New tools: Uncertainty-based data evaluation

 The principles of uncertainty-based data evaluation are explained. Based on a brief review of recent publications on the topic, examples for application to standard procedures in analytical chemistry – calibration, method validation, standard addition etc., – are given. The performance and the advantages of uncertainty-based data evaluation are discussed. Received: 4 July 1998 · Accepted: 6 July 1998     

Temperature measurement and control

Several factors in temperature measurement that can affect the precision of melting points and phase-change phenomena are discussed. In many cases, critical errors may arise in the measurement and control of temperatures due to incorrect placement and/or interpretation of the output of temperature sensors in the various system types that are in current use. Advantages can be obtained by using one temperature sensor only for temperature measurement and temperature control in a low mass infrared gold image fumace for the analytical studies in both the constant rate and stepwise isothermal thermoanalytical heating and cooling modes. Illustrations of the use of this instrumentation for measurements in both modes are given.     

C2-C8 hydrocarbon measurement and quality control procedures at the Global Atmosphere Watch Observatory Hohenpeissenberg

A new automated on-line GC-flame ionization detection system for long-term stationary measurements of atmospheric C2-C8 hydrocarbons in the lower ppt range is described. The system is operated at the Global Atmosphere Watch Observatory Hohenpeissenberg (47 degrees 48'N, 11 degrees 01'E) in rural south Germany. Atmospheric mixing ratios of more than 40 different hydrocarbons can be continuously measured in 80 min time intervals. Corresponding detection limits are below 3 ppt, except for propene, butenes and benzene (about 10 ppt). Detailed quality assurance and quality control protocols are described which are applied to routine operation and data analysis. The various error contributions, overall precision, and accuracy for all measured compounds are discussed in detail. Typical ambient air mixing ratios are in the range of a few ppt to a few ppb, and corresponding measurement accuracies are below 10% or 10 ppt. For less than 20% of the analyzed compounds measurement accuracies are worse, mainly because of insufficient peak separation, blank values or reduced reproducibilities. The present system was tested in international intercomparison experiments (NOMHICE, AMOHA). For most of the C2-C8 hydrocarbons analyzed, our results agreed better than +/- 10% (20% NOMHICE phase 5) or +/- 10 ppt with the corresponding reference values.     

Thermoplastic polymers quality control

A technique is proposed for improving the accuracy of the heat of fusion of semicrystalline polymers by DSC. The results of three commercially available instruments are compared.     

A proficiency test scheme for the quality control of black tea and development of quality control material for internal quality control

A proficiency test (PT) was organized for quality control analysis of black tea. Test materials for the analyses of total content of powder tea, moisture, total ash, acid-insoluble ash, water-soluble ash, alkalinity of water-soluble ash, water extract, crude fiber and caffeine were sent to the participant laboratories (n:43) in 2009. The assigned value, standard deviation of the parameters and z-scores of the participant laboratories were calculated using the data reported by the participants. The percentage of the reported results for analytes was found to be ranged from 67.5 to 100%. Acceptable z-scores were achieved by 80.5–97.5% of the participant laboratories. More than 15% of unacceptable results were obtained for acid-insoluble ash and caffeine analyses. The quality control material for quality control analysis of black tea was developed from the remaining material.     

A journey through quality control

The Euroanalysis VII conference in Vienna included a two-day session: Quality Assurance in Analytical Chemistry. The contributions comprised 15 lectures devoted to: intra-laboratory quality measures, inter-laboratory control, formal aspects and accreditation and implementation. The paper presents an overview of the main items developed by the contributors.A survey on the session on Quality Assurance in Analytical Chemistry of Euroanalysis VIIThe authors thank the organizers of EUROANALYSIS VII and in particular Dr. B. Griepink and Dr. E. Maier of the Community Bureau of Reference (BCR) of the CEC for their support and considerable contributions.     

Chemometric quality control of chromatographic purity

It is common practice in chromatographic purity analysis of pharmaceutical manufacturing processes to assess the quality of peak integration combined by visual investigation of the chromatogram. This traditional method of visual chromatographic comparison is simple, but is very subjective, laborious and seldom very quantitative. For high-purity drugs it would be particularly difficult to detect the occurrence of an unknown impurity co-eluting with the target compound, which is present in excess compared to any impurity. We hypothesize that this can be achieved through Multivariate Statistical Process Control (MSPC) based on principal component analysis (PCA) modeling. In order to obtain the lowest detection limit, different chromatographic data preprocessing methods such as time alignment, baseline correction and scaling are applied. Historical high performance liquid chromatography (HPLC) chromatograms from a biopharmaceutical in-process analysis are used to build a normal operation condition (NOC) PCA model. Chromatograms added simulated 0.1% impurities with varied resolutions are exposed to the NOC model and monitored with MSPC charts. This study demonstrates that MSPC based on PCA applied on chromatographic purity analysis is a powerful tool for monitoring subtle changes in the chromatographic pattern, providing clear diagnostics of subtly deviating chromatograms. The procedure described in this study can be implemented and operated as the HPLC analysis runs according to the process analytical technology (PAT) concept aiming for real-time release.     

Key requirements for introducing quality assurance in measurement laboratories

 The implementation of a quality assurance system is fraught with difficulties. However, these difficulties may be overcome if the laboratory uses suitable means to facilitate the process. It is necessary to mobilise the intelligence and energy of all members of the laboratory. In order to command adherence, the project must be shared, and this necessitates a major effort by all concerned. Communication is a major factor in obtaining the support of all parties. Six important steps must be distinguished: – Defining quality policy – Creating awareness, information, training – Creating a quality structure – Establishing a deadline for obtaining accreditation – Progressive implementation – Experimentation and validation. Even if the task of obtaining and maintaining accreditation remains difficult, it clearly promotes a minimum level of organisation and stepwise progress in quality assurance. The laboratory must keep improving its quality system, using European Standard EN 45001 as an effective management model. Received: 9 April 1997 · Accepted: 11 September 1997     

Radiochemical quality control of99mTc-phytate

Several chromatographic methods have been used for determining the radiochemical purity of^99mTc-phytate. Good separation of^99mTc-phytate from radiochemical impurities was performed using gel column chromatography packed with Sephadex G-10. Reduced^99mTc-complexes and^99mTc-phytate were not separated by paper and thin layer chromatography.This work has been presented at the Fifth International Symposium on Radiopharmaceutical Chemistry, Tokyo, July 9–12, 1984.     

Automated quality control by IR spectroscopy

IR spectroscopy is widely used for quality control of materials in industrial laboratories, with an increasing demand for procedures that are fast and can be carried out by unskilled personnel. PECDS II is a high level programming language designed to provide a high degree of flexibility in manipulating spectroscopic data.     

Chemical measurement and the law: metrology and quality issues

To facilitate just and sound decisions legal measurements must be reliable. The aim of this paper is to explore how this is currently achieved and how it might be better done. It considers the different types of legal proceedings, the role of chemical measurement, level of proof, the different types of chemical measurement, measurement units, the role of government, the chemical measurement industry and its control, legal metrology and the development of a measurement system based on metrological principles. It is argued that recent developments provide the basis for a robust support system, that but more needs to be done. It is also argued that the conventional approach to legal metrology has little place in chemical measurement, but that some controls are needed in some areas. In particular, a harmonised approach to international measurement standards is advocated. Received: 29 December 2000 Accepted: 8 January 2001     

The use of internal quality control materials for the preparation and maintenance of reliable methods for the measurement of lead in blood

Summary The performance of a group of reference laboratories measuring lead in blood, has been monitored by an intensive external quality assessment programme, since 1974. Performance was similar to that observed in other, larger quality control surveys but rapidly improved following detailed investigations of critical factors in the analytical methodology. The introduction of a rigorous internal quality control protocol, with all laboratories using the same well-characterised materials, has produced external quality control results that are both accurate and very tightly distributed. Between-laboratory coefficients of variation of less than 5%, less than 6% and less than 20% are now obtained at concentrations of over 1.0 mol/l (20.7 g/dl), 0.5–1.0 mol/l (10–20 g/dl) and less than 0.5 umol/l (10 g/dl), respectively. These results represent the best that can be achieved by current methodology and instrumentation in regular, daily use.

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Verwendung interner Qualitätskontrollmaterialien für die Erarbeitung und Anwendung zuverlässiger Methoden zur Messung von Blei in Blut

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Presented on behalf of the Trace Elements Sub-group of the Supraregional Assay Service (SAS) of the UK National Health Service     

Internal quality control in forensic DNA analysis

The trail from initial evidence examination to a DNA profile reported to match a suspect is long and complex. The different nature and great variability in the biological and DNA evidence to be recovered and analyzed, add to this complexity. Internal quality controls play an important role in maintaining a high-quality performance in daily forensic biology and DNA profiling practice. In many cases are empirical rather than analytical approaches adopted. Obviously, despite the fact of being necessary, the internal quality controls performed still need to be kept rational at a limited, yet acceptable level. Quality control from a forensic biology and DNA profiling horizon has a wider context and does not only concern obvious fit-for-purpose verifications of analytical processes, chemicals, or reagents in daily routine practice. It also includes control on computerized laboratory management and expert systems, laboratory environmental DNA monitoring, and the use of elimination DNA databases. In addition, a structured recording and handling of non-conformances and “near failures” is essential. Proper management of the non-conformances supports continuous quality improvements by learning from the errors occurring in daily practice. High transparency of non-conformances is important not only for internal improvements, but also for the criminal justice system as well as to maintain public confidence and trust. Together the quality controls used aim at maintaining evidence and DNA sample integrity and to accomplish correct results and interpretations by verifying that methods used data transfers and interpretations made are correct and performed according to validated and accredited conditions.     

Radiochemical quality control of67Ga-citrate radiopharmaceuticals

A rapid, miniaturized chromatography system has been developed to determine the possible contaminants of⁶⁷Ga-citrate. This method is simple, inexpensive and suitable for laboratory routine tests. By classical paper chromatography the analysis takes several hours to complete.