CN107748213A - The detection method of diethanol monoisopropanolamine - Google Patents
The detection method of diethanol monoisopropanolamine Download PDFInfo
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- CN107748213A CN107748213A CN201710974442.XA CN201710974442A CN107748213A CN 107748213 A CN107748213 A CN 107748213A CN 201710974442 A CN201710974442 A CN 201710974442A CN 107748213 A CN107748213 A CN 107748213A
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- diethanol monoisopropanolamine
- detection method
- absolute ethyl
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- 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
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- 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
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Abstract
The invention discloses a kind of detection method of diethanol monoisopropanolamine, is related to detection and analysis technical field, and the present invention is detected using gas chromatography, and solvent selects absolute ethyl alcohol, and chromatographic column is quartz capillary column；Column temperature is 150 DEG C (2min), 10 DEG C/min, 250 DEG C (10min)；The room temperature that gasifies is 250 DEG C, and detector temperature is 270 DEG C；Carrier gas nitrogen flow velocity is 30ml/min, and air velocity is 300 ml/min, and hydrogen flow rate is 30 ml/min, sample size 0.24ul.Gas chromatograph is debugged by chromatographic condition, takes diethanol monoisopropanolamine fluid sample absolute ethyl alcohol to dilute and be well mixed after stable, carries out data analysis with data logger, be computed drawing the content of diethanol monoisopropanolamine.The present invention can improve detection efficiency and accuracy of detection, reduce cost, safe fanout free region.
Description
Technical field
The present invention relates to detection and analysis technical field, more particularly to a kind of detection method of diethanol monoisopropanolamine.
Background technology
At present, diethanol monoisopropanolamine uses diethanol amine to be produced for initiator addition 1mol propylene oxide process.
The detection of diethanol monoisopropanolamine content is mainly carried out using chemical titration, and principle is diethanol monoisopropanolamine in methanol
Acetylization reaction does not occur with acetic anhydride in medium, nonaquepous tration is carried out with hydrochloric acid-ethanol standard liquid, so as to be calculated two
The content of ethanol monoisopropanolamine, the main agents of use include：Absolute methanol, acetic anhydride, hydrochloric acid, ethanol, methyl orange, diformazan
Benzene cyanogen FF mixing indicator solutions, and do parallel laboratory test twice, it is desirable to the absolute difference of parallel determinations is not more than 0.3%.
But there is following defect in this detection method：1st, human factor is excessive on result influence causes to repeat to test, and examines
Time length is surveyed, data are inaccurate；2nd, the reagent used has larger volatility, and portion of reagent also has sizable toxicity, damage
The health of evil testing staff；3rd, reagent deposits influence titration results for a long time, and product quality control band is influenceed.
The content of the invention
The technical problems to be solved by the invention are to provide high two of a kind of detection efficiency height, safety and environmental protection, accuracy of detection
The detection method of ethanol monoisopropanolamine.
In order to solve the above technical problems, the technical solution used in the present invention is：
A kind of detection method of diethanol monoisopropanolamine, is detected using gas chromatography, including gas chromatograph and data note
Instrument is recorded, step is as follows：
（One）Sample prepares：Solvent is absolute ethyl alcohol, chromatographic column material selection quartz capillary column；
（Two）Chromatographic condition is set：Column temperature is 150 DEG C (2min), and 10 DEG C/min, 250 DEG C (10min), gasification room temperature is 250
DEG C, detector temperature is 270 DEG C；Carrier gas nitrogen flow velocity is 30ml/min, and air velocity is 300 ml/min, hydrogen flow rate 30
ml/min；Sample size is 0.2-0.4ul；
（Three）Detection operation：（1）Start gas chromatograph, by the chromatographic condition adjusting instrument of above-mentioned setting, start after stable into
Sample is analyzed；（2）2ml diethanol monoisopropanolamine fluid samples are taken, is diluted and is well mixed with 6ml absolute ethyl alcohols, use injector
Sample introduction is analyzed, and Data Analysis Services are carried out with data logger；（Pay attention to：Etoh solvent peak is deducted when peak is handled）（3）Meter
Calculate the content for drawing diethanol monoisopropanolamine.
Preferably, the absolute ethyl alcohol is AR level absolute ethyl alcohols.
Preferably, the hydrogen volume fraction is not less than 99.99%, and nitrogen volume fraction is not less than 99.999%.
Preferably, hydrogen, nitrogen and the air used is respectively through silica gel and molecular sieve drying, purification.
Preferably, the chromatographic column selects KB-30M quartz capillary column, and specification is 30m × 0.32mm × 1.0 μm.
Preferably, with area normalization method with the content of calculated by peak area diethanol monoisopropanolamine.
Preferably, the gas chromatograph of selection is flame ionization detector；The data logger, including at chromatographic data
Reason machine and chromatographic work station.
It is using beneficial effect caused by above-mentioned technical proposal：Compared with prior art, the present invention can improve inspection
Efficiency is surveyed, detection time was shorten to 40 minutes by original 4 hours；Only absolute ethyl alcohol has volatility in detection reagent, is dropping
Also avoid damaging the health of testing staff while inexpensive；Accuracy of detection is improved, eliminates human factor, using same
The same product examine colour examining modal data control errors improve the confidence level of product quality within 0.3%.
Brief description of the drawings
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description.
Fig. 1 is the chromatography figure of diethanol monoisopropanolamine provided in an embodiment of the present invention.
Embodiment
With reference to embodiments of the invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only the part of the embodiment of the present invention, rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made,
Belong to the scope of protection of the invention.
A kind of detection method of diethanol monoisopropanolamine provided by the invention, is detected using gas chromatography, including gas
Chromatography and data logger, wherein, the gas chromatograph of selection is flame ionization detector, its machine sensitivity and stably
Property meets the pertinent regulations in GB/T9722；The data logger, including chromatographic data processor and chromatographic work station.
Comprise the following steps：
（One）Sample prepares：Solvent selects AR level absolute ethyl alcohols, chromatographic column material selection KB-30M quartz capillary column, specification
For 30m × 0.32mm × 1.0 μm.
（Two）Chromatographic condition is set：Column temperature is 150 DEG C (2min), 10 DEG C/min, 250 DEG C (10min), and gasification room temperature is
250 DEG C, detector temperature is 270 DEG C；Flow rate of carrier gas is 30ml/min, and air velocity is 300 ml/min, hydrogen flow rate 30
ml/min；Sample size is 0.24ul.Shown in table 1 specific as follows：
Wherein, hydrogen volume fraction is not less than 99.99%, and nitrogen volume fraction is not less than 99.999%；The hydrogen that uses, nitrogen and
Air is respectively through silica gel and molecular sieve drying, purification.
（Three）Detection operation：
（1）Start gas chromatograph, by the chromatographic condition adjusting instrument of above-mentioned setting, start sample introduction analysis after stable；
（2）2ml diethanol monoisopropanolamine fluid samples are taken, is diluted and is well mixed with 6ml absolute ethyl alcohols, use feeder
Analysis, Data Analysis Services are carried out with data logger.Pay attention to：Etoh solvent peak is deducted when peak is handled.
（3）The content of diethanol monoisopropanolamine is calculated, with area normalization method with calculated by peak area diethanol Dan Yi
The content of Propanolamine.
The mass fraction wi of each component, numerical value is represented with %, respectively by formula（1）Calculate：
…………………………………………………(1)
In formula：
Ai --- tested component i peak area, unit is square millimeter（mm2）;
Fi --- tested component i relative mass correction factor；
The arithmetic mean of instantaneous value for taking parallel determinations twice is report result.The parallel determination knot twice of diethanol monoisopropanolamine
The difference of fruit is not more than 0.3%.
Fig. 1 is the chromatography figure that diethanol monoisopropanolamine is detected using gas chromatography.
In summary, the present invention has the advantages of easy to operate, accuracy of detection is high, detection efficiency is high, and detection time is by original
That comes shorten to 40 minutes for 4 hours, and the volatile materials of use only has absolute ethyl alcohol, is also avoided while testing cost is reduced
The health of testing staff is damaged, testing result is eliminated man's activity, improves accuracy in detection, examined using same sample
Colour examining modal data control errors improve the confidence level of product quality within 0.3%.
Many details are elaborated in superincumbent description to facilitate a thorough understanding of the present invention, still the present invention can be with
It is different from other manner described here using other to implement, those skilled in the art can be without prejudice to intension of the present invention
In the case of do similar popularization, therefore the present invention is not limited by particular embodiments disclosed above.
Claims (7)
1. a kind of detection method of diethanol monoisopropanolamine, is detected using gas chromatography, including gas chromatograph and data
Recorder, it is characterised in that step is as follows：
（One）Sample prepares：Solvent is absolute ethyl alcohol, chromatographic column material selection quartz capillary column；
（Two）Chromatographic condition is set：Column temperature is 150 DEG C (2min), and 10 DEG C/min, 250 DEG C (10min), gasification room temperature is 250
DEG C, detector temperature is 270 DEG C；Carrier gas nitrogen flow velocity is 30ml/min, and air velocity is 300 ml/min, hydrogen flow rate 30
ml/min；Sample size is 0.2-0.4ul；
（Three）Detection operation：（1）Start gas chromatograph, by the chromatographic condition adjusting instrument of above-mentioned setting, start after stable into
Sample is analyzed；（2）2ml diethanol monoisopropanolamine fluid samples are taken, is diluted and is well mixed with 6ml absolute ethyl alcohols, use injector
Sample introduction is analyzed, and Data Analysis Services are carried out with data logger；（3）The content of diethanol monoisopropanolamine is calculated.
2. the detection method of diethanol monoisopropanolamine according to claim 1, it is characterised in that：The absolute ethyl alcohol is
AR level absolute ethyl alcohols.
3. the detection method of diethanol monoisopropanolamine according to claim 1, it is characterised in that：The hydrogen integration
Number is not less than 99.99%, and nitrogen volume fraction is not less than 99.999%.
4. the detection method of diethanol monoisopropanolamine according to claim 1, it is characterised in that：Hydrogen, the nitrogen used
Gas and air are respectively through silica gel and molecular sieve drying, purification.
5. the detection method of diethanol monoisopropanolamine according to claim 1, it is characterised in that：The chromatographic column is selected
KB-30M quartz capillary column, specification are 30m × 0.32mm × 1.0 μm.
6. the detection method of diethanol monoisopropanolamine according to claim 1, it is characterised in that：With area normalization method with
The content of calculated by peak area diethanol monoisopropanolamine.
7. the detection method of diethanol monoisopropanolamine according to claim 1, it is characterised in that：The gas-chromatography of selection
Instrument is flame ionization detector；The data logger, including chromatographic data processor and chromatographic work station.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110794048A (en) * | 2019-10-11 | 2020-02-14 | 宁波卫生职业技术学院 | High performance liquid detection method for alcamines cement grinding aid |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106706776A (en) * | 2016-11-23 | 2017-05-24 | 华润水泥技术研发有限公司 | Method for detecting grinding additive raw material solution |
| CN106918669A (en) * | 2017-02-21 | 2017-07-04 | 华润水泥技术研发有限公司 | The detection method of alcohols, alcamine compound in grinding aid |
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2017
- 2017-10-19 CN CN201710974442.XA patent/CN107748213A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106706776A (en) * | 2016-11-23 | 2017-05-24 | 华润水泥技术研发有限公司 | Method for detecting grinding additive raw material solution |
| CN106918669A (en) * | 2017-02-21 | 2017-07-04 | 华润水泥技术研发有限公司 | The detection method of alcohols, alcamine compound in grinding aid |
Non-Patent Citations (1)
| Title |
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| 郑荣平等: "气相色谱法定量分析助磨剂中的醇胺类物质", 《水泥》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110794048A (en) * | 2019-10-11 | 2020-02-14 | 宁波卫生职业技术学院 | High performance liquid detection method for alcamines cement grinding aid |
| CN110794048B (en) * | 2019-10-11 | 2022-08-23 | 宁波卫生职业技术学院 | High performance liquid detection method for alcamines cement grinding aid |
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