CN109738529A - The method that dynamic air-distributing demarcates low-boiling point liquid and admixture of gas - Google Patents
The method that dynamic air-distributing demarcates low-boiling point liquid and admixture of gas Download PDFInfo
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Abstract
A kind of method that dynamic air-distributing demarcates low-boiling point liquid and admixture of gas, steps are as follows: diluent gas and the gas mixing for being bubbled sweeping method preparation are obtained the mixed gas of various concentration, mixed gas is obtained into corresponding spectrogram and peak area with gas chromatographic analysis, drafting obtains the standard curve between gas concentration and peak area.The present invention has the advantages that it is higher than the static volumetric method accuracy by gas diffusion effect to prepare gas using dynamic method；Dynamic air-distributing device is in parallel using multiple units, realizes liquid substance and gas distribution simultaneously, demarcates simultaneously conducive to various ingredients, improves and demarcate efficiency and accuracy, and test substance is avoided to influence each other caused error, and practical application value is bigger；Insulating box is added in dynamic air-distributing device, can be adjusted by temperature, make with gas concentration it is bigger, application range is wider.
Description
Technical field
The invention belongs to gas chromatographic analysis technique field, it is related to a kind of Specification Curve of Increasing method, more particularly to a kind of
The method that dynamic air-distributing demarcates low-boiling point liquid and admixture of gas.
Background technique
Gas chromatograph is that a kind of more mixtures separate, analyze tool, it is using gas as mobile phase, using punching
Wash the Column chromatography techniques of method.Gas-chromatography major function is not only to separate the various composition in mixture, but also wants
Qualitative and quantitative analysis is carried out to result.The quantitative analysis of gas-chromatography refers under given conditions, the response of instrument detection system
It is worth directly proportional to respective components concentration.Substantially it is exactly to measure chromatographic peak area and determine quantitative correction factor, mark is calculated
Directrix curve.Theoretically correction factor is only related with the type of measured object and reference substance and detector, but actually correction factor
There is relationship with gas composition and gas concentration, so standard curve is surveyed according to practical composition concentration range with standard gas as far as possible
It is fixed.
Various concentration effumability organic gas are prepared using Devince By Dynamic Gas Ration Method in patent CN104415675B, and are carried out
Line monitoring, is accurately obtained the concentration of required organic gas, prepares gas concentration error less than 3%.But used by this patent
Dynamic air-distributing method be only applicable to single volatile organic matter micro-concentrations measurement, have certain limitation.And in reality
Gas in production is mostly mixture, and for a kind of substance, mixed component influences the correction factor of this kind of substance, standard
Curve changes.
In order in the light of actual conditions demarcate to mixed component, the error generated when one pack system calibration one by one is avoided, originally
The admixture of gas of multicomponent volatile liquid is prepared in invention by bubbling/sweeping method, and is mixed with diluent gas component laggard
Enter gas chromatographic detection, solves the problems, such as that multi-component liquid substance is difficult to demarcate simultaneously with gaseous matter.It will sealing in the present invention
Tank is put into insulating box, prepare gas concentration range is wide, the standard curve error for demarcating drafting is smaller.
Summary of the invention
The purpose of the present invention is the gas-chromatographic titer methods of low-boiling point liquid and admixture of gas, using Devince By Dynamic Gas Ration Method
It prepares a variety of low-boiling point liquids simultaneously and the gas mixture of diluent gas enters gas chromatographic analysis, obtain the side of standard curve
Method.
In order to achieve the above object, the present invention is realized using following technical solutions:
Low-boiling point liquid prepares a series of various concentration gases by bubbling/sweeping method, and diluent gas and bubbling/sweeping method are matched
The gas mixing of system obtains new various concentration gas, obtains corresponding spectrogram and peak area subsequently into gas chromatographic analysis, draws
Standard curve between concentration processed and peak area.
This method includes distribution circuit design and builds, prepares gas concentration and draw three steps of standard curve, specifically
Implementation steps are as follows: (1) it is using dynamic air-distributing device n liquid, m diluent gas is in parallel, it is mixed according to certain flow；(2)
Liquid is prepared by bubbling/sweeping method, and diluent gas controls flow by flowmeter, is mixed to get a series of gas concentrations；(3)
Gas obtains the standard curve between concentration and peak area through gas chromatographic analysis, drafting after mixing.
(1) design of distribution pipeline and operating method (as shown in Figure 1) is built in:
Unit is 1.: low-boiling point liquid being placed in hermetically sealed can, hermetically sealed can is put into insulating box, and hermetically sealed can top is gas, carrier gas
Enter sealing tank level hereinafter, exit pipeline is more than liquid level by flowmeter 101, eluting gas passes through flowmeter 102
Flow is monitored, is equipped with blow valve after flowmeter 102, liquid reduction amount is measured using weight method.
Unit is 2.: diluent gas controls flow by flowmeter 01.
1. 2. parallel connection obtains mixed gas and enters gas chromatographic analysis n unit with m unit.
(2) gas concentration is prepared
The middle preparation gas concentration operating method of implementation steps (2) at a certain temperature, is passed through certain for insulating box into hermetically sealed can
Flow carrier gas is taken liquid out of using bubbling/purging in gaseous form, measures in a period of time liquid in hermetically sealed can by weight method
The reduction amount of body passes through the meter monitoring gas flow of outgoing quality flow 102 at this temperature and flow；Unit 2. in diluent gas
Gas is quantitatively passed through by flowmeter 01.The influence factor that bubbling/sweeping method prepares gas concentration has calorstat temperature and carrier gas
Body flow fixes a factor, and changing another factor can be obtained a series of gas with various concentration.
First by unit 1. in blow valve open, insulating box is passed through carrier gas into hermetically sealed can at certain temperature T, carries
Throughput is Vn01, liquid is taken out of in gaseous form using bubbling/purging, hermetically sealed can in a period of time t is measured by weighing method
The reduction amount of interior liquid is mn.It is then shut off blow valve, containing gas flow by the monitoring of exit flowmeter is Vn02；Unit
2. middle diluent gas is passed through quantitative gas, flow V by mass flow meters control0m, wherein mixed gas flow VIt is mixed totalFor all units
Middle Vn02With V0mThe sum of, CLiquid nFor unit 1. in the molar concentration of liquid in the mixture, MnFor the amount of the substance of respective liquid, CGas n
For unit 2. in the molar concentration of gas in the mixture.The molar concentration of each component in gaseous mixture are as follows:
,
,
The influence factor that bubbling/sweeping method prepares gas concentration has calorstat temperature T and diluting gas flow V0m, fix one
Factor, changing another factor can be obtained a series of gas with various concentration.
(3) standard curve is drawn
A series of mixed gas of various concentrations is obtained, through gas Chromatographic Determination, obtains a series of not cospectral graphs and in contrast
The peak area answered draws the standard curve between concentration and peak area.
Preferably, the low-boiling point liquid be under normal pressure be in liquid condition, boiling point at 250 DEG C or less such as: water, second
Sour methyl esters, ethyl acetate, ethyl alcohol, methanol, propyl alcohol, butanol, the tert-butyl alcohol, toluene, tert-butylamine, dimethylamine, tetrahydrofuran and acetic acid
Equal low-boiling point materials.
Preferably, the diluent gas is the substance for being under normal pressure gaseous state, boiling point is at 20 DEG C hereinafter, such as first
The gases such as alkane, ethylene, ethane, propane, n-butene, isobutene, butadiene, propylene, dimethyl ether, nitrogen, hydrogen and ammonia.
Preferably, described 1. 2. in parallel with m unit by n unit, wherein quantity n is more than or equal to 1, most preferably in 1-
5, quantity m is more than or equal to 0, most preferably at 1-5；
Preferably, the insulating box is at a certain temperature, temperature is at 0-300 DEG C, 20-60 DEG C of optimum temperature；
Preferably, described be passed through certain flow carrier gas into hermetically sealed can, wherein carrier gas flux is 10-1000ml/min, most preferably
Flow is 50-800ml/min；
Preferably, the diluent gas is controlled as quantitative by flowmeter, wherein diluting gas flow is 0-1000ml/min, most
Good flow is 10-800ml/min.
Compared with prior art, the advantages and positive effects of the present invention are:
The present invention relates to the methods that low-boiling point liquid and dilute gas mixture carry out gas-chromatographic titer simultaneously, and of the invention is excellent
Point is: (1) it is higher than the static volumetric method accuracy by gas diffusion effect to prepare gas using dynamic method；(2) dynamic
Air distributing device is in parallel using multiple units, realizes liquid substance and gas distribution simultaneously, demarcates, mention simultaneously conducive to various ingredients
Height calibration efficiency and accuracy, avoids test substance from influencing each other caused error, and practical application value is bigger；(3) dynamically match
Insulating box is added in device of air, can be adjusted by temperature, make with gas concentration it is bigger, application range is wider.
Detailed description of the invention
Fig. 1 is distribution flow chart of tube,
Fig. 2 is methanol calibration curve,
Fig. 3 is toluene calibration curve,
Fig. 4 be tert-butylamine and ammonia calibration curve,
Fig. 5 is ethyl alcohol, ethyl acetate and dimethyl ether calibration curve.
Specific embodiment
To better understand the objects, features and advantages of the present invention, right combined with specific embodiments below
The present invention is described further.It should be noted that in the absence of conflict, the spy in embodiments herein and embodiment
Sign can be combined with each other.
In the following description, numerous specific details are set forth in order to facilitate a full understanding of the present invention, still, the present invention may be used also
To be implemented using other modes described herein are different from, therefore, the present invention is not limited to the specific of specification is described below
The limitation of embodiment.
Embodiment 1
The calibration of methanol
(1) design of distribution pipeline with build
Unit is 1.: 50g methanol being placed in hermetically sealed can, hermetically sealed can is put into insulating box, and carrier gas enters sealing by flowmeter 101
In tank, prepare gas by 102 detection flows of flowmeter, methanol reduction amount is measured using weight method.Unit is 2.: diluent gas
Nitrogen controls flow by flowmeter 01 by pipeline.
(2) compounding methanol gas
First by unit 1. in blow valve open, insulating box is passed through carrier gas into hermetically sealed can at T=30 DEG C, and carrier gas flux is
V101For 50.00ml/min, methanol is taken out of in gaseous form using bubbling/purging, 240min hermetically sealed can is measured by weighing method
The reduction amount m of interior liquid1For 14.23g, it is then shut off blow valve, the gas stream containing methanol is monitored by exit flowmeter
Measure V102For 61.01ml/min；
2. middle nitrogen is controlled the flow V being passed through by flowmeter to unit01Respectively 10ml/min, 50ml/min, 100ml/min,
300ml/min and 500ml/min.
Methanol Molar concentration in gaseous mixture is calculated by formula (1) are as follows: 0.0261mol/L, 0.0167mol/L,
0.0115mol/L、0.0051mol/L、0.0033mol/L。
(3) standard curve is drawn
A series of mixed gas of various concentrations is obtained, through gas Chromatographic Determination, obtains a series of not cospectral graphs and in contrast
The peak area answered draws the standard curve (see figure 2) between Methanol Molar concentration and peak area.
Embodiment 2
The calibration of toluene
(1) design of distribution pipeline with build
Unit is 1.: 200g toluene being placed in hermetically sealed can, hermetically sealed can is put into insulating box, and carrier gas is entered close by flowmeter 101
In sealed cans, prepare gas by 102 detection flows of flowmeter, toluene reduction amount is measured using weight method.
Unit is 2.: not using diluent gas to dilute.
(2) toluene gas is prepared
First by unit 1. in blow valve open, insulating box is respectively at T=10 DEG C, 20 DEG C, 30 DEG C, 40 DEG C, 50 DEG C, Xiang Mi
Carrier gas, carrier gas flux V are passed through in sealed cans101For 200.00ml/min, toluene is taken out of in gaseous form using bubbling/purging,
The reduction amount m that 100min seals pot liquid is measured by weighing method1 differenceFor 6.13g, 11.87g, 26.62g, 66.08g,
100.46g is then shut off blow valve, and gas flow V containing toluene is monitored by exit flowmeter 102102Respectively
209.79ml/min、218.95ml/min、242.51ml/min、305.51ml/min、392.34ml/min。
Toluene molar concentration in gaseous mixture is calculated by formula (1) are as follows: 0.0030mol/L, 0.0048mol/L,
0.0084mol/L、0.0118mol/L、0.0147mol/L。
(3) standard curve is drawn
A series of mixed gas of various concentrations is obtained, through gas Chromatographic Determination, obtains a series of not cospectral graphs and in contrast
The peak area answered draws the standard curve (see figure 3) between toluene molar concentration and peak area.
Embodiment 3
The calibration in parallel of tert-butylamine and ammonia
(1) design of distribution pipeline with build
Unit is 1.: 150g tert-butylamine being placed in hermetically sealed can, hermetically sealed can is put into insulating box, and carrier gas is entered by flowmeter 101
In hermetically sealed can, prepare gas by flowmeter 102 monitor flow, using weight method measure tert-butylamine reduction amount.
Unit is 2.: diluent gas ammonia controls flow by flowmeter 01 by pipeline.
(2) mixed gas compounding
First by unit 1. in blow valve open, insulating box is passed through carrier gas into hermetically sealed can at T=30 DEG C, and carrier gas flux is
V101For 50.00ml/min, tert-butylamine is taken out of using bubbling/purging in gaseous form, 300min sealing is measured by weighing method
The reduction amount m of pot liquid1For 18.73g, it is then shut off blow valve, tert-butylamine is contained by the monitoring of exit flowmeter 102
Gas flow V102For 63.21ml/min；
Unit 2. in ammonia by flowmeter 01 control flow V01Respectively 20ml/min, 50ml/min, 100ml/min, 400ml/
Min and 700ml/min.
Tert-butylamine molar concentration in gaseous mixture is calculated by formula (1) and formula (2) are as follows: 0.0101mol/L, 0.0074mol/L,
0.0052mol/L,0.0018mol/L,0.0011mol/L；Ammonia molar concentration are as follows: 0.0153mol/L, 0.0281mol/L,
0.0390mol/L、0.0550mol/L、0.0584mol/L。
(3) standard curve is drawn
A series of mixed gas of various concentrations is obtained, through gas Chromatographic Determination, obtains a series of not cospectral graphs and in contrast
The peak area answered draws the standard curve (see figure 4) between tert-butylamine and ammonia molar concentration and peak area.
Embodiment 4
The calibration of ethyl alcohol, ethyl acetate and dimethyl ether
(1) design of distribution pipeline with build
Unit is 1.: 200g ethyl alcohol being placed in hermetically sealed can, hermetically sealed can is put into insulating box, and carrier gas is entered close by flowmeter 101
In sealed cans, prepare gas by 102 detection flows of flowmeter, ethyl alcohol reduction amount is measured using weight method.
200g methyl acetate is placed in hermetically sealed can, pipeline is built with identical air distributing method with ethyl alcohol, and by two units
It is in parallel.
Unit is 2.: diluent gas dimethyl ether controls flow by flowmeter 01 by pipeline.
(2) mixed gas compounding concentration
First by unit 1. in blow valve open, insulating box is passed through carrier gas, carrier gas flux into hermetically sealed can at T=40 DEG C
V101For 100.00ml/min, ethyl alcohol is taken out of using bubbling/purging in gaseous form, 180min sealing is measured by weighing method
The reduction amount m of pot liquid1For 28.56g, it is then shut off blow valve, the gas containing ethyl alcohol is monitored by exit flowmeter 102
Body flow V102For 150.49ml/min；
Methyl acetate is under similarity condition, gas of carrier gas flow V201For 150ml/min, 180min reduction amount m is measured2For
34.67g monitoring V202For 187.94ml/min.
2. middle dimethyl ether gas is controlled the flow V being passed through by flowmeter to unit01Respectively 20ml/min, 80ml/min,
150ml/min, 300ml/min and 400ml/min.
Ethyl alcohol molar concentration in gaseous mixture is calculated by formula (1) and formula (2) are as follows: 0.0096mol/L, 0.0082mol/L,
0.0071mol/L,0.0054mol/L,0.0047mol/L；Ethyl acetate molar concentration are as follows: 0.0061mol/L, 0.0052mol/
L,0.0045mol/L,0.0034mol/L,0.0030mol/L；Dimethyl ether molar concentration is 0.0038mol/L, 0.0130mol/
L、0.0209mol/L、0.0321mol/L、0.0369mol/L。
(3) standard curve is drawn
A series of mixed gas of various concentrations is obtained, through gas Chromatographic Determination, obtains a series of not cospectral graphs and in contrast
The peak area answered, the standard curve (see figure 5) between drafting ethyl alcohol, methyl acetate and dimethyl ether molar concentration and peak area.
The above described is only a preferred embodiment of the present invention, being not that the invention has other forms of limitations, appoint
What those skilled in the art changed or be modified as possibly also with the technology contents of the disclosure above equivalent variations etc.
It imitates embodiment and is applied to other fields, but without departing from the technical solutions of the present invention, according to the technical essence of the invention
Any simple modification, equivalent variations and remodeling to the above embodiments, still fall within the protection scope of technical solution of the present invention.
Claims (9)
1. a kind of method of dynamic air-distributing calibration low-boiling point liquid and admixture of gas, it is characterised in that, steps are as follows: will dilute
Gas and the gas mixing for being bubbled sweeping method preparation obtain the mixed gas of various concentration, by mixed gas gas chromatographic analysis
Corresponding spectrogram and peak area are obtained, drafting obtains the standard curve between gas concentration and peak area.
2. the method for dynamic air-distributing calibration low-boiling point liquid according to claim 1 and admixture of gas, it is characterised in that,
Specific step is as follows:
(1) using dynamic air-distributing device that n liquid and m diluent gas is in parallel；
(2) under flowmeter control, m diluent gas is used to the various concentration gas for being bubbled sweeping method and being precipitated with n liquid
Body mixing, obtains mixed gas；
(3) by mixed gas gas chromatographic analysis, the standard curve between gas concentration and peak area is obtained.
3. the method for dynamic air-distributing calibration low-boiling point liquid according to claim 2 and admixture of gas, it is characterised in that,
Specific step is as follows for n liquid bubbling sweeping method in the step (2): low-boiling point liquid being placed in hermetically sealed can, hermetically sealed can
It is put into insulating box, hermetically sealed can top is gas, and carrier gas enters sealing tank level hereinafter, exit is managed by inlet flow rate meter
More than liquid level, eluting gas monitors flow by outlet stream meter on road, blow valve is equipped with after outlet stream meter, using weight method
Measure liquid reduction amount.
4. the method for dynamic air-distributing calibration low-boiling point liquid according to claim 3 and admixture of gas, it is characterised in that,
Various concentration gas is obtained by control calorstat temperature or diluting gas flow in the step (2).
5. the method for dynamic air-distributing calibration low-boiling point liquid according to claim 3 or 4 and admixture of gas, feature exist
In the low-boiling point gas is to be in a liquid state under normal temperature and pressure, and for boiling point in 250 DEG C of substances below, the diluent gas is room temperature
It is gaseous state under normal pressure, boiling point is in 20 DEG C of substances below.
6. the method for dynamic air-distributing calibration low-boiling point liquid according to claim 2 and admixture of gas, it is characterised in that,
The n numerical value is more than or equal to 1, and preferably 1-5, m numerical value is more than or equal to 0, preferably 1-5.
7. the method for dynamic air-distributing calibration low-boiling point liquid according to claim 3 or 4 and admixture of gas, feature exist
In the calorstat temperature is 0-300 DEG C, preferably 20-60 DEG C.
8. the method for dynamic air-distributing calibration low-boiling point liquid according to claim 3 or 4 and admixture of gas, feature exist
In the carrier gas flux is 10-1000ml/min, preferably 50-800ml/min.
9. the method for dynamic air-distributing calibration low-boiling point liquid according to claim 3 or 4 and admixture of gas, feature exist
In the diluting gas flow is 0-1000ml/min, preferably 10-800ml/min.
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Cited By (1)
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Application publication date: 20190510 |