High purity silver - Materials / Alfa Chemistry

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High purity silver

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ACMA00021093

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High purity silver

Determination of the total purity of high-purity silver materials for elemental determination

$Mean values and standard deviation s of mass fractions of impurities in silver shot by ICP-MS$ Zhou, Tao, et al. Accreditation and quality assurance 18 (2013): 341-349.

Candidate materials for use as primary standards for silver determination were characterized for their total purity. All possible impurities were considered, with the exception of radioactive elements and He. The demonstrated total purity and its standard uncertainty, based on GDS, ICP-MS and carrier gas hot extraction measurements, is w(Ag) = (99.999 52 ± 0.000 11) %. The purity value and its uncertainty are dominated by the contribution of the non-metallic impurities measured, namely S, N, C and O.
The high-purity silver was cleaned by the following procedure: in methanol (ultrasound for 3 min), water, 1% nitric acid (ultrasound for 1 min), 3 times in water (ultrasound for 1 min) and methanol, followed by drying under an infrared lamp. There was no measurable mass loss in the sample after cleaning. It was later demonstrated that this cleaning procedure did not result in the lowest possible surface oxygen content. However, it is important that for all measurements and subsequent use the same cleaning procedure is applied to always leave the material in the same defined surface state. All samples were measured under the same conditions, with a typical discharge current and discharge gas flow rate of 40 mA and 405 mL/min, respectively. The intensity of Ag was about 10 cps in low resolution mode with optimized parameters. The calibration of the GDMS is based on the Standard Relative Sensitivity Factors (SRSF) supplied with the instrument. SI-traceable measurements were performed using pressed powder pellets of pure matrix powders to determine 57 metallic and semi-metallic trace elements in the matrix Cu and Fe. These powders were doped with calibration solutions of the 57 elements at different concentration levels and dried before pressing.

Real low-field Hall coefficient studies for high-purity silver at low temperatures

Specimen information Barnard, R. D. Journal of Physics F: Metal Physics 7.4 (1977): 673.

Previous low-temperature Hall measurements on nominally pure noble metals have involved transitions to the high-field regime. We report here the results of the Hall coefficient (RH) for several high-purity silver samples and for silver samples containing low concentrations of gold. The Cd and dislocations in the field were as low as 0.0085 T (85 G), sufficient to ensure truly low-field conditions. The results are examined in terms of the variation of the relaxation time anisotropy factor for two sets of models in the neck (N) and belly (B) regions of the Fermi surface. The characteristic peak Hall coefficient, which is a single function of temperature, is characteristic of pure metals and is the locus of the peak observed in RH on dilute alloys, independent of the nature or concentration of nonmagnetic impurities or defects present. The application of the theory enables the acquisition of new R-relative curves for dilute silver-based alloys, as well as values of the phonon scattering factor in pure silver down to 10 K. The field variation of R at 4.2 K is also measured for most samples.
The silver used in the study was nominally 6 N pure and after annealing had an RRR of approximately 500. After rolling to the desired thickness, each sample was spark machined into a 50 x 5 mm rectangle but with two 1 x 3mm tabs in the middle along the long sides of the sample where the Hall voltage is developed. The aspect ratio was sufficient not to reduce the magnitude of the Hall voltage. Larger RRR's were produced in the pure silver samples by annealing two of the three samples at -760°C in the presence of oxygen. After evacuation, oxygen was leaked into the vacuum furnace system to maintain the dynamic indicated pressure for approximately 16 hours. After cooling (still with oxygen present), the RRR was 4230 for sample 1 and 4120 for sample 2. The mechanism for the improvement in RRR is believed to be related to the oxidation of residual iron impurities (typically a few PPM). This significantly reduces magnetic Kondo scattering which typically produces the majority of the resistivity of high purity silver at 4.2K. Sample 2 was initially 1 mm thick and was etched to approximately 0.5 mm, with an RRR of 3550 according to Hall measurements.

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