CN106814044A - A kind of preparation method of infrared test sample - Google Patents
A kind of preparation method of infrared test sample Download PDFInfo
- Publication number
- CN106814044A CN106814044A CN201710069875.0A CN201710069875A CN106814044A CN 106814044 A CN106814044 A CN 106814044A CN 201710069875 A CN201710069875 A CN 201710069875A CN 106814044 A CN106814044 A CN 106814044A
- Authority
- CN
- China
- Prior art keywords
- test sample
- preparation
- infrared test
- infrared
- thin slice
- Prior art date
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- Pending
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- 238000012360 testing method Methods 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 19
- 230000006835 compression Effects 0.000 claims abstract description 7
- 238000007906 compression Methods 0.000 claims abstract description 7
- 239000002270 dispersing agent Substances 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 5
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 4
- 239000012634 fragment Substances 0.000 claims description 5
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical group [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 claims description 4
- 239000001103 potassium chloride Substances 0.000 claims description 2
- 235000011164 potassium chloride Nutrition 0.000 claims description 2
- 238000005070 sampling Methods 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 4
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 238000005464 sample preparation method Methods 0.000 abstract description 3
- 231100000331 toxic Toxicity 0.000 abstract description 3
- 230000002588 toxic effect Effects 0.000 abstract description 3
- 238000002203 pretreatment Methods 0.000 abstract description 2
- 238000004458 analytical method Methods 0.000 description 5
- 238000004971 IR microspectroscopy Methods 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000004820 halides Chemical class 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 206010053615 Thermal burn Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
- G01N2021/3572—Preparation of samples, e.g. salt matrices
Abstract
Pre-treatment field the present invention relates to analyze test, especially a kind of preparation method of infrared test sample.The method includes the steps of：Step one, test sample is shredded, and is dispersed evenly in compression mold, pressurization, is kept, and is taken out after pressure release, then shred；Step 2, test sample is put in mortar, adds dispersant, mixes, and is fully ground, and powder is uniformly spread on compression mold, is pressurizeed, and is kept, and takes out thin slice after pressure release., without the use of expensive accessory device and toxic reagent, process is simple, and signal is good, and consumptive material is few, low cost for the sample preparation methods that the present invention is provided.
Description
Technical field
Pre-treatment field the present invention relates to analyze test, the especially preparation method of infrared test sample.
Background technology
Infrared spectrum is one of now the most commonly used analysis means of testing.By infrared spectrum analysis, not only can be true
Molecular structure that is fixed or speculating sample, additionally it is possible to quantitative determination is carried out to a certain predetermined substance, therefore is widely used in chemistry, material
The fields such as material, environmental protection, biology.Pressed halide disk technique is most common infrared test sample preparation methods, generally with KBr institute
As diluent, sufficiently ground after mixing with a certain amount of sample, pressurization be made transparent or semitransparent thin slice carry out it is red
Outer analysis.But for part high molecular polymer, physical property stabilization, preferably, it is very big to grind difficulty, uses for ductility
Pressed halide disk technique usually can because of crush not enough, granularity it is excessive cause compared with strong scattering, absorption band distortion so that spectrogram is difficult to
Parsing, so generally requiring using infrared microscopy, ATR（Decay total reflection）GC-MS is analyzed, or with solution film casting method, hot pressing
Embrane method film-making.But infrared microscopy, ATR GC-MSs not only need expensive accessory device, also exist sensitivity it is low, can only
The shortcomings of analysis top layer drawn game portion structure.Solution film casting method usually needs to use the toxic reagents such as acetone, toluene, harm experiment people
Member is healthy, and part high polymer is difficult to find that suitable solvent.The hot pressing annex price that hot pressed disc method is used is higher, to temperature
The requirement of the conditions such as degree, pressure, sample size is higher, generally requires just obtain suitable sample by repeatedly preparation, in operating process
Also easily scald.
The patent of invention of application number 201210380845.9 provides a kind of infrared analysis preparation of sections method to be measured
And the method for determining Fc, Ec and Et.Be prepared as impact copolymer by compressing tablet, cooling, broken, compressing tablet again by sample
Thin slice to be measured.But the invention only relates to the production field of copolymer；The method uses hot pressed disc method, it is still necessary to supporting various attached
Part, it is relatively costly；Operating process need to repeatedly be heated and quickly cooled down, and process is complicated, cumbersome.
The content of the invention
The present invention proposes a kind of preparation method of infrared test sample, mainly includes the following steps that：
Step one, test sample is shredded, and is dispersed evenly in compression mold, pressurization, is kept, and is taken out after pressure release, then shred.
Step 2, test sample is put in mortar, adds dispersant, mixes, and is fully ground, and powder is uniformly spread in into compressing tablet
On mould, pressurization keeps, and takes out thin slice after pressure release.Thin slice should be translucent that shape, thickness are uniform, surface is smooth, immaculate and
Hole.If undesirable, piece crushed again, is ground, compressing tablet, until obtaining satisfactory thin slice.
Further, test sample sampling amount described in step one is 0.2 ~ 2mg.
Further, it is that test sample is cut into fragment of the length of side no more than 2mm that sample described in step one is shredded.
Further, pressurization described in step one and step 2 refers to and is forced into 8-20MPa.
Further, step one is to maintain 1 ~ 5min with holding described in step 2.
Further, dispersant described in step 2 is KBr or sodium chloride, potassium chloride.
Further, dispersant dosage described in step 2 is 40 ~ 400mg.
Further, whole film-making process is carried out under infrared lamp.
The sample preparation methods that the present invention is provided, make test sample fully extend by first time pressurization, destruction test sample
Physical arrangement, does not interfere with the molecular spectrum test of test sample, substantially reduces the difficulty of subsequent grinding operation.The method compressing tablet enters
The spectrogram quality that row infrared scan is obtained sets better than the spectrogram that infrared microscopy, ATR technologies are obtained without the use of expensive annex
Standby and toxic reagent, process is simple, and consumptive material is few, low cost.
Specific embodiment
With reference to embodiment, the present invention will be further described, but the present invention is any limitation as never in any form, base
In any change or improvement that the present invention is made, protection scope of the present invention is belonged to.
Embodiment 1
Step one, takes polytetrafluoroethylsample sample 2mg, and it is 1mm × 1mm fragments to shred, and is dispersed evenly in compression mold, is forced into
15MPa, keeps 3min, is taken out after pressure release, then shred the fragment for 1mm × 1mm.
Step 2, the polytetrafluoroethylene (PTFE) fragment in step one is put in agate mortar, adds dry spectroscopic pure KBr
Powder 400mg, is fully ground, and mixes, and the powder of acquisition is uniformly spread on compression mold, is forced into 10MPa, is kept
1min, takes out thin slice after pressure release.Check thin slice and should be translucent that shape, thickness are uniform, surface is smooth, immaculate and hole.If
Do not meet, piece is crushed again, is ground, compressing tablet, until obtaining satisfactory thin slice.
The present invention is used above-described embodiment for illustrative purposes only, is not the limitation to patent of the present invention.It should be pointed out that right
In one of ordinary skill in the art, in the case where present inventive concept scope is not departed from, can be so that various changes can be made and becomes
Type, these belong to protection scope of the present invention.
Claims (8)
1. a kind of preparation method of infrared test sample, it is characterised in that mainly include the following steps that：
Step one, test sample is shredded, and is dispersed evenly in compression mold, pressurization, is kept, and is taken out after pressure release, then shred；
Step 2, test sample is put in mortar, adds dispersant, mixes, and is fully ground, and powder is uniformly spread in into compression mold
On, pressurization keeps, and takes out thin slice after pressure release；The good thin slice of proterties should be translucent, and shape, thickness are uniform, surface is smooth, nothing
Spot and hole；If undesirable, piece crushed again, is ground, compressing tablet, until obtaining satisfactory thin slice.
2. a kind of preparation method of infrared test sample as claimed in claim 1, it is characterised in that test sample described in step one
Sampling amount is 0.2 ~ 2mg.
3. a kind of preparation method of infrared test sample as claimed in claim 1, it is characterised in that being shredded described in step one is
Test sample is cut to fragment of the length of side no more than 2mm.
4. a kind of preparation method of infrared test sample as claimed in claim 1, it is characterised in that step one and step 2 institute
It refers to be forced into 8 ~ 20MPa to state pressurization.
5. a kind of preparation method of infrared test sample as claimed in claim 1, it is characterised in that step one and step 2 institute
State holding and be to maintain 1 ~ 5min.
6. a kind of preparation method of infrared test sample as claimed in claim 1, it is characterised in that dispersant described in step 2
It is KBr, sodium chloride or potassium chloride.
7. a kind of preparation method of infrared test sample as claimed in claim 1, it is characterised in that dispersant described in step 2
Consumption is 40 ~ 400mg.
8. a kind of preparation method of infrared test sample as claimed in claim 1, it is characterised in that whole film-making process is red
Carried out under outer lamp.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710069875.0A CN106814044A (en) | 2017-02-08 | 2017-02-08 | A kind of preparation method of infrared test sample |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710069875.0A CN106814044A (en) | 2017-02-08 | 2017-02-08 | A kind of preparation method of infrared test sample |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106814044A true CN106814044A (en) | 2017-06-09 |
Family
ID=59112997
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710069875.0A Pending CN106814044A (en) | 2017-02-08 | 2017-02-08 | A kind of preparation method of infrared test sample |
Country Status (1)
| Country | Link |
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| CN (1) | CN106814044A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108407371A (en) * | 2018-02-08 | 2018-08-17 | 东南大学 | A kind of infrared spectrum automatic tableting press device people and its application |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85108131A (en) * | 1984-09-17 | 1987-05-13 | 埃尔塔克系统公司 | Method for making inorganic-polymer composite fibers and uses thereof (including use as dimensionally stable separators) |
| CN102879247A (en) * | 2012-10-09 | 2013-01-16 | 神华集团有限责任公司 | Method for manufacturing to-be-measured film for infrared analysis and method for measuring Fc, Ec and Et |
| WO2015195479A1 (en) * | 2014-06-16 | 2015-12-23 | Murphy Brown, Llc | Method and system for in-line analysis of products |
-
2017
- 2017-02-08 CN CN201710069875.0A patent/CN106814044A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85108131A (en) * | 1984-09-17 | 1987-05-13 | 埃尔塔克系统公司 | Method for making inorganic-polymer composite fibers and uses thereof (including use as dimensionally stable separators) |
| CN102879247A (en) * | 2012-10-09 | 2013-01-16 | 神华集团有限责任公司 | Method for manufacturing to-be-measured film for infrared analysis and method for measuring Fc, Ec and Et |
| WO2015195479A1 (en) * | 2014-06-16 | 2015-12-23 | Murphy Brown, Llc | Method and system for in-line analysis of products |
Non-Patent Citations (5)
| Title |
|---|
| 吴瑾光等: "《近代傅里叶变换红外光谱技术及应用 上》", 31 December 1994, 科学技术文献出版社 * |
| 曾幸荣等: "《高分子近代测试分析技术》", 31 May 2007, 华南理工大学出版社 * |
| 杨建国等: "《建筑装饰材料》", 31 May 2014, 西安电子科技大学出版社 * |
| 王万智等: "《工程材料》", 30 September 1989, 轻工业出版社 * |
| 钱知勉: "《塑料性能应用手册 修订版》", 31 March 1987, 上海科学技术文献出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108407371A (en) * | 2018-02-08 | 2018-08-17 | 东南大学 | A kind of infrared spectrum automatic tableting press device people and its application |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
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Application publication date: 20170609 |