CN114646714A - Rapid analysis method for detecting content of pinacolone - Google Patents
Rapid analysis method for detecting content of pinacolone Download PDFInfo
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- PJGSXYOJTGTZAV-UHFFFAOYSA-N pinacolone Chemical compound CC(=O)C(C)(C)C PJGSXYOJTGTZAV-UHFFFAOYSA-N 0.000 title claims abstract description 106
- 238000004458 analytical method Methods 0.000 title claims abstract description 41
- 238000001514 detection method Methods 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 230000008016 vaporization Effects 0.000 claims abstract description 25
- 238000009834 vaporization Methods 0.000 claims abstract description 22
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000001257 hydrogen Substances 0.000 claims abstract description 19
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 19
- 238000010926 purge Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 abstract description 6
- 238000004364 calculation method Methods 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 39
- 230000000694 effects Effects 0.000 description 10
- 238000000926 separation method Methods 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000010813 internal standard method Methods 0.000 description 5
- 239000012488 sample solution Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- RMOGWMIKYWRTKW-UONOGXRCSA-N (S,S)-paclobutrazol Chemical compound C([C@@H]([C@@H](O)C(C)(C)C)N1N=CN=C1)C1=CC=C(Cl)C=C1 RMOGWMIKYWRTKW-UONOGXRCSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 239000005985 Paclobutrazol Substances 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 239000012086 standard solution Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- YNWVFADWVLCOPU-MDWZMJQESA-N (1E)-1-(4-chlorophenyl)-4,4-dimethyl-2-(1H-1,2,4-triazol-1-yl)pent-1-en-3-ol Chemical compound C1=NC=NN1/C(C(O)C(C)(C)C)=C/C1=CC=C(Cl)C=C1 YNWVFADWVLCOPU-MDWZMJQESA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- -1 dibenzyltriazole ketone Chemical class 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- WURBVZBTWMNKQT-UHFFFAOYSA-N 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)butan-2-one Chemical compound C1=NC=NN1C(C(=O)C(C)(C)C)OC1=CC=C(Cl)C=C1 WURBVZBTWMNKQT-UHFFFAOYSA-N 0.000 description 1
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 1
- 239000005583 Metribuzin Substances 0.000 description 1
- 239000005846 Triadimenol Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- KCXMKQUNVWSEMD-UHFFFAOYSA-N benzyl chloride Chemical compound ClCC1=CC=CC=C1 KCXMKQUNVWSEMD-UHFFFAOYSA-N 0.000 description 1
- 229940073608 benzyl chloride Drugs 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229940127554 medical product Drugs 0.000 description 1
- FOXFZRUHNHCZPX-UHFFFAOYSA-N metribuzin Chemical compound CSC1=NN=C(C(C)(C)C)C(=O)N1N FOXFZRUHNHCZPX-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000005648 plant growth regulator Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- BAZVSMNPJJMILC-UHFFFAOYSA-N triadimenol Chemical compound C1=NC=NN1C(C(O)C(C)(C)C)OC1=CC=C(Cl)C=C1 BAZVSMNPJJMILC-UHFFFAOYSA-N 0.000 description 1
- 150000003852 triazoles Chemical class 0.000 description 1
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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
-
- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
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- 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)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a rapid analysis method for detecting the content of pinacolone.A pinacolone sample enters a capillary column and a hydrogen flame ionization detector for detection, and is directly injected with a sample amount of 0.4ul at an N2000 chromatographic workstation; the detector is 180-220 ℃; the temperature of the vaporization chamber is 180-230 ℃; the temperature of the column chamber is 160-200 ℃; the split ratio is (30: 1) - (60: 1); purging for 5ml/min for 5 minutes; n is a radical of2：H2: the volume ratio of Air is 1:1:1, the calculation formula W ═ 100-WWater (W)) Sum of peak areas of pinacolone chromatogram/peak areas of components, wherein, percentage content of pinacolone in W-sample, WWater (W)Knowing the percentage of moisture contained in the sample, the method allows for rapid, efficient analysis to provide real-time data on pinacolone.
Description
Technical Field
The invention relates to a rapid analysis method for detecting the content of pinacolone.
Background
Pinacolone is mainly used for producing triazole pesticides, such as triadimefon, paclobutrazol, uniconazole, metribuzin, benzyl chloride triadimenol, dibenzyltriazole ketone, octazolinone and the like, and plant growth regulators such as paclobutrazol, uniconazole, imadazole, paclobutrazol and the like, and is also used for herbicides and medical products.
At present, the intermediate control of the pinacolone production occupies a large part of work of a laboratory, the real-time control analysis data processing is needed in the pinacolone production, and the existing intermediate analysis method for the pinacolone production is commonly used by an internal standard method.
Internal standard method, which requires the preparation of internal standard: ethyl acetate solution (5.00 in 500ml chloroform and to mark); pinacolone standard substance (content is more than or equal to 99.5%), hydrogen flame ionization detectorThe column was aged by heating to 250 ℃ using OV-101 stainless steel column (1m x 3mm) and nitrogen gas at a flow rate of 30ml/min, the gas flow rate being: nitrogen gas: hydrogen gas: air 1: 35, accurately weighing 0.04g (accurate to 0.0002g) of a pinacolone standard sample in a 15ml bottle with a plug during detection, accurately adding 4ml of internal standard solution by using a pipette in the second step, shaking up, accurately weighing 0.04g (accurate to 0.0002g) of a pinacolone sample in a 15ml bottle with a plug, accurately adding 4ml of internal standard solution by using a pipette in the third step, and shaking up. After the baseline of the instrument is stable, continuously injecting a plurality of needle standard sample solutions, calculating the repeatability of the relative response value of each needle, measuring according to the sequence of the standard sample solutions and the sample solutions after the relative response value of two adjacent needles changes by less than 1.5%, and calculating the result X-R1*M1*P/R2*M2Wherein, R1 represents the average value of peak area ratio of pinacolone and internal standard substance in the standard sample solution; r2 represents the average value of peak area ratio of the pinacolone to the internal standard substance in the sample solution, M represents the mass of the pinacolone standard sample, and P represents the mass percentage content of the pinacolone standard sample. The internal standard method has the advantages of multiple operation steps, multiple sampling times and long time consumption, and greatly influences the provision of real-time data in the industrial production of the pinacolone.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the method can provide the real-time data of the pinacolone quickly and efficiently, and solves the problems that an internal standard method of the existing analysis method needs to prepare an internal standard solution, pipette liquid transfer, repeated sample injection steps are complicated, the detection time is long, and the real-time data of the pinacolone is not beneficial to being provided in production.
In order to solve the technical problems, the technical scheme of the invention is as follows: a rapid analysis method for detecting the content of pinacolone, wherein a pinacolone sample enters a capillary column and a hydrogen flame ionization detector for detection, direct sample introduction is carried out, the sample introduction amount is 0.4ul, and an N2000 chromatographic workstation is selected; the temperature of the detector is 180-220 ℃; the temperature of the vaporization chamber is 180-230 ℃; the temperature of the column chamber is 160-200 ℃; the split ratio is (30: 1) - (60: 1); purging for 5ml/min for 5 minutes; n is a radical of2：H2: the volume ratio of Air is 1:1:1,
W＝(100-Wwater (I)) Sum of peak areas of pinacolone chromatograms/peak areas of each component,
wherein, the percentage content of the pinacolone in the W-sample,
Wwater (W)-the percentage content of moisture contained in the known sample.
Preferably, OV-1701(30m 0.53mm 1.0um) is used as the capillary column.
Preferably, the capillary column is SE-54 (30m 0.32mm 0.5 um).
Preferably, the chromatograph of the hydrogen flame ionization detector is selected from the type 8890 of the Shanghai extensive instrumentation, Inc.
Preferably, the temperature of the detector is 200 ℃, the temperature of the vaporizing chamber is 230 ℃, the temperature of the column chamber is 160 ℃, and the split ratio is 60: 1.
Preferably, the temperature of the detector is 180 ℃, the temperature of the vaporization chamber is 180 ℃, the temperature of the column chamber is 180 ℃, and the split ratio is 60: 1.
Preferably, the temperature of the detector is 200 ℃, the temperature of the vaporizing chamber is 200 ℃, the temperature of the column chamber is 160 ℃, and the split ratio is 60: 1.
Preferably, the temperature of the detector is 220 ℃, the temperature of the vaporization chamber is 220 ℃, the temperature of the column chamber is 200 ℃, and the split ratio is 60: 1.
Preferably, the temperature of the detector is 200 ℃, the temperature of the vaporization chamber is 220 ℃, the temperature of the column chamber is 160 ℃, and the split ratio is 60: 1.
Preferably, the temperature of the detector is 200 ℃, the temperature of the vaporizing chamber is 200 ℃, the temperature of the column chamber is 160 ℃, and the split ratio is 30: 1.
After the technical scheme is adopted, the invention has the effects that: a rapid analysis method for detecting the content of pinacolone directly samples, does not need to heat up, formula calculation, and can rapidly and efficiently provide real-time data of pinacolone while saving energy.
Drawings
The invention is further illustrated with reference to the following figures and examples.
FIG. 1 is a detection map and analysis of pinacolone in example 1 of the present invention;
FIG. 2 is a detection map and analysis of pinacolone in example 2 of the present invention;
FIG. 3 is a detection profile and analysis of pinacolone in example 3 of the present invention;
FIG. 4 is a detection map and analysis of pinacolone in example 4 of the present invention;
FIG. 5 is a detection map and analysis of pinacolone in example 5 of the present invention;
FIG. 6 is a detection map and analysis of pinacolone in example 6 of the present invention;
FIG. 7 is a detection map and analysis of pinacolone in example 7 of the present invention;
FIG. 8 is a detection map and analysis of pinacolone in example 8 of the present invention;
FIG. 9 is a detection map and analysis of pinacolone in example 9 of the present invention;
Detailed Description
The present invention is described in further detail below with reference to specific examples.
A rapid analysis method for detecting the content of pinacolone is characterized in that a pinacolone sample enters a capillary column and a hydrogen flame ionization detector for detection, is directly injected with a sample amount of 0.4ul, and selects an N2000 chromatographic workstation; the temperature of the detector is 180-220 ℃; the temperature of the vaporization chamber is 180-230 ℃; the temperature of the column chamber is 160-200 ℃; the split ratio is (30: 1) - (60: 1); purging for 5ml/min for 5 minutes; n is a radical of2：H2: the volume ratio of Air is 1:1:1,
W＝(100-Wwater (I)) Sum of peak areas of pinacolone chromatogram/peak areas of components, wherein, percentage content of pinacolone in W-sample, WWater (W)Knowing the percentage content of water contained in the sample, WWater (I)Is measured in advance by a trace moisture tester.
Example 1
A rapid analysis method for detecting the content of pinacolone, a pinacolone sample 1 enters a capillary column and a hydrogen flame ionization detector for detection, direct sample introduction is carried out, the sample introduction amount is 0.4ul, and an N2000 chromatographic workstation is selected; the temperature of the detector is 200 ℃; the temperature of the vaporization chamber is 230 ℃; the temperature of the column chamber is 160 ℃; the split ratio is 60:1; purging for 5ml/min for 5 minutes; n is a radical of2：H2: the volume ratio of Air is 1:1:1, wherein the capillary column is OV-1701(30m 0.53mm 1.0um), and the chromatograph of the hydropneumatic ionization detector is selected from the model 8890 of the Shanghai fender Instrument Limited.
Formula W ═ 100-WWater (W)) Sum of area of pinacolone chromatographic peak/area of peak of each component, so W1＝(100-WWater 1) Sum of peak areas of pinacolone chromatograms/peak areas of components
＝(100-0.11)*15504112/15908524＝99.89*15504112/15908524＝97.35。
As can be seen from FIG. 1, the detection of pinacolone is fast and the separation effect is good.
Example 2
A rapid analysis method for detecting the content of pinacolone, a pinacolone sample 2 enters a capillary column and a hydrogen flame ionization detector for detection, direct sample introduction is carried out, the sample introduction amount is 0.4ul, and an N2000 chromatographic workstation is selected; the temperature of the detector is 180 ℃; the temperature of the vaporization chamber is 180 ℃; the temperature of the column chamber is 180 ℃; the split ratio is 60: 1; purging for 5ml/min for 5 minutes; n is a radical of2：H2: the volume ratio of Air is 1:1:1, wherein the capillary column is OV-1701(30m 0.53mm 1.0um), and the chromatograph of the hydropneumatic ionization detector is selected from the model 8890 of the Shanghai fender Instrument Limited.
Formula calculates W ═ 100-WWater (W)) Sum of area of pinacolone chromatographic peak/area of peak of each component, so W2＝(100-WWater 2) Sum of peak areas of pinacolone chromatograms/peak areas of components
＝(100-0.11)*15003000/15304140＝97.92。
As can be seen from FIG. 2, the error of pinacolone is small, and the separation effect is good.
Example 3
A rapid analysis method for detecting the content of pinacolone, a pinacolone sample 3 enters a capillary column and a hydrogen flame ionization detector for detection, direct sample introduction is carried out, the sample introduction amount is 0.4ul, and an N2000 chromatographic workstation is selected; the temperature of the detector is 200 ℃; the temperature of the vaporization chamber is 200 ℃; the temperature of the column chamber is 160 ℃; the split ratio is 60:1; purging for 5ml/min for 5 minutes; n is a radical of2：H2: the volume ratio of Air is 1:1:1, wherein the capillary column is OV-1701(30m 0.53mm 1.0um), and the chromatograph of the hydropneumatic ionization detector is selected from the model 8890 of the Shanghai fender Instrument Limited.
Formula W ═ 100-WWater (W)) Sum of peak area of pinacolone chromatogram/peak area of each component, so W3 ═ 100-WWater 3) Sum of peak areas of pinacolone chromatograms/peak areas of components
＝(100-0.11)*16182227/16508537＝97.92。
As can be seen from FIG. 3, the error of the detection result of pinacolone is small, the separation effect is good, and the number of the impurity peaks is large.
Example 4
A rapid analysis method for detecting the content of pinacolone, a pinacolone sample 4 enters a capillary column and a hydrogen flame ionization detector for detection, direct sample introduction is carried out, the sample introduction amount is 0.4ul, and an N2000 chromatographic workstation is selected; the temperature of the detector is 220 ℃; the temperature of the vaporization chamber is 220 ℃; the temperature of the column chamber is 200 ℃; the split ratio is 60: 1; purging for 5ml/min for 5 minutes; n is a radical of hydrogen2：H2: the volume ratio of Air is 1:1:1, wherein the capillary column is OV-1701(30m 0.53mm 1.0um), and the chromatograph of the hydropneumatic ionization detector is selected from the model 8890 of the Shanghai fender Instrument Limited.
Formula calculates W ═ 100-WWater (W)) Sum of peak area of pinacolone chromatogram/peak area of each component, so W4 ═ 100-WWater 4) Sum of peak areas of pinacolone chromatograms/peak areas of components
＝(100-0.11)*17533822/17689282＝99.01。
As can be seen from FIG. 4, the effect of pinacolone separation was not good.
Example 5
A rapid analysis method for detecting the content of pinacolone, a pinacolone sample 5 enters a capillary column and a hydrogen flame ionization detector for detection, direct sample introduction is carried out, the sample introduction amount is 0.4ul, and an N2000 chromatographic workstation is selected; the temperature of the detector is 200 ℃; the temperature of the vaporization chamber is 220 ℃; the temperature of the column chamber is 160 ℃; the split ratio is 60: 1; the air is purged by 5ml/min,5 minutes; n is a radical of2：H2: the volume ratio of Air is 1:1:1, wherein the capillary column is OV-1701(30m 0.53mm 1.0um), and the chromatograph of the hydrogen flame ionization detector is selected from the type 8890 of the Shanghai fender-Ind.
Formula calculates W ═ 100-WWater (W)) Sum of area of pinacolone chromatographic peak/area of peak of each component, so W5＝(100-WWater 5) Sum of peak areas of pinacolone chromatograms/peak areas of components
＝(100-0.11)*18107656/18470940＝97.93。
As can be seen from FIG. 5, the error of the detection result of pinacolone is small, and the separation effect is good.
Example 6
A rapid analysis method for detecting the content of pinacolone, a pinacolone sample 6 enters a capillary column and a hydrogen flame ionization detector for detection, direct sample introduction is carried out, the sample introduction amount is 0.4ul, and an N2000 chromatographic workstation is selected; keeping the initial temperature of the column chamber at 60 deg.C for 1min at 200 deg.C, heating to 180 deg.C at 30 deg.C/min, and keeping for 10 min; a vaporization chamber of 200 ℃; the split ratio is 60: 1; n is a radical of2：H2: the volume ratio of Air is 1:1:1, wherein the capillary column is OV-1701(30m 0.53mm 1.0um), and the chromatograph of the hydropneumatic ionization detector is selected from the model 8890 of the Shanghai fender Instrument Limited.
Formula calculates W ═ 100-WWater (W)) Sum of area of pinacolone chromatographic peak/area of peak of each component, so W6＝(100-WWater 6) Sum of peak areas of pinacolone chromatograms/peak areas of components
＝(100-0.11)*22555336/23041831＝97.78。
As can be seen from figure 6, although the detection result error is small in the detection process of the pinacolone, the separation effect is good, the heating method is long in time consumption, real-time data of the pinacolone cannot be provided in time, and the production requirement of the pinacolone cannot be met.
Example 7
A rapid analysis method for detecting the content of pinacolone, wherein a pinacolone sample 7 enters a capillary column and a hydrogen flame ionization detector for detection and direct sample introduction,the sample injection amount is 0.4ul, and an N2000 chromatographic workstation is selected; the temperature of the detector is 200 ℃; the temperature of the vaporization chamber is 220 ℃; the temperature of the column chamber is 200 ℃; the split ratio is 60: 1; purging for 5ml/min for 5 minutes; n is a radical of2：H2: the volume ratio of Air is 1:1:1, wherein the capillary column is selected from SE-54 (30m 0.32mm 0.5 um); the split ratio is 60: 1; the chromatograph of the hydrogen flame ionization detector is preferably of the type 8890 from the epifender instrument co.
Formula W ═ 100-WWater (W)) Sum of area of pinacolone chromatographic peak/area of peak of each component, so W7＝(100-WWater 7) Sum of peak areas of pinacolone chromatograms/peak areas of components
＝(100-0.11)*17533822/17689282＝99.02。
As can be seen from fig. 7, the separation effect of pinacolone was poor, and the main peak was not well separated from both the front and rear hetero peaks.
Example 8
A rapid analysis method for detecting the content of pinacolone, a pinacolone sample 8 enters a capillary column and a hydrogen flame ionization detector for detection, direct sample introduction is carried out, the sample introduction amount is 0.4ul, and an N2000 chromatographic workstation is selected; the temperature of the detector is 200 ℃; the temperature of the vaporization chamber is 200 ℃; the temperature of the column chamber is 160 ℃; the split ratio is 30: 1; purging for 5ml/min for 5 minutes; n is a radical of2：H2: the volume ratio of Air is 1:1:1, wherein the capillary column is OV-1701(30m 0.53mm 1.0um), and the chromatograph of the hydropneumatic ionization detector is selected from the model 8890 of the Shanghai fender Instrument Limited.
Because W is (100-W)Water (W)) Sum of area of pinacolone chromatographic peak/area of peak of each component, so W8＝(100-WWater 8) Sum of peak areas of pinacolone chromatograms/peak areas of components
＝(100-0.11)*16849648/16998255＝99.02。
As can be seen from FIG. 8, the separation effect of pinacolone is not good, and the main peak is not well separated from the front miscellaneous peak and the back impurities.
Example 9
Rapid analysis method for detecting pinacolone content, and pinacolone sample9, entering a capillary column and a hydrogen flame ionization detector for detection, directly injecting samples with the sample injection amount of 0.4ul, and selecting an N2000 chromatographic workstation; a detector at 200 ℃; a vaporization chamber of 200 ℃; the split ratio is 30: 1; blowing at the tail for 30ml/min for 5 min; purging for 5ml/min for 5 minutes; n is a radical of2:H2Air 1:1: 1; initial temperature of the column chamber is 50 deg.C, holding for 1min, heating to 160 deg.C at 30 deg.C/min, and holding for 10min, wherein OV-1701(30m 0.53mm 1.0um) is selected as capillary column, and 8890 model of Shanghai neuro-analytical instrument is selected as chromatograph of hydrogen flame ionization detector.
Formula calculates W ═ 100-WWater (W)) Sum of area of pinacolone chromatographic peak/area of peak of each component, so W9＝(100-WWater 9) Sum of peak areas of pinacolone chromatograms/peak areas of components
＝(100-0.11)*23829402/24447935＝97.37。
As can be seen from figure 9, the pinacolone detection adopts the temperature rising method and is time-consuming, and real-time data of the pinacolone cannot be provided in time.
From the above embodiments, it can be seen that, by adopting the analysis and detection method of the present invention, the detection of pinacolone can provide the real-time data of pinacolone by calculating the time consumption of 2-3 minutes through a formula, the error is small, the separation effect is good, compared with an internal standard method, the analysis and control time of pinacolone is greatly shortened, and the method is favorable for popularization and use in the production of pinacolone.
The above-mentioned embodiments are merely descriptions of the preferred embodiments of the present invention, and are not intended to limit the scope of the present invention, and various modifications and alterations made to the technical solution of the present invention without departing from the spirit of the present invention are intended to fall within the scope of the present invention defined by the claims.
Claims (10)
1. A rapid analysis method for detecting the content of pinacolone is characterized in that: the pinacolone sample enters a capillary column and a hydrogen flame ionization detector for detection, direct sample introduction is carried out, the sample introduction amount is 0.4ul, and an N2000 chromatographic workstation is selected; the temperature of the detector is 180-220 ℃; the temperature of the vaporization chamber is 180-230 ℃; the temperature of the column chamber is 160-200 ℃; flow diversionThe ratio (30: 1) to (60: 1); purging for 5ml/min for 5 minutes; n is a radical of2：H2: the volume ratio of Air is 1:1:1,
formula calculates W ═ 100-WWater (W)) Sum of peak areas of pinacolone chromatograms/peak areas of each component,
wherein, the percentage content of the pinacolone in the W-sample,
Wwater (W)-the percentage content of moisture contained in the known sample.
2. The rapid analysis method for detecting the content of pinacolone according to claim 1, which is characterized in that: OV-1701(30m 0.53mm 1.0um) was selected as the capillary column.
3. The rapid analysis method for detecting the content of pinacolone according to claim 1, which is characterized in that: the capillary column was SE-54 (30m 0.32mm 0.5 um).
4. The rapid analysis method for detecting the content of pinacolone according to claim 1, which is characterized in that: the chromatograph of the hydrogen flame ionization detector is preferably of the type 8890 from the epihain fender instrument ltd.
5. The rapid analysis method for detecting the content of pinacolone according to claim 1, which is characterized in that: the temperature of the detector is 200 ℃, the temperature of the vaporization chamber is 230 ℃, the temperature of the column chamber is 160 ℃, and the split ratio is 60: 1.
6. The rapid analysis method for detecting the content of pinacolone according to claim 1, which is characterized in that: the temperature of the detector is 180 ℃, the temperature of the vaporization chamber is 180 ℃, the temperature of the column chamber is 180 ℃, and the split ratio is 60: 1.
7. The rapid analysis method for detecting the content of pinacolone according to claim 1, which is characterized in that: the temperature of the detector is 200 ℃, the temperature of the vaporization chamber is 200 ℃, the temperature of the column chamber is 160 ℃, and the split ratio is 60: 1.
8. The rapid analysis method for detecting the content of pinacolone according to claim 1, which is characterized in that: the temperature of the detector is 220 ℃, the temperature of the vaporization chamber is 220 ℃, the temperature of the column chamber is 200 ℃, and the split ratio is 60: 1.
9. The rapid analysis method for detecting the content of pinacolone according to claim 1, which is characterized in that: the temperature of the detector is 200 ℃, the temperature of the vaporization chamber is 220 ℃, the temperature of the column chamber is 160 ℃, and the split ratio is 60: 1.
10. The rapid analysis method for detecting the content of pinacolone according to claim 1, which is characterized in that: the temperature of the detector is 200 ℃, the temperature of the vaporization chamber is 200 ℃, the temperature of the column chamber is 160 ℃, and the split ratio is 30: 1.
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