钇化学回收率、加标实验、空白试验以及~(90)Y探测效率等方面与之对比验证,取得如下成果:
     1、一般放置法是将土壤中锶―钇进行分离,除去土壤中本身带有的~(90)Y,将~(90)Sr保留下来放置14天以上使新衰变得到的~(90)Y与之达到放射性平衡,再将钇分离出来进行测量,得出~(90)Sr的活度浓度。本课题在利用快速法分离锶钇之后又进行了两次锶钇分离,并从放置法分析得到的钇化学回收率上看出色层柱对钇的损失较小,这使其分离更为彻底,将溶液中~(90)Y的再次生成所受到的干扰降低。
     2、两次加标验证实验中,标准锶钇活度浓度为8.693Bq/ml,本方法分析程序测定出的标准锶钇活度浓度为7.514Bq/ml、7.823Bq/ml,加标活度回收率为86.44%、90.00%;锶回收率为67.95%、61.40%,钇的化学回收率为53.02%、58.25%,相对误差为13.56%、10.01%,平均标准偏差为11.74%,而一般快速法锶钇活度为5.938Bq/ml、4.098Bq/ml,加标活度回收率为68.31%、47.14%,钇的化学回收率34.57%、30.79%,相对误差为31.69%、52.86%,平均标准误差为43.40%,可见放置法的实验效果比一般快速法的更为理想和准确。
     3、分析得出的江西省国家监控点位土壤样中~(90)Sr的活度,在放置法的相较快速法测得的值较大,这是由于快速法测定的是在土壤中原有的~(90)Y,而该~(90)Y含量在分离的化学前处理中有较大损失,而放置法所测定的再次生成~(90)Y至生成到仪器测定的过程较为简单,处理方便,钇含量损失较少。而这两种方法的准确性从图5 1中放置法、快速法钇回收率与锶回收率的测定值吻合度可以看出。
     4、低本底α、β测量仪对~(90)Y探测效率的验证实验中,放置法的探测效率一路、二路分别为0.2707、0.3120,完全满足仪器的要求。
     5、在最后的土壤锶浓度计算中,本课题在前人所编写的放置法计算公式上引入了β标准源效率的修正值参与计算,这是根据不同仪器对β粒子的探测灵敏度而修正的,本次实验中的二路低本底α、β测量仪(BH1216Ⅲ型)中修正后的β标准源效率分别为0.2833、0.3126,这也符合仪器中要到达0.2500的要求。引入该值后使加标试验中的标准活度更接近真实值。
     本次土壤中~(90)Sr的放置法分析程序的研究,从活度、回收率等发面上的测定都取得取得较为满意的结果,验证了该方法的可行性,且达到了较好精度和准确性。
In the environmental radioactivity,the soil content of ~(90)Sr analysis is more complicated with poor stability.Usually in equilibrium by measuring the daughter ~(90)Y’s activity to calculate the activity of the ~(90)Sr,and the key is the separation of the same group elements strontium and calcium,barium and radium ,especially strontium and calcium from each other.The second is how pure ~(90)Y to be isolated from the ~(90)Sr and other radioactive,for the determination ofβactivity.The subject is basded on the national standard GB/T6764~GB/T6766 1986 and GB/T1222.1 1989,and National Surveillance Point of Jiangxi soil samples ~(90)Sr,carried out a二―(2―ethylhexyl) phosphoric acid method of determination of place in the results of previous studies and made on the basis of 50g soil samples for determination of activity concentration in the determination of ~(90)Sr analysis procedures.The Placed Method was proved with the Rapid Method of the chemical recovery of Sr,Y’s chemical recovery, standard addition experiments,blank tests and the detection efficiency and ~(90)Y contrast verification,achieved the following results:
     1、The general Placed Method is to remove ~(90)Y form the soil,the ~(90)Sr is placed more than 14 days to get the new decay of radioactive ~(90)Y for achieving a balancethen. Separated and measure the new Y once again,which is obtained in the activity concentration of ~(90)Sr.The issue separate the two times Sr and Y after use of the Rapid Method.Followed by The Placed Method obtained,the loss of the chemical recovery of ~(90)Y is more smaller Y,which will make the disruption of the re ~(90)Y was reduced.
     2、In the two adding the standard experiments,the activity concentration of Sr―Y was 8.693Bq/ml.The standard Sr―Y activity concentration of the Placed Method were 7.514Bq/ml and 7.823Bq/ml;of spiked recovery were 86.44% and 90.00%;Sr’s recovery were 67.95% and 61.40%;the chemical recovery of Y were 53.02% and 58.25%,relative error were 13.56% and 10.01%,the average standard deviation was 11.74%,while the Sr―Y activity of the general Rapid Method was 5.938Bq/ml, 4.098Bq/ml,spiked recovery wre 68.31% and 47.14%,34.57% ;the chemical recovery of Y was 30.79%,the relative erroris were 31.69% and 52.86%,the average standard deviation was 43.4%,which was showing that the experimental results of the Place Method more desirable than the Rapid Method’s.
     3、Drawn from the analysis of soil samples of national surveillance points in Jiangxi Province,the ~(90)Sr’s activity by the placed method compared to the fast method is the larger measured value,which is due to the Rapid Method get the ~(90)Y have a greater loss in the separation of the chemical pre treatment.In the other hand, Generation ~(90)Y was measured by the process of the placed method is more simple,convenient,and the loss of ~(90)Y contentless.The accuracy of these two methods is showed in Figure5 1,It can be seen that Sr recovery rate fit with by the Placed Method is very different it fit with the Y recovery rate by Rapid Method.
     4、In detection efficiency of ~(90)Y verification experiment of the low backgroundα、βmeasuring instrument,the detection efficiency of the Placed Method were 0.2707、0.3120 and meet the requirements for instruments fully.
     5、In the final Sr concentration calculation of the soil,the Placed Method’s formula was added theβmeasuring standard rate beyond the prepared previous method.The correction value involved in the calculation,which is based on theβparticles of the different of the instruments and the detection sensitivity.This experiment use the two Road of low backgroundα、βmeasuring instrument (BH1216Ⅲtype) and the revised efficiency ofβwere 0.2833、0.3126。It is consistent with the instrument requirements to reach 0.2500.After the introduction of it,test value is closer to the true value in the standard test.
     The study of the process in the soil analysis of ~(90)Sr by the Placed Method obtained the satisfactory results from the determination of the activity and recovery rates and so on.The study also achieved the feasibility and good precision betteraccuracy of the placed method
引文
[1]中华人民共和国放射性污染防治法实施手册.[M]北京:中国知识出版社,2000.
    [2] http://www.examda.com/hps/84/20090725/090438789.html
    [3] http://www.people.com.cn/GB/shehui/212/3572/3574/20021029/853043.html
    [4] http://wenku.baidu.com/view/a6b34137ee06eff9aef80770.html
    [5]黄治俭.放射性污染源的调查和检测.[J]辐射防护通讯,2008.4.
    [6]http://jpkc.dhu.edu.cn/hjjc/COLUMN_5/jxnr/wljx c8 5.html
    [7]沙连茂,王治惠,王风华等.牛奶样品中Sr90、Cs137、Ca和K的测定.[J]环境科学,1990.02期
    [8]沙连茂,郭混,王治惠.水中锶90放射化学分析方法二―(2乙基已基)磷酸萃取色层法.环境与可持续发展,1986.11.
    [9]沙连茂,郭混,王治惠等.锶90、铯137、铈144的分离和测定.辐射防护,1981.02.
    [10]李芳,陆继根等.海水中90Sr分析方法的初步研究.[J]辐射防护,2008.7.
    [11]秦学祥,杜春艳,张振生.海水中锶90和铯137的同时测定.[J]海洋学报,1991.第3期.
    [12]陶月潮.应用均三溴偶氮胂测定地下水中微量锶.[J]安徽技术师范学院学,2003.04.
    [13]引用GB6765 86水中锶90放化分析方法—离子交换法.放射性物质测定方法国家标准.
    [14]引用标准GB14883.1食品中放射性物质检验总则3锶90测定方法—发烟硝酸法
    [15]Anal.Chem.Gregory L P.A Separation of Strontium,Radium and Lead from Environmental Media by Precipitation Followed by Fractional Elution.,1972.44(12):2113.
    [16]Juznic.K.Radiochemical Determination of Sr 90 and Sr 89 insoil.Anal.Chem.1986.
    [17]This test method is under the jurisdiction of ASTM Committee C26 on Nuclear Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods ofTest.2001.8.10
    [18]2 Annual Book of ASTM Standards, Vol 12.01.
    [19]3 Annual Book of ASTM Standards, Vol 11.01.
    [20]谢金成,何宗莉.火焰原子吸收法测定富锶食品中的锶.[J]中国卫生检验杂质,2010.4.
    [21]张凌等.FAAS法测定丰城鸡血藤中锶含量的方法探讨.[J]光谱学与光谱分析,2010.12.
    [22]赵希文,李洁.ICP AES法测定硅铝钙钡合金中的铜锰镁锶量.武钢技术,2009.05.
    [23]李艳苹,潘献辉,刘小骐.ICP AES法测定海水中钾、钠、钙、镁、锂、锶、锰. [J]中国给水排水,2010.2
    [24]成琼,ICP AES法测定环境水样中锶的技术研究.[J]中国核科技报告,2009.01.
    [25]焦志兰,孟莉.ICP AES法测定土壤和地下水中Sr、Nd、C,[J]辐射防护通讯,2005.2,第25卷第1期.
    [26]隋诚运.关于ICP AES中最佳载气流量的研究.[J]分析化学,1985年05期.
    [27]朱泽民,杜治国,葛恒波.X射线荧光光谱法无标样分析工业碳酸锶.理化检验化学分册,2010年第46卷.
    [28]胡舜媛.快速测定环中的放射性锶90.国外核新闻,1995.第4期.
    [29]Kn?chel, Arndt.Cation Binding by Humic Substances By Edward Tipping.Angewandte Chemie International Edition,2003.42卷25期.
    [30]张佩聪,倪师军,张成江等.土壤电化学性能对铀、锶、铯分配系数的影响及机理探讨.[J]化学研究与应用,2008.第10期.
    [31]李瑞东,张志利,侯立安等.无机离子交换材料吸附锶、铯研究进展.[J]北方环境,2010.05.
    [32]齐文启,陈光,席俊清.放射性核素污染及监测.环境监测管理与技术,2008.3
    [33]张晔,郁丹炯,孙亚敏.1995—2006年我国部分地区动物样品中放射性核素水平监测.辐射防护通讯,2010.8.
    [34]韩素清,迟翔.土壤污染的类型及影响和危害.安全与环境,2007.
    [35]曹钟港,陈赵飞,吴虞华等.我国部分地区植物样品中放射性核素水平监测.辐射防护通讯,2010.30.(3):17.
    [36]放射化学技术培训会议资料.浙江省辐射环境监测站.杭州:2010.9.
    [37]党磊.低水平90Sr的分析方法研究进展.核化学与放射化学,2010.3
    [38]辐射环境监测中心.环境监测基础与基础应用研究.中国原子能科学研究院年报,北京:2003
    [39]王迎军,杨学慧.浅谈环境监测的重要性.吉林农业,2010.
    [40]祝霖.放射化学.[M]北京:原子能出版社,1985.
    [41]GB14883.1锶-90测定方法―发烟硝酸法.食品中放射性物质检验总则.
    [42]Butler F E.Sr 90 Monitoring at the Savannah River Plant.Health Phys.1962.8:273.
    [43]Carmon B.An Ion Exchange Separation Procedure for Radiostrontium from Calcium rich Soil Samples.Int.J.Appl.Radiat.Isotopes,1977.28:435.
    [44]贾国纲.土壤中Sr 90的测定.原子能科学技术,1989.23(4):34.
    [45]Baratta E J.Separation of Calcium strontium Investigated by the Use of Tracers. Anal. Chem., 1971.43(8):1138.
    [46]JiaGuogang,A Rapid And Aeeurate Method for the Determination of Strontiu 90 in Environmetal soil.J Radioanal Nuel Chem,1994,185(2):255 264.
    [47]Martin D B. Determination of Sr 89 and Sr 90 in Soil with Total Sample Decomposition. Anal.Chem.,1979.51:1968
    [48]沙连茂,郑鸿,韩玉虎.土壤中90Sr的测定.[J]辐射防护通讯,1993年第3期
    [49]北京核仪器厂.低本底α、β测量仪培训说明(内部资料),2006.
    [50]阳俊.放射性核素衰变规律的几个概念及其应用.[J]重庆教育学院学报,2002.11.
    [51]王丽君,王文焱,李致清.ICP AES光谱仪的技术特点.现代仪器,2005.
    [52]朱树中,隆绍贤,肖振红.食品和环境中Sr 90的快速分析.见:中国核化学与放射化学学会第一次全国放射化学学术讨论会论文摘要集,桂林:1992.13.
    [53]程念祖,陈雅珍.分析化学中回收率计算方法的讨论.[J]冶金分析,1985.6
    [54]放射性物质测定方法国家标准.GB 11222.1 89生物样品灰中锶90的放射化学分析方法二磷酸酯萃取色层法.2006.10
    [55]贾国纲.土壤中90Sr含量测定的改进方法.[J].辐射防护,1996.5

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