CN112697908A - Method for detecting alcohol and alcohol amine compounds in grinding aid - Google Patents
Method for detecting alcohol and alcohol amine compounds in grinding aid Download PDFInfo
- Publication number
- CN112697908A CN112697908A CN202011457457.7A CN202011457457A CN112697908A CN 112697908 A CN112697908 A CN 112697908A CN 202011457457 A CN202011457457 A CN 202011457457A CN 112697908 A CN112697908 A CN 112697908A
- Authority
- CN
- China
- Prior art keywords
- alcohol
- grinding aid
- detection
- detecting
- gas chromatograph
- 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
- 238000000227 grinding Methods 0.000 title claims abstract description 57
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 48
- -1 alcohol amine compounds Chemical class 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000012086 standard solution Substances 0.000 claims abstract description 50
- 239000012488 sample solution Substances 0.000 claims abstract description 37
- 150000001875 compounds Chemical class 0.000 claims abstract description 28
- 150000001298 alcohols Chemical class 0.000 claims abstract description 16
- 238000001514 detection method Methods 0.000 claims description 77
- 239000007789 gas Substances 0.000 claims description 39
- 239000000523 sample Substances 0.000 claims description 23
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- 239000000126 substance Substances 0.000 claims description 21
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 17
- 239000002904 solvent Substances 0.000 claims description 14
- 238000005303 weighing Methods 0.000 claims description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 13
- 239000001257 hydrogen Substances 0.000 claims description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims description 13
- 239000012159 carrier gas Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- HXKKHQJGJAFBHI-UHFFFAOYSA-N 1-aminopropan-2-ol Chemical compound CC(O)CN HXKKHQJGJAFBHI-UHFFFAOYSA-N 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 8
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 7
- 238000002347 injection Methods 0.000 claims description 7
- 239000007924 injection Substances 0.000 claims description 7
- 238000004458 analytical method Methods 0.000 claims description 6
- 238000001471 micro-filtration Methods 0.000 claims description 6
- 238000001728 nano-filtration Methods 0.000 claims description 6
- 238000001223 reverse osmosis Methods 0.000 claims description 6
- 238000000108 ultra-filtration Methods 0.000 claims description 6
- 238000011895 specific detection Methods 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 230000002349 favourable effect Effects 0.000 abstract description 2
- 230000001988 toxicity Effects 0.000 abstract description 2
- 231100000419 toxicity Toxicity 0.000 abstract description 2
- 235000019441 ethanol Nutrition 0.000 description 59
- 238000004448 titration Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 239000004568 cement Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- SLINHMUFWFWBMU-UHFFFAOYSA-N Triisopropanolamine Chemical compound CC(O)CN(CC(C)O)CC(C)O SLINHMUFWFWBMU-UHFFFAOYSA-N 0.000 description 2
- ALOUNLDAKADEEB-UHFFFAOYSA-N dimethyl sebacate Chemical compound COC(=O)CCCCCCCCC(=O)OC ALOUNLDAKADEEB-UHFFFAOYSA-N 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000007792 addition Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005251 capillar electrophoresis Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 229940014772 dimethyl sebacate Drugs 0.000 description 1
- 238000010813 internal standard method Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004832 voltammetry Methods 0.000 description 1
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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- 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
- G01N30/14—Preparation by elimination of some components
-
- 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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
- G01N2030/045—Standards internal
-
- 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
- G01N2030/062—Preparation extracting sample from raw material
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)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a method for detecting alcohols and alcamines compounds in grinding aid, which mainly comprises the following steps: firstly, preparing a standard solution; secondly, preparing a sample solution; thirdly, detecting a standard solution; fourthly, detecting the sample solution; fifthly, outputting a result; the method for detecting the alcohol and the alcohol amine compounds in the grinding aid is favorable for completely separating the alcohol and the alcohol amine compounds, and has the advantages of good recovery rate and high precision; and the cost is low, the toxicity is low, and the environmental pollution is favorably reduced.
Description
Technical Field
The invention relates to the technical field of grinding aid component detection, in particular to a method for detecting alcohol and alcohol amine compounds in a grinding aid.
Background
The grinding aid is composed of one or more substances with surface activity and other chemical additives, and mainly comprises a cement grinding aid, a powder grinding aid and a liquid grinding aid, wherein the cement grinding aid can obviously reduce the surface energy of ground powder in the grinding process of a cement material, overcome the attraction among the ground powder, reduce the grinding resistance, prevent the grinding from being pasted with balls and pasted with balls, and improve the fluidity of the ground powder, thereby reducing the power consumption of a grinding machine and improving the grinding efficiency, and the performance of the grinding aid is mainly dependent on alcohols or alcohol amine substances, such as triethanolamine, triisopropanolamine, diethanol monoisopropanolamine, ethylene glycol, glycerol and the like; the existing methods for measuring triethanolamine and triisopropanolamine mainly comprise a non-aqueous titration method, a gas chromatography, a capillary electrophoresis method, a voltammetry method, a gas-mass combination method, a neutralization titration method and the like, wherein the non-aqueous titration method is complex in operation and slow in measurement speed and cannot respectively measure the content of two components in a grinding aid, and the gas chromatography is characterized in that a grinding aid sample and absolute ethyl alcohol are uniformly mixed by a centrifugal machine, a filter membrane is used for filtering and then collecting a filtrate, dimethyl sebacate is used as an internal standard substance and added into the filtrate, a chromatographic column is selected, the content of alcohol and alcohol amine compounds in the grinding aid sample is obtained by means of gas chromatograph detection and internal standard method calculation, the detection method has higher requirement on the accuracy of pretreatment of the grinding aid sample and is inconvenient to be carried out in a common laboratory, the relative correction factor of each object to be measured is about 2-3, and the detection error is amplified, the chromatographic peak has obvious trailing phenomenon, and the accuracy of the detection result is poor, so the invention of the method for detecting the alcohol and the alcohol amine compounds in the grinding aid is particularly important.
At present, the detection method for the alcohol and alcohol amine compounds in the grinding aid is complex in operation, slow in detection speed, incapable of quantifying the amount of the alcohol and alcohol amine compounds in the grinding aid respectively, poor in accuracy of detection results, incomplete in separation and low in recovery rate, and therefore the method for detecting the alcohol and alcohol amine compounds in the grinding aid is provided.
Disclosure of Invention
In order to overcome the technical problems, the invention provides a method for detecting alcohol and alcohol amine compounds in a grinding aid.
The purpose of the invention can be realized by the following technical scheme:
a detection method of alcohols and alcamines compounds in grinding aid mainly comprises the following steps:
(1) preparing a standard solution: accurately weighing alcohol and alcamines compounds, pouring the alcohol and alcamines compounds into a centrifuge tube which is cleaned and dried in advance, and fully shaking up to obtain a standard solution;
(2) preparing a sample solution: weighing a grinding aid, pretreating by purifying, extracting and concentrating, then placing into a color comparison tube with a plug, adding a solvent into the color comparison tube with the plug for dissolving, standing for 10min, and finally filtering through a filter to obtain a sample solution;
(3) and (3) standard solution detection: adding an internal standard substance into the standard solution, and then inputting the standard solution into a gas chromatograph by using a sample injector for detection; obtaining a standard solution detection result and a standard curve I;
(4) and (3) sample solution detection: adding an internal standard substance into the sample solution, and then inputting the standard solution into a gas chromatograph by using a sample injector for detection; obtaining a sample solution detection result and a standard curve II;
(5) and (4) outputting a result: and outputting the detection result of the gas chromatograph and the analysis quasi-curve by a computer to obtain the content of the corresponding alcohol and alcohol amine compounds in the grinding aid.
Further, the gas chromatograph comprises a carrier gas system, a sample introduction system, a chromatographic column, a column incubator, a detection system and a data recording system; the chromatographic column is specifically a capillary chromatographic column, and the injection port temperature of a gas chromatograph is 250-300 ℃; the detector temperature is 250 ℃ to 300 ℃.
Further, the filter is specifically one or more of a reverse osmosis filter, a nanofiltration filter, an ultrafiltration filter and a microfiltration filter.
Further, the detection system comprises a detector, which is specifically a hydrogen flame ionization detector.
Further, the alcohol and alcamine compound is specifically triethanolamine and diethanol monoisopropanolamine, and the solvent is specifically one of absolute ethyl alcohol, methanol, acetone and cyclohexane.
Further, the parameter settings of the gas chromatograph are as follows: the carrier gas flow is 1-2.5 mL/min; the air flow is 350-400 mL/min; the hydrogen flow is 35-45 mL/min; temperature program of chromatographic column: keeping the temperature at 110-120 ℃ for 2-5 min, and then heating to 170-190 ℃ at a heating rate of 20-25 ℃/min and keeping the temperature for 2-6 min.
Further, the internal standard substance is triethanolamine.
The invention has the beneficial effects that:
(1) the invention relates to a method for detecting alcohols and alcamines compounds in a grinding aid, which comprises the following steps of: accurately weighing alcohol and alcamines compounds, pouring the alcohol and alcamines compounds into a centrifuge tube which is cleaned and dried in advance, and fully shaking up to obtain a standard solution; second step, sample solution preparation: weighing a grinding aid, pretreating by purifying, extracting and concentrating, then placing into a color comparison tube with a plug, adding a solvent into the color comparison tube with the plug for dissolving, standing for 10min, and finally filtering through a filter to obtain a sample solution; and step three, standard solution detection: adding an internal standard substance into the standard solution, and then inputting the standard solution into a gas chromatograph by using a sample injector for detection; obtaining a standard solution detection result and a standard curve I; and fourthly, detecting the sample solution: adding an internal standard substance into the sample solution, and then inputting the standard solution into a gas chromatograph by using a sample injector for detection; obtaining a sample solution detection result and a standard curve II; and fifthly, outputting results: the detection method adopts a capillary chromatographic column and a hydrogen flame ionization detector as detection tools, and is favorable for completely separating alcohols from alcohol amine compounds, and has good recovery rate and high reproducibility.
(2) According to the method for detecting the alcohol and alcohol amine compounds in the grinding aid, triethanolamine is selected as an internal standard substance to detect the alcohol and alcohol amine compounds in the grinding aid, one of absolute ethyl alcohol, methanol, acetone and cyclohexane is selected as a solvent, so that the separation effect is good, the cost is low, the toxicity is low, and the environmental pollution is reduced.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A detection method of alcohols and alcamines compounds in grinding aid mainly comprises the following steps:
(1) preparing a standard solution: accurately weighing alcohol and alcamines compounds, pouring the alcohol and alcamines compounds into a centrifuge tube which is cleaned and dried in advance, and fully shaking up to obtain a standard solution;
(2) preparing a sample solution: weighing a grinding aid, pretreating by purifying, extracting and concentrating, then placing into a color comparison tube with a plug, adding a solvent into the color comparison tube with the plug for dissolving, standing for 10min, and finally filtering through a filter to obtain a sample solution;
(3) and (3) standard solution detection: adding an internal standard substance into the standard solution, and then inputting the standard solution into a gas chromatograph by using a sample injector for detection; obtaining a standard solution detection result and a standard curve I;
(4) and (3) sample solution detection: adding an internal standard substance into the sample solution, and then inputting the standard solution into a gas chromatograph by using a sample injector for detection; obtaining a sample solution detection result and a standard curve II;
(5) and (4) outputting a result: and outputting the detection result of the gas chromatograph and the analysis quasi-curve by a computer to obtain the content of the corresponding alcohol and alcohol amine compounds in the grinding aid.
The gas chromatograph comprises a carrier gas system, a sample introduction system, a chromatographic column, a column incubator, a detection system and a data recording system; the chromatographic column is specifically a capillary chromatographic column, and the injection port temperature of a gas chromatograph is 250 ℃; the detector temperature was 250 ℃.
The filter is one or more of reverse osmosis filter, nanofiltration filter, ultrafiltration filter and microfiltration filter.
The detection system comprises a detector, and the detector is specifically a hydrogen flame ionization detector.
The alcohol and alcamine compound is triethanolamine and diethanol monoisopropanolamine, and the solvent is one of absolute ethanol, methanol, acetone and cyclohexane.
The parameters of the gas chromatograph are set as follows: the carrier gas flow is 1 mL/min; the air flow is 350 mL/min; hydrogen flow rate is 35 mL/min; temperature program of chromatographic column: keeping the temperature at 110 ℃ for 2-5 min, and then heating to 170 ℃ at the heating rate of 20 ℃/min and keeping the temperature for 2 min.
The internal standard is triethanolamine.
Example 2
A detection method of alcohols and alcamines compounds in grinding aid mainly comprises the following steps:
(1) preparing a standard solution: accurately weighing alcohol and alcamines compounds, pouring the alcohol and alcamines compounds into a centrifuge tube which is cleaned and dried in advance, and fully shaking up to obtain a standard solution;
(2) preparing a sample solution: weighing a grinding aid, pretreating by purifying, extracting and concentrating, then placing into a color comparison tube with a plug, adding a solvent into the color comparison tube with the plug for dissolving, standing for 10min, and finally filtering through a filter to obtain a sample solution;
(3) and (3) standard solution detection: adding an internal standard substance into the standard solution, and then inputting the standard solution into a gas chromatograph by using a sample injector for detection; obtaining a standard solution detection result and a standard curve I;
(4) and (3) sample solution detection: adding an internal standard substance into the sample solution, and then inputting the standard solution into a gas chromatograph by using a sample injector for detection; obtaining a sample solution detection result and a standard curve II;
(5) and (4) outputting a result: and outputting the detection result of the gas chromatograph and the analysis quasi-curve by a computer to obtain the content of the corresponding alcohol and alcohol amine compounds in the grinding aid.
The gas chromatograph comprises a carrier gas system, a sample introduction system, a chromatographic column, a column incubator, a detection system and a data recording system; the chromatographic column is specifically a capillary chromatographic column, and the injection port temperature of a gas chromatograph is 250 ℃; the detector temperature was 300 ℃.
The filter is one or more of reverse osmosis filter, nanofiltration filter, ultrafiltration filter and microfiltration filter.
The detection system comprises a detector, and the detector is specifically a hydrogen flame ionization detector.
The alcohol and alcamine compound is triethanolamine and diethanol monoisopropanolamine, and the solvent is one of absolute ethanol, methanol, acetone and cyclohexane.
The parameters of the gas chromatograph are set as follows: the carrier gas flow is 1.5 mL/min; the air flow is 400 mL/min; the hydrogen flow is 40 mL/min; temperature program of chromatographic column: keeping the temperature at 110 ℃ for 3min, and then heating to 175 ℃ at the heating rate of 20 ℃/min and keeping the temperature for 3 min.
The internal standard is triethanolamine.
Example 3
A detection method of alcohols and alcamines compounds in grinding aid mainly comprises the following steps:
(1) preparing a standard solution: accurately weighing alcohol and alcamines compounds, pouring the alcohol and alcamines compounds into a centrifuge tube which is cleaned and dried in advance, and fully shaking up to obtain a standard solution;
(2) preparing a sample solution: weighing a grinding aid, pretreating by purifying, extracting and concentrating, then placing into a color comparison tube with a plug, adding a solvent into the color comparison tube with the plug for dissolving, standing for 10min, and finally filtering through a filter to obtain a sample solution;
(3) and (3) standard solution detection: adding an internal standard substance into the standard solution, and then inputting the standard solution into a gas chromatograph by using a sample injector for detection; obtaining a standard solution detection result and a standard curve I;
(4) and (3) sample solution detection: adding an internal standard substance into the sample solution, and then inputting the standard solution into a gas chromatograph by using a sample injector for detection; obtaining a sample solution detection result and a standard curve II;
(5) and (4) outputting a result: and outputting the detection result of the gas chromatograph and the analysis quasi-curve by a computer to obtain the content of the corresponding alcohol and alcohol amine compounds in the grinding aid.
The gas chromatograph comprises a carrier gas system, a sample introduction system, a chromatographic column, a column incubator, a detection system and a data recording system; the chromatographic column is specifically a capillary chromatographic column, and the injection port temperature of a gas chromatograph is 300 ℃; the detector temperature was 250 ℃.
The filter is one or more of reverse osmosis filter, nanofiltration filter, ultrafiltration filter and microfiltration filter.
The detection system comprises a detector, and the detector is specifically a hydrogen flame ionization detector.
The alcohol and alcamine compound is triethanolamine and diethanol monoisopropanolamine, and the solvent is one of absolute ethanol, methanol, acetone and cyclohexane.
The parameters of the gas chromatograph are set as follows: the carrier gas flow is 2 mL/min; the air flow is 400 mL/min; the hydrogen flow is 40 mL/min; temperature program of chromatographic column: keeping the temperature at 120 ℃ for 4min, and then heating to 180 ℃ at the heating rate of 25 ℃/min and keeping the temperature for 5 min.
The internal standard is triethanolamine.
Example 4
A detection method of alcohols and alcamines compounds in grinding aid mainly comprises the following steps:
(1) preparing a standard solution: accurately weighing alcohol and alcamines compounds, pouring the alcohol and alcamines compounds into a centrifuge tube which is cleaned and dried in advance, and fully shaking up to obtain a standard solution;
(2) preparing a sample solution: weighing a grinding aid, pretreating by purifying, extracting and concentrating, then placing into a color comparison tube with a plug, adding a solvent into the color comparison tube with the plug for dissolving, standing for 10min, and finally filtering through a filter to obtain a sample solution;
(3) and (3) standard solution detection: adding an internal standard substance into the standard solution, and then inputting the standard solution into a gas chromatograph by using a sample injector for detection; obtaining a standard solution detection result and a standard curve I;
(4) and (3) sample solution detection: adding an internal standard substance into the sample solution, and then inputting the standard solution into a gas chromatograph by using a sample injector for detection; obtaining a sample solution detection result and a standard curve II;
(5) and (4) outputting a result: and outputting the detection result of the gas chromatograph and the analysis quasi-curve by a computer to obtain the content of the corresponding alcohol and alcohol amine compounds in the grinding aid.
The gas chromatograph comprises a carrier gas system, a sample introduction system, a chromatographic column, a column incubator, a detection system and a data recording system; the chromatographic column is specifically a capillary chromatographic column, and the injection port temperature of a gas chromatograph is 300 ℃; the detector temperature was 300 ℃.
The filter is one or more of reverse osmosis filter, nanofiltration filter, ultrafiltration filter and microfiltration filter.
The detection system comprises a detector, and the detector is specifically a hydrogen flame ionization detector.
The alcohol and alcamine compound is triethanolamine and diethanol monoisopropanolamine, and the solvent is one of absolute ethanol, methanol, acetone and cyclohexane.
The parameters of the gas chromatograph are set as follows: the carrier gas flow is 2.5 mL/min; the air flow is 400 mL/min; hydrogen flow rate is 45 mL/min; temperature program of chromatographic column: keeping the temperature at 120 ℃ for 5min, and then heating to 190 ℃ at the heating rate of 25 ℃/min and keeping the temperature for 6 min.
The internal standard is triethanolamine.
Comparative example 1
This comparative example is a non-aqueous titration test method.
The grinding aid with 12.5% triethanolamine and 16.5% diethanol monoisopropanolamine was tested by the testing methods of example 1, example 2, example 3, example 4 and comparative example 1, and the testing results are shown in the following table:
the grinding aid containing 12.5% of triethanolamine and 16.5% of diethanol monoisopropanolamine is used as a test object, and as can be seen from the above table in examples 1-4 and comparative example 1, compared with a non-aqueous titration test method in the market, the detection method disclosed by the invention has a better using effect, and the detection method disclosed by the invention is used for detecting alcohols and alcohol amine compounds in the grinding aid, so that the measured result is high in precision and recovery rate, and the detection method disclosed by the invention is simple and reliable and is easy to popularize.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (7)
1. A method for detecting alcohols and alcamines compounds in a grinding aid is characterized in that the specific detection process mainly comprises the following steps:
(1) preparing a standard solution: accurately weighing alcohol and alcamines compounds, pouring the alcohol and alcamines compounds into a centrifuge tube which is cleaned and dried in advance, and fully shaking up to obtain a standard solution;
(2) preparing a sample solution: weighing a grinding aid, pretreating by purifying, extracting and concentrating, then placing into a color comparison tube with a plug, adding a solvent into the color comparison tube with the plug for dissolving, standing for 10min, and finally filtering through a filter to obtain a sample solution;
(3) and (3) standard solution detection: adding an internal standard substance into the standard solution, and then inputting the standard solution into a gas chromatograph by using a sample injector for detection; obtaining a standard solution detection result and a standard curve I;
(4) and (3) sample solution detection: adding an internal standard substance into the sample solution, and then inputting the standard solution into a gas chromatograph by using a sample injector for detection; obtaining a sample solution detection result and a standard curve II;
(5) and (4) outputting a result: and outputting the detection result of the gas chromatograph and the analysis quasi-curve by a computer to obtain the content of the corresponding alcohol and alcohol amine compounds in the grinding aid.
2. The method for detecting the alcohols and the alcohol amines in the grinding aid according to claim 1, wherein the gas chromatograph comprises a carrier gas system, a sample injection system, a chromatographic column, a column oven, a detection system and a data recording system; the chromatographic column is specifically a capillary chromatographic column, and the injection port temperature of a gas chromatograph is 250-300 ℃; the detector temperature is 250 ℃ to 300 ℃.
3. The method for detecting alcohols and alcamines compounds in grinding aid according to claim 2, wherein the filter is one or more of a reverse osmosis filter, a nanofiltration filter, an ultrafiltration filter and a microfiltration filter.
4. The method for detecting alcohols and alcohol amines in grinding aid according to claim 2, wherein the detection system comprises a detector, and the detector is specifically a hydrogen flame ionization detector.
5. The method for detecting the alcohols and the alcamines in the grinding aid according to claim 1, wherein the alcohols and the alcamines are triethanolamine and diethanol monoisopropanolamine, and the solvent is one of absolute ethanol, methanol, acetone and cyclohexane.
6. The method for detecting the alcohol and alcohol amine compounds in the grinding aid according to claim 1, wherein the parameters of the gas chromatograph are set as follows: the carrier gas flow is 1-2.5 mL/min; the air flow is 350-400 mL/min; the hydrogen flow is 35-45 mL/min; temperature program of chromatographic column: keeping the temperature at 110-120 ℃ for 2-5 min, and then heating to 170-190 ℃ at a heating rate of 20-25 ℃/min and keeping the temperature for 2-6 min.
7. The method for detecting the alcohol and alcohol amine compounds in the grinding aid according to claim 1, wherein the internal standard substance is triethanolamine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011457457.7A CN112697908A (en) | 2020-12-10 | 2020-12-10 | Method for detecting alcohol and alcohol amine compounds in grinding aid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011457457.7A CN112697908A (en) | 2020-12-10 | 2020-12-10 | Method for detecting alcohol and alcohol amine compounds in grinding aid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112697908A true CN112697908A (en) | 2021-04-23 |
Family
ID=75507468
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011457457.7A Pending CN112697908A (en) | 2020-12-10 | 2020-12-10 | Method for detecting alcohol and alcohol amine compounds in grinding aid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112697908A (en) |
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 |
-
2020
- 2020-12-10 CN CN202011457457.7A patent/CN112697908A/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 |
|---|
| 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》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104792901B (en) | A kind of method for quantitative measuring of lithium-ion battery electrolytes solvent | |
| CN105699572A (en) | Method for simultaneously determining content of 6 types of water-soluble vitamins by HPLC-MS/MS (High Performance Liquid Chromatography-Mass Spectrometry/Mass Spectrometry) | |
| CN110702832B (en) | Application of high-content 4-hydroxyquinoline as characteristic marker of jujube honey | |
| CN106198832B (en) | A kind of quality of production control method of intensified loquet distillate | |
| CN110808203A (en) | Device and method for quickly and accurately detecting impurities in high-purity hydrogen for hydrogen fuel cell | |
| CN103743844B (en) | The assay method of ethanol content in methyl alcohol | |
| CN104345096A (en) | Method for rapidly detecting polyols in cosmetic | |
| CN102608246B (en) | Method for measuring moisture content in glyceryl triacetate | |
| CN103713066A (en) | Method for extracting and detecting vanillin, methyl vanillin, ethyl vanillin and coumarin in milk powder | |
| CN106918669B (en) | The detection method of alcohols, alcamine compound in grinding aid | |
| CN103592251A (en) | Method for directly measuring potassium sorbate in soybean sauce | |
| CN107884484A (en) | A kind of assay method of electrodes of lithium-ion batteries NMP contents | |
| CN110940746A (en) | Determination method for analyzing monosaccharide composition in cinnamon polysaccharide | |
| CN113804799A (en) | Pretreatment method and method for testing NMP content in lithium ion battery pole piece | |
| CN105606435A (en) | Pretreatment method for measuring content of mercury in soil and detection method using same | |
| CN112697908A (en) | Method for detecting alcohol and alcohol amine compounds in grinding aid | |
| CN110501394B (en) | Preparation of electrolytic solution and application of electrolytic solution in electrochemical rapid detection of content of sanshoamides | |
| CN105319303A (en) | Determination method of content of fusel in ethylene carbonate | |
| CN108037215B (en) | Detection method for measuring ammonia content in tipping paper water-based ink by using ion chromatography | |
| CN108645949A (en) | A kind of method of beet alkali content in detection zymotic fluid | |
| CN112147261A (en) | High performance liquid detection method for R-4-chloro-3-hydroxy ethyl butyrate in L-carnitine reaction solution | |
| CN111830185A (en) | Ultra-high performance liquid chromatography tandem mass spectrometry detection method of quinclorac | |
| CN216646367U (en) | VOCs gas chromatography-detector detecting system | |
| CN100543456C (en) | A kind of lithium bis (oxalato) borate content ultraviolet spectrophotometry | |
| CN105784891B (en) | A kind of hydroxyethyl/hydroxypropyl methylcellulose content assaying method |
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: 20210423 |
|
| RJ01 | Rejection of invention patent application after publication |