CN202075160U - Single-hole sample preparing mold for preparing viscous solid substance sample - Google Patents
Single-hole sample preparing mold for preparing viscous solid substance sample Download PDFInfo
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- CN202075160U CN202075160U CN2010206964402U CN201020696440U CN202075160U CN 202075160 U CN202075160 U CN 202075160U CN 2010206964402 U CN2010206964402 U CN 2010206964402U CN 201020696440 U CN201020696440 U CN 201020696440U CN 202075160 U CN202075160 U CN 202075160U
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- viscous solid
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Abstract
The utility model provides a single-hole sample preparing mold for preparing a viscous solid substance sample, which comprises a single-hole sample preparing plate with a single through hole, and an isolation device covered at the two sides of the single-hole sample preparing plate, wherein the single-hole sample preparing plate has the thickness which is the same as the thickness of a sample to be prepared, and the single through hole of the single-hole sample preparing plate is used for containing the sample formed by a viscous solid substance, and detecting the sample in an analytical instrument under the condition that the sample is contained.
Description
Technical field
The utility model relates to a kind of for example single hole sample preparation mould of rubber polymer of viscous solid material that is used for.Prepared sample can be used for the assay determination of low content component, for example infrared qualitative, quantitative test.
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.
It is to be noted especially, for the viscous solid material, 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
For the defective of the method for making sample that overcomes above-mentioned prior art, the inventor has proposed a kind of method for making sample that is used for the viscous solid material, and this method comprises:
A) a certain amount of described 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.
Related viscous solid material can be sticky polymers, for example rubber polymer in the above-mentioned method for making sample.Especially, described rubber polymer comprises butyl rubber and ethylene-propylene-diene rubber.
Corresponding to above-mentioned method for making sample, the utility model relates to a kind of single hole sample preparation mould that is used for the viscous solid material, described single hole sample preparation mould comprises the single hole sample preparation plate with single through hole and covers the spacer assembly of described single hole sample preparation plate both sides, wherein, described single hole sample preparation plate has the thickness identical with sample to be made, 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, and is holding the assay determination of carrying out sample under the situation of described sample in analytical instrument.
For the spacer assembly that covers described single hole sample preparation plate both sides, for example, it can be a for example polytetrafluoroethylene film of one deck barrier film; Perhaps, it can be for example a polytetrafluoroethylene film and one deck dividing plate that is positioned on the described barrier film of one deck barrier film.Described dividing plate can be a sheet metal, and for example corrosion resistant plate, copper coin, cast iron plate, sheet tin, aluminium sheet etc. are preferably corrosion resistant plate.
Preferably, described single hole sample preparation plate is made by metal material, for example stainless steel, copper, cast iron, tin, aluminium etc.
Thickness for described single hole sample preparation plate is generally 0.1mm-1cm, and when described single hole sample preparation plate was used for infrared analysis, in general, the sample preparation plate was thick more, and the absorption peak on the infrared spectrogram is strong more, but then, also makes the spectrogram degradation; And the sample preparation plate thickness is too thin, make absorption peak strength too again a little less than, the result that influence is measured.Therefore, the thickness of described single hole sample preparation plate for example can be 0.1-1mm, preferably 0.5-0.8mm when being used for infrared analysis.
Single through hole on the described single hole sample preparation plate can have arbitrary shape, for example circle, polygon etc.Preferably, described single through hole is circular.
Should point out that use single hole sample preparation mould of the present utility model to carry out sample preparation and have easy, characteristics fast, its important difference and beneficial effect with respect to prior art mainly comprises following 3 points:
1) by using single hole sample preparation mould of the present utility model, can directly carry out compressing tablet, not need to use KBr as dispersion medium with a certain amount of viscous solid material to be measured.That is to say that the sample that makes is the pure sample product.This not only can simplify technological process, saves time and expense, and also significant for the low component concentration of measuring in the viscous solid material.As mentioned above, in the time need analyzing the low component concentration in the viscous solid material, if use KBr to carry out sample preparation as dispersion medium, then low component concentration is wherein further diluted, thereby is difficult to guarantee the accuracy of measurement result.On the contrary, use the pure sample product to prevent that low component concentration from further being diluted, thereby improved the accuracy of measurement result.
2) the single hole sample preparation plate in the single hole sample preparation mould of the present utility model has identical thickness with sample to be made.Like this, can make the certain sample of thickness exactly, avoid thickness of sample is measured.Therefore As mentioned above, for the viscous solid material, Determination of thickness is difficulty very, can not guarantee the accuracy of thickness measurement, this so that have influence on the accuracy of analysis result.On the contrary, according to the utility model,, therefore can guarantee the accuracy of thickness of sample, thereby can improve the accuracy of analysis result because the thickness of single hole sample preparation plate is sample thickness.
3) when using single hole sample preparation mould of the present utility model to carry out sample preparation, after making, sample do not need to take out the sample that makes from single hole sample preparation plate, but the single hole sample preparation plate of load sample is directly placed on the special sample holder, on analytical instrument, carry out assay determination then.As mentioned above, the viscous solid material is because easy bonding, so its sample can not separate well with mould, is easy to generate distortion.Therefore, after making sample, sample is retained in and not only omitted sample in the single hole sample preparation plate and take out operation, significantly saved the running time, and prior meaning also is to have avoided the sample distortion, thereby improved the accuracy of analysis result.
Description of drawings
Fig. 1 is the decomposing schematic representation according to the single hole sample preparation mould of preferred embodiment of the present 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; And
Fig. 2 is the synoptic diagram that is loaded with the single hole sample preparation plate of the viscous solid material sample that completes.
Embodiment
With reference to Fig. 1, wherein show decomposing schematic representation according to the single hole sample preparation mould of a preferred embodiment 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.
Using single hole sample preparation mould of the present utility model to carry out in the preferred embodiment of sample preparation, used hot sheeter is the CARVER-3800 hot press, (U.S. laboratory equipment company), and used balance is METTLER AL-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.Described sample can perform well in for example infrared analysis.
Claims (11)
1. single hole sample preparation mould that is used for the sample preparation of viscous solid material, described single hole sample preparation mould comprises the single hole sample preparation plate with single through hole and covers the spacer assembly of described single hole sample preparation plate both sides, wherein, 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.
2. according to claims 1 described single hole sample preparation mould that is used for the sample preparation of viscous solid material, it is characterized in that described viscous solid material is a sticky polymers.
3. according to claims 1 described single hole sample preparation mould that is used for the sample preparation of viscous solid material, it is characterized in that described spacer assembly comprises one deck barrier film.
4. according to claims 3 described single hole sample preparation moulds that are used for the sample preparation of viscous solid material, it is characterized in that described barrier film is a polytetrafluoroethylene film.
5. according to claims 1 described single hole sample preparation mould that is used for the sample preparation of viscous solid material, it is characterized in that described spacer assembly comprises one deck barrier film and one deck dividing plate that is positioned on the described barrier film.
6. according to claims 5 described single hole sample preparation moulds that are used for the sample preparation of viscous solid material, it is characterized in that described barrier film is a polytetrafluoroethylene film, described dividing plate is a sheet metal.
7. according to claims 6 described single hole sample preparation moulds that are used for the sample preparation of viscous solid material, it is characterized in that described sheet metal is selected from corrosion resistant plate, copper coin, cast iron plate, sheet tin, aluminium sheet.
8. according to claims 1 described single hole sample preparation mould that is used for the sample preparation of viscous solid material, it is characterized in that described single hole sample preparation plate is made by metal material.
9. according to claims 8 described single hole sample preparation moulds that are used for the sample preparation of viscous solid material, it is characterized in that described metal material is selected from stainless steel, copper, cast iron, tin, aluminium.
10. according to claims 2 described single hole sample preparation moulds that are used for the sample preparation of viscous solid material, it is characterized in that described sticky polymers is a rubber polymer.
11., it is characterized in that described rubber polymer is butyl rubber or ethylene-propylene-diene rubber according to claims 10 described single hole sample preparation moulds that are used for the sample preparation of viscous solid material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010206964402U CN202075160U (en) | 2010-12-23 | 2010-12-23 | Single-hole sample preparing mold for preparing viscous solid substance sample |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010206964402U CN202075160U (en) | 2010-12-23 | 2010-12-23 | Single-hole sample preparing mold for preparing viscous solid substance sample |
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| CN202075160U true CN202075160U (en) | 2011-12-14 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2010206964402U Expired - Fee Related CN202075160U (en) | 2010-12-23 | 2010-12-23 | Single-hole sample preparing mold for preparing viscous solid substance sample |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102564816A (en) * | 2010-12-23 | 2012-07-11 | 中国石油化工股份有限公司 | Sample preparation method of viscous solid matter and one-hole sample preparation mold used by same |
| CN106501047A (en) * | 2016-12-06 | 2017-03-15 | 铜陵有色金属集团股份有限公司金冠铜业分公司 | A kind of pelletized powder samples method for xrf analysis |
-
2010
- 2010-12-23 CN CN2010206964402U patent/CN202075160U/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102564816A (en) * | 2010-12-23 | 2012-07-11 | 中国石油化工股份有限公司 | Sample preparation method of viscous solid matter and one-hole sample preparation mold used by same |
| CN106501047A (en) * | 2016-12-06 | 2017-03-15 | 铜陵有色金属集团股份有限公司金冠铜业分公司 | A kind of pelletized powder samples method for xrf analysis |
| CN106501047B (en) * | 2016-12-06 | 2019-06-07 | 铜陵有色金属集团股份有限公司金冠铜业分公司 | A kind of pelletized powder samples method for xrf analysis |
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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: 20111214 Termination date: 20121223 |