CN109490445A - A method of oxygen and nitrogen content in measurement acetylene gaseous mixture - Google Patents
A method of oxygen and nitrogen content in measurement acetylene gaseous mixture Download PDFInfo
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- CN109490445A CN109490445A CN201811630870.1A CN201811630870A CN109490445A CN 109490445 A CN109490445 A CN 109490445A CN 201811630870 A CN201811630870 A CN 201811630870A CN 109490445 A CN109490445 A CN 109490445A
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- G—PHYSICS
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- G01N30/02—Column chromatography
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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Abstract
The invention discloses a kind of methods of oxygen and nitrogen content in measurement acetylene gaseous mixture, use high purity acetylene gas as background gas first, certain amount of air is added and prepares Standard Gases, after ten-way valve converts sample introduction, go out the peak area of each component by gas Chromatographic Determination, the content of oxygen in Standard Gases, nitrogen, acetylene and carbon dioxide is derived according to calculation relational expression simultaneously, analysis method is demarcated using each component content and corresponding peak area, the content of oxygen, nitrogen, acetylene and carbon dioxide in acetylene gaseous mixture is determined with this standard method.The present invention measures the content of oxygen, nitrogen, acetylene and carbon dioxide in acetylene gaseous mixture by area normalization method, and the method preci-sion and accuracy is high, reproducible and easy to operate, quick.
Description
Technical field
The present invention relates to a kind of measuring method, oxygen and nitrogen content in specifically a kind of measurement acetylene gaseous mixture
Method.
Background technique
Acetylene (HC ≡ CH) is simplest alkynes.Pure acetylene is a kind of colourless, tasteless, flammable gas, is slightly soluble in water,
It is soluble in ethyl alcohol, acetone and other organic solvent.Industrial production acetylene gas is mainly the following method: carbide, methane cracking method,
Hydrocarbon cracking method etc..It is that hydrolysis occurs by calcium carbide and water to generate using calcium carbide method acetylene production gas, easy band in production process
There are a small amount of oxygen, nitrogen and carbon dioxide.If oxygen content is excessively high, easily explode, there are security risks;If nitrogen
(inert gas), carbon dioxide gas content are excessively high, and nitrogen, carbon dioxide gas accumulation, equal conditions are also easy to produce in reactor
Acetylene and acetic acid mole ratio reduce in lower reactor, and reaction rate slows down, and seriously affect product quality.Therefore production process
The middle content for needing each component in strict control acetylene gaseous mixture.
By literature search, each component Content Test method is chemical analysis method in domestic acetylene gaseous mixture at present, is first
Acetone acetylene gas is selected, remaining a small amount of acetylene gas is absorbed with silver nitrate, then uses KOH absorption titanium dioxide
Carbon gas, then oxygen is absorbed with alkaline pyrogallic acid, it is nitrogen that residue, which does not participate in reaction gas,.Change as can be seen from the above
It learns method of inspection and has the disadvantage in that 1. reaction solution concentration proportion control is inaccurate, easily causes inspection result error, accuracy
Difference, inspection result can not effective Instructing manufactures;2. examining frequently, checkout procedure largely consumes reaction solution, and reaction solution can not follow
Ring utilizes, and improves production cost;3. checkout procedure is cumbersome, the period is long, human and material resources are largely consumed;4. reaction result cannot and
When Instructing manufacture;5. reaction solution discharge easily causes environmental pollution.Physical method there is no to measure acetylene gaseous mixture at present by literature search
The analysis method of middle each component.
Summary of the invention
The present invention is directed to above-mentioned existing deficiencies in the technology, provides oxygen in a kind of measurement acetylene gaseous mixture
It with the method for nitrogen content, is measured using physical method, instrument can accurately determine each component in acetylene gaseous mixture
Content, sample energy consumption is few, and batch processing sample analysis speed is fast, and inspection result is accurate.
The method that the present invention measures oxygen and nitrogen content in acetylene gaseous mixture, includes the following steps:
Step 1: the preparation of Standard Gases
The preparation of Standard Gases uses static volumetric method.Prepare the syringe and vacuum that 100ml and 5ml is clean, dry respectively
Airbag is extracted in the high purity acetylene gas injection vacuum airbag of 98ml twice in succession with the syringe of 100ml, then with the injection of 5ml
Device is drawn 4ml air and is injected in the vacuum bag equipped with 196ml high purity acetylene gas, shakes up to get Standard Gases, this Standard Gases is
200ml, volume fraction shared by oxygen, nitrogen, acetylene and carbon dioxide is respectively 0.42%, 1.56%, 97.9%, 0.06%.
Step 2: gas Chromatographic Determination
The Standard Gases that step 1 is prepared are measured by gas-chromatography, determine the peak area of each component, while in gas
The volume fraction and archive of each component are inputted in phase chromatographic work station, are measured 3 times under equal conditions, are taken being averaged for 3 peak areas
Value;
Gas chromatograph parameters are adjusted, after stablizing, acetylene gaseous mixture to be measured is converted into sample introduction, benefit by ten-way valve
Acetylene gas and carbon dioxide are detained with Q column, oxygen, nitrogen first pass through 13X molecular sieve column and separated, the dioxy of delay
Change carbon, acetylene are converted into GDX-102 chromatographic column again by ten-way valve separated at the appointed time, and detector will separate
Constitutional changes record out chromatogram at electric signal, by recorder, obtain peak area according to respective components chromatographic peak, are returned using area
One, which changes method, measures constituent content, replication 3 times, takes measurement result average value three times;
Step 3: the calculating of relative correction factor
Calculation formula is as follows:
In formulaThe relative amount correction factor of-component to be measured to reference substance;
gwiThe Absolute Calibration factor of-component to be measured;
gwsThe Absolute Calibration factor of-reference substance component;
mi- volume components percentage to be measured, %;
msThe percentage by volume of-reference substance, %;
AiThe peak area of-component to be measured;
AsThe peak area of-reference substance.
Step 4: the calculating of constituent content in acetylene gaseous mixture to be measured
Calculation formula is as follows:
In formula: wiContent of-component the i to be measured in acetylene gaseous mixture;
A1、A2...Ai...AnThe peak area of each component to be measured in-acetylene gaseous mixture;
g1、g2...gi...gnThe Absolute Calibration factor of each component to be measured in-acetylene gaseous mixture;
gsThe Absolute Calibration factor of-reference substance component;
G1、G2...Gi...GnRelative mass correction factor of each component to be measured to reference substance in-acetylene gaseous mixture.
In the present invention, when being measured by gas chromatography, location parameter is provided that
Gas chromatograph: SP-3420A, TCD detector;
Chromatographic column: Q column, 4m × 3mm;
13X molecular sieve column, 3m × 3mm;
GDX-102 chromatographic column, 3m × 3mm;
Temperature programming:, keeping 3min by 50 DEG C of initial temperature, rises to 100 DEG C with 10 DEG C/min, keeps 5min;
Sample injector temperature: 100 DEG C;
Spare furnace temperature: 100 DEG C;
Detector temperature: 150 DEG C;
Hot-wire temperature: 180 DEG C;
Bridge stream stationary value: 206mA;
Sensitivity: 0.5;
Carrier gas: hydrogen, flow rate of carrier gas: 30ml/min;
Air velocity: 300ml/min;
Ten-way valve conversion parameter: original state -1, -2 keep conversion after 0.02s extremely to connect 13X molecular sieve column state 1,2,
Keep 1.6min after, go back to initially with GDX-102 chromatographic column on-state -1, -2.
Measuring method of the present invention, suitable for measuring each component industrial acetylene (acetylene gas concentration >=90%) gaseous mixture
Content.
The method of the present invention selects high purity acetylene gas to demarcate as background gas and divides component content comparable Standard Gases in sample,
The content of each component in acetylene gaseous mixture is measured by gas chromatography, preci-sion and accuracy is high, reproducible, and operates letter
Just, quickly.
Detailed description of the invention
Fig. 1 is the device of each component content method in the industrial acetylene gaseous mixture of chromatographic.
Fig. 2 (a) is the chromatogram of standard specimen, and Fig. 2 (b) is the chromatogram of Specimen Determination of the present invention.Peak in Fig. 2 (a), Fig. 2 (b)
1 is the chromatographic peak of oxygen, and peak 2 is the chromatographic peak of nitrogen, and peak 3 is the chromatographic peak of acetylene gas, and peak 4 is the chromatographic peak of carbon dioxide.
Specific embodiment
As best seen in figure 1, in the present embodiment utilize gas chromatograph device, including carrier gas device, regulating valve, sample injector,
Ten-way valve, chromatographic column, detector.
Chromatographic condition:
Gas chromatograph: SP-3420A, TCD detector;
Chromatographic column: Q column, 4m × 3mm;
13X molecular sieve column, 3m × 3mm;
GDX-102 chromatographic column, 3m × 3mm;
Temperature programming:, keeping 3min by 50 DEG C of initial temperature, rises to 100 DEG C with 10 DEG C/min, keeps 5min;
Sample injector temperature: 100 DEG C;
Spare furnace temperature: 100 DEG C;
Detector temperature: 150 DEG C;
Hot-wire temperature: 180 DEG C;
Bridge stream stationary value: 206mA;
Sensitivity: 0.5;
Carrier gas: hydrogen, flow rate of carrier gas: 30ml/min;
Air velocity: 300ml/min;
Acetylene gas: high-purity
Using the content of each component in area normalization method measurement acetylene gaseous mixture in the present embodiment, the specific steps are as follows:
Step 1: the preparation of Standard Gases
The preparation of Standard Gases uses static volumetric method.Prepare the syringe and vacuum that 100ml and 5ml is clean, dry respectively
Airbag is extracted in the high purity acetylene gas injection vacuum airbag of 98ml twice in succession with the syringe of 100ml, then with the injection of 5ml
Device is drawn 4ml air and is injected in the vacuum bag equipped with 196ml high purity acetylene gas, shakes up to get Standard Gases, this Standard Gases is
200ml, volume fraction shared by oxygen, nitrogen, acetylene and carbon dioxide is respectively 0.42%, 1.56%, 97.9%, 0.06%.
Step 2: gas Chromatographic Determination
The Standard Gases that step 1 is prepared are measured by gas-chromatography, determine the peak area of each component, while in gas
The volume fraction and archive of each component are inputted in phase chromatographic work station, are measured 3 times under equal conditions, are taken being averaged for 3 peak areas
Value;
Gas chromatograph parameters are adjusted, after stablizing, acetylene gaseous mixture to be measured is converted into sample introduction, benefit by ten-way valve
Acetylene gas and carbon dioxide are detained with Q column, oxygen, nitrogen first pass through 13X molecular sieve column and separated, the dioxy of delay
Change carbon, acetylene are converted into GDX-102 chromatographic column again by ten-way valve separated at the appointed time, and detector will separate
Constitutional changes record out chromatogram at electric signal, by recorder, obtain peak area according to respective components chromatographic peak, are returned using area
One, which changes method, measures constituent content, replication 3 times, takes measurement result average value three times;
Step 3: the calculating of relative correction factor
Calculation formula is as follows:
In formulaThe relative amount correction factor of-component to be measured to reference substance;
gwiThe Absolute Calibration factor of-component to be measured;
gwsThe Absolute Calibration factor of-reference substance component;
mi- volume components percentage to be measured, %;
msThe percentage by volume of-reference substance, %;
AiThe peak area of-component to be measured;
AsThe peak area of-reference substance.
Step 4: the calculating of constituent content in acetylene gaseous mixture to be measured
Calculation formula is as follows:
In formula: wiContent of-component the i to be measured in acetylene gaseous mixture;
A1、A2...Ai...AnThe peak area of each component to be measured in-acetylene gaseous mixture;
g1、g2...gi...gnThe Absolute Calibration factor of each component to be measured in-acetylene gaseous mixture;
gsThe Absolute Calibration factor of-reference substance component;
G1、G2...Gi...GnRelative mass correction factor of each component to be measured to reference substance in-acetylene gaseous mixture.
(2) method applicability and accuracy test
1, the preparation of Standard Gases
The preparation of Standard Gases uses static volumetric method.It is true to prepare 100ml and 5ml cleaning, dry syringe and 3 parts respectively
Air bag, with 100ml syringe respectively to injection 196ml, 296ml, 396ml high purity acetylene gas in vacuum bag, then the note with 5ml
Emitter injects the air of 4ml into vacuum bag respectively, oxygen, nitrogen, acetylene and carbon dioxide in 3 parts of Standard Gases at this time after mixing
Volume fraction be all respectively (1) 0.42%, 1.56%, 97.9%, 0.06%;(2) 0.28%, 1.04%, 98.6%,
0.04%;(3) 0.21%, 0.78%, 98.95%, 0.03%.
2, the system suitability of method
The Standard Gases 100ml prepared in above-mentioned steps is extracted in drying, clean syringe, sealing.By above-mentioned gas phase color
Spectral condition is measured, and sees Fig. 2 (a).The chromatographic peak separating degree of each component is good, show chromatographic column to the selectivity of each component and
The system suitability of method is good.
3, linear relationship is tested
Take 3 parts of above-mentioned series standard gas 100ml and industrial sample to be tested in having numbered and dried, clean syringe respectively
In, sealing.By above-mentioned chromatographic condition sequentially determining, peak area of each component is successively recorded.With each group in Standard Gases and sample to be tested
Swarming area ratio is ordinate, and the concentration of each component is abscissa in Standard Gases and sample to be tested, carries out linear regression.As a result see
Table 1.In the range of linearity shown in table 1, each component area ratio is with measurement concentration in good in each Standard Gases and each sample to be tested
Linear relationship.Correlation coefficient r is respectively 0.9995 and 0.9999.
Table 1
Regression equation | r | The range of linearity (%) |
Y=0.0820X+0.0286 | 0.9995 | 0.02-99 |
Y=0.0089X+0.0037 | 0.9999 | 0.02-99 |
4, minimum detectability is tested
Industrial acetylene gaseous mixture is selected, by identical GC conditions continuous sample introduction six times, according to the side of Standard Gases calibration
Method is measured, and with 3 times of calculating of baseline noise, each component limit of identification is respectively 0.04% and 0.1%.
5, accuracy test
No. 2 Standard Gases are selected, are measured by identical GC conditions, are repeated sample introduction 3 times, normative reference method pair
3 times sample introduction result is measured, and lower deviation is not more than 0.02 in measurement result three times, it is sufficient to illustrate that this method accuracy is good.
Claims (5)
1. a kind of method of oxygen and nitrogen content in measurement acetylene gaseous mixture, it is characterised in that include the following steps:
Step 1: the preparation of Standard Gases
The preparation of Standard Gases uses static volumetric method.Prepare the syringe and vacuum airbag that 100ml and 5ml is clean, dry respectively,
It is extracted in the high purity acetylene gas injection vacuum airbag of 98ml twice in succession with the syringe of 100ml, then drawn with the syringe of 5ml
It during vacuum bag of the 4ml air injection equipped with 196ml high purity acetylene gas is interior, shakes up to get Standard Gases, this Standard Gases is 200ml, oxygen
Volume fraction shared by gas, nitrogen, acetylene and carbon dioxide is respectively 0.42%, 1.56%, 97.9%, 0.06%;
Step 2: gas Chromatographic Determination
The Standard Gases that step 1 is prepared are measured by gas-chromatography, determine the peak area of each component, while in gas phase color
The volume fraction and archive for inputting each component in work station are composed, is measured 3 times under equal conditions, takes the average value of 3 peak areas;
Gas chromatograph parameters are adjusted, after stablizing, acetylene gaseous mixture to be measured is converted into sample introduction by ten-way valve, utilizes Q
Column is detained acetylene gas and carbon dioxide, and oxygen, nitrogen first pass through 13X molecular sieve column and separated, the titanium dioxide of delay
Carbon, acetylene are converted into GDX-102 chromatographic column again by ten-way valve separated at the appointed time, and detector will separate group
Divide and be transformed into electric signal, chromatogram is recorded out by recorder, peak area is obtained according to respective components chromatographic peak, utilizes area normalization
Change method measures each component content, replication 3 times, takes measurement result average value three times.
2. according to the method described in claim 1, it is characterized by:
The calculation formula of relative correction factor is as follows:
In formulaThe relative amount correction factor of-component to be measured to reference substance;
gwiThe Absolute Calibration factor of-component to be measured;
gwsThe Absolute Calibration factor of-reference substance component;
mi- volume components percentage to be measured, %;
msThe percentage by volume of-reference substance, %;
AiThe peak area of-component to be measured;
AsThe peak area of-reference substance.
3. according to the method described in claim 2, it is characterized by:
The calculation formula of constituent content is as follows in acetylene gaseous mixture to be measured:
In formula: wiContent of-component the i to be measured in acetylene gaseous mixture;
A1、A2...Ai...AnThe peak area of each component to be measured in-acetylene gaseous mixture;
g1、g2...gi...gnThe Absolute Calibration factor of each component to be measured in-acetylene gaseous mixture;
gsThe Absolute Calibration factor of-reference substance component;
G1、G2...Gi...GnRelative mass correction factor of each component to be measured to reference substance in-acetylene gaseous mixture.
4. according to the method described in claim 1, it is characterized by:
In step 2, when being measured by gas chromatography, location parameter is provided that
Gas chromatograph: SP-3420A, TCD detector;
Chromatographic column: Q column, 4m × 3mm;
13X molecular sieve column, 3m × 3mm;
GDX-102 chromatographic column, 3m × 3mm;
Temperature programming:, keeping 3min by 50 DEG C of initial temperature, rises to 100 DEG C with 10 DEG C/min, keeps 5min;
Sample injector temperature: 100 DEG C;
Spare furnace temperature: 100 DEG C;
Detector temperature: 150 DEG C;
Hot-wire temperature: 180 DEG C;
Bridge stream stationary value: 206mA;
Sensitivity: 0.5;
Carrier gas: hydrogen, flow rate of carrier gas: 30ml/min;
Air velocity: 300ml/min.
5. according to the method described in claim 1, it is characterized by:
Ten-way valve conversion parameter: original state -1, -2, conversion is kept to 13X molecular sieve column state 1,2 is connected after keeping 0.02s
After 1.6min, go back to initially with GDX-102 chromatographic column on-state -1, -2.
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Cited By (3)
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CN112098537A (en) * | 2020-08-25 | 2020-12-18 | 茌平信发华宇氧化铝有限公司 | Method for detecting content of oxygen and nitrogen in acetylene |
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