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生物样品中超低水平239Pu和240Pu的分析

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  • 国家科技期刊平台
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建立了一种生物样品中超低水平239Pu和240Pu的分析方法.以碳酸钠为皂化剂、乙酸镁为助灰化剂,对大质量的生物样品进行灰化,再使用Fe(OH)2-Fe(OH)3,通过共沉淀分离富集方法从灰化的样品中酸浸取得到钚,然后以硝酸铝为掩蔽剂消除样品中大量磷对钚在阴离子交换分离过程中的干扰,采用TEVA萃取色谱进一步除去铀等干扰组分,整个流程钚的平均回收率大于 73%,对 238U的去污因子为 3.3×104～5.4×105.利用APEX-Ω高效进样系统,使用高灵敏度的电感耦合等离子体质谱(ICP-MS/MS),以NH3-He为碰撞/反应气体测定钚同位素,使用样品分离前加入的242Pu标准为产率示踪剂和同位素稀释剂,计算样品中239Pu和240Pu的浓度.本方法有效地抑制了238U峰拖尾以及238U1H+的干扰,并将钚的分析灵敏度从850 cps/(pg/g)(ICP-MS/MS)大幅度提升至8000 cps/(pg/g).本方法对鱼虾样品(采样量3.5 kg鲜重)中239Pu和240Pu的检出限分别为2.56×10-4 mBq/(kg·wet)和7.33×10-4 mBq/(kg·wet);对海藻样品(采样量为300 g鲜重(30 g干重))中239Pu和240Pu的检出限分别为2.98×10-3 mBq/(kg·wet)和8.55×10-3 mBq/(kg·wet).采用本方法分析了我国海域海洋生物样品中的239Pu和240Pu浓度.
Determination of Ultra-Low Levels of 239Pu and 240Pu in Biological Samples
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.

Plutonium isotopeBiological samplesRapid ashingExtraction chromatographyInductively coupled plasma-mass spectrometry

王永昌、张梦婷、侯小琳

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中国科学院地球环境研究所,黄土与第四纪地质国家重点实验室,西安加速器质谱中心,西安 710061

中国科学院大学,北京 100049

西安地球环境创新研究院,西安 710061

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

中国科学院重点部署项目中国科学院战略性先导科技专项(B类)中国科学院国际合作项目国家自然科学基金国家自然科学基金

ZDBS-SSW-DQC003XDB40020104132B61KYSB201800031187526142207313

2024

10.19756/j.issn.0253-3820.231483

分析化学
中国化学会 中国科学院长春应用化学研究所

分析化学

CSTPCD北大核心
影响因子：1.423
ISSN：0253-3820
年,卷(期)：2024.52(5)
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