Sample preparation method used for determining abundance of <15>N isotope of nitrite
A technology of isotopic abundance and nitrite, which is applied in the field of sample preparation for the determination of nitrite 15N isotopic abundance, can solve problems such as low test results and inapplicability, achieve a wide range of sampling amounts, improve accuracy, and test The effect of high data accuracy and precision
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Embodiment 1
[0052] Sodium nitrite- 15 N chemical reagent isotope abundance analysis, comprising the following steps:
[0053] (1) Preparation 15 NO gas
[0054] The reaction equipment adopted in the present invention is such as figure 1 In the double-ball reaction tube shown, one side of the double-ball reaction tube is two bulbs communicated by pipelines, and the liquid in the second bulb 2 can be entered into the first bulb 3 by tilting, and the double-ball reaction The other side of the tube can communicate with other equipment outside.
[0055] The sampling connector adopted in the present invention is as figure 2 As shown, there are two vacuum cock valves 5 in series in sequence, one end of which can be connected to the vacuum system or testing equipment, and the other end can be connected to the inlet port 1 of the double-ball reaction tube to vacuumize the double-ball reaction tube, and pass Close the vacuum stopcock 5 to realize the maintenance of vacuum degree.
[0056] Ta...
Embodiment 2
[0062] Nitrite in water samples 15 N isotope abundance analysis, including the following steps:
[0063] (1) Pretreatment of water quality samples
[0064] Water quality samples need to add a small amount of sodium carbonate solution to make the pH 7-8. When the nitrite content is lower than 20ppm (volume> 50mL), heat and concentrate at 90°C to about 6mL.
[0065] (2) Preparation 15 NO gas
[0066] Take 0.5mL of 2mol / L potassium iodide solution and 2mL of the treated sample in the first bulb 3 of the double bulb reaction tube, add 2mL of 5mol / L acetic acid solution in the second bulb 2, connect the inlet port 4 of the sampling connector Connect the vacuum system, the outlet port 6 of the sampling connector is connected to the inlet port 1 of the double-ball reaction tube, after the vacuum degree is lower than 50Pa, close the vacuum cock valve 5, and add the sulfuric acid in the second bulb 2 to the first bulb 3, and placed in a hot water bath at 60°C to 80°C for 5 minutes,...
Embodiment 3
[0072] Nitrite in soil samples 15 N isotope abundance analysis, including the following steps:
[0073] (1) Pretreatment of soil samples
[0074] The soil samples were dried at 70°C, crushed and ground after 3 hours, passed through a 0.25mm aperture soil sieve, and 10g of soil was added to 10mL of aqueous solution to adjust the pH to 7-8 with sodium carbonate, ultrasonically dissolved, and after standing for 30min, take the supernatant and seal it for later use. use;
[0075] (2) Preparation 15 NO gas
[0076] Take 0.5mL of 2mol / L potassium iodide solution and 2mL of the treated sample in the first bulb 3 of the double bulb reaction tube, add 2mL of 5mol / L acetic acid solution in the second bulb 2, connect the inlet port 4 of the sampling connector Connect the vacuum system, the outlet port 6 of the sampling connector is connected to the inlet port 1 of the double-ball reaction tube, after the vacuum degree is lower than 50Pa, close the vacuum cock valve 5, and add the sul...
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