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Synthetic standards for determination of trace elements in steels by solid sampling techniques
RISE, Swerea, Swerea KIMAB.
RISE, Swerea, Swerea KIMAB.
2015 (English)Report (Refereed)
Abstract [en]

Accurate determination of trace elements in steels is of importance for several reasons. Some trace elements are added on purpose to influence the metallurgy of the steel, and it is important to control the content to the correct level. Other trace elements are deleterious to certain steel properties and must be controlled to be below maximum levels in order to ensure the quality. In more recent years, national and international legislation demand from steel producers to declare the content of certain environmentally hazardous elements, mainly heavy metals such as Hg, Pb and Cd. Multi-element techniques based on direct solid sampling is of great interest due to the short analysis times, but there is a lack of suitable reference materials (RM) for calibration. Bundesanstalt für Materialprüfung (BAM) in Berlin has therefore developed a technique to produce synthetic solid RM’s for trace analysis. The technique is based on mixing metal powder with small amounts of trace elements in liquid solution, drying and compacting the powder into solid briquettes. A few stainless steel RM’s produced at BAM were used at KIMAB to determine Ce, La, Nd and Pr in a stainless steel CRM, using an LA-ICPMS instrument. The results showed very good agreement with certified values. Six RM’s of the same type were subsequently prepared at KIMAB, doped with Pb, Cd and Hg at levels from 0,1 μg/g to 30 μg/g. The RM’s were first analysed by wet chemical ICP-MS at ALS in Luleå. The results showed nearly 100% recoveries of Pb and Cd, while most of the Hg had been lost in the sample preparation. The samples were then used to calibrate the LA-ICPMS instrument for Pb and Cd. It was found that the signals from the top surface of the samples were very high, indicating a considerable degree of “elemental fractionation. A “preburn” in the form of an ablation linear scan across the sample surface was therefore needed prior to the analysis scan. Very good linear calibration curves were obtained for Pb and Cd, but with apparently higher background levels than in solid steel. Three stainless steels with previously determined contents of Pb just below 2 μg/g were analysed together with the synthetic RM’s, giving intensities significantly below the calibration curve. Assuming a zero background level give calculated mass fractions in near agreement with certified values, but this is not a satisfactory calibration method. It is therefore concluded that in present form, synthetic RM’s are only reliable as calibration samples for LA-ICPMS measurements at trace levels larger than 10 μg/g. Further work is necessary in order to reduce this limit

Place, publisher, year, edition, pages
Swerea KIMAB AB , 2015.
Series
Rapport / Institutet för metallforskning, ISSN 1403-848X ; KIMAB-2015-101
National Category
Materials Engineering
Identifiers
URN: urn:nbn:se:ri:diva-12993OAI: oai:DiVA.org:ri-12993DiVA, id: diva2:973187
Available from: 2016-09-22 Created: 2016-09-22Bibliographically approved

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CiteExportLink to record
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  • apa
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