Elemental concentrations in nbs biological and environmental standard reference materials

Elemental concentrations reported by 325 investigators in 16 NBS SRM's are summarized. Mean values, standard deviations and comparative data from NBS and other reviews are provided.     

Elements very rapidly measurable by INAA in biological and environmental materials

In connection with the increasing usage of reference materials in INAA work, and with the continuing interest in this laboratory in rapid analyses via very short-lived induced activities, 13 biological and 8 environmental reference materials have been processed, under rapid analysis conditions, by the reactor-flux INAA Advance Prediction Computer Program. The results described show that a total of 33 induced (n, ) activities of 26 elements are detectable in these 21 reference materials, in total analysis times ranging from 1.5 to 192 seconds.     

Analysis of standard reference materials by absolute INAA

Three standard reference materials were analyzed by a method of absolute INAA. Two different light water pool-type reactors were used to produce equivalent analytical results even though the epithermal to thermal flux ratio in one reactor was higher than that in the other by a factor of two.     

Input of missing trace elements in some IAEA/NBS biological certified reference materials using INAA

IAEA and NBS biological certified reference materials have been analyzed by instrumental neutron activation analysis and concentration of 17 elements was determined. The elements determined were either completely missing or their certified values were not given in the original compilations. For quality assurance of our work, a comparison of data on missing trace elements in some of the CRMs has been presented. It seems that second round of analysis for the certification of these elements would be useful.     

The preparation of biological and environmental reference materials

The facilities of the Institute for Reference Materials and Measurements for the preparation of biological and environmental reference materials are discussed under the aspect of satisfying important parameters for the preparation of candidate reference materials. The choice of transformation methods and their possible influences on quality and long-term conservation, the need for automation as well as the importance of quality control are particularly emphasized.     

The production of powdered candidate biological and environmental reference materials in the laboratories of the Joint Research Centre

The production of candidate biological and environmental reference materials in the laboratories of the Joint Research Centre, mainly on behalf of BCR, started in 1972 in Ispra and became concentrated in 1984 in Geel. Today, dedicated facilities for the transformation of biological and solid or liquid materials into dry powder samples are in use. The major guidelines followed in the conception of these facilities are described. Some typical examples of facilities developed or adapted to fulfil the specific requirements of professional CRM preparation are discussed, e.g. the whole-Teflon cryo-grinding equipment, the in-line controlled freeze-drier, the special facility for clean and dry handling of powders, the milling with classification equipment and the automation of bottling and labelling operations.     

Preparation of biological and environmental reference materials at CBNM

Summary Since 1984, CBNM has been officially responsible for supporting the BCR programme for CRM storage, distribution and sale activities for the development of methods for preparation, conditioning and packing for reference materials, as well as actually preparing candidate CRMs. This has allowed CBNM to set up a new laboratory with unique facilities for the preparation of biological and environmental reference materials, in particular for organic and inorganic trace analysis. The main technical facilities developed at CBNM and additional equipment built to CBNM specifications by external companies are described. They have been used for the preparation of a variety of reference materials including cod fish, pig liver, offal, spiked milk, curd, orange juice, clover, lettuce, paprika, tomato, fly ash, soils and sediments.     

Elemental concentrations in the spinach reference material determined by k0-based INAA

The IAEA-331 spinach material NIST SRM 1570a Spinach Leaves, submitted to an intercomparison run by the IAEA, has been analysed by k₀-based INAA with counting using both low and high energy photon detectors. The results have been compared with (i) the certified values of the NIST SRM 1570a; the agreement is good, taking into account the uncertainties; and (ii) the certified and consensus values of the former NIST SRM 1570 Spinach Leaves, their composition in minor and trace-elements are quite similar; however a lower content has been observed for Co, Fe and Sc in the IAEA-331 and for Zn in the SRM 1570. For quality control, the NIST 1573 Tomato Leaves and the NIST 1575 Pine Needles have been analysed using the same conditions as for the IAEA-331. The results agree quite well with the certified and consensus values given in the literature.     

The determination of iodine in biological and environmental standard reference materials

Iodine is an element with excellent intrinsic sensitivity when determined by thermal neutron activation. However, in most real samples, the preponderance of chlorine and bromine, relative to iodine, makes the direct determination of iodine virtually impossible. Over the past 20 years, there probably have been as many publications on the separation of iodine as there have been for any other radionuclide. Upon review, however, the methods are essentially the same. After irradiation, the samples are subjected to a rapid destructive process to free the iodine from the matrix and then the iodine is separated from the other halides either by liquid-liquid extraction or by liquid ion exchange. Both of these procedures are, however, rather complex and do not effect a complete separation of the halides in one pass. In the work presented here, a simple procedure is described for the quantitative separation of iodine from chlorine. The procedure utilizes a gas phase separation on hydrated manganese dioxide with iodine collected on silvered quartz wool. The described procedure has been used for the determination of iodine in numerous new and old SRM's at the NBS.     

Methyl mercury determination in environmental and biological reference and other materials by quality control with certified reference materials (CRMs)

Summary Two concentration methods — HCl extraction and extraction followed by water vapour distillation — prior to anion exchange separation and cold-vapour atomic absorption spectrometry were used for the quantification of methyl mercury in a number of reference materials of biological and environmental origin with reference or certified total mercury contents. The applied methods were validated by the analysis of three marine reference materials, certified for methyl mercury. The results obtained in the materials with methyl mercury contents ranging from less than 1 g/kg to a few hundred g/kg showed good agreement between both methods for biological materials, whereas extraction/anion exchange resulted in somewhat too high values for a number of environmental materials. These findings, however, require further confirmation by additional methods and by other laboratories.Dedicated to Professor Dr. Wilhelm Fresenius on the occasion of his 80th birthday     

INAA and flame AAS of various vegetable reference materials

Summary INAA and flame AAS have been used for the analysis of a large number of vegetable reference materials. Out of all determined elements (28 by INAA and 11 by AAS) nine are common for both methods (Ca, Cd, Co, Cu, Fe, Mg, Mn, Na, Zn) and for these the possibilities of the two methods have been compared.     

Homogeneity studies of reference materials by solid sampling – AAS and INAA

The necessity to quantify a natural material's homogeneity with respect to its elemental distribution prior to chemical analysis of a given aliquot is emphasised. The instruments and methods which are currently available are described. Additionally, the calculation of element specific, relative homogeneity factors, H _E and the minimum sample mass, M _5%, to achieve 5% precision on a 95% confidence level is given. Especially, in the production and certification of certified reference materials (CRMs) this characteristic information should be determined in order to provide the user with additional inherent properties of the CRM, to enable more economic use of the expensive material and to evaluate further systematic bias of the applied analytical technique.     

Determination of element concentrations in biological reference materials by solid sampling and other analytical methods

Summary Using solid sampling with graphite furnace atomic absorption spectrometry (GFAAS), values for cadmium, copper, lead and zinc in six biological reference materials were obtained from up to four laboratories participating in three collaborative studies. These results are compared with those obtained with other methods used in routine analysis from laboratories of official food control. Under certain conditions solid sampling with GFAAS seems to be suitable for routine analysis as well as conventional methods.     

Determination of perfluorinated alkyl acid concentrations in biological standard reference materials

Standard reference materials (SRMs) are homogeneous, well-characterized materials used to validate measurements and improve the quality of analytical data. The National Institute of Standards and Technology (NIST) has a wide range of SRMs that have mass fraction values assigned for legacy pollutants. These SRMs can also serve as test materials for method development, method validation, and measurement for contaminants of emerging concern. Because inter-laboratory comparison studies have revealed substantial variability of measurements of perfluoroalkyl acids (PFAAs), future analytical measurements will benefit from determination of consensus values for PFAAs in SRMs to provide a means to demonstrate method-specific performance. To that end, NIST, in collaboration with other groups, has been measuring concentrations of PFAAs in a variety of SRMs. Here we report levels of PFAAs and perfluorooctane sulfonamide (PFOSA) determined in four biological SRMs: fish tissue (SRM 1946 Lake Superior Fish Tissue, SRM 1947 Lake Michigan Fish Tissue), bovine liver (SRM 1577c), and mussel tissue (SRM 2974a). We also report concentrations for three in-house quality-control materials: beluga whale liver, pygmy sperm whale liver, and white-sided dolphin liver. Measurements in SRMs show an array of PFAAs, with perfluorooctane sulfonate (PFOS) being the most frequently detected. Reference and information values are reported for PFAAs measured in these biological SRMs.

Elemental concentrations in the spinach reference material determined by k0-based INAA

The IAEA-331 spinach material NIST SRM 1570a Spinach Leaves, submitted to an intercomparison run by the IAEA, has been analysed by k₀-based INAA with counting using both low and high energy photon detectors. The results have been compared with (i) the certified values of the NIST SRM 1570a; the agreement is good, taking into account the uncertainties; and (ii) the certified and “consensus” values of the former NIST SRM 1570 Spinach Leaves, their composition in minor and trace-elements are quite similar; however a lower content has been observed for Co, Fe and Sc in the IAEA-331 and for Zn in the SRM 1570. For quality control, the NIST 1573 Tomato Leaves and the NIST 1575 Pine Needles have been analysed using the same conditions as for the IAEA-331. The results agree quite well with the certified and “consensus” values given in the literature.     

Overview about biological and environmental certified reference materials in the database COMAR

The Database COMAR now includes data from more than 8640 CRMs supplied by 180 producers in 24 countries. These data are divided into 8 main categories, containing up to 10 sub-categories. Quality of life as well as biological and clinical CRMs are two main categories where a great increase could be observed in the past years. These fields represent approximately 20|X% of the data records. Therefore it will be possible to gather different statistical information from these data.