BELLE物理实验DAQ系统中的精确时序调整

介绍了一个基于ＥＣＬｉｎＰＳ电路产生高精度程控延时脉冲信号的ＶＭＥ插件,该插件将用于ＢＥＬＬＥ物理实验ＤＡＱ系统中的精确时序调整,产生分辨率为１０ｎｓ的时序控制符号,其时间抖动的均方根值小于１００ｐｓ。     

痕量锂同位素的热表面电离质谱高精度测量

建立了痕量锂同位素的高精度热电离质谱测量技术。通过双带测量、加入磷酸发射剂及采用预烧处理方法等途径,抑制了分馏效应,提高了痕量锂质谱分析的精度。采用浓缩锂同位素标准样品考察了测量效果,对于100ng锂样品,测量相对标准偏差好于0.086%;对于10ng锂样品,相对标准偏差好于0.90%。     

超薄型丙氨酸／ESR剂量计特性的研究

报道了自制的丙氨酸／ＥＳＲ剂量计的研究结果。该系统包括４部分：丙氨酸探测器的制备；照射设备；ＥＳＲ波谱的测读和刻度方法。研究了这种超薄（０．５ｍｍ）型剂量计的一般特性和剂量学特性：包括，样品密度的均匀性；最小可达厚度；可探测下限；方法的重复性；线性范围；分散性等。为了刻度电子剂量，利用一个经标准装置外推电离室刻度过的旋转式９０°Ｓｒ＋９０Ｙ面源构成的参考辐射场，大大提高了均匀性、稳定性、重复性以及量值的可溯源性。利用精密温、湿度长时间自动控制系统和６０Ｃｏ板源辐射场，在严格控制实验中的有影响因素和有关参数的条件下，对丙氨酸／电子自旋共振剂量计的灵敏度与照射温度的关系进行了系统地研究，得到了在辐照剂量为１．４×１０３、１．４×１０４、和１．０×１０５Ｇｙ、照射温度在１０一７０℃时灵敏度的温度系数，以及平均温度系数，其值为０．２４％℃－１。     

Development of anodic stripping voltammetry for determination of gallium in U–Ga alloy

Deposition potential, deposition time, square-wave frequency, rotation speed of the rotating disc electrode and gallium concentration have been studied in detail, for trace concentration level determination of gallium metal in U–Ga alloy by square-wave voltammetry anodic stripping analysis, in 1 M NaClO₄ + 0.5 M NaSCN at mercury film electrode (MFE). Optimum conditions have been found for Ga(III) determination by obtaining calibration graphs for the range 1–10 × 10⁻⁷ M gallium. Error and standard deviation less than 1% were assessed of this method with all gallium standard solutions. The developed methodology was applied successfully as a subsidiary method for the determination of gallium content in synthetic U–Ga samples with very good precision and accuracy (under 1% error and std. dev.).     

ALANINE/ESR DOSIMETRY FOR MEASUREMENT OF ELECTRON DOSES IN INDUSTRIAL APPLICATIONS

In this report, the results of preliminary research on L-alanine/ESR electron dosimeters are described. They include the designs of modelling tools and experimental capsules, the preparation and irradiation of very thin dosimeters, the measurement of ESR signal spectrum and the calibration method. The physical, chemical and dosimetric properties of the alanine free radical dosimeters, such as the smallest thickness, average density, lowest detectable limit, repeatability of the method, reproducibility resulted in directivity and location in resonance cavity, linearity regions as well as relative scattering of the response to identical doses, are summarized.     

EDXRF方法测量菱镁矿中镁元素含量

采用间接测量的方法,对菱镁矿的化学分析过程进行处理,建立目标元素Mg与中间观测元素Ba之间的对应关系,以Ba的能量色散X射线荧光(Energy Dispersive X-ray Fluorescence,EDXRF)测量结果,计算出菱镁矿测试样品中镁的含量为29.43%,相对标准偏差为0.58%。借助于具有含量梯度的验证样品对方法的准确性进行了验证,得到的定标曲线具有良好的线性关系,测量结果显示准确度和可靠性高、稳定性和重复性好。该方法克服了EDXRF对轻元素直接探测效率低、结果精度差的缺点,为镁的测量提供了一种快速、准确、经济的检测思路和方法。     

Determination of boron in Zr–Nb alloys by glow discharge quadrupole mass spectrometry

Direct determination of boron in Zr–2.5%Nb, Zr–1%Nb alloys and zirconium metals which are extensively used as structural materials in nuclear reactors has been carried out by glow discharge quadrupole mass spectrometer (GD-QMS). Relative sensitive factor (RSF) values for boron were determined using different solid standard reference materials (Zircaloy and steel). A comparison of the GD-QMS results obtained using these RSF values, with DC–Arc-AES (direct current arc atomic emission spectrometry)/certified values showed reasonably good agreement in all the Zr-based materials analysed for boron in the range of 0.1–7 mg kg⁻¹. Quantitation of boron in Zr matrix is possible even with a steel standard when certified for Zr and B. Internal precision (intra-sample precision) was found to be typically ±4% RSD (relative standard deviation) and the inter-sample precision was ±10% RSD for boron at 0.1 mg kg⁻¹ levels. The overall accuracy of the procedure was found to be ±8% at 0.5 mg kg⁻¹ levels of boron using Zircaloy and steel standards. Under optimised experimental conditions the detection limit for boron was found to be ±13 μg kg⁻¹.     

Thermoluminescent characteristics of topaz from Sabser mine near Sakardu in northern Pakistan

Topaz, a naturally occurring aluminium fluorosilicate mineral, shows thermo-luminescence (TL) after irradiation to gamma rays. The TL characteristics (glow curve, dose response/intensity, sensitivity, energy response, fading, reusability and mechanical stability) of topaz collected from the Sabser mine in the vicinity of Sakardu in northern Pakistan were studied. The purpose of this study was to design and develop a TLD (thermoluminescence dosimeter) based on topaz. The samples of topaz from this mine were cut into square chips of dimensions 3.2 × 3.2 mm with thickness 0.9 mm, which are suitable for the TLD reader. Gamma dose was given to the chips from ⁶⁰Co and/or ¹³⁷Cs gamma irradiators. The TL glow curves of the chips revealed stable peak at about 260 °C. The height of this peak rose linearly with increase of dose levels. The TL response versus dose (calibration curve) showed the linear behaviour between 10⁻² and 10² Gy without saturation. Dose response was independent of gamma energies of ⁶⁰Co and ¹³⁷Cs. The response of standard sized chips of topaz remained constant within ±11% deviation from initial value after 30 cycles of reuse. The rate of fading of topaz chips of this mine were studied up to four months, which was fast for initial few hours and slowed after a few days. The chips remained mechanically stable during handling in all types of experiments. Standard sized topaz chips of Sabser mine can effectively and efficiently be used as a TLD.     

稳定同位素氘标记苏丹红I的同位素丰度和化学纯度分析

为建立高灵敏度、高选择性的食品中非法添加物的分析检测方法,采用"质量簇"计算分类方法,利用液质联用仪检测稳定同位素氘标记苏丹红Ⅰ的同位素丰度,用于同位素稀释质谱法的内标试剂。针对不同操作人员、不同仪器进行重复性和再现性实验,RSD均0.1%,重复性和再现性良好。对结果进行了F检验和t检验,结果表明,苏丹红I-D_5的同位索丰度分析方法的准确度和精密度良好。利用高效液相色谱仪,采用外标法,建立标准曲线,确立稳定同位素氘标记苏丹红I-D_5的化学纯度分析方法。结果表明,制备的稳定同位素氘标记苏丹红I-D_5可作为同位素稀释质谱法的内标物质。     

可作为校准检定用标准剂量计的能量补偿型高气压电离室改进

在电离辐射计量检定工作中,标准剂量计的测量结果通过检定逐级传递到工作计量器具,以实现单位统一和量值准确可靠。由于环境水平γ射线剂量率较低,国际上常用的PTW-UNIDOS系列标准剂量计无法满足需要。针对这一特点,结合蒙特卡罗方法对高气压电离室的X射线、γ射线和宇宙射线响应特性进行模拟计算,进行了能量补偿型高气压电离室改进。测试结果表明:剂量率约30 μGy/h时,能量补偿型高气压电离室在87 keV～1.25 MeV能量范围内相对于¹³⁷Cs γ射线的响应偏差不大于6%,宇宙射线和¹³⁷Cs γ射线的响应偏差不大于10%,在0.5 μGy/h～1 mGy/h范围内相对固有误差为-3%,0.5 μGy/h时的重复性为0.7%,校准因子的不确定度为4%(k=2),可作为环境水平标准剂量计在校准检定工作中使用。     

Optically stimulated luminescence: Searching for new dosimetric materials

Optically stimulated luminescence (OSL) is increasingly being used as a dosimetric technique in various fields such as medical, environmental and space dosimetry, and sediment and archaeological dating. Nevertheless few compounds are suitable as OSL materials. In this work, a survey was made of various insulators, searching for candidates for new OSL dosimeters. Natural and synthetic crystals and glasses from numerous sources are included. Luminescence was stimulated with blue LEDs (470 nm) and with IR laser (830 nm) provided by an automatic reader. Irradiation was performed with a ⁹⁰Sr/⁹⁰Y beta source, and the emitted light was measured with a photomultiplier tube, protected with suitable optical filters. Thermoluminescence (TL) of the samples was also measured, with the same equipment, to evaluate the thermal and optical stability of the defects related to OSL and TL. Among the various investigated materials, Al₂O₃:Cr, Mg, Fe, MgAl₂O₄ spinels, Mg₂SiO₄:Tb, and natural fluorite show potential as OSL dosimeters. Some materials, as barium aluminoborate glasses, although showing intense OSL signals, present a high fading at room temperature. In that situation the OSL signal is related to low temperature TL peaks that also fade at room temperature. None of the investigated materials was specially prepared to be used as an OSL dosimeter, which means that work can be done, mainly in the impurity nature and content, in order to improve OSL signals and to overcome some of the shortcomings that were noticed.     

燃料棒包壳管内表面残留氟含量测定方法研究

锆合金管材内表面残留氟可能会加速锆合金表面微裂纹的应力腐蚀,为准确测定锆合金管材内表面残留氟含量,本文通过试验研究,研制了专用的内表面残留氟提取装置并进行了高温水解条件试验;采用离子色谱法对提取出的氟离子进行测定,建立的分析方法可以实现快速连续测定,分析范围为0.05~1.0 μg/mL,最后采用该方法对锆合金管材内表面残留氟含量进行了测定。结果表明,研制的装置可以完全提取内表面残留氟;本文提出的测定方法的加标回收率为98%~104%,最大相对标准偏差为3.9%,精密度和准确度高,测量结果满足生产需求。      

ICP-OES测定环境水样中的钾-40

建立了利用电感耦合等离子体发射光谱仪(ICP-OES)测定环境水样中钾-40的方法。此方法标准工作曲线线性关系良好,检出限为0.001 Bq/L,相对标准偏差小于1.5%,相对误差小于4.0%,加标回收率在94.1%~105.5%之间,具有前处理简单、检出限低、精密度和准确度高、干扰小等优点,值得推广应用。     

自然循环反应堆全寿期流量分配多目标优化研究

堆芯流量分配设计是自然循环反应堆堆芯结构优化的重点内容,对提升堆芯经济性和安全性具有重要意义。基于反应堆闭式并联多通道模型构建了局部最优流量分配计算模型,并对现有的流量分配方案进行分析,针对其局限性,提出了一种基于最佳时区的多目标综合评价法,可实现反应堆全寿期多目标流量分配优化计算;根据所提出的理论,结合TOPSIS综合评价法,以自然循环下最大输出功率、反应堆寿期内出口最大温差以及最大温差随时间变化标准偏差为属性值,开展小型长寿命自然循环铅铋快堆SPALLER-100的堆芯流量分配方案优化研究。研究结果表明,基于运行时间为3182 d功率分布所得SPALLER-100反应堆堆芯流量分配方案最佳,与基于寿期初功率分布所得流量分配方案相比,所得方案堆芯出口最大温差降低30 K,堆芯出口最大温差随时间变化的标准偏差降低41%,反应堆自然循环最大输出功率提高2.35%。      

The precision of product consistency tests conducted with a glass-bonded ceramic waste form

The product consistency test (PCT) that is used for qualification of borosilicate high-level radioactive waste (HLW) glasses for disposal can be used for the same purpose in the qualification of the glass-bonded sodalite ceramic waste form (CWF). The CWF was developed to immobilize radioactive salt wastes generated during the electrometallurgical treatment of spent sodium-bonded nuclear fuels. An interlaboratory study was conducted to measure the precision of PCTs conducted with the CWF for comparison with the precision of PCTs conducted with HLW glasses. The six independent sets of triplicate PCT results generated in the study were used to calculate the intralaboratory and interlaboratory consistency based on the concentrations of Al, B, Na, and Si in the test solutions. The results indicate that PCTs can be conducted as precisely with the CWF as with HLW glasses. For example, the values of the reproducibility standard deviation for Al, B, Na, and Si were 1.36, 0.347, 3.40, and 2.97 mg/l for PCT with CWF. These values are within the range of values measured for borosilicate glasses, including reference HLW glasses.     

萃取光度法精密测定铀

在精密测定铀含量的过程中,滴定剂浓度太低或太高均对测定结果的精密度有影响,且存在电极响应迟缓及电位拖后现象,从而影响铀含量测定结果的准确度和精密度。为克服这些不利因素,建立一种溯源链清晰,结果准确、可靠的精密测定小量铀的方法尤为重要,对铀标准物质的研制及铀样品的精密分析具有重要意义。本文以异戊醇为萃取剂,对Cr(Ⅵ)与显色剂二苯卡巴肼(DPC)生成的紫红色配合物进行了萃取实验研究,并确定了最佳萃取条件,建立了萃取光度法精密测定铀含量的方法。铀取样量为100mg时,相对标准偏差为0.025%。     

应用微波消解-ICP-MS法分析环境水样中的钍

采用微波消解对环境水样进行前处理、应用电感耦合等离子体质谱法(ICP-MS)快速测定环境水样中钍含量,对测量条件和微波消解条件进行了优化,并从内标的选择、检出限、精密度、准确度、回收率以及实际样品测量等方面对结果进行分析。结果表明：以209Bi为内标分析水中钍时,测量结果的相对偏差最小,为0.2%～1.3%;该方法检出限为0.003 μg/L;考察了4个浓度水平下的方法精密度,相对标准偏差（s_r）均小于6.0%(n=6);进行了3个不同浓度水平下的标准物质测量和加标回收率实验,测定值与标准值基本吻合,加标回收率为93.4%～106.2%;对20个实际环境水样中钍质量浓度进行了测量,测定结果在2016年测量值范围之内,验证了该法测量环境水样中钍含量的实用性。     

Experimental determination of the absorbed dose to water in a scanned proton beam using a water calorimeter and an ionization chamber

The absorbed dose to water is the reference physical quantity for the energy absorbed in tissue when exposed to beams of ionizing radiation in radiotherapy. The SI unit of absorbed dose to water is the gray (Gy = 1 J/kg). Ionization chambers are used as the dosimeters of choice in the clinical environment because they show a high reproducibility and are easy to use. However, ionization chambers have to be calibrated in order to convert the measured electrical charge into absorbed dose to water. In addition, protocols require these conversion factors to be SI traceable to a primary standard of absorbed dose to water. We present experimental results where the ionization chamber used for the dosimetry for the scanned proton beam facility at PSI is compared with the direct determination of absorbed dose to water from the METAS primary standard water calorimeter. The agreement of 3.2% of the dose values measured by the two techniques are within their respective statistical uncertainties.     

能量色散X射线荧光谱仪在土壤中40K活度分析中的应用

对粉末样品进行压片制样,建立了能量色散X射线荧光（EDXRF）谱仪测定环境土壤样品中⁴⁰K放射性活度的方法。方法标准曲线的相关系数为0.991 0,测量的精密度为2.98%,测量标准样品的最大相对偏差为6.40%。采用本方法和γ谱仪同时测量7个土壤样品,并对这两种分析方法的测量结果采用配对t检验SPSS程序计算。结果表明,两种方法所得数据无显著性差异（P＞0.05）,可使用X射线荧光谱仪法分析土壤中40K的放射性活度。这种方法操作简便,精密度和准确度较好,具有广泛的实用性。