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用放射化学中子活化分析法测定人血清中的锡。

Determination of tin in human blood serum by radiochemical neutron activation analysis.

作者信息

Versieck J, Vanballenberghe L

机构信息

Department of Internal Medicine, University Hospital, Ghent, Belgium.

出版信息

Anal Chem. 1991 Jun 1;63(11):1143-6. doi: 10.1021/ac00011a016.

Abstract

A method was developed for the determination of tin in human serum by radiochemical neutron activation analysis, using the long-lived radioisotope Sn(T1/2 = 115.09 days). This radioisotope decays to a daughter isotope 113mIn, the most suitable nuclide for counting (T1/2 = 1.658 h, gamma-ray of 391.7 keV). Experience showed that, with the exception of the serum samples with the lowest tin levels, in the experimental conditions of the present study tin could mostly also be determined by using its radioisotope 117mSn(T1/2 = 13.61 days, gamma-ray of 158.5 keV). Samples were collected and prepared by using the procedure elaborated by the authors, which proved its effectiveness in preventing significant sample contamination on several occasions. Because samples had to be irradiated at 10(14) n.cm-2.s-1, dry ashing was necessary. After irradiation, tin was separated by solvent extraction of tin(IV) iodide from a sulfuric acid-ammonium iodide solution with toluene. The dry ashing and solvent extraction steps were exhaustively tested by means of radioactive tracer experiments whereas the accuracy and precision of the analytical method were thoroughly checked by analyzing biological reference materials (Bowen's kale powder, the NBS' bovine liver, the NBS' nonfat milk powder, and the "second-generation" biological reference material--freeze-dried human serum--for trace element determinations, developed by the authors).(ABSTRACT TRUNCATED AT 250 WORDS)

摘要

开发了一种用放射化学中子活化分析法测定人血清中锡的方法,使用长寿命放射性同位素Sn(半衰期=115.09天)。这种放射性同位素衰变成子同位素113mIn,它是最适合计数的核素(半衰期=1.658小时,γ射线能量为391.7keV)。经验表明,在本研究的实验条件下,除了锡含量最低的血清样品外,大部分情况下也可以使用其放射性同位素117mSn(半衰期=13.61天,γ射线能量为158.5keV)来测定锡。样品采用作者精心制定的程序进行收集和制备,该程序已多次证明其在防止样品受到显著污染方面的有效性。由于样品必须在10(14) n.cm-2.s-1的条件下进行辐照,因此需要进行干灰化。辐照后,通过用甲苯从硫酸-碘化铵溶液中溶剂萃取碘化锡(IV)来分离锡。通过放射性示踪实验对干灰化和溶剂萃取步骤进行了全面测试,而通过分析生物参考物质(鲍恩羽衣甘蓝粉、美国国家标准局的牛肝、美国国家标准局的脱脂奶粉以及作者开发的用于微量元素测定的“第二代”生物参考物质——冻干人血清)对分析方法的准确性和精密度进行了全面检查。(摘要截于250字)

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