Practical method validation: Validation sufficient for an analysis method

Validation of an analysis method depends on the purpose of the method, the chosen technique and the procedure in question. Methods are used for different research, product development, process control and quality control purposes. The human and economical importance of results vary. Each of the techniques used, such as chromatography-(HPLC, HRGC, TLC), capillary electrophoresis-(CE), spectrophotometry-(UV/VIS, IR, fluorescence, AAS, ICP) or spectrometric techniques (NMR, MS) as well as the hyphenated methods, have their own special features and deficiencies which must be considered. The method can include a simple pretreatment or it may include many demanding steps, it can use automation and data processing in various ways, it can have an official status, it can be a thoroughly verified or less studied one. How should these differences be accounted for during the validation? What would be a sufficient certainty that the method does what is expected, that the method fits for the purpose it was intended? The client (or authority) decides the required timetable, cost and quality level. This is why within a laboratory different quality levels and associated levels of validation exist. This paper tries to outline a practical test frame for validation efforts to assist the analyst when planning validation of a method.     

紫外可见分光光度计主要技术指标及其检定方法

介绍了紫外可见分光光度计的主要技术指标如波长准确度、波长重复性、光度准确度、光度重复性、杂散光,以及这些指标的检定方法。     

神光Ⅲ主机通用诊断搭载平台的研制

 神光Ⅲ主机通用诊断搭载平台提供各种诊断系统送进和收回的搭载功能,便于诊断系统的拆装和维护保养,同时提供精确的径向、指向瞄准能力,能将诊断系统送至靶室内指定位置,并且能在不破坏靶室真空的状态下安装、调试和维护诊断系统。将通用诊断搭载平台安装在神光Ⅲ原型装置上进行精度检测,得到其真空状态下的径向、X和Y方向指向定位精度分别为36,13,8 μm,全行程的径向复位精度、X和Y方向指向复位精度分别达到20,30,12 μm。搭载分幅相机诊断包进行激光打靶考核,实验结果表明:其指向瞄准精度、真空性能、接口等均满足使用要求,并具备了对抗强电磁干扰与辐射的能力。     

Composition of structural carbohydrates in biomass: precision of a liquid chromatography method using a neutral detergent extraction and a charged aerosol detector

We adapted and optimized a method to quantify the cellulose, hemicellulose, xylan, arabinan, mannan, galactan contents in lignocellulosic biomass. This method is based on a neutral detergent extraction (NDE) of the interfering biomass components, followed by a sulfuric acid hydrolysis (SAH) of the structural polysaccharides, and a liquid chromatography with charged aerosol detection (LC-CAD) to analyze the released monosaccharides. The first step of this NDE-SAH-LC-CAD method aims at removing all compounds that interfere with the subsequent sulphuric acid hydrolysis or with the subsequent chromatographic quantification of the cellulosic and hemicellulosic monosaccharides. This step includes starch hydrolysis with an analytical thermostable α-amylase followed by an extraction of soluble compounds by a Van Soest neutral detergent solution (NDE). The aim of this paper was to assess the precision of this method when choosing fiber sorghum (Sorghum bicolor (L.) Moench), tall fescue (Festuca arundinacea Schreb.) and fiber hemp (Cannabis sativa L.) as representative lignocellulosic biomass. The cellulose content of fiber sorghum, tall fescue and fiber hemp determined by the NDE-SAH-LC-CAD method were 28.7 ± 1.0, 29.7 ± 1.0 and 43.6 ± 1.2 g/100 g dry matter, respectively, and their hemicellulose content were 18.6 ± 0.5, 16.5 ± 0.5 and 14.5 ± 0.2 g/100 g dry matter, respectively. Cellulose, mannan and galactan contents were higher in fiber hemp (dicotyledon) as compared to tall fescue and fiber sorghum (monocotyledons). The xylan, arabinan and total hemicellulose contents were higher in tall fescue and fiber sorghum as compared to fiber hemp. The precision of the NDE-SAH-LC-CAD method was better for polysaccharide concentration levels above 1 g/100 g dry matter. Galactan analysis offered a lower precision, due to a lower CAD response intensity to galactose as compared to the other monosaccharides. The dispersions of the results (expanded uncertainty) of the NDE-SAH-LC-CAD method were smaller as compared to the Van Soest (VS) method. In addition, the NDE-SAH-LC-CAD method was able to provide additional information on the composition of the hemicellulose (xylan, arabinan, mannan and galactan content) that is not provided by the Van Soest method. The NDE-SAH-LC-CAD method offers also the advantage of a better specificity for hemicellulose and cellulose, as compared to the NREL and Uppsala methods.     

CSR二极磁铁积分磁场测量系统

介绍了兰州重离子加速器冷却储存环(HIRFL CSR)积分磁场测量系统以及积分测量的基本原理和数据处理方法,对测量结果的分析表明整个系统运行可靠稳定,可用于CSR磁铁的积分测量.This article presents the basic principle of dipole integral magnetic field measurement . The integral coil which has the same radius with the dipole magnets was used to measure the integral magnetic field of different magnets in Cooler Storage Ring(HIRFL CSR). The article also generally introduced the software and hardware systems of the automatic measurement device. According to the repetitive experiments, a suit of better measurement got to be summarized. On the other hand, the article recommends the...