Report (1984) on Two GIT-IWG Geochemical Reference Samples: Albite from Italy, AL-I And Iron Formation Sample from Greenland, IF-G

Two reference samples, Albite AL-I and Iron Formation sample IF-G were analysed for their chemical composition by the International Working Group "Analytical Standards of Minerals, Ores and Rocks" (GIT-IWG). AL-I was processed in 189 kg and IF-G and 760 kg. 103 GIT-IWG laboratories participated in this collaborative study along with 171 geoanalysts. This study lasted 15 months (September 1982 - December 1983) and is the second undertaken by the GIT-IWG. Over 2400 units of data were collated. As a result of this international study, the major and minor elements have been well characterized in both the samples; however, more data on trace elements will be very welcome for a better definition of trace elements, although working values have been proposed for about forty trace elements in each sample. The first and the second collaborative studies undertaken by GIT-IWG demonstrate well the immense analytical potential of the GIT-IWG.     

SECOND REPORT (1993) ON THE FIRST THREE GIT-IWG ROCK REFERENCE SAMPLES: ANORTHOSITE FROM GREENLAND, AN-G; BASALTE D'ESSEY-LA-CÔTE, BE-N; GRANITE DE BEAUVOIR, MA-N

The first report (1980) on the three samples, Anorthosite AN-G, Basalt BE-N and Granite MA-N resulted in the chemical characterization of major, minor and 30 trace elements. The present report confirms the validity of a great majority of these working values, in addition to presenting working values for 20 more trace elements for each sample. Only compiled data on trace elements are presented, followed by Tables of statistical parameters used as a basis for their evaluation, both statistical and subjective. A plea is made to obtain more data on platinum group elements and on other "difficult" trace elements (Au, B, Bi, Se, Te, TI, …). The three samples have been processed in 900 kg amounts and, therefore, they are likely to remain available for some decades to come. As such, it is certainly worthwhile to take pains to characterize them well for even these difficult trace elements.     

1987 Compilation Report on Ailsa Craig Granite AC-E With the Participation of 128 GIT-IWG Laboratories

Third in the series of collaborative studies launched by the International Working Group "Analytical Standards of Minerals, Ores and Rocks" (IWG), the study on Ailsa Craig Granite AC-E has attracted the participation of 128 laboratories from 29 countries. Tables of compiled data, 3212 results in all, are presented with working values, recommended or proposed, for seventy major, minor and trace elements. The success of this study which lasted for only one year from the distribution of sample to the release of the present report is to be attributed entirely to the record participation of the IWG-Member laboratories.     

Reference Values Following ISO Guidelines for Frequently Requested Rock Reference Materials

We present new reference values for nineteen USGS, GSJ and GIT‐IWG rock reference materials that belong to the most accessed samples of the GeoReM database. The determination of the reference values and their uncertainties at the 95% confidence level follows as closely as possible ISO guidelines and the Certification Protocol of the International Association of Geoanalysts. We used analytical data obtained by the state‐of‐the‐art techniques published mainly in the last 20 years and available in GeoReM. The data are grouped into four categories of different levels of metrological confidence, starting with isotope dilution mass spectrometry as a primary method. Data quality was checked by careful investigation of analytical procedures and by the application of the Horwitz function. As a result, we assign a new and more reliable set of reference values and respective uncertainties for major, minor and a large group of trace elements of the nineteen investigated rock reference materials.     

Report (1967–1981) on Four ANRT Rock Reference Samples: Diorite DR-N, Serpentine UB-N, Bauxite BX-N and Disthene DT-N

All data reported by 200 analysts (106 laboratories) are presented for the four ANRT samples: Diorite DR-N, Serpentine UB-N, Bauxite BX-N and Disthène DT-N. Recommended values are given for the major and minor elements. As far as the as trace elements are concerned, DR-N has been characterized for 35 elements whereas the other three samples have been for only 20 elements. Wherever possible, brief comments have been inserted so as to explain our way of assigning recommended or proposed values.
After more than a decade of existence the total number of data reported for all the four samples reach only 3200 units which are not sufficient enough for a valid evaluation of compiled data. It is also pointed out that these samples are most likely to be available even during the next century as they have been prepared in large quantities of the order of one ton. A plea is therefore made for contribution of more data particularly for trace elements and for major elements which are present as trace elements in UB-N, BX-N and DT-N.     

Petrological considerations for the demineralization of Rajmahal coals with <Emphasis Type="Italic">Pseudomonas mendocina</Emphasis> B6-1

The present study entails the results of the petrological coniderations for demineralization of Rajmahal Gondwana coals with Psudomonas mendocina B6-1. Inertinite group macerals are the dominant constituents of these coals, followed by vitrinite group, while liptinite occurs in low concentration. The amount of Mineral matter is moderately high. The concentration of major, minor and trace elements is high when compared with Clarke values. After the treatment of these coals with Pseudomonas mendocina strain B6-1, a significant reduction in the elemental content of oxygen, hydrogen and sulphur was observed. A gradual reduction of pyrite phase due to bioleaching was identified and its signatures were reflected in the XRD spectra and FTIR absorption bands. Over 5 % reduction in the ash content and decrease of major, minor and trace element to variable degrees were also noticed. Fe, As, and Ca positively correlate with the ash removal percentage indicating that the samples with high concentration of these elements were prone to demineralization with Pseudomonas mendocina strain B6-1 whereas Ni, Zn, Cr and Cu, negatively correlate with the ash removal percentage and shows that their enrichment impeded the process of demineralization. With increasing concentration of vitrinite the removal of major/minor/trace elements also increased which is attributed to the possible association of these elements with the mineral matter occurring as superficial mounting and superficial blanketing over the vitrinite macerals. This could facilitate the bacterial access to the elements to act upon and remove it to the variable extent. Some minerals occur intergrown with inertinites causing restricted bacterial action owing to the nonexposure of the mineral particles and less surface area available to the bacteria for bioleaching. Sulfur removal strongly relates with increase in inertinite content and decrease in liptinite content. This appears that sulfur associated with liptinites have shown difficult removal condition. The maximum removal of the trace elements like Cd, Cu, Co, Zn and Pb was observed from the ‘banded dull coal’ samples of the Rajmahal basin while maximum removal of major/minor elements like Fe, Ca and Mg was noticed from the ‘banded bright coal’ samples. However, maximum removal of Mn and As was also observed in the samples of ‘banded coal’.     

First Co-Operative Study on Four Tropical Soil Samples and One Lateritic Bauxite (Suriname) Proposed as Geochemical Reference Samples

Five samples from Suriname have been analysed for their chemical composition by 18 laboratories. The proposed reference samples are four soil samples and one lateritic bauxite. The samples were analyzed for major and minor elements as well as for 36 trace elements. More data are needed for better characterization of these samples, particularly for trace elements.     

1996 COMPILATION OF ANALYTICAL DATA ON NINE GSJ GEOCHEMICAL REFERENCE SAMPLES, "SEDIMENTARY ROCK SERIES"

Analytical data compiled on nine Geological Survey of Japan (GSJ) reference samples, "Sedimentary rock series" received by February 1996 are reported. After excluding outliers and examining critically the analytical procedures employed, the data were evaluated statistically. Recommended or preferable values for fifteen major and sixty minor and trace elements are proposed.     

Three Marine Sediment Reference Samples: SDO-1, SDO-2 and SDO-3

The study of three marine sediments is the first in a series of reference samples to be developed for characterizing the bottom sediments of the Pacific Ocean and the Red Sea. The three samples were certified for their contents of major, minor and some trace elements. These values were assigned on the basis of statistical processing of the data obtained from an interlaboratory experiment conducted with the use of physical, physico-chemical and chemical methods of analysis. The Soviet, Czechoslovakian and Bulgarian laboratories took part in the interlaboratory experiment.     

1986 Values for Fifteen GSJ Rock Reference Samples, "Igneous Rock Series"

During the five-year period (April 1981 - March 1986), a series of fifteen rock reference samples, "Igneous rock series", has been prepared by the Geological Survey of Japan (GSJ). Based on the data available (published and communicated), consensus values for major, minor and trace elements have been derived; these values are presented for this second series of samples as well as for the first series of two samples, Granodiorite JG-1 and Basalt JB-1.     

1994 COMPILATION OF ANALYTICAL DATA FOR MINOR AND TRACE ELEMENTS IN SEVENTEEN GSJ GEOCHEMICAL REFERENCE SAMPLES, "IGNEOUS ROCK SERIES"

Analytical data for minor and trace elements published or communicated to us, on seventeen GSJ (Geological Survey of Japan) reference samples, "Igneous rock series" received up to April 1994 are compiled. The data were evaluated statistically in consideration of analytical methods. Based on the selected available data, 1994 recommended and proposed values for 65 minor and trace elements are presented.     

Geochemical Reference Samples, Drainage Sediment GSD 1 - 8 from China

A set of eight geochemical standard reference samples of stream sediments was prepared. The original purpose was to use these samples as primary standards for the data quality monitoring of a nation-wide regional geochemical survey program in China. But their use has been soon extended to other fields. Forty-one laboratories in China have joined in a collaborative venture to analyse these samples, using a variety of analytical procedures. Recommended values for over 50 trace and minor elements were derived by a method of repetitive elimination of outliers and calculation of central "tendency" from several central values.     

Certification of four North-American Gypsum Rock Samples Type: Calcium Sulphate Dihydrate, CaSO4.2H2O, GYP-A, GYP-B, GYP-C and GYP-D

Four natural gypsum rock samples were prepared and certified for major elements and some trace elements by the Analytical Group of Domtar Inc., Research Centre in Senneville (Montréal), Québec, Canada with the cooperation of Domtar Gypsum Products Laboratory in Caledonia, Ontario, Canada. The analytical round-robin results received from 29 participating laboratories were statistically evaluated, summarized, and form the basis of this paper. These certified reference materials are primarily intended as calibration standards for the determination of major and minor elements in gypsums and gypsum related minerals and products. As certified gypsum rock samples were not available on the North-American or world markets, these may be particularly important not only to the gypsum and cement industries, but also to geochemists, geologists and analysts of minerals and ores.     

Homogeneity of the Geochemical Reference Material BRP-1 (Paraná Basin Basalt) and Assessment of Minimum Mass

Reference materials (RM) are required for quantitative analyses and their successful use is associated with the degree of homogeneity, and the traceability and confidence limits of the values established by characterisation. During the production of a RM, the chemical characterisation can only commence after it has been demonstrated that the material has the required level of homogeneity. Here we describe the preparation of BRP-1, a proposed geochemical reference material, and the results of the tests to evaluate its degree of homogeneity between and within bottles. BRP-1 is the first of two geochemical RM being produced by Brazilian institutions in collaboration with the United States Geological Survey (USGS) and the International Association of Geoanalysts (IAG). Two test portions of twenty bottles of BRP-1 were analysed by wavelength dispersive-XRF spectrometry and major, minor and eighteen trace elements were determined. The results show that for most of the investigated elements, the units of BRP-1 were homogeneous at conditions approximately three times more rigorous than those strived for by the test of "sufficient homogeneity". Furthermore, the within bottle homogeneity of BRP-1 was evaluated using small beam (1 mm²) synchrotron radiation XRF spectrometry and, for comparison, the USGS reference materials BCR-2 and GSP-2 were also evaluated. From our data, it has been possible to assign representative minimum masses for some major constituents (1 mg) and for some trace elements (1-13 mg), except Zr in GSP-2, for which test portions of 74 mg are recommended.     

Report (1968–1978) on Two Mica Reference Samples: Biotite Mica-Fe and Phlogopite Mica-Mg

Since 1967–68, two mica reference samples, Biotite Mica-Fe and Phlogopite Mica-Mg, were made available to several geochemical laboratories. The analytical data reported during the past ten years by 142 geoanalysts belonging to 74 international laboratories are presented and assessed for deriving preferred values. Reaomrmended or proposed values are assigned for major, minor and several trace elements. The biotite Mica-Fe is better characterized for its chemical composition than the Phlogopite Mica-Mg. Both the samples are also proposed as geochronological standards. Because very few mica reference samples have been processed in large quantities, the international geochemiaal community is invited to contribute further useful data.     

THREE NEW GSJ ROCK REFERENCE SAMPLES: RHYOLITE JR-3, GABBRO JGB-2 AND HORNBLENDITE JH-1

Three new rock reference samples, Rhyolite JR-3, Gabbro JGb-2 and Hornblendite JH-1 have been prepared by the Geological Survey of Japan for collaborative studies on their chemical composition. Twenty-eight major, minor and trace elements were determined and presented. The results of homogeneity tests showed that all elements are considered to be distributed homogeneously in each reference sample. Geological and mineralogical characteristics are also described.     

Trace Element Analysis of Natural Gold by Laser Ablation ICP-MS: A Combined External/Internal Standardisation Approach

For the trace element analysis of gold by laser ablation ICP-MS, external calibration samples of differing matrix composition have been used in previous studies. Data presented here suggest that even for calibration samples and unknowns with closely-matched matrices, discrepancies arise due to variations in the coupling behaviour of the laser with the sample at different power deliveries, and can lead to erroneous trace element determinations. Internal standardisation for gold is complicated because Au and Ag, the most common major elements, do not have minor isotopes that can be used as internal standards. This problem was overcome for natural gold samples by using an external calibration sample only for the major elements Au and Ag, then defocussing the ion path and using ¹⁰⁷Ag in each sample as an internal standard against which μg g^-1 levels of Te, Sb, Hg, Bi, and Cu were determined. The results suggest that trace elements can occupy lattice sites in gold rather than occurring only as micro-inclusions of other phases. The analytical approach taken here may be used in trace element analysis where adequate external calibration samples are not readily available.     

1998 Compilation of Analytical Data for Five GSJ Geochemical Reference Samples: The "Instrumental Analysis Series"

Analytical data for five GSJ (Geological Survey of Japan) reference samples, the "Instrumental analysis series" received by October 1998, are compiled. The data reported in publications and personal communications were evaluated statistically, taking into account the analytical method and sample preparation. Based on the selected available data, recommended and preferred values for fourteen major and fifty one minor and trace elements are proposed.     

The “North American shale composite”: Its compilation,major and trace element characteristics

The compilation and major element composition of the “North American shale composite” (NASC) are reported for the first time, along with redeterminations for the REE and selected other elements by modern, high precision analytical methods. The NASC is not strictly of North American origin; 5 of the constituent samples are from Africa and Antarctica, and 15 are from unspecified locations. The major element composition of the NASC compares quite closely with other average shale compositions. New analyses of the NASC document that significant portions of the REE and some other trace elements are contained in minor phases (zircon and possibly other minerals) and that their uneven distribution in the NASC powder appears to have resulted in heterogeneity among analyzed aliquants. The results of this study show that the REE distributions of detrital sediments can be dependent to some extent on their minor mineral assemblages and the sedimentological factors that control these assemblages. Consequently, caution should be exercised in the interpretation of the REE distributions of sediment samples as they may be variable and biased relative to average REE distribution of the crustal rocks supplying detritus. These effects appear to be largely averaged out in sediment composites, with the result that their REE distributions are more likely to be representative of their provenances.