CN114924000A - Method for detecting content of diisopropyl ether in crude phenol - Google Patents
Method for detecting content of diisopropyl ether in crude phenol Download PDFInfo
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- CN114924000A CN114924000A CN202210514531.7A CN202210514531A CN114924000A CN 114924000 A CN114924000 A CN 114924000A CN 202210514531 A CN202210514531 A CN 202210514531A CN 114924000 A CN114924000 A CN 114924000A
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- diisopropyl ether
- crude phenol
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- ZAFNJMIOTHYJRJ-UHFFFAOYSA-N Diisopropyl ether Chemical compound CC(C)OC(C)C ZAFNJMIOTHYJRJ-UHFFFAOYSA-N 0.000 title claims abstract description 59
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 23
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 48
- 238000001514 detection method Methods 0.000 claims abstract description 10
- 238000004817 gas chromatography Methods 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims description 13
- 238000004821 distillation Methods 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000004364 calculation method Methods 0.000 claims description 7
- 238000011088 calibration curve Methods 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 6
- 239000007924 injection Substances 0.000 claims description 6
- 238000004458 analytical method Methods 0.000 claims description 5
- 239000012159 carrier gas Substances 0.000 claims description 4
- 238000010812 external standard method Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000012360 testing method Methods 0.000 claims description 4
- 238000013459 approach Methods 0.000 claims description 3
- 238000004587 chromatography analysis Methods 0.000 abstract description 5
- 239000012535 impurity Substances 0.000 abstract description 2
- 238000005259 measurement Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000013215 result calculation Methods 0.000 description 1
- 239000002351 wastewater Substances 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
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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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
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
- G01N2030/047—Standards external
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- 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)
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Abstract
The invention discloses a method for detecting the content of diisopropyl ether in crude phenol, which comprises the steps of firstly building a chromatographic detection device, then mixing crude phenol containing diisopropyl ether with toluene, separating most components in the diisopropyl ether and the crude phenol, reducing the interference of impurities on chromatographic analysis, and finally determining the content of trace diisopropyl ether in the crude phenol by gas chromatography.
Description
Technical Field
The invention belongs to the field of gas chromatography, and relates to a method for detecting the content of diisopropyl ether in crude phenol.
Background
The diisopropyl ether is used in coal pressure gasification wastewater for extraction dephenolization, and then the diisopropyl ether is distilled out, so that the diisopropyl ether in the crude phenol needs to be analyzed to ensure that the diisopropyl ether is completely distilled out, thereby saving the cost;
at present, no universal analysis method exists, the composition of a crude phenol sample is complex and viscous, direct sample injection analysis cannot be carried out, and even if the crude phenol sample is diluted, a PEG2 m packed column is recommended to be used in a method for chromatographic analysis, and other components cannot be separated from diisopropyl ether.
Disclosure of Invention
The invention aims to provide a method for detecting the content of diisopropyl ether in crude phenol, which is used for overcoming the problems in the prior art,
in order to achieve the purpose, the invention provides the following technical scheme:
a method for detecting the content of diisopropyl ether in crude phenol is characterized by comprising the following steps:
the method comprises the following steps: building a chromatographic detection device;
step two: mixing crude phenol containing diisopropyl ether with toluene, and distilling to obtain a sample liquid to be detected;
step three: and (3) determining the content of the trace diisopropyl ether in the sample liquid to be detected by gas chromatography.
Preferably, the chromatographic detection device is set up in the first step and comprises a split-flow sample inlet chromatographic column interface connected with a chromatographic column HP-INNOWAX, the chromatographic column HP-INNOWAX is connected with a FID detector, and nitrogen is used as carrier gas.
Preferably, in the second step, the ratio of the amount of the crude phenol containing diisopropyl ether to the amount of toluene added is 10g to 1 ml.
Preferably, in step two, the distillation rate is 1-2 drops per second.
Preferably, in the second step, the distillation device is a rectifier and a receiver, the heating is stopped when the sample liquid to be tested approaches the branch pipe of the receiver, the receiver is removed, the effluent is poured into a measuring cylinder to be mixed evenly, and the volume is read.
Preferably, in the third step, 1 microliter of the liquid sample to be tested is absorbed, and a trace amount of sample injection is adopted, and the sample injection is carried out through the sample injection port for analysis.
Preferably, the third step comprises the following specific steps:
3.1 calibration Curve
Respectively adding diisopropyl ether with different weights into 5 clean, dry and sealed 25ml ground bottles, then adding chromatographic pure toluene to 25ml, calculating the concentration value of the diisopropyl ether, determining according to chromatographic conditions, quantifying by using an external standard method, and drawing a standard curve;
3.2 determination of the samples
Pretreating a crude phenol sample, recording the distillation volume V, slightly sucking 1 microliter of distillate, determining according to the test conditions same as curve drawing, and recording the content m of diisopropyl ether in the distillate;
3.3 calculation of results
The diisopropyl ether content w in the crude phenol was calculated.
Preferably, the weight of the diisopropyl ether added to the calibration curve is 0.1g, 0.2 g, 0.4g, 0.8g, 1.6g, respectively.
Preferably, the gas chromatography is carried out under the following measurement conditions:
sample inlet temperature: 200 deg.C
The split ratio is as follows: 100
Linear velocity: 20cm/sec
A chromatographic column: HP-INNOWAX
Column temperature: starting at 50 ℃ and increasing at a rate of 20 ℃ per minute to 180 DEG C
FID temperature: at 200 ℃.
Compared with the prior art, the invention has the following beneficial effects
The invention provides a method for detecting the content of diisopropyl ether in crude phenol, which comprises the steps of firstly, building a chromatographic detection device to ensure that a sample liquid to be detected can be detected in time after being obtained, then mixing crude phenol containing diisopropyl ether with toluene, separating most of components in the diisopropyl ether and the crude phenol, reducing the interference of impurities on chromatographic analysis, and finally, measuring the content of trace diisopropyl ether in the crude phenol by a gas chromatography, thus simply and quickly measuring the result.
Drawings
FIG. 1 is a schematic diagram of a connection of a chromatography detection apparatus according to the present invention;
FIG. 2 is a schematic view of a distillation apparatus according to the present invention;
FIG. 3 is a schematic diagram of a receiver of the present invention;
FIG. 4 is a schematic representation of diisopropyl ether contained in the crude phenol in the inventive examples.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
As shown in FIGS. 1-4, a method for detecting the content of diisopropyl ether in crude phenol comprises the following steps:
the method comprises the following steps: building a chromatographic detection device;
step two: mixing crude phenol containing diisopropyl ether with toluene, and distilling to obtain a sample liquid to be detected;
step three: determining the content of trace diisopropyl ether in the crude phenol by gas chromatography of a sample liquid to be detected;
and step one, setting up a chromatographic detection device, wherein the outlet of the split-flow sample inlet is connected with a chromatographic column HP-INNOWAX, and then is connected with a FID detector, and nitrogen is used as carrier gas.
In the second step, the adding amount ratio of the crude phenol sample to the toluene is 10g to 1 ml.
In the second step, the distillation speed is 1-2 drops per second.
In step two, the heating is stopped when the sample liquid approaches the receiver branch pipe, the receiver is taken off, the effluent is poured into a measuring cylinder and mixed evenly, and the volume is read.
In the third step, 1 microliter of sample liquid to be detected is absorbed, and micro sample introduction is adopted, and sample introduction is carried out through a sample introduction port for analysis.
The third step comprises the following concrete steps:
3.1 calibration Curve
Using 5 clean, dry and sealable 25ml ground bottles, adding diisopropyl ether by a weighing method, then adding chromatographic pure toluene to 25ml to obtain the content of diisopropyl ether, measuring according to chromatographic conditions, quantifying by an external standard method, and drawing a standard curve;
3.2 determination of the samples
The crude phenol sample was pretreated, the distillate volume v (ml) was recorded, 1. mu.l of the distillate was aspirated with a trace amount, and the diisopropyl ether content m (g/ml) in the distillate was recorded by measuring under the same test conditions as the curve plotting.
3.3 calculation of results
The diisopropyl ether content w (%) in the crude phenol;
gas chromatography, the determination conditions were:
sample inlet temperature: 200 deg.C
The split ratio is as follows: 100
Linear velocity: 20cm/sec
And (3) chromatographic column: HP-INNOWAX
Column temperature: 50 ℃ (5min) -20 ℃/min-180 ℃ (10min)
FID temperature: 200 deg.C
The embodiment is as follows:
firstly, a chromatographic detection device is set up, the outlet of a shunt sample inlet is connected with a chromatographic column HP-INNOWAX, and then is connected with a FID detector, and nitrogen is used as carrier gas.
Secondly, pretreatment of a crude phenol sample:
weighing 50g of crude phenol sample into a distillation flask, adding 5ml of toluene, connecting a receiver and a condenser tube, distilling at the speed of 1-2 drops per second, stopping heating when approaching a branch tube of the receiver, removing the receiver, pouring the effluent into a measuring cylinder, mixing uniformly, and reading the volume.
Note: firstly, the purpose of adding toluene is to completely distill out diisopropyl ether and dilute the effluent;
② if the effluent flows back into the distillation flask through the receiver branch pipe, the measurement result will be small.
The chromatographic conditions are specifically as follows:
sample inlet temperature: 200 ℃; the split ratio is as follows: 100; linear velocity: 20 cm/sec; a chromatographic column: HP-INNOWAX column temperature: 50 ℃ (5min) - -20 ℃/min-180 ℃ (10min) FID: 200 ℃;
third step, chromatography
3.1 calibration curve
Using clean, dry, sealable 5 25ml ground bottles, add diisopropyl ether 0.1g, 0.2 g, 0.4g, 0.8g, 1.6g by weight, then chromatographic grade toluene to 25ml, with diisopropyl ether content of 0.004g/ml, 0.008g/ml, 0.016g/ml, 0.032g/ml, 0.064g/ml, determine according to chromatographic conditions, quantify by external standard method, draw standard curve.
3.2 measurement of samples
The crude phenol sample was pretreated, the distillate volume v (ml) was recorded, 1. mu.l of distillate was aspirated under the same test conditions as for the curve, and the diisopropyl ether content m (g/ml) in the distillate was recorded.
3.3 calculation of results
Diisopropyl ether content w (%) in crude phenol:
table 1: diisopropyl ether to toluene retention time and peak area
Peak# | Cmpd Name | Ret.Time | Area |
1 | Diisopropyl ether | 3.143 | 1621651 |
2 | Toluene | 8.400 | 184367622 |
Although embodiments of the present invention have been described above with reference to the accompanying drawings, the present invention is not limited to the above-described embodiments and application fields, and the above-described embodiments are illustrative, instructive, and not restrictive. Those skilled in the art, having the benefit of this disclosure, may effect numerous modifications to the disclosed embodiments without departing from the scope of the invention as defined by the appended claims.
Claims (10)
1. A method for detecting the content of diisopropyl ether in crude phenol is characterized by comprising the following steps:
the method comprises the following steps: building a chromatographic detection device;
step two: mixing crude phenol containing diisopropyl ether with toluene, and distilling to obtain a sample liquid to be detected;
step three: and (3) determining the content of the trace diisopropyl ether in the sample liquid to be detected by gas chromatography.
2. The method for detecting the content of diisopropyl ether in crude phenol according to claim 1, wherein the step one of setting up a chromatographic detection device comprises connecting a split-flow sample inlet chromatographic column interface with a chromatographic column HP-INNOWAX, connecting the chromatographic column HP-INNOWAX with a FID detector, and using nitrogen as carrier gas.
3. The method for detecting the content of diisopropyl ether in crude phenol according to claim 1, wherein in step two, the addition ratio of crude phenol containing diisopropyl ether to toluene is 10g:1 ml.
4. The method for detecting the content of diisopropyl ether in crude phenol according to claim 1, wherein in said second step, the distillation speed is 1-2 drops per second.
5. The method for detecting the content of diisopropyl ether in crude phenol according to claim 1, wherein in the second step, the distillation device is a rectifier and a receiver, the heating is stopped when the sample liquid to be detected approaches the branch tube of the receiver, the receiver is removed, the effluent is poured into a measuring cylinder for mixing, and the volume is read.
6. The method for detecting the content of diisopropyl ether in crude phenol according to claim 1, characterized in that in step three, 1 microliter of sample liquid to be detected is sucked, and a trace amount of sample injection is adopted and is carried out through a sample injection port for analysis.
7. The method for detecting the content of diisopropyl ether in crude phenol according to claim 1, characterized by comprising the following three specific steps:
3.1 calibration Curve
Respectively adding diisopropyl ether with different weights into 5 clean, dry and sealed 25ml ground bottles, then adding chromatographic pure toluene to 25ml, calculating the concentration value of the diisopropyl ether, measuring according to chromatographic conditions, quantifying by using an external standard method, and drawing a standard curve;
3.2 determination of the samples
Pretreating a crude phenol sample, recording the distillation volume V, slightly absorbing 1 microliter of distillate, measuring according to the test condition which is the same as the curve drawing, and recording the content m of diisopropyl ether in the distillate;
3.3 calculation of results
The diisopropyl ether content w in the crude phenol was calculated.
8. The method for detecting the content of diisopropyl ether in crude phenol according to claim 7, wherein the weight of diisopropyl ether added to said calibration curve is 0.1g, 0.2 g, 0.4g, 0.8g, 1.6g, respectively.
10. The method for detecting the content of diisopropyl ether in crude phenol according to claim 7, characterized in that the determination conditions of the gas chromatography are as follows:
sample inlet temperature: 200 deg.C
The split ratio is as follows: 100
Linear velocity: 20cm/sec
A chromatographic column: HP-INNOWAX
Column temperature: starting at 50 ℃ and increasing at a rate of 20 ℃ per minute to 180 DEG C
FID temperature: at 200 ℃.
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