脉冲阳极溶出伏安法测定钚中痕量银

本工作以Nafion树脂修饰玻碳电极为工作电极、铂片电极为对电极、饱和甘汞电极(SCE)为参比电极,进行电极修饰技术研究,建立了脉冲阳极溶出伏安法测定钚中痕量银的分析方法。实验结果表明,银的阳极溶出峰的峰电流与银离子浓度在10~100μg/L范围内呈线性关系,银离子的定量检测下限为5ng/mL,回收率为90%~109%,该方法取样量小、抗干扰能力强、重现性好。     

铀产品中镎和钚的分离与测定方法

为了提高分离效果,避免测量过程中铀基体的干扰,满足核燃料后处理质量控制分析的要求,建立了氩气加压排空阴离子交换系统用于铀产品中Np和Pu的同时分离与测定的方法.模拟样品分离与测定结果表明:采用该系统可快速有效实现铀产品中Np和Pu的分离,Np和Pu对铀的去污系数平均值分别为8.6×104,9.6×104,避免了测量过程中铀基体的干扰,Np和Pu的平均回收率分别为78%(n=6)和86%(n=6).     

Radiochemical Determination of Plutonium Isotopes and Americium-241 in a Plutonium Sample

Isotopic ratios of ²³⁸Pu, ²³⁹Pu, ²⁴⁰Pu and ²⁴¹Am in a plutonium sample were approximately determined by means of combined α- and γ-ray spectrometry without chemical separation of americium from plutonium. The intensity of α-ray followed by internal conversion was determined by measuring the intensity of LX-rays. The ratio of ²⁴⁰Pu to ²³⁹Pu was obtained from the ratio between the α-ray intensity thus determined and the total α-ray intensity from the two nuclides.     

Determination of Plutonium Isotopic Abundance

正The isotope ratio of plutonium product is an important technical index in spent fuel reprocessing process.Thermal ionization mass spectrometry is widely used in isotope ratio measurement of product in reprocessing plant because of its high sensitivity,high precision and high accuracy.     

Study on Extraction of Pu（Ⅳ） by Tri-iso-Amyl Phosphate

The extraction performance of Pu（Ⅳ） with tri-iso-amyl phosphate （TiAP） were studied. The effects of the concentration of nitric acid and the ratio of phase on the extraction efficiency of Pu（Ⅳ）, and on the formation of second organic phase were investigated. The experimental results indicate that the distribution ratios of Pu（Ⅳ） increase obviously with increasing aqueous nitric acid concentration,     

Plutonium Isotopic Determination by Gamma-ray Spectroscopy

Themethodofplutoniumisotopicdeterminationisestablishedusing94～104keVgammarayofHPGespectroscopy.100mg,16gand3.4gPusamples,whichhavedifferentisotopicabundance,aremeasuredwiththemethod.TheresultsofmeasurementareconsistentwiththeanalysisresultusingPC/FRAMsof…     

1AP中铀钚在线分析

为及时监测后处理台架实验1AP中铀和钚浓度,设计加工了1套用于铀钚浓度在线测量的X射线荧光装置,该装置几何光路入射光线与出射光线夹角为60°。为保护光管和探测器不受环境腐蚀,对装置进行了密封。采用已定值的铀和钚配制不同浓度的系列溶液作标准溶液,绘制工作曲线,在此基础上,建立了测量铀钚浓度的分析方法。经测试,本装置测量铀浓度的相对标准偏差为0.42%;连续测量3 h,相对极差为1.6%,说明该装置稳定性良好。应用该装置对台架实验1AP中铀浓度进行在线测量,能及时检测铀浓度的波动,测量值与滴定法得到的值较一致。     

痕量镎和钚的ICP-MS分析方法

经TOA萃取色层柱分离环境样品,2次上柱,将Np和Pu同时洗脱,239Pu的化学回收率为 (92.7±3.1)%,237Np为(96.8±2.7)%,实现了ICP-MS同时测定痕量Np和Pu的含量.应用稀释剂242Pu,通过同位素稀释ICP-MS法测量痕量239Pu和240Pu的含量,用IAEA标样对方法进行验证,Pu 的测定值与标样的推荐值吻合较好(标样中无Np的标准值),证明了ICP-MS同时测定痕量Np和Pu的可行性.     

Gamma-Ray Spectrometric Determination of Isotopic Ratios of Plutonium

Abstract

Plutonium samples (3–30 μg) of various isotopic compositions were measured with a high-resolution Ge(Li) detector. The γ-rays counted are the 43.5 keV of ²³⁸Pu, the 38.7, 51.6 and 129.3 keV of ²³⁹Pu, the 45.2 keV of ²⁴⁰Pu, and the 148.6 keV of ²⁴¹Pu. To estimate the relative photopeak efficiencies of the γ-rays, an empirical curve was derived from measurements of the three γ-rays of ²³⁹Pu adopted as internal standard. Data treatment is described in detail as well as the method of correction to account for the activities of ²³⁷U and ²⁴¹Am inherently accumulating in the plutonium sample. The branching ratios of the γ-rays of plutonium were also evaluated by comparing the γ-ray spectrometric results with mass-spectrometric data.     

Determination of Uranium,Neptunium and Plutonium in 1AW

正The solution in 1AW is the waste of the first separation unit in Purex process.The composition of the aqueous waste of the co-decontaminating unit is very complex.It contains almost all the radioactive fragment elements,and the spe-     

γ能谱法测定铀、钚同位素丰度

简单介绍了特殊核材料铀、钚同位素丰度测定在核材料管理和衡算中的作用;着重描述了γ能谱法测定铀、钚同位素丰度的原理和实验方法。实验结果表明,使用高分辨率的高纯锗探测器,γ能谱法测定轴、钚同位素丰度的不确定度在2%以内。     

痕量镎钚的同步分离测量

研究了痕量Np和Pu的同步分离测量方法.利用相同价态Np和Pu的化学行为和物理性质的相似性,以242Pu为指示剂,用TOA萃取色层-Dowex阴离子交换双柱联合同步分离纯化,ICP-MS同时定量237 Np和239Pu,实现237Np和239Pu的同步分离测量.实验结果表明,相同价态的Np和Pu在色层柱中的化学行为相似...     

A Method for Determination of Plutonium in Blood by Anion Exchange

The anion exchange behavior of Pu(IV) and Pu(VI) were studied in solutions of both nitric acid and of ethanol-nitric acid mixture, and a method of determining plutonium content in blood was developed. About 10 ml of blood were wet-incinerated with concentrated nitric acid and evaporated to dryness. The residue was dissolved in 8 ml of 8 N nitric acid, and 12 ml of ethanol was added. The solution was passed through a resin column of Dowex 2, X8 (9 mm diam., 3.0cm long). After washing the column with ethanol-nitric acid mixed solution, plutonium was eluted with 10 ml of 1N nitric acid containing sulfur dioxide. The eluate was transferred to a cell for electrodeposition, which was carried out with 500 mA/cm² for 3 hr using a stainless steel disk as cathode.

The plutonium yield from the ion exchange was 85~91%, and the electrodeposition quantitative. The blank activity from the reagents, resin and disk was 10^?14Ci. With this method a 10-hr count with silicone semiconductor spectrometer, will permit determination of 5 × 10^?14 10^?13Ci of plutonium in 10 ml of blood.     

质谱、α谱联合测定钚年龄

介绍了用质谱和α谱相结合测定钚材料年龄的方法.该方法利用质谱计测得试样中239Pu相对于241Pu比、用α能谱仪测得试样中239Pu相对于241Am比,利用241Pu和241Am核素级联衰变关系及其参数进行数学运算,求得钚材料的年龄.     

1BP钚在线测量装置的研制及应用

为满足热实验在线监测的需要,根据热室工艺设备台架及热室的具体情况,设计加工安装了一套1BP钚在线测量装置,该在线测量装置主要由探测系统、光路系统、样品流通池系统和控制及数据处理系统组成。采用C语言开发了控制及数据处理程序,应用无线模块使仪器和计算机之间实现无线信号传输及远程控制和数据处理。采用Pu标准溶液刻度仪器,建立了1BP溶液中钚在线分析方法。工作曲线的线性范围为0.1～5.0 g/L,R²=0.999。用该测量装置测量0.5 g/L的Pu标准溶液,结果的相对标准偏差为0.67%。该测量装置的热实验应用结果表明,其可实时监测工艺运行状况,监测结果可用于指导各相液流配比的调节。     

1BP中铀钚价态及其含量的分析方法

建立了1BP工艺点铀钚价态及其含量的分析方法。通过研究不同价态铀钚的可见吸收光谱，采用多点斜率法拟合了不同价态铀钚在414、480、600、659 nm波长下的摩尔吸光系数ε。利用摩尔吸光系数ε结合多元线性回归法（MLR），建立了1BP中Pu(Ⅲ)、U(Ⅳ)、U(Ⅵ)及Pu(Ⅳ)分析的数学模型。该方法测量了1BP模拟样品：在工艺正常情况下，Pu(Ⅲ)的质量浓度范围为0.50～8.00 g/L，测量精密度优于3.0%(n=6)，回收率为94.5%～103.9%；U(Ⅳ)的质量浓度范围为0.45～38.15 g/L，测量精密度优于3.0%（n=6），回收率为95.3%～104.7%；U(Ⅵ)的质量浓度范围为0.45～38.59 g/L，测量精密度优于3.0%（n=6），回收率为96.5%～103.0%；Pu总量的回收率为87.2%～100.6%。方法简单快速，精密度高，属于无损分析。     

1BP中铀钚价态及其含量的分析方法

建立了1BP工艺点铀钚价态及其含量的分析方法。通过研究不同价态铀钚的可见吸收光谱,采用多点斜率法拟合了不同价态铀钚在414、480、600、659 nm波长下的摩尔吸光系数ε。利用摩尔吸光系数ε结合多元线性回归法（MLR）,建立了1BP中Pu(Ⅲ)、U(Ⅳ)、U(Ⅵ)及Pu(Ⅳ)分析的数学模型。该方法测量了1BP模拟样品：在工艺正常情况下,Pu(Ⅲ)的质量浓度范围为0.50～8.00 g/L,测量精密度优于3.0%(n=6),回收率为94.5%～103.9%;U(Ⅳ)的质量浓度范围为0.45～38.15 g/L,测量精密度优于3.0%（n=6）,回收率为95.3%～104.7%;U(Ⅵ)的质量浓度范围为0.45～38.59 g/L,测量精密度优于3.0%（n=6）,回收率为96.5%～103.0%;Pu总量的回收率为87.2%～100.6%。方法简单快速,精密度高,属于无损分析。