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Preparation method of abundant <13> CO2 standard gas

A standard gas, high-abundance technology, applied in the field of carbon isotopes, can solve the problems of inconvenient storage and transportation, high cost of screening, cumbersome methods, etc.

Active Publication Date: 2017-05-17
BEIJING HUAGEN ANBANG TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, infrared spectrometers need to use standard gases for detection on a regular basis. At present, there are basically two ways to prepare standard gases used in the market: the first is to use 13 C and 12 The C isotope gas is mixed in the gas according to the ratio of the standard gas abundance to obtain the standard gas. This method needs to be mixed by a special gas mixing device and a large amount of batch preparation is required. The method is cumbersome, and after preparation, there is storage The transportation is inconvenient, resulting in a high final price, which can even reach 10,000 yuan / liter; the second is to select a large number of carbon salt manufacturers in different regions, and compare and screen them one by one with mass spectrometry after processing. Appropriate proportions of the two solids are then decomposed to produce gas, although this method can obtain a stable abundance ratio 13 C / 12 C gas; but screening requires a lot of work and the cost of screening is very high. If the manufacturer's production standards are slightly adjusted or the source of raw materials is changed, the product must be re-screened

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  • Preparation method of abundant &lt;13&gt; CO2 standard gas
  • Preparation method of abundant &lt;13&gt; CO2 standard gas
  • Preparation method of abundant &lt;13&gt; CO2 standard gas

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preparation example Construction

[0056] The present invention provides a high abundance 13 CO 2 The preparation method of gas comprises the following steps:

[0057] 1) the solid or liquid 13 After the C source reacts, we get 13 CO 2 gas, reacted again with barium hydroxide solution to obtain 13 Barium carbonate of C;

[0058] said 13 The abundance value of the C source is greater than the natural abundance and less than or equal to 100%;

[0059] 2) Get the above steps 13 After the barium carbonate of C is mixed with barium carbonate, mixture A is obtained;

[0060] 3) After the mixture A obtained in the above steps is mixed with calcium carbonate again, the mixture B is obtained;

[0061] 4) react the mixture B obtained in the above steps with an acid to obtain a high-abundance 13 CO 2 gas.

[0062] The present invention at first solid or liquid 13 After the C source reacts, we get 13 CO 2 gas, reacted again with barium hydroxide solution to obtain 13 C barium carbonate.

[0063] The presen...

Embodiment 1

[0123] 1, 13 C urea refining:

[0124] Take 20 boxes 13 Add 200mL of absolute ethanol to the solid of the C urea kit, and put the beaker into the ultrasonic wave for 0.5 hours to fully dissolve it. Filtrate under reduced pressure, repeat the dissolution of the filter cake by the above method, combine the filtrate, and concentrate the filtrate under reduced pressure (0.080-0.095MPa, 45-55°C) to obtain a white solid 13 C urea sample (contains a certain amount of auxiliary materials).

[0125] 2. High abundance 13 CO 2 gas preparation, and 13 C barium carbonate solidification:

[0126] The white solid obtained above 13 C urea sample, 2.33g sodium nitrite solid, 25mL water were added to the reaction flask, 2N dilute sulfuric acid was added dropwise, the generated gas was absorbed with a clear aqueous solution of saturated barium hydroxide, a white precipitate was produced, and the last remaining gas in the system was blown with nitrogen into a barium hydroxide solution, an...

Embodiment 2

[0142] 1, 13 C urea refining:

[0143] Take 20 boxes 13 Add 150mL of absolute ethanol to the solid of the C urea kit, and put the beaker into the ultrasonic wave for 1 hour to fully dissolve it. Filtrate under reduced pressure, repeat the dissolution of the filter cake by the above method, combine the filtrate, and concentrate the filtrate under reduced pressure (0.080-0.095MPa, 45-55°C) to obtain a white solid 13 C urea sample (contains a certain amount of auxiliary materials).

[0144] 2. High abundance 13 CO 2 gas preparation, and 13 C barium carbonate solidification:

[0145] The white solid obtained above 13 C urea sample, 2.30g sodium nitrite solid, 20mL water were added to the reaction flask, 2N dilute sulfuric acid was added dropwise, the generated gas was absorbed with a clear aqueous solution of saturated barium hydroxide, a white precipitate was produced, and the last remaining gas in the system was blown with nitrogen into a barium hydroxide solution, and f...

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Abstract

The invention provides a preparation method of abundant <13> CO2 standard gas. The method comprises steps as follows: firstly, a solid or liquid <13>C source reacts to produce <13>CO2 gas, the <13>CO2 gas reacts with a barium hydroxide solution again to produce barium carbonate of <13>C; the abundance of the <13>C source is larger than the natural abundance and smaller than or equal to 100%; then a mixture A is obtained after the barium carbonate of <13>C obtained in the last step is mixed with barium carbonate; a mixture B is obtained after the mixture A obtained in the last step is mixed with calcium carbonate again; finally, the mixture B obtained in the last step reacts with acid to produce the abundant <13>CO2 gas. The prepared gas has good uniformity, the method is high in stability, low in preparation cost and short in preparation period, the gas is easy to store and transport, can be prepared at any time as required and can be prepared in small batches, the preparation amount is controllable, and the gas is good in stability and high in accuracy when used for detecting <13>C infrared spectrometers.

Description

technical field [0001] The invention belongs to the technical field of carbon isotopes, and relates to a high-abundance 13 CO 2 The preparation method of standard gas, especially relates to a kind of high abundance 13 CO 2 Preparation method and detection of standard gas 13 C infrared spectrometer method. Background technique [0002] Different nuclides of the same element with the same number of protons and different numbers of neutrons in microscopic particles are isotopes (Isotopes). Isotopes are different atoms of the same element that have the same number of protons but different numbers of neutrons. Example: Carbon has multiple isotopes, 12 C. 13 C and 14 C (radioactive), etc. Although isotopes occupy the same position on the periodic table and have almost the same chemical properties (the properties of protium, deuterium and tritium are slightly different), their atomic mass or mass number is different, so their mass spectrometry properties, radioactive trans...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/50
CPCC01B2210/0026
Inventor 龚爱华马胜利郑君军图布新
Owner BEIJING HUAGEN ANBANG TECH CO LTD