CN106018539B - A kind of measurement N2The method of O or NO gas nitrogen isotope ratio - Google Patents
A kind of measurement N2The method of O or NO gas nitrogen isotope ratio Download PDFInfo
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- CN106018539B CN106018539B CN201610534302.6A CN201610534302A CN106018539B CN 106018539 B CN106018539 B CN 106018539B CN 201610534302 A CN201610534302 A CN 201610534302A CN 106018539 B CN106018539 B CN 106018539B
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Abstract
The invention discloses one kind to be based on elemental analyser-stable isotope mass spectrograph combined apparatus N2The detection method of O or NO gas nitrogen isotope ratio is continuously passed through inert gas from the air inlet of elemental analyser oxidation tube, and by under test gas sample N2O or NO is injected by the injection port of gas sample injection device, under test gas N2It is N that O or NO, which enters elemental analyser reduction tube by hot copper reduction with inert gas,2Later, continue to enter stable isotope mass spectrograph with inert gas, stable isotope mass spectrograph detects nitrogen isotope ratio.Measurement N of the present invention2The method of O or NO nitrogen isotope ratio, it is easy to operate it is simple and direct, data reappearance is fabulous, and have very high accuracy, can rapidly and accurately demarcate N2O, the nitrogen isotope ratio of NO.
Description
Technical field
The present invention relates to a kind of detection methods of gas isotope ratio, and in particular to one kind is steady based on elemental analyser-
Determine isotope mass spectrometer combined apparatus measurement N2The method of O or NO gas nitrogen isotope ratio.
Background technique
N2O is the mass spectrometric reference gas of common nitrogen stable isotope in laboratory, true value relationship detected sample
The accuracy of product measured value is significant to entire isotope test result.In recent years, many foreign study personnel start to analyze
N2The isotope allosterism of O15NαWith15NβBetween relationship, deepen continuously and inquire into N2The approach that O is generated.NO is as N2O isotope
Allosterism15NαReference gas, more and more widely be applied to mass spectral analysis work in, therefore, to NO, N2O working stamndard
The calibration of gas nitrogen isotope ratio is particularly significant.
Calibration to the isotopic ratio of laboratory work calibrating gas, there are three types of methods.First is that utilizing two-way sample introduction system
System carries out the measurement of two-way comparative measurement method, second is that fixed using elemental analyser and isotope mass spectrometry combined instrument (EA-IRMS) reactionary slogan, anti-communist poster
Method is measured, third is that using minimum gas pre-concentration device, it is most laggard by the gas of required calibration by the concentration of cold-trap
Enter stable isotope mass spectrograph to be measured.But since double path system is more expensive, many laboratories are not equipped with；And
The anti-scaling method of EA-IRMS can only demarcate N2And CO2Nitrogen and carbon isotope ratio, and N can not be demarcated2The nitrogen of O and NO gas
Isotopic ratio.In addition, minimum gas pre-concentration device staking-out work calibrating gas, needs to be diluted gas, gas exists
It is inevitably contaminated in dilution, the accuracy of calibration result is caused to reduce.
Summary of the invention
The purpose of the present invention is to provide one kind based on elemental analyser-stable isotope mass spectrograph combined apparatus measurement
N2The method of the nitrogen isotope ratio of O or NO gas, the measuring method are convenient, fast.Using detection method of the present invention
N can accurately be measured2The nitrogen isotope ratio of O or NO gas, testing result preci-sion and accuracy are fully able to meet
The needs of research work.
In order to complete foregoing invention purpose, present invention employs a kind of elemental analyser-stable isotope mass spectrograph combinations
Device, the combined apparatus include elemental analyser oxidation tube, elemental analyser reduction tube, stable isotope mass spectrograph and gas
Body sampling device, the gas sample injection device include connecting tube, and the connecting tube both ends are respectively fixedly connected with a washer, described
Be interspersed with a screw on the outside of connecting tube, the end of thread of the screw is directed toward washer, the gas sample injection device by screw and
Washer is threadedly coupled with the gas outlet of elemental analyser oxidation tube and elemental analyser reduction tube air inlet respectively；The gas
It is additionally provided with the cover type nut of sample feeding pipe, top equipped with injection port on sampling device, is provided with rubber at the sample feeding pipe top
Rubber spacer is fixed in cover type nut by dottle pin, the cover type nut by connecting with sample feeding pipe outside screw；The connection
A firm banking is provided on the outside of pipe, between two terminal screw of connecting tube, the bottom of the sample feeding pipe is fixed on the fixed base,
And it is connected to the connecting tube in firm banking.The gas outlet of the elemental analyser reduction tube and stable isotope are mass spectrometric
Injection port connection.
N is detected based on elemental analyser-stable isotope mass spectrograph combined apparatus2O or NO gas nitrogen isotope ratio
Method includes the following steps: that the air inlet from elemental analyser oxidation tube is continuously passed through inert gas, and by under test gas sample
N2O or NO gas is injected by the injection port of gas sample injection device, under test gas N2O or NO gas enters element point with inert gas
Analyzer reduction tube is N by hot copper reduction2Later, continue to enter stable isotope mass spectrograph, stable isotope matter with inert gas
Spectrometer detects nitrogen isotope ratio.
The connecting tube, screw and washer are stainless steel products；Firm banking, sample feeding pipe are copper product.
The N2O and NO gas is the gas of steel cylinder gas or single pure natural abundance.
The steel cylinder gas is commercially available cyclinder gas, wherein other impurities gas is not present, ingredient is single.
The single pure natural abundance gas are as follows: such as measurement N2When, sample to be tested the inside can only contain N2This one kind contains
N gas cannot contain N2The gases such as O or NO, otherwise can interference measurement, but can containing without N gas, such as CO2Deng not
The presence of the gas containing N would not influence to measure.
The inert gas is preferably helium.
The hot copper reduction temperature of elemental analyser reduction tube is 400-680 DEG C.
The under test gas sample N2O or NO gas sampling volume is 0.1-0.5mL.
It is described that sample introduction is carried out to gaseous sample to be measured using gas-tight syringe.
Elemental analyser of the gas detection method of the present invention based on inventor's designed, designed-stable isotope mass spectrograph
Combined apparatus is used in combination using elemental analyser reduction tube with stable isotope mass spectrograph, can both not have two-way sample introduction
The measurement of gaseous sample is carried out under conditions of system, and can demarcate the isotopic ratio of a variety of working stamndard gases.Using this hair
Bright the method demarcates N2When O and NO gas, it is only necessary to the N of known isotopic ratio2As reference gas.
The utility model has the advantages that using of the present invention a kind of based on elemental analyser-stable isotope mass spectrograph combined apparatus
N2The detection method of O or NO gas nitrogen isotope ratio, can either demarcate N2The nitrogen isotope ratio of the high-purity cyclinder gas of O and NO
Value, while can also measure the single pure N of natural abundance2The nitrogen isotope ratio of O and NO gaseous sample.The detection side
Method also has the advantage that
1. precision, stability are high: the method for the invention measures NO or N2The nitrogen isotope ratio of O, the δ measured15NAirFor ‰ maximum changing range only within 0.5 ‰, this has absolutely proved that detection of the present invention has very high measurement steady
It is qualitative.
2. accuracy is high: measuring NO or N using distinct methods2The result of O gas isotope ratio and side of the present invention
The result that method measures is compared, as a result between coincide it is fine, illustrate that the accuracy of the method for the invention is able to satisfy completely and grind
Study carefully requirements of one's work.
3. easy to operate: elemental analyser of the present invention-stable isotope mass spectrograph combined apparatus installation is simple, square
Just, based on the detection method of described device, operating procedure is simple, only simple sample introduction is needed to can be obtained by accurate detection number
According to.
Detailed description of the invention
Fig. 1 is a kind of elemental analyser of the invention-stable isotope mass spectrograph combined apparatus gas sample injection device
Structural schematic diagram.Wherein 1 is connecting tube；2 be firm banking；3 be screw；4 be washer；5 be rubber spacer；6 be cover type nut；
7 be sample feeding pipe；8 be injection port.
Fig. 2 is a kind of elemental analyser of the invention-stable isotope mass spectrograph combined apparatus structural schematic diagram.Its
In 9 be hot copper；10 be quartz ampoule；11 be O-ring seal；12 be gas sample injection device；13 be elemental analyser oxidation tube；14 are
Elemental analyser reduction tube.
Specific embodiment
To further illustrate the technical scheme of the present invention below with reference to the accompanying drawings and specific embodiments.
A kind of elemental analyser-stable isotope mass spectrograph combined apparatus, including elemental analyser oxidation tube 13, element
Analyzer reduction tube 14 and stable isotope mass spectrograph are additionally provided with a gas sample injection device 12 on the combined apparatus,
The gas sample injection device 12 includes connecting tube 1, and 1 both ends of connecting tube are respectively fixedly connected with a washer 4, the connecting tube
1 outside is interspersed with a screw 3, and the end of thread of the screw 3 is directed toward washer 4；The gas sample injection device 12 passes through 3 He of screw
Washer 4 is connect with the gas outlet of elemental analyser oxidation tube 13 and 14 air inlet of elemental analyser reduction tube respectively；The gas
Body sampling device 12 further includes the cover type nut 6 that the threaded sample feeding pipe 7 in an outside and a top are equipped with injection port, institute
It states and is provided with rubber spacer 5 at the top of sample feeding pipe 7, the cover type nut 6 with 7 outside screw of sample feeding pipe by connecting rubber spacer
5 are fixed in cover type nut 6.A firm banking 2, institute are provided between 1 liang of 1 outside of connecting tube, connecting tube terminal screw 3
The bottom for stating sample feeding pipe 1 is fixed on firm banking 2, and is connected to the connecting tube 1 in firm banking 2.The elemental analyser
The gas outlet of reduction tube 14 is connect with the mass spectrometric injection port of stable isotope.
The connecting tube 1, screw 3 and washer 4 are stainless steel products；Firm banking 2, sample feeding pipe 7, cover type nut 6 are
Copper product.
N used in following embodiment2O and NO gas is commercially available single pure cyclinder gas or single pure
The gas of natural abundance.
Embodiment 1:
Helium is continuously passed through from the air inlet of elemental analyser oxidation tube, and by No.1 N to be measured2O gaseous sample is by gas
The injection port of sampling device injects, No.1 N2O gas enters elemental analyser reduction tube by hot copper reduction (N with continuous helium stream2O
It is completely reduced as N2) and then by continuous helium stream by the N after conversion2Bring stable isotope mass spectrograph, stable isotope into
Mass spectrograph detects nitrogen isotope ratio.
The sample volume of under test gas is 0.3mL in the present embodiment, the temperature by controlling hot copper reduction is respectively 400 DEG C,
550 DEG C and 680 DEG C；Compare influence of the hot copper reduction temperature to nitrogen isotope ratio testing result.
It is measured under the conditions of different hot copper reduction temperature, No.1 N2The nitrogen isotope ratio result of O gaseous sample is such as
Shown in table 1:
Table 1: No.1 N is measured at a temperature of different hot copper reductions2The result of O gaseous sample nitrogen isotope ratio
When the control of hot copper reduction temperature is in 550 DEG C and 680 DEG C, the No.1 N that measures2The δ of O gaseous sample15NAir‰ is very steady
It is fixed, it varies less, precision is high.Due to consideration that the factors such as sample injection volume and concentration, we use 680 DEG C of hot copper to protect
Card under test gas is thoroughly restored.When selective reduction temperature is 680 DEG C, the No.1 N that measures2The δ of O reference gas sample15NAir‰
Average value are as follows: δ15NAir‰=- 1.75 ± 0.012.
Embodiment 2
Hot copper reduction method measures No. two N2O reference gas.
The step of with embodiment 1, is essentially identical, and difference is adjusted to 680 DEG C in the temperature of hot copper.
No. two N2The results are shown in Table 2 for the nitrogen isotope ratio of O reference gas sample:
Table 2: different hot No. two N of copper reduction temperature measuring2The result of O reference gas sample
When reduction temperature is 680 DEG C, No. two N measuring2The δ of O reference gas sample15NAir‰ average value are as follows: δ15NAir‰
=-1.73 ± 0.036.
Comparative example 3:
To No.1 N2O gaseous sample is using the result measured in the two-way comparative measurement method and embodiment 1 of isotope mass spectrometry
It is compared, the results are shown in Table 3.Wherein the temperature of hot copper reduction is adjusted to 680 DEG C, and under test gas sample volume is 0.3mL.
Table 3: distinct methods measure No.1 N2The nitrogen isotope ratio of O gaseous sample
That mutually coincide between the result that two methods obtain as can be seen from Table 3 is fine, illustrates the method for the invention
Accuracy and the prior art it is essentially identical, be able to satisfy the needs of research work completely.
Embodiment 4:
The step of implementation steps of embodiment 4 are with embodiment 1 is essentially identical, unlike, under test gas is NO gas, heat
Copper temperature is respectively set as 400 DEG C, 550 DEG C and 680 DEG C, and the sampling volume of gaseous sample is respectively 0.1mL, 0.3mL and 0.5
ML, measurement result are as shown in table 4:
Table 4: the result for the NO gas nitrogen isotope that different hot copper reduction temperature and gas sampling volume measure
Find out from the result of table 4, the either variation of reduction tube temperature or the change of sample volume, the NO reference gas measured
Body δ15NAir‰ maximum changing range is only within 1 ‰；It is most of wherein when hot copper reduction temperature is at 550 DEG C or more
The variation range of measurement result is both less than 0.5 ‰；This has been absolutely proved based on elemental analyser-stable isotope mass spectrograph connection
There is very high stability with the method for device measurement NO gas nitrogen isotope ratio.
Embodiment 5:
NO gaseous sample is compared using the result measured in the two-way comparative measurement method and embodiment 4 of isotope mass spectrometry
Compared with the results are shown in Table 4.Wherein the temperature of hot copper reduction is adjusted to 680 DEG C, and under test gas sample volume is 0.3mL.
Table 4: the nitrogen isotope ratio of distinct methods measurement NO gaseous sample
That mutually coincide between the result that two methods obtain as can be seen from Table 4 is fine, illustrates the method for the invention
Accuracy and the prior art it is essentially identical, be able to satisfy the needs of research work completely.
Claims (6)
1. a kind of based on elemental analyser-stable isotope mass spectrograph combined apparatus N2The inspection of O or NO gas nitrogen isotope ratio
Survey method, which is characterized in that the combined apparatus include elemental analyser oxidation tube (13), elemental analyser reduction tube (14),
Stable isotope mass spectrograph and gas sample injection device (12), the gas outlet and the same position of stability of the elemental analyser reduction tube
The mass spectrometric injection port connection of element；The gas sample injection device (12) includes connecting tube (1), and connecting tube (1) both ends are each logical
Cross screw (3) and washer (4) respectively with the gas outlet of elemental analyser oxidation tube and elemental analyser reduction tube air inlet spiral shell
Line connection；Sample feeding pipe (7) is additionally provided on the gas sample injection device (12), top is equipped with the cover type nut of injection port (8)
(6), at the top of the sample feeding pipe (7) at be provided with rubber spacer (5), the cover type nut (6) by with spiral shell on the outside of sample feeding pipe (7)
Rubber spacer (5) is fixed in cover type nut (6) by line connection；It is provided with a firm banking (2) outside the connecting tube (1),
The bottom of the sample feeding pipe (7) is fixed on firm banking (2), and is connected to the connecting tube (1) in firm banking (2)；
Described method includes following steps: being continuously passed through inert gas from the air inlet of elemental analyser oxidation tube (13), and will
Under test gas sample N2O or NO gas is injected by the injection port (8) of gas sample injection device (12), under test gas N2O or NO gas with
It is N that inert gas, which enters elemental analyser reduction tube (14) by hot copper reduction,2Later, N2Continue to enter with inert gas and stablize together
Position quality spectrometer, stable isotope mass spectrograph detect nitrogen isotope ratio.
2. according to claim 1 a kind of based on elemental analyser-stable isotope mass spectrograph combined apparatus N2O or NO
The detection method of gas nitrogen isotope ratio, which is characterized in that the N2O and NO gas be steel cylinder gas or it is single it is pure from
Right abundance gas.
3. according to claim 1 a kind of based on elemental analyser-stable isotope mass spectrograph combined apparatus N2O or NO
The detection method of gas nitrogen isotope ratio, which is characterized in that the inert gas is helium.
4. according to claim 1 a kind of based on elemental analyser-stable isotope mass spectrograph combined apparatus N2O or NO
The detection method of gas nitrogen isotope ratio, which is characterized in that the hot copper reduction temperature of elemental analyser reduction tube (14) is
400-680℃。
5. according to claim 1 a kind of based on elemental analyser-stable isotope mass spectrograph combined apparatus N2O or NO
The detection method of gas nitrogen isotope ratio, which is characterized in that the under test gas sample N2O or NO gas sampling volume is
0.1-0.5mL。
6. according to claim 1 a kind of based on elemental analyser-stable isotope mass spectrograph combined apparatus N2O or NO
The detection method of gas nitrogen isotope ratio, which is characterized in that using gas-tight syringe to N to be measured2O or NO gas carry out into
Sample.
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| CN110887721B (en) * | 2018-09-07 | 2024-06-11 | 核工业理化工程研究院 | Sample purification device and sample purification method for gas isotope analysis |
| CN117783378B (en) * | 2024-02-28 | 2024-05-28 | 中国科学院地球环境研究所 | Flow self-adaptive control device, mass spectrometer, nitrogen isotope determination system and method |
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