CN109060999A - The measuring method of sorbitol acetal nucleation agent content - Google Patents
The measuring method of sorbitol acetal nucleation agent content Download PDFInfo
- Publication number
- CN109060999A CN109060999A CN201811065912.1A CN201811065912A CN109060999A CN 109060999 A CN109060999 A CN 109060999A CN 201811065912 A CN201811065912 A CN 201811065912A CN 109060999 A CN109060999 A CN 109060999A
- Authority
- CN
- China
- Prior art keywords
- solution
- acetonitrile
- volumetric flask
- scale
- test
- 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
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
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)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A kind of measuring method of sorbitol acetal nucleation agent content, is belonged to organic object detecting method technical field, is substantially measured using external standard method, it is characterized in that, include the following steps: 1) to prepare blank solution: pipetting DMF 10.0ml in 100ml volumetric flask, add acetonitrile to scale, shake up；2) prepare contrast solution: precision weighs standard items 20mg in 50ml volumetric flask, and DMF10.0ml is added to dissolve, and adds acetonitrile to scale, then ultrasound 2 minutes, is cooled to room temperature, shakes up, filter；3) test solution: precision weighs test sample 20mg in 50ml volumetric flask, and DMF10.0ml is added to dissolve, and adds acetonitrile to scale, then ultrasound 2 minutes, is cooled to room temperature, shakes up, filter, every batch of prepares 2 parts；4) high performance liquid chromatography is tested: after instrument balance, taking test solution sample introduction, every part of test solution sample introduction is primary, and standard solution is not greater than 2.0% into 5 needles, main peak area RSD deviation.The invention has the advantages that providing the quantitative measuring method of sorbitol acetal nucleating agent.
Description
Technical field
The present invention relates to a kind of measuring methods of sorbitol acetal nucleation agent content, belong to organic matter detection technique field.
Background technique
Polyol acetal class nucleating agent is spread out with polyalcohol (generally sorbierite or xylitol) and benzaldehyde or its substitution
Biology is occurred the resulting product of aldol reaction, is spread out with sorbierite and benzaldehyde or its substitution under the action of acid catalyst
Biology is that the general structure of the acetals nucleating agent of Material synthesis is:
Wherein, R1, R2 H, alkyl (C1~C6), alkoxy, hydroxyl or halogen atom.
In the prior art, following several modes are generallyd use to the structural characterization of the nucleating agent:
1) measurement of fusing point the measurement of fusing point: is carried out using display micro melting point apparatus nucleating agent；
2) FTIR spectrum is tested: carrying out FTIR spectrum test, scanning range to the nucleating agent of preparation
4000~500cm-1, resolution ratio 2cm-1。
In addition, also on the books in the prior art swept using petrographic microscope, scanning electron microscope, X-ray diffraction, differential
Retouch the modes such as thermometric analysis, thermogravimetic analysis (TGA).
As far as the applicant is aware, there is no the method for carrying out quantitative analysis to the nucleating agent.
Summary of the invention
The measuring method that the present invention provides a kind of sorbitol acetal nucleation agent content uses high-efficient liquid phase color using external standard method
Spectrum, realizes the quantitative analysis to sorbitol acetal nucleating agent.
The present invention it is specific the technical solution adopted is that:
A kind of measuring method of sorbitol acetal nucleation agent content, is substantially measured using external standard method, characterized in that
Include the following steps:
1) prepare blank solution: pipetting DMF 10.0ml in 100ml volumetric flask, add acetonitrile to scale, shake up；
2) prepare contrast solution: precision weighs standard items 20mg in 50ml volumetric flask, adds DMF10.0ml to dissolve, adds second
Nitrile is cooled to room temperature, shakes up, filter to scale, then ultrasound 2 minutes；
3) test solution: precision weighs test sample 20mg in 50ml volumetric flask, adds DMF10.0ml to dissolve, adds acetonitrile
To scale, then ultrasound 2 minutes, it is cooled to room temperature, shakes up, filter, every batch of prepares 2 parts；
4) high performance liquid chromatography is tested: after instrument balance, taking test solution sample introduction, every part of test solution sample introduction
Once, standard solution is not greater than 2.0% into 5 needles, main peak area RSD deviation.
Further, the test condition is: chromatographic column: 4.6 × 250mm of C18 5um
Mobile phase: it 1. matches: acetonitrile-water=580:420；
2. preparation method: measuring acetonitrile 580ml, 420ml water is added, mix, filter, degassing is spare.
3. mobile phase ratio can be adjusted, suitably when necessary to meet separation needs.
4. according to sample size how much, expand or shrink in proportion, prepare the mobile phase of different volumes.
Wavelength: 266nm；
Flow velocity: 1.0~1.2ml/min；
Sample volume: 20ul；
Column temperature: 35 DEG C；
Compared with the prior art, the advantages of the present invention are as follows: provide the quantitative test of sorbitol acetal nucleation agent content
Method.
Specific embodiment
Sorbitol acetal nucleation agent content is quantitative determined using external standard method, is included the following steps:
1) prepare blank solution: pipetting DMF 10.0ml in 100ml volumetric flask, add acetonitrile to scale, shake up；
2) prepare contrast solution: precision weighs standard items 20mg in 50ml volumetric flask, adds DMF10.0ml to dissolve, adds second
Nitrile is cooled to room temperature, shakes up, filter to scale, then ultrasound 2 minutes；
3) test solution: precision weighs test sample 20mg in 50ml volumetric flask, adds DMF10.0ml to dissolve, adds acetonitrile
To scale, then ultrasound 2 minutes, it is cooled to room temperature, shakes up, filter, every batch of prepares 2 parts；
4) high performance liquid chromatography is tested: after instrument balance, taking test solution sample introduction, every part of test solution sample introduction
Once, standard solution is not greater than 2.0% into 5 needles, main peak area RSD deviation.
Further, the test condition is: chromatographic column: 4.6 × 250mm of C18 5um
Mobile phase: it 1. matches: acetonitrile-water=580:420；
2. preparation method: measuring acetonitrile 580ml, 420ml water is added, mix, filter, degassing is spare.
3. mobile phase ratio can be adjusted, suitably when necessary to meet separation needs.
4. according to sample size how much, expand or shrink in proportion, prepare the mobile phase of different volumes.
Wavelength: 266nm；
Flow velocity: 1.0~1.2ml/min；
Sample volume: 20ul；
Column temperature: 35 DEG C.
Claims (2)
1. a kind of measuring method of sorbitol acetal nucleation agent content, is substantially measured using external standard method, characterized in that packet
Include following steps:
1) prepare blank solution: pipetting DMF 10.0ml in 100ml volumetric flask, add acetonitrile to scale, shake up；
2) prepare contrast solution: precision weighs standard items 20mg in 50ml volumetric flask, and DMF10.0ml is added to dissolve, and adds acetonitrile extremely
Scale, then ultrasound 2 minutes, it is cooled to room temperature, shakes up, filter；
3) test solution: precision weighs test sample 20mg in 50ml volumetric flask, and DMF10.0ml is added to dissolve, and adds acetonitrile to quarter
Degree, then ultrasound 2 minutes, it is cooled to room temperature, shakes up, filter, every batch of prepares 2 parts；
4) high performance liquid chromatography is tested: after instrument balance, taking test solution sample introduction, every part of test solution sample introduction one
Secondary, standard solution is not greater than 2.0% into 5 needles, main peak area RSD deviation.
2. the measuring method of sorbitol acetal nucleation agent content according to claim 1, characterized in that, the test-strips
Part is:
Chromatographic column: C184.6 × 250mm 5um
Mobile phase: it 1. matches: acetonitrile-water=580:420；
2. preparation method: measuring acetonitrile 580ml, 420ml water is added, mix, filter, degassing is spare；
Wavelength: 266nm；
Flow velocity: 1.0~1.2ml/min；
Sample volume: 20ul；
Column temperature: 35 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811065912.1A CN109060999A (en) | 2018-09-13 | 2018-09-13 | The measuring method of sorbitol acetal nucleation agent content |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811065912.1A CN109060999A (en) | 2018-09-13 | 2018-09-13 | The measuring method of sorbitol acetal nucleation agent content |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109060999A true CN109060999A (en) | 2018-12-21 |
Family
ID=64761508
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811065912.1A Pending CN109060999A (en) | 2018-09-13 | 2018-09-13 | The measuring method of sorbitol acetal nucleation agent content |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109060999A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1984949A (en) * | 2004-04-26 | 2007-06-20 | 美利肯公司 | Method of nucleating a polyolefin composition with acetal-based compounds |
| WO2010039865A2 (en) * | 2008-10-01 | 2010-04-08 | Cornell University | Biodegradable chemical delivery system |
| CN105203682A (en) * | 2015-09-10 | 2015-12-30 | 中华人民共和国台州出入境检验检疫局 | Method for determining specific migration quantity of 3 aromatic organic acids/salts in liquid chromatography-ultraviolet method |
| CN106084488A (en) * | 2016-06-07 | 2016-11-09 | 神华集团有限责任公司 | Transparent polypropylene resin and preparation method thereof |
| WO2017174546A1 (en) * | 2016-04-08 | 2017-10-12 | Solvay Specialty Polymers Usa, Llc | Photocurable polymers, photocurable polymer compositions and lithographic processes including the same |
-
2018
- 2018-09-13 CN CN201811065912.1A patent/CN109060999A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1984949A (en) * | 2004-04-26 | 2007-06-20 | 美利肯公司 | Method of nucleating a polyolefin composition with acetal-based compounds |
| WO2010039865A2 (en) * | 2008-10-01 | 2010-04-08 | Cornell University | Biodegradable chemical delivery system |
| CN105203682A (en) * | 2015-09-10 | 2015-12-30 | 中华人民共和国台州出入境检验检疫局 | Method for determining specific migration quantity of 3 aromatic organic acids/salts in liquid chromatography-ultraviolet method |
| WO2017174546A1 (en) * | 2016-04-08 | 2017-10-12 | Solvay Specialty Polymers Usa, Llc | Photocurable polymers, photocurable polymer compositions and lithographic processes including the same |
| CN106084488A (en) * | 2016-06-07 | 2016-11-09 | 神华集团有限责任公司 | Transparent polypropylene resin and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| LUCAS STERNBAUER 等: "Determination of nucleating agents in plastic materials by GC/MS after microwave-assisted extraction with in situ microwave-assisted derivatization", 《TALANTA》 * |
| 段元超 等: "聚丙烯成核剂DMDBS的合成工艺研究", 《化学工业与工程》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Li et al. | Hydrophobic deep eutectic solvents as extractants for the determination of bisphenols from food-contacted plastics by high performance liquid chromatography with fluorescence detection | |
| Andanson et al. | Quantification of the impact of water as an impurity on standard physico-chemical properties of ionic liquids | |
| CN108827998B (en) | Method for accurately measuring purity of volatile substance by adopting quantitative nuclear magnetic resonance hydrogen spectrum | |
| Xie et al. | Deep eutectic solvent-based liquid-liquid microextraction for the HPLC-DAD analysis of bisphenol A in edible oils | |
| Losetty et al. | Synthesis, spectroscopic characterization and acoustic, volumetric, transport and thermal properties of hydroxyl ammonium based ionic liquids | |
| CN103499549A (en) | Method for measuring content of trace cadmium in rice by utilizing flame atomic absorption spectrometry | |
| CN105223223A (en) | The raw quantitative detecting method for effective constituent in Buddhist nun's bulk drug of two p-toluenesulfonic acid edge | |
| CN105301031B (en) | The method that one-dimensional nuclear magnetic resonance hydrogen spectrometry determines containing hydrogen silicone oil residual quantity in trisiloxane surfactant | |
| CN111624283A (en) | Method for detecting water content in rubber | |
| CN102768263B (en) | The assay method of pentaerythrite solution concentration in a kind of production of polyester | |
| Faraji et al. | Development of a deep eutectic solvent-based dispersive liquid–liquid microextraction method followed by back-extraction and diazotization coupled to spectrophotometry for determination of total primary aromatic amines from food simulants | |
| CN109060999A (en) | The measuring method of sorbitol acetal nucleation agent content | |
| Zhou et al. | A molecularly imprinted fiber array solid-phase microextraction strategy for simultaneous detection of multiple estrogens | |
| Ulenberg et al. | Understanding performance of 3D-printed sorbent in study of metabolic stability | |
| Fitzpatrick et al. | Fabrication of solid calibration standards by a sol–gel process and use in laser ablation ICPMS | |
| CN102854264B (en) | Method for determining methanol content and methyl acetate content in polyvinyl alcohol | |
| CN116626087A (en) | Method for quantitatively analyzing allyl sucrose ether content through nuclear magnetic resonance hydrogen spectrum | |
| CN103743690A (en) | Quantitative fullerene analysis method | |
| CN104950049B (en) | A kind of analysis method of copolyamide PUR relative molecular weight and its distribution | |
| CN109912512A (en) | A kind of new Telmisartan impurity compound and its preparation method and application | |
| Fang et al. | The solid-liquid equilibrium behavior of 2, 7-dihydroxynaphthalene in eleven organic solvents: Thermodynamic analysis and molecular simulation understanding | |
| CN109738555B (en) | Method for measuring content of orthoformate in crude orthoformate | |
| CN100535657C (en) | Method for measuring purity of 9-fluorenemethanol | |
| CN105424642A (en) | Method for measuring content of alkyl groups or alkoxy groups in polysiloxane | |
| CN106442841B (en) | The method for separating and detecting of cationic surfactant in a kind of drug |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20181221 |