University of North Florida
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Stuart Chalk, Ph.D.
Department of Chemistry
University of North Florida
Phone: 1-904-620-1938
Fax: 1-904-620-3535
Email: schalk@unf.edu
Website: @unf

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NIST 365

Classification: Reference Material -> NIST -> 365 -> Iron

Citations 2

"Determination Of Trace Elements In Unalloyed Steels By Flow Injection Inductively Coupled Plasma Mass Spectrometry"
J. Anal. At. Spectrom. 1995 Volume 10, Issue 6 Pages 449-453
Aurora G. Coedo and Teresa Dorado

Abstract: Steel (250 mg) was treated with 7 mL 65% HNO3, 200 µL 40% HF and 3 mL water and the mixture was digested in a microwave oven (program details given). The oven was cooled, the contents were transferred to a calibrated flask and 2.5 µg each of Be, Tl and Rh (internal standards) were added. The solution was diluted to 50 mL with 1% HNO3 and a 250 µL portion of the solution was pumped into the nebulizer (2.8 ml/min), mixed with the nebulizer gas (1.1 ml/min) and analyzed by ICP-MS (operating conditions given). The RSD was 3% for all analytes at concentrations 1 µg/g. The method was applied to the analysis of two pure Fe reference materials (BCR CRM 097 and NIST SRM 365). Results agreed well with certified values.
Trace elements Mass spectrometry Sample preparation Internal standard Reference material

"Isotope Dilution Analysis For Flow Injection ICP-MS Determination Of Microgram Per Gram Levels Of Boron In Iron And Steel After Matrix Removal"
Anal. Chem. 1996 Volume 68, Issue 6 Pages 991-996
Aurora G. Coedo, Teresa Dorado, Bernardo J. Fernandez, and Francisco J. Alguacil

Abstract: Steel or Fe (0.25 g) was mixed with HCl, HNO3, H2SO4 and water in a high-pressure digestion vessel and dissolved using a microwave oven. A 10B spike solution was added (250 ng B) and the solution was evaporated to form solid salts, which were redissolved in water. The solution was extracted with acetylacetone/CHCl3 (1:1) at pH 1.4, the organic phase was discarded, and the extraction procedure was repeated on the aqueous phase. The aqueous layer was mixed with 1 mL HNO3, the solution was evaporated to 2 mL and diluted to 5 mL with water. The resulting test solution corresponded to 50 mg/ml sample, with the total B and Fe contents 1 µg/ml. Flow injection sampling minimized problems arising from the total salt concentration. The ICP-MS detection limit was 0.02 µg/g and the RSD values for concentrations 10 times this limit were 1% (n = 4). Good accuracy was obtained for eight Fe reference materials with B contents 10 µg/g.
Boron Mass spectrometry Sample preparation Reference material Interferences Matrix removal