CS252298B1 - Method for preparing argon for quantum analysis - Google Patents

Abstract

The purpose of the solution is to dry and purify argon for quantummetric analysis in metallurgy. Argon is subjected to the action of a filling consisting of a molecular sieve and granulated nickel activated by hydrogen. The active surface of the granulated nickel is 1 to 10 m2 at an argon flow rate of 1 to 5 l/min.

Description

The invention relates to a process for preparing argon for quantometric analysis by purifying it with a molecular sieve in the presence of hydrogen.

In quantometric analysis, i.e. optical-emission vacuum quantitative spectral analysis, most commonly used in metal production and processing, excitation is performed. the sample to be analyzed in an inert gas stream, generally formed by argon. In order to achieve the desired excitation quality of the material of the sample to be analyzed, the flowing argon gas must have the necessary parameters, in particular be clean.

The methods known to date for preparing argon consist either of selecting the purest production batches from conventional argon production, or of using argon-hydrogen mixtures in quantometric analysis.

Further, it is known to purify argon using scrubbers in which undesirable impurities bind to metal chips such as magnesium, copper and titanium at high temperatures. It is also known to purify and dry argon using zeolite molecular sieves. Alternatively, the purification and drying of the argon is performed using a catalytically activated surface silica gel. Combinations of all these known methods are also known.

These known methods of preparing argon for quantometric analysis have the common disadvantage that they are unable to maintain the same in the long term. argon quality and thus eliminate the effect of oxygen transported by the discharge from the analyzed sample. This results in variations in the accuracy and accuracy of the results of the quantometric analysis.

The present invention overcomes these drawbacks by providing a method for preparing argon for quantometric analysis by purifying it with a molecular sieve in the presence of hydrogen. Its essence is that argon

2S2 298 is subjected to a molecular sieve charge and granulated nickel-activated hydrogen, the active surface of granulated nickel being 1 to 10 m @ 2 at an argon flow rate of 1 to 5 l / minute.

The main advantage of the process according to the invention lies in the achievement of long-term stability of the quality of the argon to be prepared and thus the required accuracy and precision of the quantometric analyzes. This advantage results primarily from the favorable time constant of the hydrogen diffusion process from nickel and, more recently, from the filling capacity »

The method according to the invention is described in more detail below by way of example of a suitable device and its function according to the attached drawing and a specific embodiment.

The apparatus comprises a vessel χ having an inlet port χ for raw argon and an outlet port χ for the treated argon. The container 1 is loaded with a charge sieve consisting of a molecular sieve and finely granulated nickel. The molecular sieve is regenerated in a conventional manner and free of moisture and adsorbed impurities of oxygen, nitrogen, carbon dioxide and the like. The granulated nickel is activated by hydrogen, around the vessel 1 a heating system is provided.

The device works by passing crude argon into the vessel χ through the inlet χ and gradually flowing through the charge,, i.e., the molecular sieve and the fine granulated nickel, which is activated by hydrogen · Here argon desiccates and purifies along with controlled hydrogen sorption from activated hydrogen nickel. This control is provided by the heating system χ. Pure argon enters the inter-electrode space with a small amount of hydrogen from the outlet opening of the vessel 4 to ensure displacement of the oxygen transported at the discharge of the sample to be analyzed. Sufficient absorbency of the molecular sieve and the time hydrogen diffusion constant ensures long-term stability.

- 3 Example

252 298

Crude argon having a purity of 99.95% by volume of argon was purified. The filler consisted of a 20 kg molecular sieve and 20 kg granulated hydrogen activated nickel. The flow rate of argon ranged from 0.5 to <1.5 L / min. In comparison with argon with a purity of 99.99% by volume, it was found that the purification of argon had better results than the argon compared.

Claims (1)

Process for preparing argon for quantometric analysis by purifying it with a molecular sieve in the presence of hydrogen, characterized in that argon is subjected to a molecular sieve charge and granulated nickel-activated hydrogen, wherein the active area of granulated nickel is 1 to 10 at argon / minute.