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.
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[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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