JPS5849431A - Production of water standard gas - Google Patents

Abstract

PURPOSE:To obtain a water standard gas of a prescribed moisture concn. easily and surely by supplying gaseous raw materials of a prescribed concn. continuously from a bomb, allowing the gases to react to produce water and humidifying the remaining gases with said water. CONSTITUTION:Gaseous raw materials such as, for example, an inert gas contg. oxygen of a prescribed concn. and hydrogen of a concn. higher than twice equiv. the concn. of oxygen, or air contg. a hydrogen-contg. compd. such as hydrocarbon or the like which is a source for supplying hydrogen of a prescribed concn, or gaseous hydrogen contg. an oxygen-contg. compd. which is a source for supplying oxygen of a prescribed concn. are filled in a gas bomb 1 filled with the gaseous raw materials. The gaseous raw materials are fed to a reactor 4, where the materials are heated and the water corresponding to the content of the oxygen or hydrogen contained in the gaseous raw materials is produced continuously. Since the remaining gases which do not contribute to the reaction are humidified by the produced water, the water standard gas of a prescribed moisture concn. is produced continuously. Said gas is discharged through a discharge port 7.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing a standard gas containing water at a predetermined concentration. synthesize,
The present invention relates to a method for producing a water standard gas containing a stoichiometrically calculated moisture content by humidifying a certain amount of residual gas with this water.

Conventionally, there are devices such as infrared gas analyzers and gas chromatographs that continuously measure moisture in gas, but this
When measuring moisture concentration using a standard gas, a standard gas containing a certain concentration of moisture (water standard gas) is required to calibrate the device.

However, water is highly corrosive, highly adsorbent, and has a relatively high boiling point, so preparing a water standard gas is very introspective.
Moreover, it is almost impossible to fill a cylinder with a certain concentration of water standard gas and store it, and then take it out of the cylinder and use it when necessary. The sample gas is introduced into the measurement device before calibration, and the indicated value of this device is recorded, and the same sample gas f:@@ is introduced into the collection liquid and the moisture in the sample gas is absorbed by the absorption liquid, and then analyzed using the Karl Fischer method. Calibrate the scale of the measuring device using 20, or determine the water concentration by letting an absorbent absorb the water in the sample gas and find the weight change, and use the same method. The scale of the measuring device is calibrated.

However, these methods require an absorbent solution or absorbent, which is expensive and cumbersome to store, requires a long time to determine the water concentration, and requires indirect calibration, making it unreliable. However, there was a strong desire for a simple production of a water standard gas with extremely high concentrations.

The present invention has been developed in consideration of the above-mentioned circumstances, and therefore, a water standard gas that continuously supplies a raw material gas with a predetermined concentration from a cylinder and uses this raw material gas to continuously produce a water standard gas with a predetermined concentration. The purpose is to provide a manufacturing method.

That is, the present invention combines a gas containing oxygen or an oxygen-containing compound at a predetermined concentration and a gas containing hydrogen or a hydrogen-containing compound at a predetermined concentration, which are filled into the same or different cylinders, into a gas phase in the presence of a balance gas if necessary. A water standard gas containing a predetermined concentration of water calculated chemically is produced by continuously reacting and synthesizing water.

Hereinafter, one embodiment of the present invention will be described with reference to FIG.

FIG. 1 shows an example of a water standard gas production apparatus used in carrying out the present invention, and in the figure, 1 is a gas cylinder filled with raw material gas. This cylinder contains, for example, an inert gas containing oxygen at a predetermined concentration and hydrogen at a concentration more than twice that of oxygen (in this case, since the concentration of oxygen and hydrogen is low, there is no risk of drying out). air containing a hydrogen-containing compound such as a hydrocarbon, which is a supply source of hydrogen at a predetermined concentration, or a raw material gas such as hydrogen gas containing an oxygen-containing compound, which is a supply source of oxygen at a predetermined concentration. Examples of hydrogen-containing compounds include low-boiling hydrocarbons having 1 to 4 carbon atoms, and examples of oxygen-containing compounds include carbon oxides such as carbon dioxide and carbon dioxide.
Low boiling point gaseous fluorides such as sulfur oxides such as sulfur dioxide gas and nitrogen oxides such as nitrous chloride are preferred. These hydrogen, oxygen-containing compounds, or hydrogen-containing compounds are usually diluted to a predetermined concentration with an inert gas such as nitrogen or a balance gas such as air. The raw material gas in the cylinder 1 is The bales pass through the wrinkle adjustment valve 2, the flow rate of which is adjusted to a predetermined value, and flow into the reactor 4 via the pressure meter 6.

This reactor 4 has a heat-resistant pipe 5 made of quartz or the like and a nichrome wire 6.
When the raw material gas is heated in this reactor 4, oxygen or oxygen in the oxygen-containing compound and hydrogen or hydrogen in the hydrogen-containing compound are combined. In this case, the amount of water produced can be arbitrarily set by selecting the concentration of the oxygen-containing compound, hydrogen, or hydrogen-containing compound in the raw material gas. In addition, this reactor 4 can be filled with a catalyst that promotes the reaction. For example, a palladium-based catalyst can be used to oxidize hydrocarbons (05118
COo +3a2-rTp'm
, o + al14 omitted), and furthermore, it is also possible to fill the container with a compound capable of supplying oxygen, such as copper oxide, and send leaf gas at a predetermined concentration to generate water.

The heating temperature varies depending on whether or not a catalyst is used, but is usually 300°C or higher, preferably 350°C or higher.

In this way, the raw material gas is sent to the reactor 4, where it is heated and the oxygen or hydrogen contained in the raw material gas is
Water corresponding to the amount of water is continuously produced, and the residual gas that does not react to the reaction that is colored in the raw material gas is humidified and the predetermined water content is 1llI! The water standard gas is continuously produced and taken out from the water standard gas take-out lower.

In this example, a raw material gas set in advance at a predetermined temperature is introduced into a reactor, where oxygen (oxygen-containing compound) and water TE (hydrogen-containing compound) in the raw material gas are reacted to continuously produce water. is generated and the residual gas is thereby humidified, so that a water-monomer gas having a predetermined moisture content can be easily and reliably obtained regardless of the flow rate of the raw material gas. Also, special effects are easy because the raw material gas is filled in a cylinder, and because of this, water standard gas can be generated at any time at any location in Renci, and the supplied raw material gas always has a constant composition. ,
As a result, the water concentration of the water standard gas is kept accurately constant and does not fluctuate. Furthermore, the water concentration of the produced water standard gas is approximately twice the concentration of the raw material gas in the low-dose range, 1iI! The secret is chemistry fiI11i! This value is a direct value that is different from the indirect leakage value.

Figure 2 shows another example of the water standard gas production apparatus used in the implementation of the present invention. In this case, one cylinder is filled with a balance gas such as nitrogen and oxygen (or oxygen containing The other cylinder IBk: is filled with *lF+ gas, which is a mixture of balance gas such as violet and hydrogen (or hydrogen-containing compound) at a predetermined a degree. After mixing the raw material gases supplied from the two cylinders one by one, they are led to the reactor 4, and the other kojic acid and effects are the same as in the above example. 1. The same reference numerals are given to the same parts and the explanation thereof will be omitted.

In addition, in the above-mentioned example, an electric heater was used to heat the reaction furnace, but the hydrogen-containing compound and the oxygen-containing compound are not limited to the above-mentioned compounds, and other compounds may be used without departing from the gist of the present invention. There is no problem with deformation.

On the other hand, the present invention provides a system in which a predetermined mL of an acid-based or oxygen-containing compound-containing gas and a predetermined concentration of hydrogen or a hydrogen-containing compound-containing gas filled in the same or different cylinders are placed in a gas phase. By chemically reacting to synthesize water and using this water to cool down the residual gas from the reaction, it is possible to easily generate a water sub-gas with a predetermined concentration calculated chemically. In this case, since the raw material gas is supplied from a cylinder and has a constant composition, the water standard gas produced thereby has the advantage that the composition is also constant and highly reliable without fluctuations.

[Brief explanation of the drawing]

FIGS. 1 and 2 are schematic A-plane views showing specific examples of a water standard gas production apparatus used in carrying out the present invention. 1, IA# IB...Cylinder, 2.2Al 2B・
...Wrinkle #valve adjustment, 6.6mm, 5B...pressure meter,
4...Anti-Si C1 furnace, 5...Pipe, 6...Nichrome wire, 7-...Water standard gas extraction [Io Applicant: wt% Chemical Drying Equipment Co., Ltd. Agent Masuji Naohata Hata World Patent Attorney Takashi Kojima

Claims (1)

[Claims] Water is synthesized by continuously reacting a gas containing oxygen or an oxygen-containing compound at a predetermined concentration with a gas containing hydrogen or a hydrogen-containing compound at a predetermined concentration in a gas phase filled in the same or a similar cylinder. A method for producing a water standard gas, which comprises: humidifying residual gas from the reaction with this water to generate a water-containing gas having a predetermined concentration calculated stoichiometrically.