CN103776674A - Nitrogen extracting and purifying device of nitrogen isotope sample in water - Google Patents
Nitrogen extracting and purifying device of nitrogen isotope sample in water Download PDFInfo
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- CN103776674A CN103776674A CN201410024988.5A CN201410024988A CN103776674A CN 103776674 A CN103776674 A CN 103776674A CN 201410024988 A CN201410024988 A CN 201410024988A CN 103776674 A CN103776674 A CN 103776674A
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Abstract
The invention relates to a nitrogen extracting and purifying device of a nitrogen isotope sample in water. The nitrogen extracting and purifying device comprises a nitrogen bottle (1), a carbon dioxide absorption cold trap A (2), a carbon dioxide absorption cold trap B (5), a water-vapor absorption cold trap (6) and a U-shaped gas sample collector (8), which are successively connected end to end, wherein the gas outlet end of the U-shaped gas sample collector (8) is communicated with a long needle B (19) through a rubber tube, and the long needle B (19) enters below the liquid level in a gas monitoring cup B (10). The device has the advantages that a tedious chemical treatment process is avoided, and the device is time-saving and labor-saving and simple and efficient; the nitrate, nitrite and solubleness nitrogen in the water are completely converted into pure nitrous oxide gas or pure nitrogen which can be completely collected, so that the isotope fractionation is avoided; the CO2 and water-vapor can be removed, and the interference in testing is avoided; the device can be widely applied to the scientific search and production of colleges, scientific research institutions, industrial and mining enterprises, and the like.
Description
Technical field
The present invention relates to nitrogen isotope sample in a kind of water nitrogen extract and purifying plant, be mainly used in nitrate in water, nitrite, dissolubility nitrogen nitrogen stable isotope (
15n) pre-treatment of composition, belongs to element and isotope field tests in chemistry.
Background technology
In water, nitrate and nitrite are the pollutants that is difficult to removal.Nitrate In Drinking Water and content of nitrite are too high, can cause poisoning, the easy cancer stricken of long-term drinking.The source of understanding fully nitrate and nitrite in water is important environmental science problem.Due to the nitrate of separate sources and the nitrogen stable isotope of nitrite (
15n) composition is different, nitrogen stable isotope (
15n) become the important tool in nitrate and nitrite source in research water.
In water, nitrogen isotope pre-treatment is a loaded down with trivial details process slowly at present, its ultimate principle is that nitrate in water and nitrite are carried out to enrichment and precipitation, then the pressed powder of bone dry is sent into after stable isotope mass spectrometer (as MAT253) Pintsch process, generated nitrogen (N
2), then measure nitrogen stable isotope (
15n) composition.Subject matter: in (1) water, nitrate and nitrite carry out enrichment and precipitation needs super-clean environment, wastes time and energy, and must use the deionized water of high-quality in processing procedure; (2) use Zeo-karb when enrichment, exist ion-exchange not thorough, thereby cause nitrogen isotope fractionation; (3) if precipitation is not exclusively thorough, also can cause nitrogen isotope fractionation; (4) pressed powder Pintsch process in stable isotope mass spectrometer is not exclusively thorough, has nitrogen isotope fractionation.
Summary of the invention
The object of the invention is to overcome the shortcoming of prior art, provide the nitrogen of nitrogen isotope sample in a kind of water to extract and purifying plant, this device can be converted into pure nitrous oxide (N by nitrate, nitrite, dissolubility nitrogen in water
2o) gas or pure nitrogen (N
2), for stable isotope mass spectrometer (as MAT253) directly measure nitrogen stable isotope (
15n), there is not isotope fractionation in composition in processing procedure.
Object of the present invention is achieved through the following technical solutions: in a kind of water, the nitrogen of nitrogen isotope sample extracts and purifying plant, it comprises helium tank, carbon dioxide absorption cold-trap A, gas monitor cup A, carbon dioxide absorption cold-trap B, water vapor absorption cold-trap, temperature control cup A, U-shaped gaseous sample gatherer, temperature control cup B and gas monitor cup B, described helium tank is connected with carbon dioxide absorption cold-trap A, between helium tank and carbon dioxide absorption cold-trap A, be disposed with valve, tensimeter and flowmeter, carbon dioxide absorption cold-trap A is connected with carbon dioxide absorption cold-trap B, on pipeline between carbon dioxide absorption cold-trap A and carbon dioxide absorption cold-trap B, be provided with piston A, the inlet end of piston A is communicated with by minute hand A with gas monitor cup A, the outlet side of piston A is communicated with by hour hand with gas monitor cup A, carbon dioxide absorption cold-trap B is communicated with water vapor absorption cold-trap, and water vapor absorption cold-trap is placed in temperature control cup A, water vapor absorption cold-trap is communicated with the inlet end of U-shaped gaseous sample gatherer, and U-shaped gaseous sample gatherer is placed in temperature control cup B, and the outlet side of U-shaped gaseous sample gatherer is connected with minute hand B, and minute hand B stretches under the liquid level in gas monitor cup B.
Minute hand A in described sealed sample bottle and hour hand be all on the liquid level in sealed sample bottle, and minute hand A approaches liquid level, and hour hand approaches the bottleneck of sealed sample bottle.
Minute hand in gas monitor cup A and hour hand are all under the liquid level in gas monitor cup A.
The temperature range of described temperature control cup A is-70 ℃～0 ℃.
Described temperature control cup B is liquid nitrogen cup.
There are piston B and piston C in the inlet end of described U-shaped gaseous sample gatherer and outlet side respectively welding.
From above technical scheme, in water, nitrate, nitrite, dissolubility nitrogen are converted into pure nitrous oxide (N
2o) gas or pure nitrogen (N
2) after, this device is transferred to them in gaseous sample gatherer by cryogenic freezing under carrier gas condition, and guarantees to remove CO
2and steam, stable isotope mass spectrometer (as MAT253) mensuration nitrogen stable isotope for elimination (
15n) interference causing while composition.
The present invention has the following advantages:
1, without loaded down with trivial details chemical treating process, time saving and energy saving, simply efficient.
2, due to nitrate, nitrite, dissolubility nitrogen in water are converted into pure nitrous oxide (N completely
2o) gas or pure nitrogen (N
2), this device can be collected them completely, has avoided isotope fractionation.
3, this device can guarantee to remove CO
2and steam, the interference while having avoided test.
4, in water, the nitrogen of nitrogen isotope sample extracts and purifying plant, nitrate, nitrite, dissolubility nitrogen in water can be converted into pure nitrous oxide (N
2o) gas or pure nitrogen (N
2), for stable isotope mass spectrometer (as MAT253) directly measure nitrogen stable isotope (
15n) composition, in processing procedure, there is not isotope fractionation, high efficient and reliable, to the source of nitrate and nitrite in research water, solve a series of relevant environment problem in science significant, therefore apparatus of the present invention can be widely used in scientific research and the production of colleges and universities, scientific research institutions, industrial and mining enterprises etc.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention;
In figure: 1-helium tank, 2-carbon dioxide absorption cold-trap A, 3-sealed sample bottle, 4-gas monitor cup A, 5-carbon dioxide absorption cold-trap B, 6-water vapor absorption cold-trap, 7-temperature control cup A, 8-U shape gaseous sample gatherer, 9-temperature control cup B, 10-gas monitor cup B, 11-valve, 12-tensimeter, 13-flowmeter, 14-piston A, 15-minute hand A, 16-hour hand, 17-piston B, 18-piston C, 19-minute hand B.
Embodiment
Below in conjunction with accompanying drawing, the present invention will be further described, but protection scope of the present invention is not limited to the following stated.
As shown in Figure 1, in a kind of water, the nitrogen of nitrogen isotope sample extracts and purifying plant, it comprises helium tank 1, carbon dioxide absorption cold-trap A2, gas monitor cup A4, carbon dioxide absorption cold-trap B5, water vapor absorption cold-trap 6, temperature control cup A7, U-shaped gaseous sample gatherer 8, temperature control cup B9 and gas monitor cup B10, described helium tank 1 is connected with carbon dioxide absorption cold-trap A2, between helium tank 1 and carbon dioxide absorption cold-trap A2, be disposed with valve 11, tensimeter 12 and flowmeter 13, carbon dioxide absorption cold-trap A2 is connected with carbon dioxide absorption cold-trap B5, on pipeline between carbon dioxide absorption cold-trap A2 and carbon dioxide absorption cold-trap B5, be provided with piston A14, the inlet end of piston A14 is communicated with by minute hand A15 with gas monitor cup A4, the outlet side of piston A14 is communicated with by hour hand 16 with gas monitor cup A4, carbon dioxide absorption cold-trap B5 is communicated with water vapor absorption cold-trap 6, and water vapor absorption cold-trap 6 is placed in temperature control cup A7, water vapor absorption cold-trap 6 is communicated with the inlet end of U-shaped gaseous sample gatherer 8, and U-shaped gaseous sample gatherer 8 is placed in temperature control cup B9, and the outlet side of U-shaped gaseous sample gatherer 8 is connected with minute hand B19, and minute hand B19 stretches under the liquid level in gas monitor cup B10.
Minute hand A15 in described sealed sample bottle 3 and hour hand 16 be all on the liquid level in sealed sample bottle 3, and minute hand A15 approaches liquid level, and hour hand 16 approaches the bottleneck of sealed sample bottle 3.
The temperature range of described temperature control cup A7 is-70 ℃～0 ℃.
Described temperature control cup B9 is liquid nitrogen cup.
There are piston B17 and piston C18 in the inlet end of described U-shaped gaseous sample gatherer 8 and outlet side respectively welding.
The course of work of the present invention is as follows:
(1) sealed sample bottle 3 is evacuated, then injects appropriate water sample;
(2), if process nitrate or nitrite in water, inject and transform nitrous oxide (N to sealed sample bottle 3
2or nitrogen (N O)
2) denitrifying bacteria, under normal temperature, keep more than 6 hours.If dissolubility nitrogen in processing water, without adding any material to sealed sample bottle 3;
(3) minute hand A15 and hour hand 16 are put into gas monitor cup A4, minute hand B19 is put into gas monitor cup B10, the gas outlet of all pins is all below the liquid level in gas monitor cup;
(4) by filling CO in carbon dioxide absorption cold-trap A2 and carbon dioxide absorption cold-trap B5
2solid absorbent, opens piston A14, piston B17, piston C18;
(5) open valve 11, regulate tensimeter 12, make top hole pressure be not more than 0.6MP;
(6) adjust flux meter 13, maintenance gas flow is 20mL/s～50mL/s, at this moment can see in gas monitor cup A4 that minute hand A15 and hour hand 16 emit bubble, in gas monitor cup B10, minute hand B19 emits bubble.
(7) keep stable aeration status 5～15 minutes;
(8) put temperature control cup A7 at water vapor absorption cold-trap 6 places, the temperature range of temperature control cup A7 is-70～0 ℃;
(9) put temperature control cup B9 at U-shaped gaseous sample gatherer 8 places, temperature control cup B9 is liquid nitrogen cup;
(10) first hour hand 16 is taken out from gas monitor cup A4, lunge in sealed sample bottle 3, allow the gas outlet of hour hand 16 approach the bottleneck of sealed sample bottle 3.Then minute hand A15 is taken out from gas monitor cup A4, lunge in sealed sample bottle 3, allow the gas outlet of minute hand A15 approach water sample liquid level in sealed sample bottle 3;
(11) closure piston A14, adjust flux meter 13, maintenance gas flow is 10mL/s～40mL/s;
(12) keep stable aeration status 10～20 minutes;
(13) first closure piston C18, then closure piston B17, removes temperature control cup B9 from U-shaped gaseous sample gatherer 8, takes off U-shaped gaseous sample gatherer 8, completes pretreatment process.
Adopt the nitrogen extraction of nitrogen isotope sample in water of the present invention to verify with purifying plant, select high-purity KNO
3, KNO
2, N
2laboratory standard material, adopts respectively direct method of testing (Pintsch process of MAT253) and the inventive method to carry out contrast experiment, and experimental result is as follows:
From confirmatory experiment result, within the scope of measuring error (1 σ), the nitrogen stable isotope that adopts direct method of testing (Pintsch process of MAT253) and the inventive method to carry out pre-treatment to obtain (
15n) composition value is consistent.Therefore, in water of the present invention the nitrogen of nitrogen isotope sample extract with purifying plant can high efficient and reliable ground process nitrate, nitrite, dissolubility nitrogen in water, for nitrogen stable isotope (
15n), there is not isotope fractionation in the mensuration of composition in pretreatment process.
Claims (6)
1. in a water, the nitrogen of nitrogen isotope sample extracts and purifying plant, it is characterized in that: it comprises helium tank (1), carbon dioxide absorption cold-trap A(2), gas monitor cup A(4), carbon dioxide absorption cold-trap B(5), water vapor absorption cold-trap (6), temperature control cup A(7), U-shaped gaseous sample gatherer (8), temperature control cup B(9) and gas monitor cup B(10), described helium tank (1) and carbon dioxide absorption cold-trap A(2) be connected, helium tank (1) and carbon dioxide absorption cold-trap A(2) between be disposed with valve (11), tensimeter (12) and flowmeter (13), carbon dioxide absorption cold-trap A(2) with carbon dioxide absorption cold-trap B(5) be connected, carbon dioxide absorption cold-trap A(2) and carbon dioxide absorption cold-trap B(5) between pipeline on be provided with piston A(14), piston A(14) inlet end and gas monitor cup A(4) by minute hand A(15) be communicated with, piston A(14) outlet side and gas monitor cup A(4) be communicated with by hour hand (16), carbon dioxide absorption cold-trap B(5) be communicated with water vapor absorption cold-trap (6), water vapor absorption cold-trap (6) is placed in temperature control cup A(7) in, water vapor absorption cold-trap (6) is communicated with the inlet end of U-shaped gaseous sample gatherer (8), U-shaped gaseous sample gatherer (8) is placed in temperature control cup B(9) in, the outlet side of U-shaped gaseous sample gatherer (8) and minute hand B(19) be connected, and minute hand B(19) stretch into gas monitor cup B(10) in liquid level under.
2. in a kind of water according to claim 1, the nitrogen of nitrogen isotope sample extracts and purifying plant, it is characterized in that: the minute hand A(15 in described sealed sample bottle (3)) and hour hand (16) all on the liquid level in sealed sample bottle (3), and minute hand A(15) approach liquid level, hour hand (16) approaches the bottleneck of sealed sample bottle (3).
In a kind of water according to claim 1 the nitrogen of nitrogen isotope sample extract and purifying plant, it is characterized in that: described gas monitor cup A(4) in minute hand (15) and hour hand (16) all in gas monitor cup A(4) in liquid level under.
In a kind of water according to claim 1 the nitrogen of nitrogen isotope sample extract and purifying plant, it is characterized in that: described temperature control cup A(7) temperature range be-70 ℃～0 ℃.
5. in a kind of water according to claim 1, the nitrogen of nitrogen isotope sample extracts and purifying plant, it is characterized in that: described temperature control cup B(9) be liquid nitrogen cup.
6. in a kind of water according to claim 1, the nitrogen of nitrogen isotope sample extracts and purifying plant, it is characterized in that: there is piston B(17 the inlet end of described U-shaped gaseous sample gatherer (8) and outlet side respectively welding) and piston C(18).
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| CN201410024988.5A CN103776674A (en) | 2014-01-20 | 2014-01-20 | Nitrogen extracting and purifying device of nitrogen isotope sample in water |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104569220A (en) * | 2015-01-11 | 2015-04-29 | 中国科学院地理科学与资源研究所 | Pretreatment device for online determination of nitrate nitrogen isotope in liquid |
| CN105300765A (en) * | 2015-10-27 | 2016-02-03 | 中国科学院广州地球化学研究所 | Atmospheric aerosol organic carbon (OC)/element carbon (EC) visualized separation and preparation device |
| CN106501401A (en) * | 2016-10-21 | 2017-03-15 | 中国地质大学（北京） | A kind of device and method of quick measure water body ammonium nitrogen isotopics |
| CN109632412A (en) * | 2018-12-05 | 2019-04-16 | 中国科学院亚热带农业生态研究所 | One kind converting N for trace nitrogen2The auxiliary device of O |
| CN115046834A (en) * | 2022-08-17 | 2022-09-13 | 中国科学院地理科学与资源研究所 | Nitrite nitrogen isotope sample preparation device and method |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104569220A (en) * | 2015-01-11 | 2015-04-29 | 中国科学院地理科学与资源研究所 | Pretreatment device for online determination of nitrate nitrogen isotope in liquid |
| CN105300765A (en) * | 2015-10-27 | 2016-02-03 | 中国科学院广州地球化学研究所 | Atmospheric aerosol organic carbon (OC)/element carbon (EC) visualized separation and preparation device |
| CN105300765B (en) * | 2015-10-27 | 2018-10-30 | 中国科学院广州地球化学研究所 | A kind of atmospheric aerosol organic carbon (OC)/elemental carbon (EC) visualization separation preparation facilities |
| CN106501401A (en) * | 2016-10-21 | 2017-03-15 | 中国地质大学（北京） | A kind of device and method of quick measure water body ammonium nitrogen isotopics |
| CN106501401B (en) * | 2016-10-21 | 2020-02-28 | 中国地质大学（北京） | Device and method for rapidly determining water body ammonium nitrogen isotope composition |
| CN109632412A (en) * | 2018-12-05 | 2019-04-16 | 中国科学院亚热带农业生态研究所 | One kind converting N for trace nitrogen2The auxiliary device of O |
| CN109632412B (en) * | 2018-12-05 | 2021-07-27 | 中国科学院亚热带农业生态研究所 | A auxiliary device for trace nitrogen conversion N2O |
| CN115046834A (en) * | 2022-08-17 | 2022-09-13 | 中国科学院地理科学与资源研究所 | Nitrite nitrogen isotope sample preparation device and method |
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Application publication date: 20140507 |