CN105866159A - Testing method of specific surface area of particulate matter in suspension system - Google Patents
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- 239000000725 suspension Substances 0.000 title claims abstract description 45
- 238000012360 testing method Methods 0.000 title claims abstract description 23
- 239000013618 particulate matter Substances 0.000 title claims abstract description 18
- 239000002904 solvent Substances 0.000 claims abstract description 47
- 238000001514 detection method Methods 0.000 claims abstract description 14
- 238000000685 Carr-Purcell-Meiboom-Gill pulse sequence Methods 0.000 claims abstract description 12
- 238000005481 NMR spectroscopy Methods 0.000 claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 11
- 239000002245 particle Substances 0.000 claims description 52
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 6
- 125000004494 ethyl ester group Chemical group 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000007788 liquid Substances 0.000 abstract description 7
- 229910052681 coesite Inorganic materials 0.000 description 5
- 229910052906 cristobalite Inorganic materials 0.000 description 5
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 229910052682 stishovite Inorganic materials 0.000 description 5
- 229910052905 tridymite Inorganic materials 0.000 description 5
- 239000008187 granular material Substances 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100000027 toxicology Toxicity 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N24/00—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
- G01N24/08—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using nuclear magnetic resonance
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- Physics & Mathematics (AREA)
- High Energy & Nuclear Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a testing method of the specific surface area of a particulate matter in a suspension system. The testing method comprises the following steps: (1) carrying out nuclear magnetic resonance detection on a solvent, controlling the temperature of the solvent by virtue of a metal bath, carrying out CPMG impulse sequence testing on the solvent to obtain T2 relaxation time of the solvent, and calculating relaxation rate R2f of the solvent; (2) adding a particulate matter sample into the solvent, so as to obtain suspension liquid containing the particulate matter sample; (3) carrying out the nuclear magnetic resonance detection on the suspension liquid containing the particulate matter sample, controlling the temperature of the suspension liquid by virtue of the metal bath, carrying out the CPMG impulse sequence testing on the suspension liquid to obtain T2 relaxation time of the particulate matter sample, and calculating the average relaxation rate according to a formula: R2=PbR2b+PfR2f; and (4) calculating the specific surface area of the particulate matter according to the following formula: Sa=(R2sp*R2f)/(Psi*Kp). According to the testing method, the specific surface area of the particulate matter in a suspension state can be tested.
Description
Technical Field
The invention relates to a method for testing the specific surface area of particles in a suspension system.
Background
It is well known that the surface chemistry, affinity, wettability and specific surface area under wet conditions between particles and solvents in a liquid in suspension are of great technical importance in numerous fields of industry and research: the pharmaceutical field (drug dissolution rate and toxicology properties are directly related to the surface area of the drug); electronic materials (properties of the polishing liquid such as dispersibility, stability); coating (the formula design needs to consider dispersing agent and flow characteristic); energy field (chemical and physical state of particle surface, dispersion of carbon nanotubes and slurry); biological fields (change in specific surface area after coupling of biomaterials), and the like.
The particle interface properties will affect many properties of the material: the hiding power of the coating, the activity of the catalyst, the taste of the food, the efficacy of the drug, etc. The techniques currently used mainly include gas adsorption, mercury intrusion, gravity and osmosis. In practice, all these methods have a limitation: only "dry powder" samples can be analyzed.
Most samples, whether during manufacture or at the end of use, are dispersed in a liquid, in suspension. Measurement methods such as gas adsorption are suitable for those samples of dry powder, and cannot effectively provide information on the interfacial properties of these samples in a suspension state.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a method for measuring the specific surface area of particles in a suspension system, which can detect the specific surface area of a particle sample in the suspension in a use state.
In order to solve the problems in the prior art, the technical scheme provided by the invention is as follows:
the method for testing the specific surface area of the particles in the suspension system is characterized by comprising the following steps of:
(1) performing nuclear magnetic resonance detection on the solvent, controlling the temperature of the solvent by using a metal bath, performing CPMG pulse sequence test on the solvent, and measuring the T of the solvent2Relaxation time, calculating the solvent relaxation rate R2f;
(2) Placing a particle sample in a solvent to obtain a suspension containing particles;
(3) performing nuclear magnetic resonance detection on the suspension containing the particle sample in the step (2), controlling the temperature of the suspension by using a metal bath, performing CPMG pulse sequence test on the suspension, and measuring the T of the particle sample2Relaxation time, calculating the mean relaxation rate R of the suspension according to the formula2=PbR2b+PfR2fIn which P isbTo restrict the solvent ratio, PfIs the ratio of free solvents, R2bRelaxation rate for tethered solvents;
(4) the specific surface area of the particulate matter was calculated according to the following formula:
Sa=(R2sp*R2f)/(Ψ*Kp)
wherein,
R2spas relative relaxation rate, R2sp=(R2-R2f)/R2f;
KpIs a specific surface area relative coefficient;
psi is material volume ratio, psi ═ Vp/VL=(ω*ρL)/[ρp*(1-ω)]Weight concentration omega,
Density of solvent rhoLParticle density of a particle sample ρpAre all known.
In some embodiments, the solvent is one of water, ethanol, acetone, toluene, and ethyl ester.
In some embodiments, the temperature of the solvent in step (1) is 20-80 ℃ and the temperature of the suspension in step (3) is 20-80 ℃.
Compared with the prior art, the invention has the advantages that:
by adopting the technical scheme of the invention, the specific surface area of the particulate matter in the suspension can be tested to evaluate the interface characteristic of the particulate matter in an actual state, the testing process is simple, the testing result is stable, and the repeatability is good.
Detailed Description
The above-described scheme is further illustrated below with reference to specific examples. It should be understood that these examples are for illustrative purposes and are not intended to limit the scope of the present invention. The conditions used in the examples may be further adjusted according to the conditions of the particular manufacturer, and the conditions not specified are generally the conditions in routine experiments.
Example 1
Detection of SiO2Specific surface area of the particles in water, SiO2The particle size of the particles was 162.7nm, the particle weight density, i.e. the solids content of the suspension, was 0.255, the solvent density was 1g/ml and the particle density was 1.176 g/ml.
(1) Performing nuclear magnetic resonance detection on the solvent water, keeping the water temperature at 20-80 ℃ by using a metal bath, performing CPMG pulse sequence test on the solvent water, and measuring the T of the solvent water2The relaxation time was 2681ms and,
(2) mixing SiO2Placing the granules in solvent water to obtain the product containing SiO2A suspension of particles;
(3) to SiO-containing2Performing nuclear magnetic resonance detection on the suspension of the particles, keeping the temperature of the suspension at 20-80 ℃ by using a metal bath, and performing CPMG pulse sequence detection on the suspensionTest, T of particle samples2The relaxation time was 135.232ms which was,
(4) the specific surface area of the particulate matter was calculated according to the following formula:
Sa=(R2sp*R2f)/(Ψ*Kp)
wherein,
R2spas relative relaxation rate, R2sp=(R2-R2f)/R2f;
KpIs a specific surface area relative coefficient;
psi is material volume ratio, psi ═ Vp/VL=(ω*ρL)/[ρp*(1-ω)]Weight concentration omega,
Density of solvent rhoLParticle density of a particle sample ρpAre all known;
measuring SiO2The specific surface area of the particles in water was 96.5m2/g。
Example 2
Detection of WO3Specific surface area of particles in Ethyl ester, WO3The particle size of the particles was 59nm, the particle weight density, i.e. the solids content of the suspension, was 0.3, the solvent density was 0.901g/ml, and the particle density was 1.3 g/ml.
(1) Performing nuclear magnetic resonance detection on the ethyl ester solvent, maintaining the temperature of the solvent at 20-80 ℃ by using a metal bath, performing CPMG pulse sequence test on the solvent, and measuring the T of the solvent2Relaxation time 2482.817ms
(2) Mixing WO3Placing the granules in ethyl ester solvent to obtain the product containing WO3A suspension of particles;
(3) for containing WO3The suspension of particles is subjected to NMR measurements, the temperature of the suspension being maintained atPerforming CPMG pulse sequence test on the suspension at 20-80 ℃, and measuring T of the particle sample2Relaxation time 88.611ms
(4) The specific surface area of the particulate matter was calculated according to the following formula:
Sa=(R2sp*R2f)/(Ψ*Kp)
wherein,
R2spas relative relaxation rate, R2sp=(R2-R2f)/R2f;
KpIs a specific surface area relative coefficient;
psi is material volume ratio, psi ═ Vp/VL=(ω*ρL)/[ρp*(1-ω)]Weight concentration omega,
Density of solvent rhoLParticle density of a particle sample ρpAre all known;
measured WO3The specific surface area of the particles in water was 40.71m2/g。
Example 3
Detection of Fe2O3Specific surface area of the particles in toluene, Fe2O3The particle size of the particles was 59nm, the particle weight density, i.e. the solids content of the suspension, was 0.3, the solvent density was 0.87g/ml, and the particle density was 5.24 g/ml.
(1) Performing nuclear magnetic resonance detection on a toluene solvent, keeping the temperature of the toluene solvent at 20-80 ℃ by using a metal bath, performing CPMG pulse sequence test on the toluene solvent, and measuring the T of the toluene solvent2The relaxation time is 2704 ms;
(2) mixing Fe2O3Placing the granules in toluene to obtain the granules containing Fe2O3A suspension of particles;
(3) to pair ofFe2O3Performing nuclear magnetic resonance detection on the suspension of the particles, keeping the temperature of the suspension at 20-80 ℃ by using a metal bath, performing CPMG pulse sequence test on the suspension, and measuring the T of a particle sample2The relaxation time was 4.858 ms;
(4) the specific surface area of the particulate matter was calculated according to the following formula:
Sa=(R2sp*R2f)/(Ψ*Kp)
wherein,
R2spas relative relaxation rate, R2sp=(R2-R2f)/R2f;
KpIs a specific surface area relative coefficient;
psi is material volume ratio, psi ═ Vp/VL=(ω*ρL)/[ρp*(1-ω)]Weight concentration omega,
Density of solvent rhoLParticle density of a particle sample ρpAre all known;
measuring Fe2O3The specific surface area of the particles in water was 51.17m2/g。
The above examples are only for illustrating the technical idea and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the content of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (3)
1. The method for testing the specific surface area of the particles in the suspension system is characterized by comprising the following steps of:
(1) performing nuclear magnetic resonance detection on the solvent, controlling the temperature of the solvent by using a metal bath, performing CPMG pulse sequence test on the solvent, and measuring the T of the solvent2Relaxation time, calculating the solvent relaxation rate R2f;
(2) Placing a particle sample in a solvent to obtain a suspension containing particles;
(3) subjecting the suspension containing the particulate sample of step (2) to NMR detectionControlling the temperature of the suspension by using a metal bath, performing CPMG pulse sequence test on the suspension, and measuring the T of the particle sample2Relaxation time, calculating the relaxation rate R of the suspension according to the formula2=PbR2b+PfR2fIn which P isbTo restrict the solvent ratio, PfIs the ratio of free solvents, R2bRelaxation rate for tethered solvents;
(4) the specific surface area of the particulate matter was calculated according to the following formula:
Sa=(R2sp*R2f)/(Ψ*Kp)
wherein,
R2spas relative relaxation rate, R2sp=(R2-R2f)/R2f;
KpIs a specific surface area relative coefficient;
psi is material volume ratio, psi ═ Vp/VL=(ω*ρL)/[ρp*(1-ω)]Weight concentration omega,
Density of solvent rhoLParticle density of a particle sample ρpAre all known.
2. The method for testing the specific surface area of particulate matter in a suspension system according to claim 1, wherein: the solvent is one of water, ethanol, acetone, toluene and ethyl ester.
3. The method for testing the specific surface area of particulate matter in a suspension system according to claim 1, wherein: the temperature of the solvent in the step (1) is 20-80 ℃, and the temperature of the suspension in the step (3) is 20-80 ℃.
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Cited By (10)
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CN108872288A (en) * | 2017-05-13 | 2018-11-23 | 上海健康医学院 | Nonferromagnetic powder reuniting degree measuring method in a kind of suspension system |
CN108872026A (en) * | 2017-05-13 | 2018-11-23 | 上海健康医学院 | Powder reuniting degree measuring method in a kind of organic group suspension system |
CN108872025A (en) * | 2017-05-13 | 2018-11-23 | 上海健康医学院 | Powder reuniting degree measuring method in a kind of suspension system |
CN108872287A (en) * | 2017-05-13 | 2018-11-23 | 上海健康医学院 | Ferromagnetism powder reuniting degree measuring method in a kind of suspension system |
CN108956411A (en) * | 2018-04-09 | 2018-12-07 | 上海利物盛企业集团有限公司 | A kind of test method of graphene dispersing solution wet type specific surface area |
CN109269449A (en) * | 2018-10-12 | 2019-01-25 | 重庆大学 | Stockpile specific surface area test method |
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CN108872025A (en) * | 2017-05-13 | 2018-11-23 | 上海健康医学院 | Powder reuniting degree measuring method in a kind of suspension system |
CN108872287A (en) * | 2017-05-13 | 2018-11-23 | 上海健康医学院 | Ferromagnetism powder reuniting degree measuring method in a kind of suspension system |
CN108872288A (en) * | 2017-05-13 | 2018-11-23 | 上海健康医学院 | Nonferromagnetic powder reuniting degree measuring method in a kind of suspension system |
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CN110514687A (en) * | 2019-09-19 | 2019-11-29 | 上海景瑞阳实业有限公司 | A kind of method of inspection and system of silver powder dispersion shelf-life |
CN111257220A (en) * | 2020-02-26 | 2020-06-09 | 上海景瑞阳实业有限公司 | Method for judging bonding strength of putty powder |
CN115248226A (en) * | 2022-07-20 | 2022-10-28 | 苏州纽迈分析仪器股份有限公司 | Method for testing specific surface area of material based on nuclear magnetic resonance technology |
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