共查询到19条相似文献，搜索用时 46 毫秒
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摘要：介绍检测和校准方法证实与确认的概念。从版本的有效性、人员、设备、材辅料、样品、作业指导书、设施和环境条件等方面介绍标准方法的证实内容;介绍非标准方法的确认方法、步骤以及非标准方法确认应有的文件和确认记录。列举了非标准方法特性量的测定示例。校准方法的证实与确认能有效确保检测和校准的准确性。 相似文献
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回顾了我国稀土化学分析方法标准化工作的历史,并介绍了近年来我国稀土化学分析方法标准化工作的进展.指出目前已初步形成了较为完善的稀土化学分析方法国家标准体系. 相似文献
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《理化检验(化学分册)》2011,(8)
本汇编共收集了100项钢铁及合金化学分析相关国家标准,内容包括冶金化学分析方法综合、钢铁及合金化学分析方法等。本汇编新增了7项冶金化学分析方法综合部分标准方法,将原钢铁产品分析方法部分更名为钢铁及合金化学分析方法,并废止3项标准方法, 相似文献
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《理化检验(化学分册)》2010,(4)
<正>本汇编共收集了100项钢铁及合金化学分析相关国家标准,内容包括冶金化学分析方法综合、钢铁及合金化学分析方法等。本汇编新增了7项冶金化学分析方法综合部分标准方法,将原钢铁产品分析方法 相似文献
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王冠杰;黄海伟;项新华;张河战;肖镜;田利 《化学分析计量》2015,(5)
摘要：建立气相色谱仪性能验证新方法,为申请 WHO药品预认证提供保障。根据欧洲药品质量管理局《质量控制文件》提供的方法,结合《中国药典》要求,与我国计量检定规程进行对比,总结气相色谱仪性能验证参数要求,建立气相色谱仪性能验证检测方法,并用该方法对 5台气相色谱仪进行检测,结果符合实际。 相似文献
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摘要：为探讨比对法在计量标准考核验证中的可行性,将 5家实验室分别对同一分度吸量管的检定结果进行比对,同时采用具有溯源性的传递比较法进一步验证比对法的可靠性。验证结果显示,采用比对法和传递比较法对被考核实验室的验证结果一致,说明采用比对法对检定结果的验证是有效的、可行的。 相似文献
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《液相色谱法及相关技术杂志》2012,35(4):454-469
A new, simple, and stability indicating thin layer chromatographic (TLC) method has been developed for estimation of norfloxacin. Study was performed on precoated silica gel F254 TLC plate using environmentally safe mobile phase consisting of n-butanol:methanol:ammonia (33%) (8:1:3.5 v/v). A Camag TLC Scanner 3 set at 282 nm was used for direct determination of the chromatograms in the reflectance/absorbance mode. Method was validated according to ICH guidelines. Determination coefficient of the calibration curve was 0.9962 in the range 6–150 ng/band with limit of detection and limit of quantification of 1.01 ng/band and 3.06 ng/band, respectively. Statistical comparison of the results with those of the official HPLC method showed good agreement between the official and the proposed methods with respect to accuracy and precision. Norfloxacin was subjected to forced degradation at 150°C with 2 M HCl or 2 M NaOH, and the degradation rate in both cases was studied. The calculated first order rate constant for the degradation were determined at 0.056 and 0.023 hour−1 and the t1/2 were 12.28 and 30.09 hr for acid and base degradation, respectively. The method has the potential to determine norfloxacin in different dosage forms and in quality control laboratories. 相似文献
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Luke Taylor Lili Sask&#x;y Tara Brodie Vytautas Reme&#x;kevi
ius Hannah Jayne Moir James Barker John Fletcher Baljit Kaur Thatti Gavin Trotter Brian Rooney 《Molecules (Basel, Switzerland)》2022,27(15)
Ethanol is the most commonly used recreational drug worldwide. This study describes the development and validation of a headspace gas chromatography flame ionisation detection (HS-GC-FID) method using dual columns and detectors for simultaneous separation and quantitation. The use of a dual-column, dual-detector HS-GC-FID to quantitate ethanol is a common analytical technique in forensic toxicology; however, most analytical systems utilise pressure-balance injection rather than a simplified gas-tight syringe, as per this technique. This study is the first to develop and validate a technique that meets the specifications of the United Kingdom’s requirements for road traffic toxicology testing using a Shimadzu GC-2014 gas-tight syringe. The calibration ranged from 10 to 400 mg/100 mL, with a target minimum linearity of r2 > 0.999, using tertiary butanol as the internal standard marker. The method has an expanded uncertainty at 99.73% confidence of 3.64% at 80 mg/100 mL, which is the blood alcohol limit for drink driving in England and Wales. In addition, at 200 mg%—the limit at which a custodial sentence may be imposed on the defendant—the expanded uncertainty was 1.95%. For both the 80 mg% and 200 mg% concentrations, no bias was present in the analytical method. This method displays sufficient separation for other alcohols, such as methanol, isopropanol, acetaldehyde, and acetone. The validation of this technique complies with the recommended laboratory guidelines set out by United Kingdom and Ireland Association of Forensic Toxicologists (UKIAFT), the recently issued Laboratory 51 guidelines by the United Kingdom Accreditation Service (UKAS), and the criteria set out by the California Code of Regulations (CCR), 17 CCR § 1220.1. 相似文献
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我国粘度计量工作中存在的问题 总被引：1，自引：0，他引：1
指出我国粘度计量工作中存在的一些问题,在修订粘度计检定规程,规范标准粘度的名称和有效期以及加强对粘度计检定工作的管理等方面的出了建议,强调了在标准粘度液证书中应给出不同温度下的运动粘度和粘度值,以满足粘度计检定工作的需要。 相似文献
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叠加法是由内标法衍生而来的一种气相色谱定量方法。对于较复杂混合物的分析,当选择内标物困难时,用叠加法定量更为方便。本文在大量实验的基础上,提出了叠加法定量过程中应注意的一些问题。 相似文献
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为了加深学生对标准加入法（standard addition methods,SAM）的理解,将其列为“分析化学英文文献选读”选修课的一个专题,在学习资源开放、学习方式开放和学习结果开放的环境下,经过学习阶段、展示阶段和拓展阶段等密不可分的3阶段式问题导引下的主动学习和讨论,获得了有别于目前教科书内容的、鲜活的SAM内容：（1）由目前的2种类型拓展为9种类型的SAM;（2）由目前的外推法SAM拓展为内插法SAM;（3）由目前的容量法SAM拓展为重量法SAM;（4）新近出现的“稀释标准加入校准法”与这里讨论的SAM存在本质差别。在开放的环境下将传统的教学问题与新思路和新应用结合起来是一种行之有效的教学方法。它至少有以下3个优点：（1）以学生已有的知识为切入点,易于学生接受;（2）所选择的材料紧密跟踪分析化学的新进展,可以激发学生的兴趣;（3）课程以专题的形式展开,逻辑线索清晰。 相似文献
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The old debate is revived: Definite differences can be observed in suggestions of estimation for prediction performances of models and for validation variants according to the various scientific disciplines. However, the best and/or recommended practice for the same data set cannot be dependent on the field of usage. Fortunately, there is a method comparison algorithm, which can rank and group the validation variants; its combination with variance analysis will reveal whether the differences are significant or merely the play of random errors. Therefore, three case studies have been selected carefully to reveal similarities and differences in validation variants. The case studies illustrate the different significance of these variants well. In special circumstances, any of the influential factors for validation variants can exert significant influence on evaluation by sums of (absolute) ranking differences (SRDs): stratified (contiguous block) or repeated Monte Carlo resampling and how many times the data set is split (5‐7‐10). The optimal validation variant should be determined individually again and again. A random resampling with sevenfold cross‐validations seems to be a good compromise to diminish the bias and variance alike. If the data structure is unknown, a randomization of rows is suggested before SRD analysis. On the other hand, the differences in classifiers, validation schemes, and models proved to be always significant, and even subtle differences can be detected reliably using SRD and analysis of variance (ANOVA). 相似文献