scholarly journals 30 years of IRMM-1027 reference materials for fissile material accountancy and control: development, production and characterisation

2021 ◽  
Author(s):  
Rožle Jakopič ◽  
Kalman Toth ◽  
Jeroen Bauwens ◽  
Renata Buják ◽  
Carmel Hennessy ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Isotopic Composition ◽  
Reference Materials ◽  
Isotope Dilution ◽  
Organic Substance ◽  
Certified Reference Materials ◽  
Isotope Dilution Mass Spectrometry ◽  
Fissile Material ◽  
High Quality ◽  
And Control

AbstractThe IRMM-1027 Large-sized dried (LSD) spikes are certified reference materials applied to measure the uranium and plutonium content of dissolved fuel solutions using isotope dilution mass spectrometry. High quality starting metals of uranium and plutonium are dissolved to produce a stock solution, which is dispensed into individual vials and dried down. The present spikes are mixtures of typically 50 mg 20% enriched U and 2 mg enriched 239Pu as dried nitrates, conditioned in an organic substance for stability. Each vial of an IRMM-1027 LSD spike comes with certified masses of uranium (235U and 238U) and 239Pu and isotopic composition with associated uncertainty. This article will discuss major developments since the production of the first batch of LSD spikes and will reflect on the current preparation and certification approaches.

Development, validation, and certification by isotope dilution gas chromatography-mass spectrometry of lyophilized human serum reference materials for cortisol (CRM 192 and 193) and progesterone (CRM 347 and 348)

1991 ◽  
Vol 37 (4) ◽  
pp. 540-546 ◽  
Author(s):  
Linda Thienpont ◽  
Lothar Siekmann ◽  
Alexander Lawson ◽  
Elisabeth Colinet ◽  
Andrȳ De Leenheer
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Reference Materials ◽  
Isotope Dilution ◽  
Certified Reference Materials ◽  
Collaborative Study ◽  
Gas Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry ◽  
Coefficients Of Variation

Abstract The Community Bureau of Reference of the European Communities has produced four batches of lyophilized serum Certified Reference Materials, two for cortisol (CRM 192 and 193) and two for progesterone (CRM 347 and 348). For cortisol, one of the pools consisted of serum from healthy blood donors, whereas the second batch was supplemented with pure cortisol. The progesterone Reference Materials contained only endogenous hormone concentrations. Assessment of vial-to-vial variability in the cortisol and progesterone concentrations showed no between-sample inhomogeneity, and the materials were stable. The quality of the materials was therefore considered sufficient for certification of the values for the cortisol and progesterone concentrations by a collaborative study involving several laboratories from the European Communities, using isotope dilution gas chromatography-mass spectrometry. Inaccuracy in reconstitution of the lyophilized materials was less than 0.3%; imprecision of sampling was less than 0.2%. For determinations of cortisol and progesterone concentrations, the mean within-laboratory coefficients of variation (CVs) were 1.76% (CRM 192), 1.19% (CRM 193), 1.64% (CRM 347), and 1.75% (CRM 348). The between-laboratory CVs were greater: CRM 192, 1.79%; CRM 193, 1.48%; CRM 347, 2.08%; and CRM 348, 2.16%. The concentrations in the reconstituted Reference Materials were certified to be 273 nmol/L in CRM 192 and 763 nmol/L in CRM 193 for cortisol and 10.13 nmol/L in CRM 347 and 40.3 nmol/L in CRM 348 for progesterone. Uncertainties at the 0.95 confidence level--6 (CRM 192), 14 (CRM 193), 0.21 (CRM 347), and 1.0 nmol/L (CRM 348)--were considered compatible with the intended use of the materials.

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