The purity of laboratory chemicals with regard to measurement uncertainty.
ABSTRACT The purity P of laboratory chemicals is often declared in the form P > or = xy% (e.g., P > or = 97%). With a randomly chosen set of 40 compounds we found that their purity is generally closer to 100% than to the lower limit. The distribution of the purity data as found in the laboratory depends on the analytical technique used. Whereas purities determined by chromatography do not exceed 100% (because the sum of all observed peak areas is set to 100%), the purities obtained by titration can exceed 100% (because the functionality of the compound is measured). Therefore, the data for these two groups need to be dealt with in different ways. For purities based on titration we propose to use a rectangular distribution with a range from Pmin to 101%, an expected purity value which is the mean and a standard uncertainty of the purity u(P) of 29% of the range. Purities determined by chromatography can be described with a triangular distribution (ramp function). One leg of the triangle represents the range from Pmin to 100% and the right-angle is located at 100%. The expected value is the median and the uncertainty u(P) is 24% of the range. These proposals match the experimental data well.
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ABSTRACT: In this study the validity and suitability of differential scanning calorimetry (DSC) to determine the purity of selected polycyclic aromatic hydrocarbons and chloramphenicol has been investigated. The study materials were two candidate certified reference materials (CRMs), 6-methylchrysene and benzo[a]pyrene, and two different batches of commercially available highly pure chloramphenicol. The DSC results were compared with those obtained by other methods, namely gas and liquid chromatography with mass spectrometric detection, liquid chromatography with diode array detection, and quantitative nuclear magnetic resonance. The purity results obtained by these different analytical methods confirm the well-known challenges of comparing results of different method-defined measurands. In comparison with other methods, DSC has a much narrower working range. This limits the applicability of DSC as purity determination method, for instance during the assignment of the purity value of a CRM. Nevertheless, this study showed that DSC can be a powerful technique to detect impurities that are structurally very similar to the main purity component. From this point of view, and because of its good repeatability, DSC can be considered as a valuable technique to investigate the homogeneity and stability of candidate purity CRMs.Thermochimica Acta - THERMOCHIM ACTA. 01/2011; 524(1):1-6.
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ABSTRACT: Concern that human impacts on the environment may be harmful to natural resources such as soils as well as to living conditions is the major motivation for long-term environmental monitoring. However, the evidence that measurement bias is not constant through time affects time series as an artifact; this also holds true for chemical soil monitoring. Measurement instabilities occur along the whole measurement chain, from soil sampling to the expression of results. The first step in controlling measurement instability is to identify its relevant sources, and the second is to control it by stabilizing, minimizing, or quantifying measurement instability. For all five steps in the measurement process, from soil sampling to the expression of the analytical results, sources of measurement instability are identified and measures of control discussed, leading to the main conclusion concerning the requirement to continuously control the relevant environmental and measurement boundary conditions that may affect measurement instability. The innovative aspect of this paper consists in explicitly addressing measurement instability in chemical soil monitoring and tracking it along the whole measurement chain. The paper is also a plea for a change of paradigm in long-term environmental monitoring, namely to consider temporal measurements as unstable unless their degree of stability is traceably demonstrated, adequately quantified, and included in interpretation.Environmental Monitoring and Assessment 03/2011; 184(1):487-502. · 1.68 Impact Factor
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ABSTRACT: Quantitative chromatographic analyses do not belong to the class of primary methods, but the analyst needs to calibrate the obtained signals with well-known solutions made of high-purity reference materials. Every analyte, to be quantified by a non-primary method, needs the chemically identical compound as its reference. It is not necessary that the content of the reference is 100.0%, but it is crucial that its purity is known, together with the uncertainty of this value (e.g., 99.9±0.05%). Any high-quality analytical result should include information about the associated measurement uncertainty, and the purity uncertainty of the reference is a parameter which always appears in the overall measurement uncertainty calculation of the measurand (such as the concentration or content of an analyte). Our general postulation is that the purity and the uncertainty of all reference materials must be known. It concerns all types of reference materials although we focus our discussion on the analysis of drug products. Unfortunately, at present only a few pharmaceutical reference materials are commercially available from regulatory bodies with a certificate confirming their purity with the related uncertainty. In contrast, such well-characterized materials, traceable to the International System of Units (SI), are available from various commercial suppliers.Journal of pharmaceutical and biomedical analysis 01/2013; 77C:40-43. · 2.45 Impact Factor