分析化学2024，Vol.52Issue(5)：706-716,11.DOI:10.19756/j.issn.0253-3820.231483
生物样品中超低水平239Pu和240Pu的分析
Determination of Ultra-Low Levels of 239Pu and 240Pu in Biological Samples
摘要
Abstract
In this work,a reliable analytical method for ultra-low 239,240Pu in biological samples was developed.Sodium carbonate and magnesium acetate were used as saponification agent and ashing aid,respectively,and then Fe(OH)2-Fe(OH)3 was used for co-precipitation separation and enrichment of plutonium extracted from the ashing samples.Then aluminum nitrate was used as a masking agent to eliminate the interference of a large amount of phosphorus in the loading solution on plutonium during the anion exchange separation process.The results showed that the average recovery of plutonium was more than 73%and the decontamination factor for 238U was 3.3×104-5.4×105 in biological samples.The ultimate sample introduction technology(APEX-Ω)was used in determination of plutonium isotopes by inductively coupled plasma mass spectrometry(ICP-MS/MS)with NH3-He as the collision/reaction gas.The 242Pu standard added before sample separation was used as the yield tracer and isotope diluent to calculate the concentration of 239Pu and 240Pu in samples.This method not only effectively suppressed the 238U peak tail and 238U1H+interference,but also greatly improved the analytical sensitivity of plutonium from 850 cps/(pg/g)(ICP-MS/MS)to 8000 cps/(pg/g)(APEX-ICP-MS/MS).The detection limits of 239Pu and 240Pu in 3.5 kg fresh fish samples were as low as 2.56×10-4 mBq/(kg·wet)and 7.33×10-4 mBq/(kg·wet),respectively.The detection limits of 239Pu and 240Pu in 300 g fresh seaweed samples(30 g dry weight)were 2.98×10-3 mBq/(kg·wet)and 8.55×10-3 mBq/(kg·wet).The concentrations of 239Pu and 240Pu in marine biological samples from the China Sea have been successfully analyzed by using the established analytical method.关键词
钚同位素/生物样品/快速灰化/萃取色谱法/电感耦合等离子体质谱Key words
Plutonium isotope/Biological samples/Rapid ashing/Extraction chromatography/Inductively coupled plasma-mass spectrometry引用本文复制引用
王永昌,张梦婷,侯小琳..生物样品中超低水平239Pu和240Pu的分析[J].分析化学,2024,52(5):706-716,11.基金项目
中国科学院重点部署项目(No.ZDBS-SSW-DQC003)、中国科学院战略性先导科技专项(B类)项目(No.XDB40020104)、中国科学院国际合作项目(No.132B61KYSB20180003)和国家自然科学基金项目(Nos.11875261,42207313)资助. Supported by the Key Deployment Program of Chinese Academy of Sciences(No.ZDBS-SSW-DQC003),the Strategy Priority Research Program(Category B)of Chinese Academy of Sciences(No.XDB40020104),the International Cooperation Project of Chinese Academy of Sciences(No.BZB61KYSB20180003),and the National Natural Science Foundation of China(Nos.11875261,42207313). （No.ZDBS-SSW-DQC003）
