Industrial Analytes

QUALITY MANAGEMENT IN THE INDUSTRIAL ANALYTICAL LABORATORY - DO WE GET OUR MONEY S WORTH ... 

Due to their wide range of analytical challenges centralized analytical laboratories are required to adopt a series of QM systems simultaneously. For example, the Competence Center Analytics of BASF AG in Ludwigshafen is certified and accredited to operate under four different QM systems. Undoubtedly, QM systems play a vital role in a modern industrial analytical laboratory. The sale of many products of the chemical industry is not possible without a GLP-certified analytical laboratory. However, in practical tenus the different QM systems can potentially reduce the efficiency of the analytical process and lead to increased costs. 

X-ray fluorescence (XRF) analysis is successfully used to determine chemical composition of various geological and ecological materials. It is known that XRF analysis has a high productivity, acceptable accuracy of results, developed theory and industrial analytical equipment sets. Therefore the complex methods of XRF analysis have to be constituent part of basis data used in ecological and geochemical investigations... 

It is important to understand that this material will not be presented in a theoretical vacuum. Instead, it will be presented in a particular context, consistent with the majority of the author s experience, namely the development of calibrations in an industrial setting. We will focus on working with the types of data, noise, nonlinearities, and other sources of error, as well as the requirements for accuracy, reliability, and robustness typically encountered in industrial analytical laboratories and process analyzers. Since some of the advantages, tradeoffs, and limitations of these methods can be data and/or application dependent, the guidance In this book may sometimes differ from the guidance offered in the general literature. 

Of the various methods of data presentation, the one with which starting analysts may be least familiar is trend analysis and statistical quality control. In an industrial environment, analysis is often centered around the production of batches of material. The properties of those batches may change over time due to random effects or to subtle changes in the production process. In either case, the quality of the product may change. Analysis is used to track the change in the properties of batches over time. Industrial analytical methods, therefore, need to be extremely rugged. Millions of dollars may depend on the analyst s judgment as to batch equivalence. 

Swadesh, J. K. and Kasouf, C. J., Industrial analytical operations organizational implications of automation, Crit. Rev. Analyt. Chem., 25, 195, 1995. 

Industrial analytical laboratories search for methodologies that allow high quality analysis with enhanced sensitivity, short overall analysis times through significant reductions in sample preparation, reduced cost per analysis through fewer man-hours per sample, reduced solvent usage and disposal costs, and minimisation of errors due to analyte loss and contamination during evaporation. The experience and criticism of analysts influence the economical aspects of analysis methods very substantially. 

Applications The broad industrial analytical applicability of microwave heating was mentioned before (see Section 3.4.4.2). The chemical industry requires extractions of additives (antioxidants, colorants, and slip agents) from plastic resins or vulcanised products. So far there have been relatively few publications on microwave-assisted solvent extraction from polymers (Table 3.5). As may be seen from Tables 3.27 and 3.28, most MAE work has concerned polyolefins. 

Polymer/additive analysis is a typical industrial analytical problem, and indeed not one of the easiest or least important ones. Requirements set to industrial analytical expertise vary from new analytical approaches for product innovation, to service-oriented problem solving (combination of analytical expertise and specific product knowledge), and cost-efficient analysis of a few grades (plant service) (Scheme 10.1). Reported prospects set the instrumental trends in the polymer industry (Table 10.17). For traditional quality laboratories this translates into ... 

Today s analytical methods are generally sufficiently selective and sensitive, but industrial analytical chemists are faced with changes in analytical demands ... 

Various analytical methods have made quantum leaps in the last decade, not least on account of superior computing facilities which have revolutionised both data acquisition and data evaluation. Major developments have centred around mass spectrometry (as an ensemble of techniques), which now has become a staple tool in polymer/additive analysis, as illustrated in Chapters 6 and 7 and Section 8.5. The impact of mass spectrometry on polymer/additive analysis in 1990 was quite insignificant [100], but meanwhile this situation has changed completely. Initially, mass spectrometrists have driven the application of MS to polymer/additive analysis. With the recent, user-friendly mass spectrometers, additive specialists may do the job and run LC-PB-MS or LC-API-MS. The constant drive in industry to increase speed will undoubtedly continuously stimulate industrial analytical scientists to improve their mass-spectrometric methods. 

See Selectivity, above, and Table 21.9. Industrial problems usually generate samples with complex matrices and many potential interferences. Selective analytical methods or sample preparation are normally required. Separation techniques are quite commonly used. In the average industrial analytical lab, the most numerous instruments are usually gas or liquid chromatographs because they combine separation with detection. 

Both hand washing and machine washing and drying procedures are in use in industrial analytical laboratories. The variety of available soaps include alkaline phosphate-based and phosphate-free soaps. While phosphate-based soaps are quite satisfactory for cleaning purposes because phosphate helps to... 

In the food industry analytical methods can be divided into two classes ... 

Guidance for Industry, Analytical Procedures and Method Validation Chemistry, Manufacturing and Controls Documentation, Draft, August 2000, Center for Drug Evaluation and Research, Center for Biologies Evaluation and Research, FDA, Department of Health and Human Services, 2000. 

Guidance for Industry Analytical Procedures and Methods Validation, FDA, November 1994 (http //www.fda.gov). 

Guidance for Industry, Analytical Procedures and Methods Validation, Chemistry Manufacturing and Controls Documentation, Draft Guidance, FDA, August 2000. 

This work is intended to be, as the title implies, a brief introduction to the principles of quality that are important for workers in a modem industrial analytical chemistry laboratory. It is intended to be a textbook for students preparing to become technicians or chemists in the chemical process industry. It is intended to be a quick reference for new employees in an industrial laboratory as they begin to learn the intricacies of regulations and company policies relating to quality and quality assurance. It is also intended for experienced laboratory analysts who need a readable and digestible introductory guide to issues of quality, statistics, quality assurance, and regulations. 

Cleansing-Agent and Personal-Care Industries Pharmaceutical Industry Animal-Feed Industry Analytical Applications... 

U.S. Food and Drug Administration (FDA) (2000), Guidance for industry, Analytical procedures and methods validation—Chemistry, manufacturing, and controls documentation, FDA, Rockville, MD. 

Analytical methods validation is one of the most regulated validation processes in the pharmaceutical industry. Analytical validations are required to demonstrate that the methods employed are the most indicated for each product and that the results obtained are reliably correct. All methods employed in raw and finished product materials analysis are required to be validated. 

Although industrial laboratories shied away from the technique at first, CE is now becoming more common in these labs for a variety of analyses, including ion analysis, chiral pharmaceutical analysis, and peptide mapping [1]. With the increased prevalence of CE in industrial analytical laboratories comes the need for instrument qualification to ensure the proper functioning and performance of the instrument in order to obtain consistent, reliable, and accurate data. 

The practice in many industrial analytical service laboratories is to present the analytical chemist with samples and some form of written request for analysis. Often discrepancies occur between expected values and those obtained by analysis and the blame for this is often placed on the analytical chemist. In many cases little or no thought is given to the sampling or handling of the material prior to submission for analysis. The analytical chemist is well advised to enquire into the history of samples and where possible to maintain some form of control over sampling, sample handling and storage. 

Infrared spectroscopy is now nearly 100 years old, Raman spectroscopy more than 60. These methods provide us with complementary images of molecular vibrations Vibrations which modulate the molecular dipole moment are visible in the infrared spectrum, while those which modulate the polarizability appear in the Raman spectrum. Other vibrations may be forbidden, silent , in both spectra. It is therefore appropriate to evaluate infrared and Raman spectra jointly. Ideally, both techniques should be available in a well-equipped analytical laboratory. However, infrared and Raman spectroscopy have developed separately. Infrared spectroscopy became the work-horse of vibrational spectroscopy in industrial analytical laboratories as well as in research institutes, whereas Raman spectroscopy up until recently was essentially restricted to academic purposes. 

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