CN201965085U - Sample holder - Google Patents
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- CN201965085U CN201965085U CN2010206964120U CN201020696412U CN201965085U CN 201965085 U CN201965085 U CN 201965085U CN 2010206964120 U CN2010206964120 U CN 2010206964120U CN 201020696412 U CN201020696412 U CN 201020696412U CN 201965085 U CN201965085 U CN 201965085U
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- sample
- sample holder
- single hole
- preparation plate
- sample preparation
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Abstract
The utility model provides a sample holder which is used on an analytical apparatus. The sample holder can hold a single-hole sampling plate loading a sticky solid material, so as to facilitate the analytic determination of the sticky solid material on the analytical apparatus.
Description
Technical field
The utility model relates to a kind of sample holder, and this sample holder is used to support sample to be detected, in analytical instrument sample is analyzed helping.
Background technology
In chemical field, in the time need carrying out assay determination, need to use the sample of this material usually to the component of certain chemical substance.Solid sample is with various multi-form existence, and test purpose has nothing in common with each other, thereby various solid sample preparation methods are arranged.The most frequently used is pressed halide disk technique, paste method and membrane process.For pressed halide disk technique, the most frequently used halogenide compressing tablet matrix is potassium bromide, and it is transparent fully at middle infrared, under high pressure can be changed into transparent compressing tablet.The sample that general infrared analysis is used is the small pieces about diameter 13mm, the about 1mm of thickness.Get about 1-2mg sample and add the dry levigate potassium bromide powder of 100-200mg after agate mortar or vibrations are levigate in the bowl mill, fully mix and grind, making average particle size particle size is to get final product about 2 μ m.Ground potpourri is put into equably between the backform and bed die of mould, then mould is put into sheeter, at 10T/cm
2About pressure under can obtain transparent or semitransparent sample in 1-2 minute, pressure should not be too high, otherwise can mold damage.From mould, take out sample and want extreme care in order to avoid the sample fragmentation.Best compacting when compressing tablet while vacuumizing, so that extract air between powder particle out, otherwise the sample that is pressed into suction and become opaque easily, and easily break.Potassium bromide is very big to the corrosivity on steel die surface.Mould is kept in the dry environment then with must in time cleaning up later.A shortcoming of the method is a compressing tablet process very complicated, operation must be carried out in the room of low humidity, and the potassium bromide powder is easy to suction, and the metal surface is easy to adhere to the potassium bromide powder, need water to remove potassium bromide on specimen holder, compressing tablet frame and the filtrator, use acetone drying then.Especially specimen holder, pressing potassium bromide troche mould and compressing tablet frame need be kept in the exsiccator.
For the sample that obtains by said method, can directly put into the sample cell that analytical instrument carries usually and qualitatively or quantitatively determine.The effect of described sample cell is to keep the position of sample in analytical instrument, and sample is in same position when guaranteeing to measure at every turn, reduces measuring error.For example, when described analytical instrument was spectrometer, described sample cell kept the position of sample in spectrometer, makes light beam can just in time see through sample.
It is to be noted especially, for viscous solid material rubber polymer (as butyl rubber and ethylene-propylene-diene rubber) for example, because its viscosity is big, yielding characteristics, when with above-mentioned pressed disc method sample preparation, because its viscosity is difficult to take out from mould greatly, this on the other hand taking-up is operated also can cause the very big distortion of sample generation on the one hand, thereby the result of impact analysis causes analysis result inaccurate.In addition, above-mentioned pressed disc method can not guarantee the thickness of sample compressing tablet, and must carry out the mensuration of thickness of sample, but because the viscosity of viscous solid material is big, yielding, its Determination of thickness is difficulty very, and therefore above-mentioned pressed disc method can not guarantee the accuracy of thickness of sample, and this also can have influence on analytical accuracy.
In addition, in above-mentioned pressed disc method, use potassium bromide that sample to be tested is diluted, this is perhaps feasible for analyzing higher component concentration, but for low component concentration, for example be low to moderate the butyl rubber degree of unsaturation of 0.5%～3.3% (mol), it is difficult to draw measurement result accurately by analytical instrument after further being diluted by potassium bromide.
The utility model content
In order to overcome the defective of above-mentioned prior art, the inventor has proposed to use a kind of new method for making sample to prepare the sample of viscous solid material, so that on analytical instrument described viscous solid material is analyzed accurately and rapidly, the information feedback of in time carrying out industrial installation is to instruct next step production.
Described method for making sample comprises:
A) a certain amount of viscous solid material is put into the single through hole of a single hole sample preparation plate, and at the both sides of described single hole sample preparation plate covering spacer assembly, wherein said single hole sample preparation plate has the thickness identical with sample to be made, and described single hole sample preparation plate and described spacer assembly are formed single hole sample preparation mould jointly;
B) the single hole sample preparation mould that will be loaded with described viscous solid material is put into sheeter and is carried out compressing tablet;
C) after compressing tablet is finished, cool off, remove described spacer assembly then, thereby obtain being loaded in the sample of the described viscous solid material on the described single hole sample preparation plate.
Owing to adopted above-mentioned new method for making sample, especially sample keeps being loaded on the sample preparation plate rather than from the sample preparation plate taking out after making, therefore the sample cell that being generally used for of carrying on the analytical instrument placed sample may become unavailable, thereby need a kind of special sample holder to keep sample, sample is in same position when guaranteeing to measure at every turn, reduce measuring error, guarantee the accuracy of measurement result.
Particularly, the utility model provides a kind of sample holder that is used on the analytical instrument, described sample holder is used to support the single hole sample preparation plate of the specimen preparation that is used for the viscous solid material, described single hole sample preparation plate has the thickness identical with sample to be made, and the single through hole of described single hole sample preparation plate is used to hold the sample of only being made up of described viscous solid material, wherein, described sample holder has holding device to keep the accommodating single hole sample preparation plate of described viscous solid material sample, so that on analytical instrument described viscous solid material sample is carried out assay determination.
That is to say, when adopting above-mentioned new method for making sample, after sample is made, do not take out, but be put on the sample holder of the present utility model, on analytical instrument, carry out qualitative or quantitative test then together with single hole sample preparation plate from single hole sample preparation plate.Therefore, sample holder of the present utility model has remedied the deficiency of the sample cell that analytical instrument carries, and has widened the range of application of analytical instrument.
Described analytical instrument can be spectrometer, for example infrared spectrometer.
Should point out, above-mentioned new method for making sample mainly comprises 3 points with respect to the difference and the beneficial effect of method for making sample of the prior art: at first, above-mentioned new method for making sample directly carries out compressing tablet with a certain amount of viscous solid material to be measured, does not need to use KBr as dispersion medium.So not only simplify technological process, saved time and expense, and prevented that low component concentration from further being diluted, improved the accuracy of measurement result.Next, the single hole sample preparation plate that above-mentioned new method for making sample uses has identical thickness with sample to be made.Like this, can make the certain sample of thickness exactly, avoid thickness of sample is measured, guarantee the accuracy of thickness of sample.Once more, above-mentioned new method for making sample does not need to take out the sample that makes from single hole sample preparation plate after sample is made, but the single hole sample preparation plate of load sample is directly placed on the sample holder of the present utility model, carries out assay determination then on analytical instrument.Like this, not only omit sample and taken out operation, saved the running time, and the more important thing is and avoided the sample distortion, thereby improved the accuracy of analysis result.
Preferably, the holding device of described sample holder comprises body, has groove at the top of described body, and described single hole sample preparation plate can be maintained in the described groove and can slide in described groove.
The holding device that it is also contemplated that described sample holder comprises a pair of jaw, and described single hole sample preparation plate can be by described jaw clamping.
The size and dimension of described sample holder is not particularly limited, as long as can play in effect that stably keeps described single hole sample preparation plate and the test cabinet that can be placed on analytical instrument suitably just passable.For example, the body of described sample holder can be rectangular shape.
Preferably, described sample holder has at least one leg, has roller on described leg.Like this, can be when carrying out assay determination along any direction mobile example support easily, thereby find best locating to measure rapidly.
The material of described sample holder also is not particularly limited, and for example can be made by stainless steel, copper, cast iron, aluminium, plastics etc.
It needs to be noted that be illustrated although be used for the Infrared survey method with above-mentioned sample holder in this manual, the purposes of obvious described sample holder is not limited to this.In fact, described sample holder also can be used at other analytical instrument supporting sample preparation plate.
Description of drawings
Fig. 1 is the decomposing schematic representation of the single hole sample preparation mould in the preferred embodiment of the related method for making sample of the utility model, and viscous solid material wherein to be measured also is not placed in the single through hole of single hole sample preparation plate;
Fig. 2 is the synoptic diagram that is loaded with the single hole sample preparation plate of the viscous solid material sample that completes; And
Fig. 3 is the synoptic diagram according to the sample holder of preferred embodiment of the present utility model.
Embodiment
With reference to Fig. 1, wherein show the decomposing schematic representation of the single hole sample preparation mould in the preferred embodiment of the related method for making sample of the utility model.Described single hole sample preparation mould represents with reference number 1 that totally it comprises single hole sample preparation plate 2, will cover the polytetrafluoroethylene film 3 and the steel plate 4 of single hole sample preparation plate 2 both sides successively.Described single hole sample preparation plate 2 comprises and will hold the single through hole 5 of viscous solid material 6, and has the thickness identical with sample to be made.
Fig. 2 shows the synoptic diagram of the single hole sample preparation plate 2 that is loaded with the viscous solid material sample that completes.After sample making is finished, need not from single hole sample preparation plate 2, to take out, carry out assay determination but be retained in the single hole sample preparation plate 2.
Fig. 3 shows the synoptic diagram according to the sample holder of preferred embodiment of the present utility model.This sample holder is made by stainless steel and is totally represented with reference number 7, it comprises body 8, have groove 9 at the top of this body 8, single hole sample preparation plate 2 can be placed in this groove 9 with being stabilized and can slide in this groove 9, thereby can adjust the measuring position by the slip of single hole sample preparation plate 2 when measuring on analytical instrument.
This sample holder 7 also comprises the legs 10 of two band rollers, like this, can be when carrying out assay determination along any direction mobile example support easily, thereby find best locating to measure rapidly.
In a preferred embodiment of the related method for making sample of the utility model, used hot sheeter is CARVER-3800 hot press (U.S. laboratory equipment company), and used balance is METTLERAL-204, precision 0.1mg.Used viscous solid material is synthetic butyl rubber.
Take by weighing 0.1850g butyl rubber sample, put into the single hole sample preparation plate 2 of aperture 13mm, thickness 0.6mm, both sides cover polytetrafluoroethylene film 3, and then press from both sides two steel plates 4, put into sheeter and carry out compressing tablet.The compressing tablet condition is: 7 tons of pressure, 150 ℃ of temperature, 5 minutes compressing tablet time.Randomly, can before compressing tablet, add 1 ton of pressure, put pressure then, repeatedly twice, to eliminate bubble.In addition, for thermoplastic polymer or the plasticity inorganics of chemical change does not take place, can be before compressing tablet sample be placed on the preheating regular hour in the sheeter near softening point.After compressing tablet is finished, from sheeter, take out the single hole sample preparation plate 2 that is kept by polytetrafluoroethylene film 3 and steel plate 4, place it in addition two for example thickness be in the steel plate of 2cm cooling 10 minutes so that the butyl rubber sample cooling and shaping in the through hole 5 of single hole sample preparation plate 2.After cooling, take out by the single hole sample preparation plate 2 of polytetrafluoroethylene film 3 and steel plate 4 maintenances two blocks of steel plates in addition from described, remove steel plate 4 then, take polytetrafluoroethylene film 3 off, thereby obtain being retained in the butyl rubber sample in the single through hole 5 of single hole sample preparation plate 2.
After making sample, the single hole sample preparation plate 2 that will have sample inserts in the groove 9 of sample holder 7, just can for example measure on the infrared spectrometer in analytical instrument.In the mensuration process, single hole sample preparation plate 2 can slide in groove 9, and two legs 10 of sample holder 7 can move along any direction, thereby can find best locating very soon, make light just in time can pass the center of through hole 5, carry out sample determination fast.
Claims (7)
1. sample holder that is used on the analytical instrument, described sample holder is used to support the single hole sample preparation plate of the specimen preparation that is used for the viscous solid material, described single hole sample preparation plate has the thickness identical with sample to be made, and the single through hole of described single hole sample preparation plate is used to hold the sample of only being made up of described viscous solid material, wherein, described sample holder has holding device to keep the accommodating single hole sample preparation plate of described viscous solid material sample, so that on analytical instrument described viscous solid material sample is carried out assay determination.
2. according to claims 1 described sample holder, it is characterized in that the holding device of described sample holder comprises body, have groove at the top of described body, described single hole sample preparation plate can be maintained in the described groove and can slide in described groove.
3. according to claims 1 described sample holder, it is characterized in that the holding device of described sample holder comprises a pair of jaw, described single hole sample preparation plate can be by described jaw clamping.
4. according to claims 2 described sample holders, it is characterized in that the body of described sample holder is a rectangular shape.
5. according to claims 1 described sample holder, it is characterized in that described sample holder has at least one leg.
6. according to claims 5 described sample holders, it is characterized in that, on described at least one leg, have roller.
7. according to claims 1 described sample holder, it is characterized in that the material of described sample holder is selected from stainless steel, copper, cast iron, aluminium, plastics.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010206964120U CN201965085U (en) | 2010-12-23 | 2010-12-23 | Sample holder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010206964120U CN201965085U (en) | 2010-12-23 | 2010-12-23 | Sample holder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN201965085U true CN201965085U (en) | 2011-09-07 |
Family
ID=44527631
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010206964120U Expired - Fee Related CN201965085U (en) | 2010-12-23 | 2010-12-23 | Sample holder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN201965085U (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102564988A (en) * | 2010-12-23 | 2012-07-11 | 中国石油化工股份有限公司 | Method for measuring unsaturation degree of sticky solid matter by infrared spectrometer and sample support for same |
| CN103033773A (en) * | 2011-09-29 | 2013-04-10 | 中国科学院地质与地球物理研究所 | Sample fixing device and method for intensity experiment of paleomagnetic field with the device |
| CN106772647A (en) * | 2016-11-24 | 2017-05-31 | 程燕君 | A kind of sample fixing device and the method that paleomagnetic field intensity experiment is carried out with the device |
-
2010
- 2010-12-23 CN CN2010206964120U patent/CN201965085U/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102564988A (en) * | 2010-12-23 | 2012-07-11 | 中国石油化工股份有限公司 | Method for measuring unsaturation degree of sticky solid matter by infrared spectrometer and sample support for same |
| CN103033773A (en) * | 2011-09-29 | 2013-04-10 | 中国科学院地质与地球物理研究所 | Sample fixing device and method for intensity experiment of paleomagnetic field with the device |
| CN103033773B (en) * | 2011-09-29 | 2016-08-10 | 中国科学院地质与地球物理研究所 | Sample fixing device and the method carrying out paleomagnetic field intensity experiment with this device |
| CN106772647A (en) * | 2016-11-24 | 2017-05-31 | 程燕君 | A kind of sample fixing device and the method that paleomagnetic field intensity experiment is carried out with the device |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20110907 Termination date: 20111223 |