Reference material experimental techniques

In many analyses, fhe compound(s) of inferesf are found as par of a complex mixfure and fhe role of fhe chromatographic technique is to provide separation of fhe components of that mixture to allow their identification or quantitative determination. From a qualitative perspective, the main limitation of chromatography in isolation is its inability to provide an unequivocal identification of the components of a mixture even if they can be completely separated from each other. Identification is based on the comparison of the retention characteristics, simplistically the retention time, of an unknown with those of reference materials determined under identical experimental conditions. There are, however, so many compounds in existence that even if the retention characteristics of an unknown and a reference material are, within the limits of experimental error, identical, the analyst cannot say with absolute certainty that the two compounds are the same. Despite a range of chromatographic conditions being available to the analyst, it is not always possible to effect complete separation of all of the components of a mixture and this may prevent the precise and accurate quantitative determination of the analyte(s) of interest. 

As usually viewed by the reference material producers, a fundamental philosophy of certification rests on the concept of independent methodology, which is the application of theoretically and experimentally different measurement techniques and procedures to generate concordant results leading to one reliable assigned value for the property. Such assigned values are thus method-independent. Extractable concentrations are generated by specific procedures and are thus method-dependent, an idea that has to be rationalized with the fundamental method-independent concept in reference material certification work. 

In the simplest case, experimental calibration can be carried out by direct reference measurements where the sensitivity factor b is given by the relation of measured value to concentration of a reference material (RM), b = yRvi/xRv,. Direct reference calibration is frequently used in NAA and X-ray analytical techniques (XRF, EPMA, TXRF). 

Certified reference materials (CRMs) are mainly applied to validate the analytical procedure developed for routine analysis in order to determine the accuracy of analytical data, the recovery for selected elements, the uncertainty of trace element determination and the detection limits. Otherwise, in solid-state mass spectrometric techniques, such as SSMS, LA-ICP-MS, GDMS, SNMS or SIMS, one point calibration using CRMs has been established as an important calibration strategy to obtain reliable analytical data. The one point calibration is performed using the experimentally determined relative sensitivity coefficients (RSCs) on a suitable CRM with a similar trace/matrix composition. An RSC of a chemical element is defined as the ratio of the measured element concentration (experimentally determined) divided by the certified element concentration (accepted or recommended value of element concentration) in a given matrix. 

The study of these systems have become possible thanks to the development of various preparation routes, from sophisticated routes for the preparation of model materials with controlled nanostructures to industrial routes for the production of large quantity of materials. It has benefited as well from the development of new experimental techniques, allowing the properties of matter to be quantitatively examined at the nanometre scale. These include Hall micro-probe [3] or micro-SQUID magnetometry [4], XMCD at synchrotron radiation facilities [5] and scanning probe microscopes [6]. This is not the topic of this chapter to describe in detail these various techniques. They are only quoted in the following sections. The reader may find in the associated references the detailed technical descriptions that he may need. 

This statement refers directly to the concept of the potential energy function describing interaction energy as a function of the distance sufficient to model various properties of matter that are directly or indirectly related to the intermolecular forces. Recent progress in computational and experimental techniques opens the perspective for rational de novo design of new materials with desired properties being governed by specific interactions. 

The determination of atomic weights has been preeminent in the study of the reliability of analytical methods and in the definition and development of reference materials. In the history of chemistry no significant problem has been under more continuous investigation than that of atomic weights. Determinations of atomic weights by chemical methods require highly refined experimental techniques, and only a few... 

Fourier transform infrared spectrophotometry is used widely in the semiconductor industry for the routine determination of the interstitial oxygen content of production silicon wafers. However, the lack of interlaboratory reproducibility in this method has forced the use of ad-hoc calibration methods. The sources of this lack of reproducibility are just beginning to be understood. As investigation of this problem continues and wider acceptance is gained for improved experimental and analytical techniques, a greater degree of reproducibility should be achieved. Furthermore, new standard test methods and standard reference materials being developed by the ASTM (71 ),... 

This section deals with mechanisms of electrostatic charging and charge relaxation in powders and with the important variables, such as powder size, quantity, temperature, humidity, etc., which affect these phenomena. Also considered are experimental techniques for investigating the electrostatic characteristics of sensitive materials, with particular reference to lead azide. Finally, the application of such information to the safe handling of sensitive substances is discussed. 

Contemporaneously, the Joint Research Centre established the METRE Programme (Mesures, Etalons et Techniques de Reference) in 1972 in support of its experimental activities. Both BCR and METRE focused, at the beginning, on industrial reference materials such as cokes and non-ferrous metal ores, but in 1973 METRE started with... 

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