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Trace Element Determinations in a Low-Alloy Steel Standard Reference Material by Isotope Dilution, Spark Source Mass Spectrometry (CAT#: STEM-ST-0287-LJX)

Introduction

The service uses the spark source mass spectrograph for the simultaneous determination of cerium, copper, neodymium, selenium, silver, tellurium, and zirconium in a low-alloy steel material. Except for copper, the elements were present at trace concentrations that are difficult to determine by most analytical methods. In the procedure, known amounts of the isotopically enriched elements were added to 100-mg samples, which were dissolved in perchloric and hydrofluoric acids. After evaporation of the solutions almost to dryness, dissolution of the residues, and addition of hydrofluoric acid to complex the iron, the resulting solutions were electrolyzed in polytetrafluoroethylene cells. The electrodeposit on high purity, gold cathode wires was sparked in the mass spectrograph and the isotope ratios of the isotopically equilibrated elements were measured. The concentrations, ranging from 0.041% for copper to 3.1 μg/g (ppm) for neodymium, were calculated from the general isotope dilution equation. The low-alloy steel is available from NBS as Standard Reference Material 1261.




Principle

By using vacuum spark discharge, the energy accumulated in a small volume can make the material in the volume suddenly evaporate and ionize, so as to obtain the characteristic ion current information.

Applications

(1) Solid spark source mass spectrometry: impurity analysis of high-purity materials, which can be applied to semiconductor materials, non-ferrous metals, and building materials industries;
(2) Gas isotope mass spectrometry: determination of stable isotopes C, H, N, O, S and radioactive isotopes Rb, Sr, U, Pb, K, Ar, which can be applied to geology, petroleum, medicine, environmental protection and agriculture.

Procedure

(1) An electric field is applied between the electrodes to ionize part of the carrier gas (such as argon) in the electric field;
(2) The "cathode ray" or "anode ray" generated by ionization accelerates in the direction of the opposite polarity in the residual gas, bombards the anode or cathode, and vaporizes a part of the substance to be measured on the plate;
(3) Part of the atoms of the vaporized substance are ionized in the subsequent discharge process.

Materials

• Sample Type:
Low-Alloy steel

Notes

Before starting the machine, check whether the water (water cooler), electricity, gas (argon/nitrogen), temperature, humidity, and exhaust air of the instrument are normal.
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