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  • Gravimetric preparation and characterization of primary reference solutions of molybdenum and rhodium.

Gravimetric preparation and characterization of primary reference solutions of molybdenum and rhodium.

Analytical and bioanalytical chemistry (2014-12-19)
Angela Kaltenbach, Janine Noordmann, Volker Görlitz, Carola Pape, Silke Richter, Heinrich Kipphardt, Gernot Kopp, Reinhard Jährling, Olaf Rienitz, Bernd Güttler
ABSTRACT

Gravimetrically prepared mono-elemental reference solutions having a well-known mass fraction of approximately 1 g/kg (or a mass concentration of 1 g/L) define the very basis of virtually all measurements in inorganic analysis. Serving as the starting materials of all standard/calibration solutions, they link virtually all measurements of inorganic analytes (regardless of the method applied) to the purity of the solid materials (high-purity metals or salts) they were prepared from. In case these solid materials are characterized comprehensively with respect to their purity, this link also establishes direct metrological traceability to The International System of Units (SI). This, in turn, ensures the comparability of all results on the highest level achievable. Several national metrology institutes (NMIs) and designated institutes (DIs) have been working for nearly two decades in close cooperation with commercial producers on making an increasing number of traceable reference solutions available. Besides the comprehensive characterization of the solid starting materials, dissolving them both loss-free and completely under strict gravimetric control is a challenging problem in the case of several elements like molybdenum and rhodium. Within the framework of the European Metrology Research Programme (EMRP), in the Joint Research Project (JRP) called SIB09 Primary standards for challenging elements, reference solutions of molybdenum and rhodium were prepared directly from the respective metals with a relative expanded uncertainty associated with the mass fraction of U rel(w) < 0.05 %. To achieve this, a microwave-assisted digestion procedure for Rh and a hotplate digestion procedure for Mo were developed along with highly accurate and precise inductively coupled plasma optical emission spectrometry (ICP OES) and multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) methods required to assist with the preparation and as dissemination tools.

MATERIALS
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Sigma-Aldrich
Nitric-14N acid solution, ~10 N in H2O, 99.99 atom % 14N
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Supelco
Acetone, Pharmaceutical Secondary Standard; Certified Reference Material
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LD-2391-25G25 g
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Supelco
Hydrogen peroxide solution, 30 % (w/w), for ultratrace analysis
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LD-2391-25G25 g
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Sigma-Aldrich
Hydrochloric acid solution, 32 wt. % in H2O, FCC
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LD-2391-25G25 g
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USP
Dehydrated Alcohol, United States Pharmacopeia (USP) Reference Standard
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LD-2391-5G5 g
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€558.42
LD-2391-25G25 g
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€1,721.40
Sigma-Aldrich
Hydrochloric acid, 36.5-38.0%, BioReagent, for molecular biology
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LD-2391-5G5 g
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LD-2391-25G25 g
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Supelco
Hydrochloric acid solution, volumetric, 0.1 M HCl (0.1N), endotoxin free
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LD-2391-25G25 g
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Hydrochloric acid solution, 1.0 N, BioReagent, suitable for cell culture
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LD-2391-25G25 g
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Hydrogen peroxide solution, 30 % (w/w) in H2O, contains stabilizer
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LD-2391-25G25 g
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Supelco
Hydrogen chloride – 2-propanol solution, ~1.25 M HCl (T), for GC derivatization, LiChropur
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Sigma-Aldrich
Hydrochloric acid solution, ~6 M in H2O, for amino acid analysis
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Hydrogen chloride – methanol solution, ~1.25 m HCl (T), for GC derivatization, LiChropur
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Supelco
Hydrogen peroxide solution, ≥30%, for trace analysis
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LD-2391-25G25 g
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Sigma-Aldrich
Hydrogen peroxide solution, tested according to Ph. Eur.
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Millipore
Hydrogen peroxide solution, 3%, suitable for microbiology
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Acetone, ≥99%, meets FCC analytical specifications
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Acetone, natural, ≥97%
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Hydrogen chloride – ethanol solution, ~1.25 M HCl, for GC derivatization, LiChropur
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Hydrogen peroxide solution, 34.5-36.5%
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Acetone, United States Pharmacopeia (USP) Reference Standard
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Rhodium, foil, light tested, 25x25mm, thickness 0.05mm, as rolled, 99.9%
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Rhodium, foil, not light tested, 50x50mm, thickness 0.00025mm, permanent polyester support, 99.9%
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Rhodium, wire reel, 0.05m, diameter 0.12mm, as drawn, 99.9%
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LD-2391-5G5 g
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LD-2391-25G25 g
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Rhodium, wire reel, 0.2m, diameter 0.12mm, as drawn, 99.9%
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LD-2391-1G1 g
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LD-2391-5G5 g
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€558.42
LD-2391-25G25 g
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Rhodium, foil, light tested, 25x25mm, thickness 0.075mm, as rolled, 99.9%
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LD-2391-1G1 g
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LD-2391-5G5 g
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€558.42
LD-2391-25G25 g
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€1,721.40
Rhodium, wire reel, 0.05m, diameter 0.25mm, hard, 99.9%
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LD-2391-1G1 g
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LD-2391-5G5 g
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€558.42
LD-2391-25G25 g
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€1,721.40
Rhodium, foil, 25x25mm, thickness 0.125mm, as rolled, 99.9%
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LD-2391-1G1 g
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LD-2391-5G5 g
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€558.42
LD-2391-25G25 g
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€1,721.40
Rhodium, foil, not light tested, 50x50mm, thickness 0.00075mm, permanent polyester support, 99.85%
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LD-2391-1G1 g
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€226.14
LD-2391-5G5 g
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€558.42
LD-2391-25G25 g
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€1,721.40
Rhodium, wire reel, 0.2m, diameter 0.25mm, hard, 99.9%
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LD-2391-1G1 g
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€226.14
LD-2391-5G5 g
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€558.42
LD-2391-25G25 g
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€1,721.40
Rhodium, foil, light tested, 25x25mm, thickness 0.05mm, as rolled, x-ray quality, 99.9%
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LD-2391-1G1 g
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€226.14
LD-2391-5G5 g
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€558.42
LD-2391-25G25 g
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€1,721.40