TY - CONF A1 - Riebe, Gundel A1 - Klingbeil, Patrick A1 - Pritzkow, Wolfgang A1 - Vogl, Jochen T1 - Erfahrungen mit mikrowelleninduzierten Aufschluss-Verfahren für die Elementspurenanalytik T2 - MLS-Tagesseminar CY - Berlin, Deutschland DA - 2001-03-19 PY - 2001 AN - OPUS4-1111 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogl, Jochen A1 - Klingbeil, Patrick A1 - Pritzkow, Wolfgang A1 - Riebe, Gundel T1 - High accuracy measurements of Fe isotopes using hexapole collision cell MC-ICP-MS and isotope dilution for certification of reference materials N2 - An ICP-MS equipped with collision cell, sector field and multi-collector technology has been applied to developing analytical procedures for Fe in terms of isotope ratio measurements and isotope dilution analysis. Therefore a detailed study on the reduction of molecular interferences by a variety of collision gases (He, Ar, Kr, H2, D2 and N2) was performed. The efficiency of the reduction has been checked by high resolution mass scans. The argon based interferences disturbing the determination of 54Fe and 56Fe could be completely removed when using Faraday detectors. The interferences on mass 57 could be reduced to a level which enables accurate measurements. Also, the 40Ar12C interference, which disturbs the chromium correction, could be completely removed. Reproducibilities of 0.01% could be reached for 54Fe/56Fe isotope ratios and 0.02% for 57Fe/56Fe isotope ratios. Under these measurement conditions a sensitivity of 1.2 V per 50 µg kg–1 Fe is available. This corresponds to 1.5 × 109 cps per mg kg–1. Based on these results highly accurate procedures for Fe isotope ratio determinations were set up, reaching a performance level superior to that of other ICP-MS instruments. Consequently, IDMS procedures were developed on this basis in order to perform certification measurements at the highest metrological level. The first application was the contribution to the Fe reference value by IMEP-12, an interlaboratory comparison with approximately 350 participants worldwide. The analysed Fe mass content is 0.2150 mg kg–1 with its expanded uncertainty (k= 2) of 0.0012 mg kg–1(0.56%), which is ten times less than the uncertainty of the second certification laboratory. Another application was the certification campaign of the two reference materials Tea Leaves and Polish Herbs. The results obtained with the ICP-MS procedure, 542 ± 11 mg kg–1 and 543 ± 12 mg kg–1, were compared with the results analysed by TIMS, 541 ± 12 mg kg–1 and 541 ± 13 mg kg–1, and agree very well within the stated uncertainties (k= 2). The results presented demonstrate quite well the suitability of the developed IDMS procedures for certification or reference measurements. PY - 2003 DO - https://doi.org/10.1039/b301812a SN - 0267-9477 SN - 1364-5544 VL - 18 SP - 1125 EP - 1132 PB - Royal Society of Chemistry CY - London AN - OPUS4-2739 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riebe, Gundel T1 - A comparative study in the field of soil analysis T2 - Trends in sample preparation CY - Seggauberg, Austria DA - 2004-07-04 PY - 2004 AN - OPUS4-16300 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pritzkow, Wolfgang A1 - Vogl, Jochen A1 - Berger, Achim A1 - Ecker, Klaus A1 - Grötzschel, R. A1 - Klingbeil, Patrick A1 - Persson, L. A1 - Riebe, Gundel A1 - Wätjen, U. T1 - Contribution of ICP-IDMS to the certification of antimony implanted in a silicon wafer - comparison with RBS and INAA results N2 - A thin-layer reference material for surface and near-surface analytical methods was produced and certified. The surface density of the implanted Sb layer was determined by Rutherford backscattering spectrometry (RBS), instrumental neutron activation analysis (INAA), and inductively coupled plasma isotope dilution mass spectrometry (ICP-IDMS) equipped with a multi-collector. The isotopic abundances of Sb (121Sb and 123Sb) were determined by multi-collector ICP-MS and INAA. ICP-IDMS measurements are discussed in detail in this paper. All methods produced values traceable to the SI and are accompanied by a complete uncertainty budget. The homogeneity of the material was measured with RBS. From these measurements the standard uncertainty due to possible inhomogeneities was estimated to be less than 0.78% for fractions of the area increments down to 0.75 mm2 in size. Excellent agreement between the results of the three different methods was found. For the surface density of implanted Sb atoms the unweighted mean value of the means of four data sets is 4.8121016 cm-2 with an expanded uncertainty (coverage factor k=2) of 0.0921016 cm-2. For the isotope amount ratio R (121Sb/123Sb) the unweighted mean value of the means of two data sets is 1.435 with an expanded uncertainty (coverage factor k=2) of 0.006. KW - ICP-MS KW - IDMS KW - Reference material KW - Surface analysis PY - 2001 DO - https://doi.org/10.1007/s002160100987 SN - 0937-0633 VL - 371 SP - 867 EP - 873 PB - Springer CY - Berlin AN - OPUS4-7220 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dudek, Gabriele A1 - Alber, D. A1 - Pritzkow, Wolfgang A1 - Riebe, Gundel A1 - Vogl, Jochen A1 - Görner, Wolf T1 - Determination of the beta- branching ratio of 64Cu by mass spectrometric investigations of the decay products in neutron transmuted copper N2 - The ?- branching ratio of 64Cu was determined by investigating the resulting decay products in copper doped by neutron transmutation. The numbers of 64Zn and 64Ni atoms were analyzed using isotope dilution analysis combined with thermal ionization mass spectrometry. A ?- branching ratio of (38.06±0.30)% was obtained, which agrees with the study of Kawada (Appl. Radiat. Isot. 37 (1) (1986) 7) to a higher accuracy. However, our result differs from the value cited in the NUDAT database of (39.0±0.3)%. KW - NTD KW - Copper KW - Zinc KW - Nickel KW - Branching ratio KW - Cu-64 KW - TIMS KW - IDMS KW - Isotope dilution KW - Thermal ionization mass spectrometry KW - Neutron transmutation doping PY - 2002 DO - https://doi.org/10.1016/S0969-8043(01)00180-4 SN - 0883-2889 SN - 0969-8043 N1 - Geburtsname von Dudek, Gabriele: Wermann, G. - Birth name of Dudek, Gabriele: Wermann, G. VL - 56 SP - 145 EP - 151 PB - Elsevier CY - Amsterdam AN - OPUS4-7221 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riebe, Gundel T1 - On the problems related to total of chromium determination T2 - Trends in sample preparation CY - Seggauberg, Austria DA - 2007-06-26 PY - 2007 AN - OPUS4-15012 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riebe, Gundel T1 - Bestimmung von Platin in Autokatalysatoren mit massenspektrometrischer Isotopenverdünnungsanalyse T2 - 39. Diskussionstagung der Deutschen Gesellschaft für Massenspekrometrie CY - Mainz, Germany DA - 2006-03-05 PY - 2006 AN - OPUS4-14559 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riebe, Gundel T1 - Chemische Probenvorbereitung T2 - 1. Workshop "Isotopenverdünnungsanalyse mit ICP-MS" CY - Berlin, Germany DA - 2002-11-11 PY - 2002 AN - OPUS4-2999 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riebe, Gundel T1 - Massenspektrometrische Isotopenverdünnungsanalyse unter dem Blickwinkel von Referenzanalysen für metrologische Fragestellungen T2 - 6. Symposium Massenspektrometrische Verfahren der Elementspurenanalyse / 18. ICP-MS Anwendertreffen CY - Berlin, Germany DA - 2003-10-06 PY - 2003 N1 - Geburtsname von Dudek, Gabriele: Wermann, G. - Birth name of Dudek, Gabriele: Wermann, G. AN - OPUS4-3798 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogl, Jochen A1 - Koenig, Maren A1 - Pritzkow, Wolfgang A1 - Riebe, Gundel T1 - Development of reference procedures for the quantification of toxic metals and S in plastics N2 - The quantitative analysis of toxic metals in plastics is very important for different sectors of industry and daily life. Many routine procedures have been established based on X-ray fluorescence or inductively coupled plasma atomic emission spectrometry. However, all of them require suitable reference materials to calibrate or validate. These reference materials ideally are being certified by reference procedures. The development of such reference procedures for sulfur and the four toxic elements cadmium, chromium, mercury and lead in plastics is described here. The procedures are based on double isotope dilution mass spectrometry including analyte–matrix separation. The applied mass spectrometric techniques are thermal ionization mass spectrometry as well as inductively coupled plasma mass spectrometry. Memory effects of mercury and dissolution of chromium(III) oxide have been considered especially. The expanded uncertainties have been improved from the percent range down to the per mill range during the development of the procedure from the early analysis of BCR-680/681 to the recent analysis of CCQM-P106. With the fully developed procedures expanded uncertainties (k = 2) between 0.1 and 0.4% for cadmium, chromium, lead and sulfur and around 1% for mercury can be achieved. The so developed procedures have been successfully applied to the certification of reference materials as well as to intercomparisons organized by CCQM. KW - ICPMS KW - TIMS KW - Reference materials KW - IDMS PY - 2010 DO - https://doi.org/10.1039/c0ja00034e SN - 0267-9477 SN - 1364-5544 VL - 25 IS - 10 SP - 1633 EP - 1642 PB - Royal Society of Chemistry CY - London AN - OPUS4-22044 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Vogl, Jochen A1 - Gusarova, Tamara A1 - Czerwensky, Michael A1 - Heinrich, Hans-Joachim A1 - Hioki, A. A1 - Konopelko, L.A. A1 - Methven, B. A1 - Miura, T. A1 - Petersen, O. A1 - Riebe, Gundel A1 - Sturgeon, R. A1 - Turk, G.C. A1 - Yu, L. L. T1 - Purity determination as needed for the realisation of primary standards for elemental determination: status of international comparability N2 - Within the National Metrology Institutes (NMIs) and designated laboratories, an interlaboratory comparison, CCQM-P107, was conducted to verify the degree of international comparability concerning the results of purity analysis. The mass fractions of Ag, Bi, Cd, Cr, Ni, Tl at the lower mg/kg-level in a high purity zinc material were determined, but the real measurand in metrological sense was the sum of the six mass fractions. Homogeneity was investigated by glow discharge mass spectrometry, reference values were obtained using isotope dilution mass spectrometry. Six NMIs participated, contributing eight independent data sets. The agreement amongst the results of the participants, their median and the agreement with the reference values were usually excellent and in almost all cases below the target uncertainty of 30% relative. In this manner, the accuracy of results and the comparability between the participants was demonstrated to be established. KW - Interlaboratory comparison KW - Purity analysis KW - High purity metals KW - CCQM-P107 KW - Zinc PY - 2010 DO - https://doi.org/10.1007/s00769-009-0557-0 SN - 0949-1775 SN - 1432-0517 VL - 15 IS - 1 SP - 29 EP - 37 PB - Springer CY - Berlin AN - OPUS4-20767 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Riebe, Gundel A1 - Pritzkow, Wolfgang A1 - Vogl, Jochen T1 - Schwermetallbestimmung im Boden KW - Königswasserextraktion KW - Bodenanalyse KW - Schwermetallbestimmung KW - Unsicherheitsvergleiche PY - 2006 SN - 0016-3538 IS - 8 SP - 688 EP - 690 PB - GIT-Verlag CY - Darmstadt AN - OPUS4-13725 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riebe, Gundel T1 - Hochpräzise Bestimmung von Cadmium und Blei in Sedimentproben im Rahmen von CCQM-Ringversuchen T2 - 17. ICP-MS Anwendertreffen und 2nd International Conference on High-resolution Sector Field ICP-MS CY - Vienna, Austria DA - 2001-09-10 PY - 2001 N1 - Geburtsname von Dudek, Gabriele: Wermann, G. - Birth name of Dudek, Gabriele: Wermann, G. AN - OPUS4-7714 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riebe, Gundel T1 - Combination of sophisticated sample digestion methods and highly accurate determination procedures shown for Sulphur in oil and Cadmium and Lead in sediment T2 - Trends in sample preparation 2002 CY - Seggauberg, Austria DA - 2001-06-29 PY - 2001 AN - OPUS4-7717 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riebe, Gundel T1 - Prüfung der Dekontaminierbarkeit von radioaktiv kontaminierten Oberflächen nach DIN 25 415, Teil 1 (identisch mit ISO 8690 T2 - Analytica Messe 2000 CY - Munich, Germany DA - 2000-04-11 PY - 2000 AN - OPUS4-7708 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riebe, Gundel T1 - Bestimmung von Bor-Isotopenverhältnissen in Stahl und Aluminiumlegierungen für kerntechnische Anwendungen T2 - 5. Symposium Massenspektrometrische Verfahren der Elementspurenanalyse und 16. ICP-MS Anwendertreffen CY - Jülich, Germany DA - 2000-09-18 PY - 2000 AN - OPUS4-7711 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Klingbeil, Patrick A1 - Vogl, Jochen A1 - Pritzkow, Wolfgang A1 - Riebe, Gundel A1 - Müller, J. T1 - Comparative studies on the certification of reference materials by ICPMS and TIMS using isotope dilution procedures N2 - A comparison of different isotope dilution mass spectrometric (IDMS) procedures using inductively coupled plasma mass spectrometry (ICPMS) and thermal ionization mass spectrometry (TIMS) was carried out to examine the degree of equivalence between the used procedures in terms of requirements for reference material certification. The comparison was based on the measurement results and their uncertainties. The sample used in this study is a pure zinc metal to be certified by the Bureau Communie de Référence (BCR) for amount contents of different trace elements. This study focuses on cadmium and thallium. The TIMS values contributed to the certified values. To guarantee identical conditions as far as possible for the procedures under investigation, the samples were split into subsamples after spiking and digestion took place. Thus, every IDMS procedure started with an identical set of samples. In total, four different IDMS procedures and one external calibration procedure using internal standardization as an example of routine analysis were applied. The IDMS procedures divide in a group with and a group without trace/matrix separation. Multicollector TIMS (TI-MC-MS) and multicollector ICPMS (ICP-MC-MS) were used in combination with trace/matrix separation, whereas quadrupole ICPMS (ICP-QMS) and ICP-MC-MS were also applied to nonseparated samples. All IDMS results agree well within their combined uncertainties, while some results from the external calibration procedure do not. IDMS results obtained by ICPMS without separation are comparable to those obtained by TI-MC-MS with separation regarding precision and accuracy. The smallest uncertainties were achieved using ICP-MC-MS in combination with trace/matrix separation. KW - ICP-MS KW - TIMS KW - IDMS KW - multi-collector KW - uncertainty budget KW - Certification KW - reference material PY - 2001 DO - https://doi.org/10.1021/ac001278c SN - 0003-2700 SN - 1520-6882 VL - 73 IS - 8 SP - 1881 EP - 1888 PB - American Chemical Society CY - Washington, DC AN - OPUS4-909 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riebe, Gundel A1 - Ostermann, Markus A1 - Pritzkow, Wolfgang A1 - Vogl, Jochen T1 - Combination of sophisticated sample digestion methods and highly accurate determination procedures shown for Sulphur in oil and Cadmium and Lead in sediment T2 - Internationale Konferenz "Trends in Sample Preparation 2002" CY - Seggau, Austria DA - 2002-06-30 PY - 2002 AN - OPUS4-1398 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dudek, Gabriele A1 - Pritzkow, Wolfgang A1 - Riebe, Gundel A1 - Görner, Wolf A1 - Alber, D. T1 - Characterization of neutron transmuted zinc traces in pure copper materials by isotope dilution mass spectrometry N2 - The neutron transmutation doping (NTD) of highly pure copper with zinc was investigated as a promising means of achieving controlled gradation of the zinc content in the range 1-20 wg g-1. The doping process leads to the enrichment of two stable isotopes 64Zn and 66Zn in a ratio which differs from that of natural isotopic distribution. Mass spectrometric investigations by thermal ionization mass spectrometry (TIMS) were performed to validate the results obtained by gamma spectrometry. The investigations included both determination of the isotopic ratios of the doped zinc isotopes and the analysis of the accumulated zinc contents by isotope dilution (ID) analysis. Thereby a sample-specific correction of the blank could be performed because the isotope 68Zn was not influenced, because of the transmutation process. The results obtained by TIMS prove the strict proportionality of the doped zinc content, in the range 5 to 20 wg g-1, to the neutron fluence. Comparison with gamma spectrometric results showed a very good agreement within the uncertainties. PY - 2001 DO - https://doi.org/10.1007/s002160100784 SN - 0937-0633 N1 - Geburtsname von Dudek, Gabriele: Wermann, G. - Birth name of Dudek, Gabriele: Wermann, G. VL - 370 IS - 5 SP - 606 EP - 611 PB - Springer CY - Berlin AN - OPUS4-1145 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Ecker, K. H. A1 - Wätjen, U. A1 - Berger, Achim A1 - Grötzschel, R. A1 - Persson, L. A1 - Pritzkow, W. A1 - Radtke, Martin A1 - Riebe, Gundel A1 - Riesemeier, Heinrich A1 - Vogl, Jochen T1 - Certification of antimony implanted in silicon wafer with a silicon dioxide diffusion barrier - IRMM-302 and BAM-L001 N2 - This Report describes the certification of the reference material antimony implanted in Si/SiO2 intended to be used for calibration of surface and near surface analytical methods. It describes the preparation, homogeneity measurements and the analytical work performed for the certification of both Areal density of antimony Atoms (retained dose) and the isotope amount Ratio as well as giving considerations on the stability of the material. KW - Isotope ratio KW - Areal density KW - Surface analysis PY - 2002 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-355752 SP - 1 EP - 40 PB - Institute for Reference Materials and Measurements CY - Geel, Belgium AN - OPUS4-35575 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Vogl, Jochen A1 - Klingbeil, P. A1 - Pritzkow, W. A1 - Riebe, Gundel A1 - Wermann, G. A1 - Turner, P. A1 - Wortel, N. A1 - Woittiez, J. T1 - HIIRM final report N2 - Accurate analytical results have become more and more an absolute essential tool for further progresses in technology and science. Precision however, often used in this context as a quality criterion for analytical methods, is not a replacement for accuracy in any way. Therefore, analytical procedures are necessary, which will generate reliable and accurate results and can be used for evaluation of other analytical procedures and certification of reference materials (RM). Especially the certification of reference materials for the amount content of trace elements requires highly accurate results with a small combined uncertainty. The best example for an analytical procedure having this capability is undoubtedly Isotope Dilution Mass Spectrometry, for inorganic as well as for organic applications. Applied on Thermal Ionization Mass Spectrometry (TIMS) isotope dilution provides results of highest quality and proven high accuracy especially in the field of RM certifications for more than 30 years. The major drawback of this approach often is the necessity for a complex chemical separation step. A major advantage of Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is the potential to cope with a simplified or an on-line-carried-out sample preparation. A key requirement of isotope dilution analysis however is the accurate and precise determination of isotope ratios, because of its limiting factor for the accuracy and the total uncertainty of the result. Very precise isotope ratios can be determined in combination with a detection system that is capable of simultaneous detection of different isotopes, a so-called multi-collector system. The objective of the presented project is to evaluate the advantages of such a multi-collector ICP-MS for the application of IDMS in the field of trace elemental analysis in reference materials. The focus is on the development of simple and fast procedures for isotope ratio measurements in general and IDMS analysis in particular. Furthermore, it is an objective to develop and evaluate on-line spiking procedures. One of the first conclusions, which had a severe impact on the HIIRM project, arose during the early days of the project. Currently most certification experiments are accomplished by certification campaign based on a variety of participants’ results. The sample preparation, sending, analyzing and data evaluation however require lot of resources and the process may take a long time. An alternative way is given by using fewer participants with methods of higher metrological quality. For elemental amount contents such a method undoubtedly is isotope dilution analysis and multi-collector ICP-MS offers the necessary precision and matrix robustness and ruggedness as said above. Therefore, a multiple collector ICP-MS was manufactured as part of the project instead of the originally planned high-resolution instrument. Due to the novelty of the multicollector ICP-MS instrument, a lot of additional fundamental research became necessary. Especially interferences needed further attention. Fortunately, the IsoProbe is additionally equipped with a high-resolution option and with a brand new collison cell. The high-resolution option however can only be used to identify interferences but cannot be used to quantify them. On the other hand, the use of the collision cell proved to be a vital tool to overcome interferences. This is especially true because high resolution would have reduced the available sensitivity by a factor of ~100. Applying the collision cell technology the high sensitivity was maintained whilst most interferences were eliminated. However finding the right parameters of operation for the collision cell became a huge part of the method development process. A variety of gases like argon, helium, hydrogen, deuterium, nitrogen, krypton and xenon were tested for their suitability. Especially the tests accomplished for iron determinations revealed that carefully selected parameters have an incredible influence on the quality of the final results. Nonetheless collision cell technology will undoubtedly be widely used for newer ICP-MS instrumentation and contribute to eliminate wrong analytical values caused by interferences. The enhanced sensitivity of the instrument revealed also problems not detectable by other means. The control of contaminations seems to be one of the major analytical challenges in the future. Sector field based ICP-MS will give the user an opportunity to trace sources of contamination back to their origin and eliminate them. Even lower limits of detection will be the result as well as an enhanced reliability for analysts dealing with higher amount contents. The analyst will also benefit in controlling blank levels when the method of isotopically spiked procedure blanks is used as demonstrated in this project. Another main part of the project was the validation of the developed procedures. The first validation step was successfully accomplished by applying these procedures on the standard solutions provided by NRG. The main part of this validation however consisted of the evaluation of the fundamental parameters of the isotope dilution process and related measurements. This approach turned out to be superior compaired to the first step as a highly reliable uncertainty calculation can be easily performed. The best reputation and acceptance of the methods can however only be accomplished by participating in certification campaigns or in interlaboratory comparisons on highest metrological level. The results of the participations in general were brilliant. Not only the results but also the obtained realistic uncertainties were of superior quality. Direct comparisons at BAM with the results obtained by a multicollector TIMS applying the same calculation schemes showed the benefits of using multicollector ICP-MS. The main benefits of ICP-MS were identified, of which the first one is the enhanced precision of the isotope ratio measurement. For a variety of elements the values obtained by multicollector ICP-MS are even more precise than the ones obtainable by multicollector TIMS. The second important advantage identified was the simplified sample preparation. The laborious and time consuming analyte-matrix-separation step as necessary for TIMS measurements can either be omitted or at least be drastically reduced. Therefore, the advantages regarding time and enhanced sample throughput will result in further spread of ICP-MS in general and multicollector ICP-MS in particular. The third major part in terms of the method development process was mainly focused on developing an online isotope dilution system. The volumetric instead of the gravimetric IDMS approach proved difficult, if the high demands necessary for RM definition measurements are to be fulfilled. The major obstacle in this case is the missing stability and precision in terms of mass flow. Consequently, the initial development failed as the system made up of two piezoelectric droplet injectors was unable to reach the required stability as well as precision. The thereupon-created system consisting of two HPLC pumps proved to be far more valuable regarding automation and particularly the quantification of transient signals. Nevertheless, such a system will probably be rarely used in certification campaigns, as the gain of time is too small compared to the loss of reliability. However, this system proved most valuable in terms of species-specific elemental analysis as preliminary investigations showed. In this context this system will be suitable for certification measurements, as the major uncertainty contributions derive from sampling, sample treatment and species distribution and as moreover all availabel methods demonstrate far beyond. During the whole project, one of the main concerns regarding the multicollector ICP-MS instrument were software issues caused by the early development state of the original control programs. A lot of effort was necessary to accomplish the necessary data manipulations externally. The development of a new software suite by Micromass for the HIIRM project has solved this issue almost completely. With the new software suite and the validated parameters of measurement a step forward for institutes dealing with reference material certifications was achieved. Future certifications campaigns for minor elemental contents in different matrices should be performed by a small number of participants from highly qualified institutes. These institutes should apply very reliable methods of measurement like the ones developed in the HIIRM project. Many resources may be saved that way while the outcome of the certifications may easily be improved. ICP-MC-MS has the potential to be an important method in this context. Stable isotope dilution analysis in combination with a multi-detector ICP-MS, equipped with a hexapole collision cell for the suppression of important spectral interferences and for enhanced sensitivity, proved to be an advanced method of elemental analysis with a high potential for matrix independent measurements. Since ICP mass spectrometers of this type have only recently been introduced, no systematic evaluation of the capabilities of this specific application of the ICP-IDMS method has yet been made. KW - interferences KW - collision cell KW - ICPMS KW - IDMS PY - 2002 SP - 1 EP - 166 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-35579 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -