~1H、~2H核磁共振研究氘标记丙氨酸的标记位置及相对百分含量

本文利用质子及氘的核磁共振波谱技术研究氘标记丙氨酸的标记位置及相对百分含量,并指出:~1H核磁共振利用波谱高度的下降间接证明氘被富集在分子上的结果具有不确定性,而~2H核磁共振则是直观地观察到在相对应的质子谱线位置上氘被标记的信号并可计算各标记基团之间标记百分含量。     

~2H和~3H标记四氢原小檗碱的合成

四氢原小檗碱是一类天然存在的生物碱,新近研究表明其左旋异构体是脑内多巴胺受体 的拮抗剂,而右旋体则极可能是多巴胺的排空或释放剂。为了研究它们的氚标记化合物的生物活性,我们用NaBH_4还原法制备了氚代位置在C_8和C_(14)位上的三种四氢原小檗碱,即氘代四氢小檗碱(THB-d_2),氘代四氢巴马汀(THP-d_2)和氘代千金藤立定(SPD-d_2)。氘代物的质谱显示它们的分子离子峰均比非氚代物增加2,RDA产生的两碎片峰均比非氘代物增加质量1。故可推定反应中分子上了两个氘原子,氘代位置只能分别在C_8和C_(18)位上。从氘代物的′H-NMR看,C_(14)位质子信号消失,表明该位置为氘取代。C_8位质子信号由非氘代物的两组二重峰(AB型)变成氘代物的两个单峰,每单峰积分为0.5H,两单峰具有较大的化学位移值之差(Δδ=0.7),表明B/C环应为反式稠合。IR在2800cm~(-1)处Bohlmann带亦可作证。对于C_8位置质子信号可解释为由于氘负离子首先还原平面型季铵阳离子成二氢化物时没有优势进攻面,氘在横或竖键上的分布几率均等,故C_8-H两单峰积分各为0.5H。     

天然钐和浓缩钐同位素丰度比质谱测定

裂变产物~(149)Sm热中子吸收截面大,是反应堆中妨碍提高反应性的可燃毒物。用MATCH5质谱计,测定了天然氧化钐和浓缩钐同位素丰度比和百分原子浓度,~(149)Sm同位素丰度比测定精度在0.4％左右,为同位素稀释质谱法准确测定~(149)Sm绝对浓度奠定了基础。     

生产堆元件铀同位素丰度比和含量的测定

文章用同位素质谱法测定了辐照堆元件铀的同位素丰度比和含量。讨论了测定技术、方法及误差来源和误差传递等有关问题。上述各量与切片的分布相符,与其他方法的有关测量结果相一致。     

铪试剂及控制棒中铪同位素丰度测定

本文描述用 CH_5质谱计表面电离源双带组件测定天然铪同位素丰度。铪的化学形态为过氯酸盐或硝酸盐。铪离子流收集均用电子倍增器,其测量精度(除~(174)Hf/~(176)Hf 比之外)在0.5%以内。此外,该结果还与用法拉第筒收集器的测量值进行了比较。     

无源γ能谱法非破坏测定核燃料中~(235)U丰度

利用γ能谱法对 UO_2 中~(235)U 丰度进行了非破坏分析研究.测量结果与质谱分析结果对照只差3—1%,在最短测量时间为7分钟的情况下,其相对统计误差为4—1%(2σ 水平).本方法的特点是简便、快速、对样品无破坏及对各种样品的适应性强.     

~3H和~(35)S标记农药杀虫双(SCD)

杀虫双是广谱性巴丹类农药杀虫剂,化学名称为2-N,N-二甲胺基-1,3-双硫代硫酸钠基丙烷(SCD)。其合成方法如下:     

~3H和~(14)C标记常咯啉的合成

本文用合成方法制备了抗心律不齐新药常咯啉的三种不同位置~3H和~(14)C的标记化合物。以5-溴邻氨基苯甲酸按Scheme 1经5步反应得6-溴代常咯啉(Ⅵ),Ⅵ用氚经催化脱卤得[6-~3H]常咯啉(Ⅰ)用[~(14)]甲酸制成[~(14)C]甲酰胺,按Scheme 1经二步反应得[2~(14)C]5-氯代喹唑啉(V,R=H)再按Sc-heme2即得[2-~(14)C]常咯啉(Ⅱ)。以[~(14)C]甲醛为原料按Schemel的最后一步可直接制得(甲撑-~(14)C)常咯啉(Ⅲ)     

氢-氘体系的氘丰度质谱分析技术

介绍了用低分辨MAT253质谱计准确测量氢-氘体系中氘丰度的分析技术.通过建立实验室次级标准样品配气系统,并考虑氢同位素的灵敏度差异,测得了几何校正因子(k).对不同氘丰度的气体样品比对分析,2个独立检测的结果吻合较好.     

~3H、~(14)C和~(35)S标记农药渝-7802

1.~3H标记:用放电曝射法,氚标记中间体苯甲酰肼,再与二氯乙烷、25％的KOH溶液混合,在搅拌下逐渐滴加CS_2,反应温度15—20℃。其粗产品由硅胶G薄板层析分离纯化,推进剂:乙醚:氯仿=4:1,R_f=0.30,渝-7802-~3H的总放射性为321.9MBq,比活度为22.6MBq/mg,放化纯度≥90％。     

氘和氚标记ST—1435的制备

在氘或氚化溶剂中,16-次甲基-17α-乙酰氧基-19-羧基-孕甾-4-烯-3、20-二酮(Ⅰ)通过脱羧反应制得[10-~2H]ST-1435或[10-~3H]ST-1435(Ⅱ)。氘标记ST-1435经质谱分析表明有1—3个氘原子掺入到ST-1435分子中去,其中m/e 371(M~+)的氘掺入率为22.6％。氚标记ST-1435的比活度为52.5TBq/mol,放化纯度>95％。     

高纯氘中杂质的低温气相色谱分析

实验研究采用5A分子筛和氧化铝充填色谱柱分别在常温和低温（77K)下对D₂中的O₂、N₂以及H₂、HD等杂质进行定量分析测量，以建立1种准确实用的分析方法。研究结果表明，该方法对H₂、HD的最低检测浓度可达（150～200）×10^－6，能够满足高纯氘制备过程中对杂质的定量分析要求。     

密封容器中钚材料同位素丰度和年龄的测量

根据相对效率法的原理,利用PC/FRAM分析软件,开展了用高分辨γ谱仪测量密封容器中钚材料的同位素丰度和年龄的实验研究.研究结果表明,同位素丰度和年龄的分析精度随能谱测量精度的提高而提高,如果能谱的测量精度不够,通过PC/FRAM分析得出的钚材料的同位素丰度和年龄有偏低的可能.因此,在能谱测量过程中,建议通过监测某个特征峰的峰面积计数来判定239Pu丰度和年龄的测量精度是否已满足测量要求.     

采用弹性反冲分析法同时测量薄膜中氢和氘的深度分布

给出由重叠反冲能谱计算氢和氘的浓度及深度分布的解谱技术，用４．５ＭｅＶ和４．２ＭｅＶ的α粒子作入射粒子得到两个反冲能谱。在考虑和不考虑能量展宽效应的情况下分析了钛膜中氢和氘的深度分布；发现考虑能量展宽效应的影响得到的氢和氘的深度分布是令人满意的。     

Evaluation of gases'molecular abundance ratio by fiber-optic laser-induced breakdown spectroscopy with a metal-assisted method

A metal-assisted method is proposed for the evaluation of gases'molecular abundance ratio in fiber-optic laser-induced breakdown spectroscopy(FO-LIBS).This method can reduce the laser ablation energy and make gas composition identification possible.The principle comes from the collision between the detected gases and the plasma produced by the laser ablation of the metal substrate.The interparticle collision in the plasma plume leads to gas molecules dissociating and sparking,which can be used to determine the gas composition.The quantitative relationship between spectral line intensity and molecular abundance ratio was developed over a large molecular abundance ratio range.The influence of laser ablation energy and substrate material on gas quantitative calibration measurement is also analyzed.The proposed metal-assisted method makes the measurement of gases'molecular abundance ratios possible with an FO-LIBS system.     

Measurement of the isotopic abundance of boron-10 by inductively coupled plasma-quadrupole mass spectrometry

This article describes the method for measuring the isotopic abundance of ¹⁰B in nuclear grade boron carbide using inductively coupled plasma-quadrupole mass spectrometry (ICP-QMS). The results of investigation revealed that both the integration time and the dwell time have a major influence on the reproducibility of ICP-QMS measurements. As a result of optimization of the measurement conditions, reproducibility below 0.2% relative standard deviation (RSD) (0.17% RSD maximum) was achieved. In addition, the measured value of the isotopic abundance of ¹⁰B for each sample well agreed with the values measured by the TIMS. Thus, the method described in the present investigation was very effective in the analysis of isotopic abundance of ¹⁰B in B₄C or H₃BO₃. The results of this study suggest that ICP-QMS could be applied to the precise analysis of the isotopic abundance of ¹⁰B required in the field of nuclear applications.     

Retention of deuterium and tritium in Papyex graphite

The retention of 100 eV D-T ions in Papyex graphite over the temperature range 373 to 1573 K has been measured using both nuclear reaction analysis and tritium dissolution counting. Below 1000 K, the retention is characterized by saturation of the near surface region and atomic adsorption on internal porosity, both of which decrease with increasing temperature. Above 1000 K, a local maximum in the retention is seen near 1200 K due to intergranular diffusion and decoration of high energy traps.     

Abundance Analysis of13C Isotope Separation by Cryogenic Rectification Based on Dynamic Simulation

The carbon isotope (¹²CO/¹³CO) separation has a separation coefficient of only 1.007, which has typical characteristics of severe separation conditions and long equilibrium time. In order to reduce the operational risk of industrial devices, the theoretical prediction of the dynamic process of¹³C isotope enrichment is an urgent problem to be solved in industrial technology research. Therefore, the dynamic simulation of carbon isotope separation by CO cryogenic rectification was carried out by using Aspen Dynamics. Through the simulation, the abundance distribution of¹³C isotope was obtained under the conditions of total reflux, concentration and continuous rectification operation, and the visualization of the abundance change of the¹³C isotope in the two dimensions of space and time was realized. On the other hand, comparing the dynamic simulation values with the experimental data, the results show that they are agree well, and the relative errors of the enrichment equilibrium abundance and equilibrium time are both less than 15%, which indicate that the accuracy of the dynamic simulation calculation method of¹³C isotope for cryogenic rectification separation is verified, which can be further used to theoretically predict the abundance enrichment process in the production plant of high abundance¹³C isotope.