Method for detecting deuterium content in deuterium depleted water

A technology of ultra-light water and deuterium content, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of high stability requirements of instruments and huge investment in instruments and equipment, and achieve compact and reasonable design, low equipment investment, and low system cost. effect of error

Inactive Publication Date: 2010-10-13
SHANGHAI RES INST OF CHEM IND +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Mass spectrometry is widely used and has high accuracy. It can be injected directly and is not affected by oxygen isotopes. However, a standard sample is required for analysis. If the deuterium content of the sample differs greatly from the standard sample, it will cause certain errors. huge investment
Chromatography is suitable for the determination of extremely dilute heavy water samples and high-concentration heavy water samples with a deuterium content greater than 95%, and the accuracy can reach ±1ppm, but it requires high stability of the instrument

Method used

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  • Method for detecting deuterium content in deuterium depleted water
  • Method for detecting deuterium content in deuterium depleted water
  • Method for detecting deuterium content in deuterium depleted water

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Effect test

Embodiment 1

[0030] 1. Instruments: GC8800H gas chromatograph, thermal conductivity detector, HL-3000 chromatography workstation.

[0031] 2. Chromatographic conditions: high-purity hydrogen as the carrier gas, the purity of which is above 99.99%, the carrier gas flow rate is 20ml / min, the stainless steel chromatographic column, Φ3×2m, filled with 5A molecular sieve, the column temperature is 40℃, the detector is 50℃, The sample temperature is room temperature, and the bridge current is 100mA.

[0032] 3. Preparation of standard samples:

[0033] Several standard samples with different deuterium content were accurately prepared from 99.9% heavy water and Shanghai tap water by a stepwise dilution method. The atomic percentages were 194.4ppm, 234.4ppm, 278.9ppm, 320.3ppm, 360.1ppm.

[0034] 4. Drawing of standard curve:

[0035] The above-mentioned standard samples were reduced with magnesium bars under vacuum. First evacuate the system, then heat the reaction tube with magnesium bars to 500°C, inje...

Embodiment 2

[0045] 1. Instruments: GC8800H gas chromatograph, thermal conductivity detector, HL-3000 chromatography workstation.

[0046] 2. Chromatographic conditions: high-purity hydrogen as the carrier gas, its purity is above 99.99%, the carrier gas flow rate is 30ml / min, stainless steel chromatographic column, Φ3×2m, filled with 5A molecular sieve, column temperature 60℃, detector 70℃, inlet The sample temperature is room temperature, and the bridge current is 110mA.

[0047] 3. Preparation of standard samples:

[0048] Several standard samples with different deuterium content were accurately prepared from 99.9% heavy water and Shanghai tap water by a stepwise dilution method. The atomic percentages were 194.4ppm, 234.4ppm, 278.9ppm, 320.3ppm, 360.1ppm.

[0049] 4. Drawing of standard curve:

[0050] The above-mentioned standard samples were reduced with zinc under vacuum. First evacuate the system, then heat the reaction tube filled with zinc chips to 460℃, use a syringe to inject 0.1ml of ...

Embodiment 3

[0062] 1. Instruments: GC8800H gas chromatograph, thermal conductivity detector, HL-3000 chromatography workstation.

[0063] 2. Chromatographic conditions: high-purity hydrogen as the carrier gas, its purity is above 99.99%, the carrier gas flow rate is 40ml / min, stainless steel chromatographic column, Φ3mm×3m, filled with 5A molecular sieve, column temperature 40℃, detector 70℃, enter The sample temperature is room temperature, and the bridge current is 80mA.

[0064] 3. Preparation of standard samples:

[0065] Several standard samples with different deuterium content were accurately prepared from 99.9% heavy water and Shanghai tap water by a stepwise dilution method. The atomic percentages were 194.4ppm, 234.4ppm, 278.9ppm, 320.3ppm, 360.1ppm.

[0066] 4. Drawing of standard curve:

[0067] The above-mentioned standard samples were reduced with zinc under vacuum. First evacuate the system, then heat the reaction tube filled with zinc chips to 500°C, inject 0.1ml of water sample in...

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Abstract

The invention relates to a method for detecting deuterium content in deuterium depleted water. The method comprises the following steps of: reducing the deuterium depleted water into hydrogen with a reducing agent; introducing a sample and performing chromatographic detection on the sample, wherein high-purity hydrogen is used as a carrier gas by a gas chromatograph; separating HD peak from the sample gas through gas chromatographic column, wherein the peak area is directly proportional to the deuterium content in the sample gas; establishing a standard curve according to the ultra-low deuterium content in the standard heavy water sample and the area of the HD peak; reversely extending the standard curve to the range of the deuterium depleted water; and calculating the deuterium content in the water according to the area of the HD peak in the deuterium depleted water. Compared with the prior art, the invention overcomes the disadvantages of difficult separation at the low liquid nitrogen temperature during the measurement of hydrogen isotopes through the gas chromatography and complex measurement and error of volume correction factor in the area normalization method, breaks through the limitation that external standard method cannot be performed in the absence of standard deuterium depleted water sample, ensures high analysis precision and accuracy, small equipment investment, convenient operation and low analysis cost and makes the quantitative analysis of the deuterium content during the production of the deuterium depleted water convenient.

Description

Technical field [0001] The invention relates to a detection method, in particular to a method for detecting deuterium content in ultralight water. Background technique [0002] As we all know, water in nature is generally composed of 2 hydrogen atoms and 1 oxygen atom, but hydrogen atoms have 3 isotopes with different masses. The masses are 1, 2, 3 hydrogen, heavy hydrogen (deuterium), and super heavy hydrogen. (tritium). The content of deuterium in natural water is about 150 ppm. [0003] Research results show that deuterium is harmful to the survival, development and reproduction of living organisms, and no matter how much deuterium content in water is, it is toxic to living organisms. The replacement of hydrogen atoms by deuterium can generate additional stress in the helical structure of DNA, causing phase shifts, breaks, and replacements of the double helix, chaotic arrangement of ribonucleic acids, and even re-synthesis, resulting in mutations. Living organisms do not have...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 李猷陈汉文
Owner SHANGHAI RES INST OF CHEM IND
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