理化分析测试实验室仪器设备的管理

仪器设备是实验室的重要资产,仪器设备管理是实验室正常运行的重要组成部分。从仪器设备的管理架构以及仪器设备的采购、验收、量值溯源、维护维修、报废等方面讨论了理化分析测试实验室仪器设备管理工作的重点和注意事项。     

食品检测实验室大型检测设备的管理探讨

从食品实验室大型设备定义、仪器设备购置、使用管理、人员管理、共享管理、网络化管理、设备报废7个方面对食品检测实验室大型检测设备的管理进行了探讨,尤其是对量值传递/溯源、仪器使用人员管理提出了建议.     

Cleaning validation using thermogravimetry

The health authorities require that equipment used in the pharmaceutical industry is clean prior to use. The main raison is to prevent any contamination of the drug products. This article demonstrates that thermogravimetry (TG) can be used for the determination of the residual impurities during the cleaning validation of the equipment of pharmaceutical production plants. The accuracy and the recovery rate of this method are comparable with those of the classical analysis method (determination of the distillation residue using a rotary evaporator). The fully automation of the testing equipment even allows its utilization around the clock by plants operators, leading to a significant reduction of the time necessary for the cleaning validation and to an increase of the plant capacity.     

无损检测技术及应用

无损检测技术经历了3个发展阶段,即无损探伤、无损检测和无损评价。目前一般统称为无损检测(NDT),而不是特指上述的第二阶段。无损检测技术在产品质量控制中起着不可替代的作用,很多无损检测技术是从航空航天装备的制造和检验中发展起来的,在承压设备制造和焊接等工业领域也有着广泛的应用。中国航天科技有限公司旗下的乐凯医疗科技有限公司,与其他几家跨国感光材料企业一道,在传统射线检测领域服务多年,生产的立方体和T颗粒卤化银系列工业无损探伤胶片,是航天"黑科技"之一。本文介绍了无损检测技术的发展、检测方法,以及在航天和铁路桥梁上的应用。     

Performance testing activities for analytical assessment of supercritical fluid extractors

Systematic performance testing activities for supercritical fluid extractors consistent with the implementation of quality systems in analytical laboratories are proposed. In this context, supercritical fluid extraction (SFE) is used for the automatic processing of complex samples. Ensuring reproducible operation of SFE equipment is crucial with a view to obtaining traceable results. To this end, an assessment protocol including recommended preventive and corrective actions, and complementary internal quality control activities, was developed with a view to facilitating the use of SFE equipment by routine analytical laboratories.     

物理吸附系统的改造及其测试

根据测试需求和物理吸附系统的性能,对现有物理吸附系统进行功能升级改造.研制了一套气体吸附法的前处理设备,解决目前脱气设备不够用、超高表面积和超细孔径的材料脱气不彻底、因现有前处理设备温度波动大引起的金属-有机框架材料(MOF)和有机共价框架材料(COF)等新型材料内部结构坍塌等问题.搭建新的分析站,将目前效率低、测试性价比低的单站测试升级到高效率的双站测试.改善了液氮的添加工具,避免了测试人员的冻伤,避免了转移液氮工具的温度对测试数据的影响.在大量无机吸附质试验基础上,将物理吸附仪拓展到甲烷、丙烷、甲醇等有机气体吸附质试验,实现了双性吸附质的物理吸附测试,增强了仪器的功能范围.改进吸附环境装置,解决吸附过程中样品管出现冷凝现象,避免吸附量偏大,从而完善了物理吸附系统及其测试方法.     

On-line testing equipment of P–V–T properties of polymers based on an injection molding machine

In order to obtain more accurate prediction of the service performance and service life of polymers and the optimization of processing parameters, this paper presents a novel, on-line testing equipment for measuring P–V–T (Pressure–Volume–Temperature) relationships of polymers under processing conditions. This equipment is based on an injection molding machine (IMM), and it can be used to get P–V–T data of polymers directly with a special testing mold under normal processing conditions. P–V–T properties of five polymers (ABS, PS, LDPE, PA 6 and PP) were measured. The experimental results under industrial processing conditions were presented. The results were compared with those obtained by the confining fluid technique. The P–V–T curves were consistent, which proved that the new on-line measurement is feasible. The repeatability of the P–V–T measurement was within 0.3%. Consequently, a new P–V–T database on typical commercial materials could be established. Repeatability of IMM could be improved significantly.     

食品药品检验机构仪器设备计量信息的标准化管理

建立食品药品检验机构仪器设备计量的信息化规范管理方法。总结了传统人工计量管理的弊端,提出计量信息化管理的流程,将计量信息化管理分为计量计划申报、计量应急申报、计量信息登记、计量结果确认4个步骤,详细介绍了4个步骤中信息管理的主要内容及注意事项。建立食品药品检验机构仪器设备计量信息化管理的标准化规程,可以为仪器设备计量信息的动态监管提供支持。     

Assessment of parameters for simulation of thermal ageing of materials in nuclear power plants using DSC

Summary Simulation of thermal ageing is an important part of qualification of materials designed for the use in nuclear power plants (NPP). According to standards, the simulation of long-term service thermal ageing is performed isothermally at elevated temperature using Arrhenius methodology. The samples or equipment are aged in thermal chamber, to bring them to the same state as after long-term service time. To proceed a reliable simulation, the testing parameters should be taken very carefully and the accelerator factors should not be too high. The testing temperature and time and the activation energy are the most important parameters. Determination of these factors and the limitations of their use in practice are discussed.     

Sorption of organic compounds from urine in mutagenicity testing: choice of sorbent

The choice of sorbents for urine mutagenicity testing was investigated. 14C-Labelled compounds were dissolved in urine and extracted from it by sorption with seven different sorbents singly or in combination. The compounds were desorbed with acetone. Sorption was examined under various experimental conditions. Except for two strong ionic compounds satisfactory extraction was achieved with a combination of three sorbents: Amberlite XAD-2, XAD-7, and Sep-Pak Silica. Filtration of the urine or contact of it with the walls of the experimental equipment could lead to substantial losses. Implications of these results for urine mutagenicity testing and possibilities for further optimization of the method are discussed.     

Application of ICP-MS radionuclide analysis to “Real World” samples of department of Energy radioactive waste

Germanium spectrometers must be operated at liquid nitrogen temperatures. Other detectors operate better when cooled. Many applications, because of hostile environments, inaccessibility, remote location, long duration, etc., are compromised, or totally precluded, by the requirement for liquid nitrogen. A Stirling cycle refrigerator based on a linear motor design, which is acoustically and vibrationally quiet, does not require secondary cooling, and operates unattended for years, is under development. System design and specifications are presented. Applications to cooled laser monitoring equipment. SQUID-based detection systems, environmental cleanup and monitoring, medical diagnostics, non-destructive testing systems, communication equipment, computer electronics, and imaging systems are discussed.     

质量控制图用于石墨炉原子吸收光谱法检测海水中铅元素

为保证海水中重金属检测结果的准确可靠,以铅元素为例,每个工作日使用石墨炉原子吸收光谱仪平行测定铅质控样2次,收集20组有效数据后,通过计算均值、标准差得出上下控制限、警告线及辅助限,绘制出在当前实验室环境条件、仪器设备、试剂药品和人员水平等因素条件下的质量控制图。该质量控制图不仅用于实际检测过程中对检测结果进行监控,还可为该实验室的人员考核、留样复测等实验室质量控制行为提供结果判定依据。     

凝结水处理用树脂溶出物问题研究

本文在自选设计的树脂溶出物动态循环溶茁测试装置上,试验了常用的各种凝结水处理用离子交换树脂短、长期动态溶出行为、发现各种树脂的溶出物量及行为相差很远,对树脂溶出物进行的高压釜试验表明,高压釜试验前后溶的的红外光谱变化不大,溶出物主要结构、基团变化也不明显,但是,树脂溶出物在高温、高压下酸化较明显。因此,对树脂溶出物进行检测是必要的。     

Carbon sequestration and estimated carbon credit values as measured using <Superscript>13</Superscript>C labelling and analysis by means of an optical breath test analyser

Recent developments in optical systems (isotope-selective non-dispersive infrared spectrometry) for breath testing have provided a robust, low-cost option for undertaking ¹³C analysis. Although these systems were initially developed for breath testing for Helicobacter pylori, they have an enormous potential as a soil science research tool. The relatively low cost of the equipment, US$15,000–25,000, is within the research budgets of most institutes or universities. The simplicity of the mechanisms and optical nature mean that the equipment requires relatively low maintenance and minimal training. Thus methods were developed to prepare soil and plant materials for analysis using the breath test analyser. Results that compare conventional mass spectrometric methods with the breath test analyser will be presented. In combination with simple ¹³C-plant-labeling techniques it is possible to devise methods for estimating carbon sequestration under different agronomic management practices within a short time frame. This enables assessment of the carbon credit value of a particular agronomic practice, which can in turn be used by policy makers for decision-making purposes. For global understanding of the effect of agricultural practices on the carbon cycle, data are required from a range of cropping systems and agro-ecological zones. The method and the approach described will enable collection of hard data within a reasonable time.     

二级学院大型仪器管理探索与实践

各国家重点实验室及高校的校级公共测试中心的大型仪器管理已经发展的较为成熟,但是二级学院的大型仪器设备管理还有待加强.就二级学院大型仪器的科学管理进行了探索与实践,旨在提高其利用率和共享性,充分发挥大型仪器的使用效益.     

Advances in Molecular Diamagnetism

At the present state of instrumentation and quantum-mechanical approximations, diamagnetic measurements can supply information on chemical structure which complements the result of other approaches, such as infrared and NMR spectroscopy. General applicability and relatively low cost of equipment are among the advantages of this technique. There is growing interest in the relation to chemical shifts in NMR spectra and in the possibility offered by this technique for testing quantum-chemical approximations.     

Comparative study on degradation of ethylene-propylene rubber for nuclear cables from gamma and beta irradiation

Considering safety is the priority concern of nuclear power plants, equipment qualification testing of the nuclear components manufactured should be paid special attention to. Thereinto, equivalent conversion (1:1) from the absorbed beta doses to gamma doses is a rule of thumb for irradiation qualification testing of the polymers used as nuclear cables, however whether it is reasonable and applicable to Chinese domestic polymers still requires investigation. In this paper, both gamma and beta irradiation testing with the actual dose rates and total absorbed doses in China Advanced Passive (CAP) series nuclear power plant was performed upon one domestically manufactured ethylene-propylene rubber intended for nuclear cable insulation in China. The mechanical and the electrical properties before and after irradiation were measured to compare the extent and the trend of degradation between the two irradiation types, and related oxidation degradation mechanism especially its attenuation along the thickness was quantitatively addressed.     

Sound transmission testing of polymer compounds

Acoustic properties of polymer compounds are an important consideration for many applications. Currently, there are standard test methods for the determination of these properties. There is, however, no standard for the equipment used in these tests, only a specification for the test conditions. The objective of this work was to evaluate the operation and performance of a bench top laboratory sound testing system for its potential as a simple cost effective method for the initial evaluation of materials that require specific acoustic properties. The work was limited to an investigation of the property of sound transmission loss (STL). A study of the effect of the mounting conditions for the samples on the STL was carried out. Following this, a series of polymer and polymer composite samples was tested. The results presented demonstrate the potential for the testing system as an effective standard test method for the acoustic properties of polymer composites and other materials.     

波兰农产品中农药残留检测技术现状

介绍波兰农产品中农药残留检测技术。波兰的农药残留检测技术标准以欧盟标准为框架,在实际检测过程中各实验室可根据自身仪器设备条件、样品基质及目标农药的性质,自主开发检测方法,但需根据SANCO 12571:2013对方法进行验证,并向波兰认可中心提供验证报告。样品制备技术以基于乙腈提取/分配、Qu ECh ERS净化为主(EN 15662:2008),各实验室对标准中大部分步骤进行了调整和创新,以满足实际工作的需要;一些经改进的经典方法,如基质固相分散法(MSPD)和基于丙酮提取、二氯甲烷萃取的LUKE法在波兰农产品检测实验室也有较为广泛的应用;最终定性定量分析以GC–MS/MS和HPLC–MS/MS法为主,以GC,HPLC和紫外分光光度法等分析方法为辅。     

CRISPR-Cas Biochemistry and CRISPR-Based Molecular Diagnostics

Polymerase chain reaction (PCR)-based nucleic acid testing has played a critical role in disease diagnostics, pathogen surveillance, and many more. However, this method requires a long turnaround time, expensive equipment, and trained personnel, limiting its widespread availability and diagnostic capacity. On the other hand, the clustered regularly interspaced short palindromic repeats (CRISPR) technology has recently demonstrated capability for nucleic acid detection with high sensitivity and specificity. CRISPR-mediated biosensing holds great promise for revolutionizing nucleic acid testing procedures and developing point-of-care diagnostics. This review focuses on recent developments in both fundamental CRISPR biochemistry and CRISPR-based nucleic acid detection techniques. Four ongoing research hotspots in molecular diagnostics-target preamplification-free detection, microRNA (miRNA) testing, non-nucleic-acid detection, and SARS-CoV-2 detection-are also covered.