JPS59180458A - Quantitative analysis of deuterium in water - Google Patents

Abstract

PURPOSE:To enable a quantitative analysis of deuterium concentricity on a limited quantity of sample and within a limited time, by allowing steam and hydrogen of sample deuterium a mutual reaction in presence of hydrophobic catalyst and analysing deuterium in enriched hydrogen reached to exchange equilibrium. CONSTITUTION:A rapid promotion of reaction in presence of hydrophobic catalyst causes equilibrium of heavy hydrogen concentration in steam and hydrogen gas in accordance with equilibrium constant K and material balance following a reaction formula. After exchange reaction, hydrogen gas now in a balanced concentration condition is collected is subject to concentration analysis of deuterium in hydrogen gas by means of mass analyser, gas-chromatography enables determination of deuterium concentration in steam. For instance, a hydrophobic catalyst 4 supporting Pt in a cylindrical porous teflon phase body located in a stainless reacting vessel 1 and this reacting vessel is admitted in a constant temperature chamber 3 and high-purity hydrogen gas is introduced.

Description

[Detailed Description of the Invention] The present invention is designed to reduce the amount of water used in water by 11:1':・7 minutes.
This method is one type of Jj method.

Heavy water traditionally contained in water, Peno'tjii! A method called the equilibrium method has been used for Iza analysis for a long time. In this method, in a flask maintained at a constant humidity, ・i[should be determined? &7 Water is added together with a platinum catalyst, hydrogen is added to the empty space iiU in the flask, and a water-water 1111 isotope exchange reaction is caused between the sample heavy water and hydrogen gas using the platinum GjJ+ medium. As a result of that reaction, try it! 1.
, if deuterium in water moves to hydrogen gas, and in hydrogen gas, deuterium is converted to 76 and reaches an equilibrium concentration. Collect the water Z < gas that has a concentration of 1 #f, ) (i) Analyze the hydrogen concentration by 1 each, etc., and calculate the deuterium concentration of the sample water by calculating from the relationship between the equilibrium constant and mass balance. Gray calyx.

However, this conventional deuterium analysis method requires a large amount of sample (several ml in the smallest trench), and in addition, 77, J
It has the disadvantage that it takes a long time, about an hour, to reach equilibrium.

For this reason, it is important to use the equilibrium method more than once in the study of physical, chemical, biological, and other phenomena using heavy water as a tracer.1. i: 'Ji practically impossible i + 7 ability, analysis; 1 (1
Between 1 and 2 hours: (The sample is reduced to 5J compared to the previous method.)
<;51< was praised.

I [・ Store opening 1. J-d, solving the drawbacks of this sophisticated conventional method
fjj and reduce the hydrogen concentration in the water JS),
Furthermore, it is to provide a method for analyzing the treasure 111 in short poem 1 (II).

This purpose, according to the present invention, is based on trial 1? l Kame water steam) 1
(This is achieved by subjecting hydrogen to an intersectional reaction in the presence of a hydrophobic catalyst, and then electrostatically analyzing the deuterium in the enriched hydrogen of heavy water J that has reached the intersectional plane.

Here, "exchange reaction between heavy water vapor and water-based gas in the presence of a hydrophobic catalyst" specifically means that between gaseous 11↑ water-based vapor and water-based gas, a hydrophobic catalyst is This means that the reaction is abruptly completed under the presence of 111E. Therefore, the reaction preparation is the
Approximately 70 times longer than the median reaction rate. The deuterium concentration in the water vapor and water vapor is constant according to the equilibrium constant and mass balance according to the following reactor: 7:C.

HD +H20→ N2 +1 old] O gas
After the exchange reaction of vapor gas,...
・If you measure the threat level of 1 q of hydrogen in hydrogen gas using an analyzer or gas chromatography, you can calculate the amount of deuterium in 1 q of water vapor. Island degree can be determined・r#
Aqueous resistance (medium) is made by depositing a fraction of platinum gold 4 in the form of atoms in the pores of a porous polymer material such as Teflon, which has water-repellent properties. (This is called a medium. This hydrophobic 'rl: +701! You should use a medium, the water is +', the adsorption of the lk medium surface is saturated water'17,:
Even in A7, there is N11., n zukizu, and therefore, non-'r'?r has a good amount of movement, and anti-1'j';moves;1 five lines.

FIG. 1 shows the h position used when actually performing the +1 analysis according to the present invention. An example in which the method of the present invention was carried out using this equipment will be described below.

Lucid g/yytQ stainless steel reaction: 'r:i 1 with cylindrical trum X? rnrn rl] pore 'I
031j, u 'Ek ノ and 1 cent platinum was supported on fI Teflon gel jj4'9Wednesday) ・l! ! B
Assuming it・^279, llI4shi, this reaction 4k/
30? Z” Noah fi+f If K,?, fl
i, I put it in the dry bottle 3 that I had. Then, commercially available high-purity water and gas were sealed up to a pressure of 7 degrees θRmH. 4 is a wire mesh that holds the wound (1<), and 5 is a thermometer.

- To measure the blade hydrogen concentration, from sample heavy water /θθt
A sample of ti was measured with a micro syringe and injected into the reactor 1 by piercing the rubber stopper 6 of the lower insertion part of the micro syringe. In this reaction, the injected sample 4 drains, becomes vapor, and undergoes an exchange reaction (with hydrogen gas in the image) in the presence of a solvent. The required time was within 3 minutes for the exchange reaction to be completed and the hydrogen gas, r+c water in the water vapor, and French IGp degree to be equal. After the reaction, the water vapor is converted into a liquid; only the hydrogen gas is collected using a trap at a temperature of 100 nm, and the hydrogen gas is transferred to a gas chromatograph.
The heavy water level in the water was measured at 111 degrees. The time required to determine the deuterium RP degree after the exchange reaction was about 3 minutes, and the extra time required for 141" and 14" was about 140 g minutes. If we know the degree of 11-(water; And Moi Koji Teishi K (/Left 0C to -2,2 O) Which l>>
From section i, 1R hydrogen i' in water vapor, that is, in trial water.
+'! Can calculate degrees.

Save this 1 expressed overculm to 1 (1), i()rap J.
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Set Jl to 6f a F nail 1 for A<knowledge> test
1()9r:p, r'l ha, j・3', ;'i'
, l: i? '4+' ((:+1+ 144 L/
You can decide immediately.

Figure 2 shows the detected deuterium C''1 degrees (DmO/?%) determined by a heavy water sample of 4 degrees (Dmo/%).
) is shown. Trial゛γ [σ) 4 + main I or water, 1a degree is 70
%, the detected IR hydrogen concentration was related to the tj and iT lines.

[Brief explanation of the drawing]

Figure 1 shows the equipment used in the constant analysis method according to the present invention;
A schematic diagram of t, Figure 2 shows the relationship between the detected heavy water y+,'+j degree and the 4 degree relationship.1 in the figure: ・
”: IK) Biξ, 2: Fused metal, 3: Bed temperature 4): 1.
4: Gold 5'14.5'? ! ja i magazine full, 7:
Micro syringe needle insertion port. For patent use 1'jA human burial

Claims (1)

[Scope of Claims] /) An exchange reaction is performed between 4 gases of 1.It material i'Q water and hydrogen in the presence of a hydrophobic catalyst, and 1. ``U1 analysis method for deuterium in water, which is characterized by constant one-step analysis of hydrogen in G-converted water. Sword A special feature that evaporates the sample heavy water by placing the sample heavy water and hydrogen in a closed space where the temperature trap is maintained and making the exchange reaction 1 core.
i1・, 41 range of search [ilj in water described in the first term
, Mizune no U; 71 analysis method. 3) ,'i:j1. ' :lt minute iJ? Keimata & J
16th Edition Claim 1J (↑; 1) Quantitative analysis method for hydrogen in water according to 1, which involves constant 1Jt analysis by gas chromatography.