Preparation and certification of the new polish CRM: fine fly ash (CTA-FFA-1)

Abstract

About 60 kg of fine fly ash was collected from the third zone of electrofilters from the "Kozienice" power station. The material has a density of 2.53 gþcm-3 at a very fine mesh size (93% passed through the 0.06 mm sieve). The material was rotated for 16 h in a 110 L polyethylene (PE) drum placed in a specially constructed mixing device. Preliminary homogeneity checking was done by taking the samples from the drum at certain time intervals and analyzing them by XRF for their Y and Fe contents. After apportioning the material into PE containers, final homogeneity checking was performed by instrumental neutron activation analysis. Determination of Fe, Co, Cr, Cs, Sc, and Th in subsamples from six containers chosen at random, with analogous results for subsamples taken from a single container, revealed that the material can be considered homogeneous, at least for a sample size greater than or equal to 200 mg. An international intercomparison brought together nearly 60 laboratories from 19 countries employing a variety of analytical techniques as: neutron activation analysis (NAA), atomic absorption spectrometry (AAS), atomic emission spectrometry (AES), X-ray fluorescence (XRF), mass spectrometry (MS), and others, with or without sample pretreatment and preconcentration or separation procedures. In total, about 3900 pieces of chemical data (over 950 laboratory means) on 65 elements were provided by participating laboratories. Evaluation of results was done by the method previously proposed by one of us with some recent refinements. The procedure included the calculation of laboratory means, the use of four concurrent tests for outlier rejection (Dixon's, Grubbs's coefficient of skewness and coefficient of kurtosis), calculation of the overall mean and its confidence interval etc. Using a set of appropriate criteria formulated earlier with some recent modifications it was found that it will be possible to certify at least 30 elements and provide "information values" for at least a further ten. Observations on the performance of various analytical techniques and their contribution to the certification process are also presented.

Performance and frequency of use of NAA and other techniques during the certification of two new Polish CMRs prepared by INCT

“…In the years: 1987-1994 the following CRMs were issued: geological and environmental materials, i.e., Apatite Concentrate (CTA-AC-1) [8,9] and Fine Fly Ash (CTA-FFA-1) [8,9] as well as biological materials: Oriental Tobacco Leaves (CTA-OTL-1) [9,10] and Virginia Tobacco Leaves (CTA-VTL-2) [11,12], the latter being also recommended for microchemical techniques. These and former data can now be compared with the last two materials, i.e., Tea Leaves (INCT-TL-1) and Mixed Polish Herbs (INCT-MPH-2) (cf.…”

Development of a Cigarette Tobacco Filler Standard Reference Material

“…The Institute of Nuclear Chemistry and Technology has developed two reference materials for inorganic trace analysis of tobacco, designated Oriental Tobacco Leaves (CTA-OTL-1) and Virginia Tobacco Leaves (CTA-VTL-2). 29 Both materials consist of dried, ground, and sieved tobacco leaves and are certified for elemental composition. CORESTA and TASL have produced four Reference Products (CRPs) to support the determination of pH, moisture, nicotine and TSNAs in smokeless tobacco products.…”

“…These materials are characterized for alkaloids, TSNAs, and moisture content. The Institute of Nuclear Chemistry and Technology has developed two reference materials for inorganic trace analysis of tobacco, designated Oriental Tobacco Leaves (CTA-OTL-1) and Virginia Tobacco Leaves (CTA-VTL-2) . Both materials consist of dried, ground, and sieved tobacco leaves and are certified for elemental composition.…”