Analytical methods standardised

With so many variations in methodology in the literature, some sort of standardisation of analytical methods is necessary. One study of standardisation... 

For standardised instrumental analytical methods, i.e. biomarkers, biosensors and bioassays, there are well-established standard protocols on the national level, e.g. under Association Francaise de Normalisation (AFNOR), British Standard Institute (BSI), DIN (German Organisation for Standardisation), etc., and all those standards are formed by ISO-Working Groups and by validation studies into ISO - and CEN - Standards. Normal accredited and well-qualified laboratories should be able to perform the monitoring. 

In 1935, the Committee was renamed the Analytical Methods Committee (AMC) but the main analytical work was carried out by sub-committees composed of analysts with specialised knowledge of the particular application area. The earliest topics selected for study were milk products, essential oils, soap and the determination of metals in food colourants. Later applications included the determination of fluorine, crude fibre, total solids in tomato products, trade effluents and trace elements, and vitamins in animal feeding stuffs. These later topics led to the publication of standard methods in a separate booklet. All standard and recommended methods were collated and published in a volume entitled Bibliography of Standard, Tentative and Recommended or Recognised Methods of Analysis in 1951. This bibliography was expanded to include full details of the method under the title Official, Standardised and Recommended Methods of Analysis in 1976 with a second edition in 1983 and a third edition in 1994. 

The Analytical Methods Committee s own compilation of official and standardised methods of analysis is widely used and respected within the analytical community. The importance of standardised formats for method documentation has been emphasised by the AMC s guidelines for achieving quality in trace analysis. They list 17 headings for inclusion in the documentation ... 

Atomic absorption analysis made available to the routine laboratory an analytical technique which initially was intended to produce considerable simplification of procedures for the analysis of aqueous, acidic or basic solutions, and thereby contribute to a reduction in costs. Numerous reviews show the worldwide application of this technique [15, 40, 77, 126—129, 137]. Nevertheless, some 10 years passed before atomic absorption became part of the international standardisation of analytical methods. At present, there are many standard methods being developed on the basis of atomic absorption [35, 67], Some, dealing with the determination of metals in lubricating oils, are already in use [35, 66], although the overwhelming majority, for example those dealing with the analysis of iron ores [67], are still being developed. The first indication of standardisation of atomic absorption methods for iron and steel analysis was seen in 1973 [8]. 

To support the analyst in applying such controls, CEN (the European Standardisation Commission) has in TC 194 adopted and validated analytical methods for the determination of the overall migration and the migration of some specific substances. These methods are intended to be applied for testing plashc materials and articles. At national level, e.g., in The Netherlands, the methods and simulants may also be used to demonstrate compliance with national regulation of non-plastic or multilayer materials composed of plastics and non-plastics (e.g. plastic on paper, coating on metal). 

European Committee for Standardisation, CEN (1999) Food analysis— biotoxins—criteria of analytical methods for mycotoxins, Report Reference no. CR 13505 1999E... 

In accordance with Article 7a of the WHG, the AbwV (Ordinance on Requirements for the Discharge of Wastewater into Waters - Wastewater Ordinance) has been divided into a general framework section, an annex (to Article 4) with analytical methods for parameter determination and sector-specific appendices, including requirements for 53 wastewater sectors [3], Minimum requirements to be stipulated when granting a permit to discharge wastewater are described, analysis and measurement techniques are specified in the annex and sector-specific requirements in the appendices refer to the analysis and measurement techniques specified in the annex. Article 4 of the AbwV, in conjunction with the annex, lists the analysis and measurement procedures that are to be used to determine the parameters defined in the appendices. Paragraph 2 emphasises that for individual cases other equivalent procedures may be required if compliance with the requirements specified in the ordinance is to be ensured [9]. All analysis and determination procedures are standardised methods (DIN, CEN, ISO). 

Chemical analysis always involves the use of different chemicals. In order to assure accurate analysis results, the chemicals used need to he standardised, the procedures must he followed exactly and the data obtained have to he analysed statistically. If an instrument is used, it should be maintained and calibrated properly. A detailed description of analytical chemistry is not the purpose of this book. Readers can refer to analytical chemistry books in the literature. During the last five decades, sophisticated instruments in the market have made chemical analysis much easier than before. However, the price of the instruments plus high operation costs have limited their applications in many textile businesses. Therefore, the analytical methods discussed in this chapter are mainly those of traditional wet chemistry based analyses. 

Advisory Committee on Business and the Environment American Chemistry Council Association of Chartered Certified Accountants adsorbable organic halogen compounds (X = any halogen that can be identified by standardised analytical methods)... 

According to the procedure proposed. Member States were extensively consulted during 2006 for revision of CEN biologic standard methods (Table 1.3.6) for their relevance in the context of the WFD and to identify priority areas for future standardisation activities. It became apparent from this process that sampling and quality assurance methods are mostly needed at community level, and also that published standard methods often do not take into account water category type-specific features, as is required in the Directive. This consultation process enabled the identification of a number of candidate sampling and analytical methods fulfilling short-tenn standardisation needs for lakes, rivers and coastal waters. 

Visual inspection is a classical example of quality by attributes , where the batch is compared with a standard , which can be a quality perfect example of the component or a quality check list. It should be noted that the physical senses of smell and taste, where safe, are often more sensitive than many sophisticated analytical methods, but equally require validation and standardisation. 

Over the last few years, the measurement methodology of the nutritional value of feedstuffs has been the topic of concerted studies at the European level, with particular emphasis on the standardisation of in vivo methods (Perez et o/., 1995a) and on the harmonisation of analytical methods for feeds and faeces (EGRAN, 2001). This resulted in the adoption of a European reference method to determine the digestibility of diets (Perez et al., 1995b) and in the harmonisation of the procedures used to calculate the nutritional value of feed materials within mixtures of feedstuffs (Villamide et al., 2001). 

For reproducible analyses and reliable control of polycyclic aromatic hydrocarbons (PAH) and related heterocyclic compounds, the availability of standardised analytical procedures is essential. When national or international regulations are issued or developed, standardised analytical methods are usually mandatory. 

To ensure full comparability of results, all the various steps which are involved in the analytical procedures (sampling, sample extraction, enrichment, clean-up, analytical method and data presentation) should be considered in harmonisation and standardisation discussions. 

Originally, when the need for harmonisation and standardisation of analytical methods in response to international regulations arose, TLC was the preferred choice since GC and HPLC were neither fully developed nor universally available. 

Thus, a broad range of sometimes complementary analytical techniques is available at present for the characterisation of the various PAH/POM emissions. For standardisation purposes, candidate methods must be tested extensively in a collaborative exercise to determine and evaluate repeatability, reproducibility and recovery criteria before final definition and approval. (Recently, the method detection limit, defined as the concentration which can be detected at a specific confidence level, was proposed as one criterion for assessing the performance of an analytical method (18)). 

With improved analytical methods there has been a large increase in the number of compounds identified in wines. Volatile compounds from different families (such as alcohols, esters, aldehydes, terpenes, etc.) play an important role in the organoleptic characteristics of wines. This wide variety of compwimds with different chemical properties and with different concentrations makes the flavour pa-ofile of wines very complex. Therefore, it is necessary to standardise the terminology so as to facilitate the knowledge of the aromatic profile of wines. 

The aim of these standards was to improve analytical methods placing the emphasis on the use of standardised procedures to determine concentrations of micro-organisms within production facilities. It was believed that such standardisation would raise the level of health inspection and make it possible to compare and analyse working conditions in the (biotechnology) sector as a whole and at individual enterprises that use either different or identical technologies and process instrumentation . ... 

In an overview, the permeability of gloves to several cytostatic drugs was presented by Mellstrom et al. (1996). However, the procedures used were not standardised methods and the analytical methods, equipment and sensitivity vary tremendously therefore, the test results are difficult to evaluate and compare. 

Borke et al. [31] ( chromatostrip technique [104]) and Mariani and Mariaiu-Marelli [129] in their studies of opium alkaloids, were the first to draw attention to the advantages of TLC over other analytical methods, including PC. The method really developed only after Stahl [227] had introduced standardised conditions and apparatus for separation in 1956. 

Before any technique can be fully accepted it must be possible for analysts anywhere to carry out the same method and get identical results. Unfortunately, at present this is not always being implemented. However, the current trend towards globalisation in the chemical industry is stimulating method validation. Standardisation of analytical methods... 

In particular in the industrial environment, where most in-poIymer analyses are being carried out, analyst time needs to be minimised. To this extent, autosamplers, robots, fast analysis techniques (e.g. ASE , fast GC), hyphenation and standardised data output formats for further manipulation and transmission are wanted. Automation is advantageous (Table 8.4). Ideally, the whole process may be automated analysis, data reduction and output. Unfortunately, standardisation of data handling procedures is still far off. This determines continuous, multiple efforts for training of analysts. Analytical methods should also be easy to maintain caUbra-tion should be required at minimal levels. Sample preparation should minimise time, effort, materials and volume of sample consumed. Sample pretreatment is ideally superfluous. There should also be little inherent doubt on the representativity of the analysis (of special concern for those techniques employing minimal sample amounts 0.1-1 fj,g). The method should be able to qualitatively identify the specific analyte(s) of interest, on the basis of expected behaviour (e.g. retention time, colour... 

As many oils, other than those included in the official publications, are met with in pharmaceutical practice, the most useful chemical methods of analysis are given briefly below. The Analytical Methods Committee of the S,A,C, (referred to below as the S,A,C,) has carried out a considerable amount of useful work on standardisation of methods for the analysis of essential oils, and many of its recommendations have been embodied in the official monographs. 

At around the same time, much of the rest of the world was putting together regional or local performance-based method standardisation i.e. statistical performance characteristics were specified instead of analytical techniques. 

Method type and code Analytes Samples Standardisation body... 

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