CN108387653A - A kind of method of ethanol content in measurement industrial methanol - Google Patents
A kind of method of ethanol content in measurement industrial methanol Download PDFInfo
- Publication number
- CN108387653A CN108387653A CN201810123211.2A CN201810123211A CN108387653A CN 108387653 A CN108387653 A CN 108387653A CN 201810123211 A CN201810123211 A CN 201810123211A CN 108387653 A CN108387653 A CN 108387653A
- Authority
- CN
- China
- Prior art keywords
- sample
- ethanol content
- methanol
- industrial methanol
- analysis
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
- G01N30/68—Flame ionisation detectors
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The present invention relates to analysis and testing technology fields, specifically disclose a kind of method measuring ethanol content in industrial methanol.The method, under selected operating condition, after vaporization, constant temperature is detached sample by capillary chromatographic column, each component, is detected with flame ionization ditector, with quantified by external standard method, calculates the mass fraction of ethyl alcohol.Method provided by the invention, sample are not required to pre-processing, and direct injection analysis improves analysis efficiency；Sample is not required to that internal standard compound is added, and saves analysis cost, reduces the interference of isopropanol in sample；Using Constant Temperature Detection instrument stabilizer, baseline stability, the interval analyzed twice is short, and the lookup reason that goes wrong is relatively easy, and improves instrument utilization rate and service life；It is detected using not shunt method, improves Monitoring lower-cut, reinforce micro-analysis result accuracy.
Description
Technical field
The present invention relates to analysis and testing technology field more particularly to a kind of methods measuring ethanol content in industrial methanol.
Background technology
Ethyl alcohol is the homologue of methanol, and physicochemical properties are very close with methanol, and the purity of fine methanol is very high in addition
(99.96% or more), main peak is very wide, is easy to cover ethyl alcohol peak, and on most fixers, ethyl alcohol peak is after methanol peak
Outflow, is influenced seriously by main peak, this analysis for allowing for micro ethanol in methanol becomes a problem.Domestic many enterprises now
Regulation ethanol content measurement gas chromatography in methanol GB338-2011 is all used to be measured analysis.
However, the existing assay method sample preparation time is longer, sample preparation is complicated, and analysis time is long；Because it need to be added in
Object isopropanol is marked, increases analysis cost, and Chong Die with internal standard compound containing isopropanol in product；It may using temperature programming when analysis
It can cause baseline fluctuation, to impact analysis result；Split ratio is greatly affected to analysis result of content when low.
Invention content
Longer for the sample preparation time existing for existing method, sample preparation is complicated, and analysis time is long, costly, and
Using temperature programming and the problems such as analyzing easy impact analysis result is shunted, ethyl alcohol contains in a kind of measurement industrial methanol of present invention offer
The method of amount.
To achieve the above object of the invention, the embodiment of the present invention uses the following technical solution：
The method of ethanol content, includes the following steps in a kind of measurement industrial methanol：
(1) prepare chromatograph operating condition
Chromatographic column：AB-PLOT U, 30m × 0.32mm × 7um；
Detector：Flame ionization detector；
Column temperature：100℃；
Temperature of vaporization chamber：150℃；
Detector temperature：300℃；
Air mass flow：400mL/min；
Hydrogen flowing quantity：40mL/min；
Carrier gas：N2, column flow：8.0mL/min；
Sample size：0.6uL；
The chromatographic column is polarity porous polymer bonding capillary column AB-PLOT U；
(2) titer of 3 kinds of different ethanol contents is prepared, the solute of the titer is analysis straight alcohol, and solvent is color
Compose pure methanol；
(3) after chromatograph stabilization, the titer of 3 kinds of different ethanol contents is sent into chromatograph with injector and is examined
It surveys, recorder calculates correction factor f '；
(4) after chromatograph stabilization, sample to be tested feeding chromatograph is detected with injector, obtains sample to be tested
Peak area Ai, according to following formula
W=f ' × Ai × 100
Wherein, w is the content of ethyl alcohol in sample to be tested；
It repeats step (4) at least twice, calculates separately the content of ethyl alcohol in sample to be tested；
(5) it is ethanol content result in final methanol to take the arithmetic mean of instantaneous value of Parallel testing result in step (4).
Wherein, in correction factor f ' and sample to be tested ethyl alcohol content w, be the recorder by being used cooperatively with chromatograph
It is directly automatic to calculate gained.
Compared with the existing technology, the method provided by the invention for measuring ethanol content in industrial methanol, sample are not required to early period
Processing, direct injection analysis improve analysis efficiency；Sample is not required to that internal standard compound is added, and saves analysis cost, reduces isopropyl in sample
The interference of alcohol；Interval using Constant Temperature Detection instrument stabilizer, baseline stability, Parallel testing is short, and going wrong, it is opposite to search reason
Simply, and instrument utilization rate and service life are improved；It is detected using not shunt method, improves Monitoring lower-cut, reinforce micro-analysis
As a result accuracy.
Description of the drawings
It to describe the technical solutions in the embodiments of the present invention more clearly, below will be to needed in the embodiment
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for ability
For the those of ordinary skill of domain, without creative efforts, it can also be obtained according to these attached drawings other attached
Figure.
Fig. 1 is the chromatogram of sample to be tested in the embodiment of the present invention.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
The embodiment of the present invention provides a kind of method measuring ethanol content in industrial methanol.Ethyl alcohol in the measurement industrial methanol
The method of content, includes the following steps：
(1) prepare chromatograph operating condition
Chromatographic column：AB-PLOT U, 30m × 0.32mm × 7um；
Detector：Flame ionization detector；
Column temperature：100℃；
Temperature of vaporization chamber：150℃；
Detector temperature：300℃；
Air mass flow：400mL/min；
Hydrogen flowing quantity：40mL/min；
Carrier gas：N2, column flow：8.0mL/min；
Sample size：0.6uL；
The chromatographic column is polarity porous polymer bonding capillary column AB-PLOT U；
(2) titer of 3 kinds of different ethanol contents is prepared, the solute of the titer is analysis straight alcohol, and solvent is color
Compose pure methanol；
(3) after chromatograph stabilization, the titer of 3 kinds of different ethanol contents is sent into chromatograph with injector and is examined
It surveys, recorder calculates correction factor f '；
(4) after chromatograph stabilization, sample to be tested feeding chromatograph is detected with injector, obtains sample to be tested
Peak area Ai, according to following formula
W=f ' × Ai × 100
Wherein, w is the content of ethyl alcohol in sample to be tested；
It repeats step (4) at least twice, calculates separately the content of ethyl alcohol in sample to be tested；
(5) it is ethanol content result in final methanol to take the arithmetic mean of instantaneous value of Parallel testing result in step (4).
Specifically, chromatographic column AB-PLOT U are far superior to WAX maos to ethyl alcohol in industrial methanol and isopropanol separating effect
Capillary chromatographic column, AB-PLOT U post separation degree is higher than WAX chromatographic columns under the conditions of same analysis.
Column temperature uses 100 DEG C, because gas chromatograph can be carried out with 2, fashionable dress or more chromatographic column in real work
Different sample detections, if another chromatogram column analysis sample result accuracy, program can be influenced using the method for temperature programming
Heating analysis terminates to cool down and be stabilized to original state time length and distinct methods switching time is long, every ginseng in temperature-rise period
Number variation is higher to instrument requirements, and baseline is not easy to stablize, and the probability to go wrong is more, and impact analysis efficiency lowering apparatus makes
Use the service life；And industrial methanol component is relatively narrow compared with simple, boiling point distribution to use temperature programming to analyze, Constant Temperature Detection instrument
Stablize, baseline stability, the interval analyzed twice is short, and the lookup reason that goes wrong is relatively easy, can fill column on a chromatograph
Chromatographic column similar in temperature and detector detect different samples, improve instrument utilization rate and device longevity, reduce analysis cost, together
When, distinct methods switching time can shorten, and improve analysis efficiency.
Temperature of vaporization chamber is 150 DEG C, ensures that each component can gasify in methanol sample, and ensure methanol, ethyl alcohol not
It is thermal decomposited.
Detector temperature is 300 DEG C, prevents detector burning from generating the pollution of the condensation and combustion product of water.
Preferably, the high polymer is polystyrene-divinylbenzene, has effects that adsorb and detach well.
Preferably, volume fraction >=99.99% of the hydrogen ensures the precision of analysis.
Preferably, the hydrogen removes micro-moisture, carbon dioxide and oxygen in hydrogen using silica gel molecular sieve purification device,
The purity for ensureing hydrogen, helps to improve the precision of analysis.
Preferably, the N2Volume fraction >=99.99%, ensure analysis precision.
Preferably, the N2N is removed using silica gel molecular sieve purification device2Middle micro-moisture, carbon dioxide and oxygen improve
The purity of nitrogen ensures the precision of analysis.
Preferably, the air removes micro-moisture, carbon dioxide and oxygen in air using silica gel molecular sieve purification device,
Ensure the precision of analysis.
Preferably, the recorder is chromatographic work station, quickly analyzes correction factor, time saving and energy saving.
Preferably, the injector is 10uL micro syringes, completes the sample introduction of titer and sample to be tested.
Preferably, as the mass fraction ＜ 0.01% of ethyl alcohol in sample to be tested, the parallel determinations twice it is exhausted
To difference≤0.0005%；As the mass fraction ＞ 0.01% of ethyl alcohol in sample to be tested, the parallel determinations twice
Absolute difference≤0.001% ensures the precision of analysis.
The method of ethanol content, sample are not required to pre-processing in measurement industrial methanol provided in an embodiment of the present invention, directly
Sample introduction is analyzed, improves analysis efficiency；Sample is not required to that internal standard compound is added, and saves analysis cost, reduces the interference of isopropanol in sample；
Using Constant Temperature Detection instrument stabilizer, baseline stability, the interval analyzed twice is short, and the lookup reason that goes wrong is relatively easy, and carries
High instrument utilization rate and service life；It is detected using not shunt method, improves Monitoring lower-cut, it is accurate to reinforce micro-analysis result
Property.
Method in order to better illustrate ethanol content in measurement industrial methanol provided in an embodiment of the present invention, below by
Embodiment is further to be illustrated.
Embodiment 1
The method for measuring ethanol content in industrial methanol, includes the following steps：
(1) prepare chromatograph operating condition
Chromatographic column：AB-PLOT U, 30m × 0.32mm × 7um；
Detector：Flame ionization detector；
Column temperature：100℃；
Temperature of vaporization chamber：150℃；
Detector temperature：300℃；
Air mass flow：400mL/min；
Hydrogen flowing quantity：40mL/min；
Carrier gas：N2, column flow：8.0mL/min；
Sample size：0.6uL；
The chromatographic column is polarity expanded polystyrene-divinylbenzene bonding capillary column AB-PLOT U；
(2) 100mL volumetric flasks are taken, after assay balance is weighed, is weighed using pipette addition Chromatographic Pure Methanol and is denoted as m1,
Analysis straight alcohol is added using micro syringe to weigh and be denoted as m2, is diluted to groove with Chromatographic Pure Methanol and weighs and be denoted as m3, according to
Sample to be tested contains amount of alcohol, by following formula
The titer of 3 kinds of different ethanol contents is prepared, the solute of the titer is analysis straight alcohol, and solvent is chromatographically pure
Methanol；
(3) after chromatograph stabilization, the standard of 3 kinds of different ethanol contents of 0.6uL is taken respectively with 10uL micro syringes
Liquid is sent into chromatograph and is detected, and recorder calculates correction factor f '；
(4) it after chromatograph stabilization, takes 0.6uL samples to be tested to be sent into chromatograph with 10uL micro syringes and is detected,
Obtain the peak area Ai of sample to be tested, wherein the retention time of methanol and ethyl alcohol is respectively 2.014min and 8.721min, is such as schemed
1, according to following formula
W=f ' × Ai × 100
The content w of ethyl alcohol in sample to be tested is calculated；
(5) take in step (4) that the arithmetic mean of instantaneous value of parallel determinations is that ethanol content result is in final methanol twice
68.0000ppm。
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
Any modification, equivalent replacement or improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.
Claims (10)
1. a kind of method measuring ethanol content in industrial methanol, it is characterised in that：Include the following steps：
(1) prepare chromatograph operating condition
Chromatographic column：AB-PLOT U, 30m × 0.32mm × 7um；
Detector：Flame ionization detector；
Column temperature：100℃；
Temperature of vaporization chamber：150℃；
Detector temperature：300℃；
Air mass flow：400mL/min；
Hydrogen flowing quantity：40mL/min；
Carrier gas：N2, column flow：8.0mL/min；
Sample size：0.6uL；
The chromatographic column is polarity porous polymer bonding capillary column AB-PLOT U；
(2) titer of 3 kinds of different ethanol contents is prepared, the solute of the titer is analysis straight alcohol, and solvent is chromatographically pure
Methanol；
(3) after chromatograph stabilization, the titer of 3 kinds of different ethanol contents is sent into chromatograph with injector and is detected, is remembered
It records instrument meter and calculates correction factor f '；
(4) after chromatograph stabilization, sample to be tested feeding chromatograph is detected with injector, obtains the peak face of sample to be tested
Product Ai, according to following formula
W=f ' × Ai × 100
Wherein, w is the content of ethyl alcohol in sample to be tested；
It repeats step (4) at least twice, calculates separately the content of ethyl alcohol in sample to be tested；
(5) it is ethanol content result in final methanol to take the arithmetic mean of instantaneous value of Parallel testing result in step (4).
2. a kind of method measuring ethanol content in industrial methanol as described in claim 1, it is characterised in that：The polarity is more
High polymer in the high polymer bonding capillary column AB-PLOT U of hole is polystyrene-divinylbenzene.
3. a kind of method measuring ethanol content in industrial methanol as described in claim 1, it is characterised in that：The hydrogen
Volume fraction >=99.99%.
4. a kind of method measuring ethanol content in industrial methanol as claimed in claim 3, it is characterised in that：The hydrogen is adopted
Micro-moisture, carbon dioxide and oxygen in hydrogen are removed with silica gel molecular sieve purification device.
5. a kind of method measuring ethanol content in industrial methanol as described in claim 1, it is characterised in that：The N2Body
Fraction >=99.99%.
6. a kind of method measuring ethanol content in industrial methanol as claimed in claim 5, it is characterised in that：The N2Using
Silica gel molecular sieve purification device removes N2Middle micro-moisture, carbon dioxide and oxygen.
7. a kind of method measuring ethanol content in industrial methanol as described in claim 1, it is characterised in that：The air is adopted
Micro-moisture, carbon dioxide and oxygen in air are removed with silica gel molecular sieve purification device.
8. a kind of method measuring ethanol content in industrial methanol as described in claim 1, it is characterised in that：The recorder
For chromatographic work station.
9. the method for measuring ethanol content in industrial methanol as claim 1-8 any one of them is a kind of, it is characterised in that：Institute
It is 10uL micro syringes to state injector.
10. the method for measuring ethanol content in industrial methanol as claim 1-8 any one of them is a kind of, it is characterised in that：
As the mass fraction ＜ 0.01% of ethyl alcohol in sample to be tested, absolute difference≤0.0005% of the Parallel testing result；When
In sample to be tested when the mass fraction ＞ 0.01% of ethyl alcohol, absolute difference≤0.001% of the Parallel testing result.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810123211.2A CN108387653A (en) | 2018-02-07 | 2018-02-07 | A kind of method of ethanol content in measurement industrial methanol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810123211.2A CN108387653A (en) | 2018-02-07 | 2018-02-07 | A kind of method of ethanol content in measurement industrial methanol |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108387653A true CN108387653A (en) | 2018-08-10 |
Family
ID=63075475
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810123211.2A Pending CN108387653A (en) | 2018-02-07 | 2018-02-07 | A kind of method of ethanol content in measurement industrial methanol |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108387653A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112526053A (en) * | 2020-12-29 | 2021-03-19 | 陕西延长石油（集团）有限责任公司 | Method for measuring mixed alcohol and mixed ester in industrial ethanol by gas chromatography internal standard method |
| CN114965765A (en) * | 2022-05-21 | 2022-08-30 | 河南龙宇煤化工有限公司 | Gas chromatography analysis method for components of acetic acid reaction liquid |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103743844A (en) * | 2014-01-27 | 2014-04-23 | 云南煤业能源股份有限公司 | Determination method of alcohol content in methanol |
-
2018
- 2018-02-07 CN CN201810123211.2A patent/CN108387653A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103743844A (en) * | 2014-01-27 | 2014-04-23 | 云南煤业能源股份有限公司 | Determination method of alcohol content in methanol |
Non-Patent Citations (4)
| Title |
|---|
| 何红莲等: "工业甲醇中微量乙醇定量测定方法的探索", 《中国氯碱》 * |
| 王铁红: "工业甲醇中微量乙醇的毛细管气相色谱分析", 《广东化工》 * |
| 王铁鸿: "工业甲醇中微量乙醇的毛细管气相色谱分析", 《泸天化科技》 * |
| 许增辉: "甲醇中微量乙醇测定方法的应用研究", 《现代商贸工业》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112526053A (en) * | 2020-12-29 | 2021-03-19 | 陕西延长石油（集团）有限责任公司 | Method for measuring mixed alcohol and mixed ester in industrial ethanol by gas chromatography internal standard method |
| CN114965765A (en) * | 2022-05-21 | 2022-08-30 | 河南龙宇煤化工有限公司 | Gas chromatography analysis method for components of acetic acid reaction liquid |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US8499614B2 (en) | Field gas chromatograph with flame ionization | |
| CN102590414B (en) | Method for analyzing contents of trace arsine and phosphine in gas-phase propylene by gas chromatograph | |
| CN105021732A (en) | Method for fast determination of oxygen isotope composition of water in beverage wine | |
| CN106990174A (en) | SVOC quick determination methods in a kind of cloth velvet sample based on full volatilization head space | |
| CN102520082A (en) | Method for determining volatile components in polyvinyl alcohol in full-evaporation headspace gas chromatography | |
| CN107167524A (en) | Method of the gas chromatography separation detection Aripiprazole about material | |
| CN108387653A (en) | A kind of method of ethanol content in measurement industrial methanol | |
| CN106153431A (en) | The detection method of a kind of quick mensuration raw gas composition and device thereof | |
| US4151741A (en) | Method and apparatus for gas chromatographic analysis | |
| CN106198405B (en) | System for monitoring hydrogen-oxygen stable isotope ratio of atmospheric water vapor | |
| CN208350726U (en) | Gas chromatographicanalyzer for VOC on-line analysis | |
| CN110895264A (en) | Method for determining ethyl bromide in tenofovir alafenamide | |
| CN108872416A (en) | A kind of method of simultaneous quantitative detection erucyl amide and ethylene bis stearamide | |
| CN105758970B (en) | A kind of method of gas chromatography detection 3- methylamino -1,2- propane diols purities | |
| CN104569174A (en) | Method for determining concentration of formic acid in carboxylic acids in working place | |
| CN111965288A (en) | Method for determining ethanol content by gas chromatography in non-aqueous medium | |
| CN108593796A (en) | A method of detection bulk pharmaceutical chemicals Austria is uncommon for organic residual solvent in Buddhist nun | |
| CN205958524U (en) | Ethyl acetate in white spirit and ethyl caproate's survey system | |
| CN106596752B (en) | A kind of method for separating and analyzing of the cis-trans-isomer of liquid crystal intermediates hexahydrobenzaldehyde and its derivative | |
| CN111458433A (en) | Method for detecting kasugamycin by high performance liquid chromatography | |
| CN106018595B (en) | The method of capillary column method detection 3- methylamino -1,2- propane diols purity | |
| CN114200067B (en) | High performance liquid chromatography analysis method for 6-bromo-3-hydroxy pyrazine-2-carboxamide and impurities | |
| CN115343399B (en) | Method for detecting residual solvent of N-alkyl pyrrolidone in bulk drug | |
| CN107748213A (en) | The detection method of diethanol monoisopropanolamine | |
| Sternberg et al. | A general method for detection and recording of component bands in chromatography with liquid eluents |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180810 |
|
| RJ01 | Rejection of invention patent application after publication |