CN105527253A - Infrared testing method for attenuated total reflection - Google Patents
Infrared testing method for attenuated total reflection Download PDFInfo
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- CN105527253A CN105527253A CN201510873304.3A CN201510873304A CN105527253A CN 105527253 A CN105527253 A CN 105527253A CN 201510873304 A CN201510873304 A CN 201510873304A CN 105527253 A CN105527253 A CN 105527253A
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- 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
- G01N21/55—Specular reflectivity
- G01N21/552—Attenuated total reflection
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Abstract
The invention discloses an infrared testing method for attenuated total reflection. The infrared testing method for attenuated total reflection is used for testing a liquid sample or powdery sample; the liquid sample or powdery sample is shaped and pressurized on a sample bearing plane; and infrared attenuated total reflection testing is carried out on the liquid sample or powdery sample in the shaped and pressurized state. The infrared testing method for attenuated total reflection disclosed by the invention shapes and pressurizes the liquid sample or powdery sample on the sample bearing plane and carries out infrared attenuated total reflection testing on the liquid sample or powdery sample in the shaped and pressurized state, so form changes of the sample are prevented from influencing testing results.
Description
Technical field
The present invention relates to attenuated total reflection infrared test technical field, particularly relate to a kind of attenuated total reflection infrared test approach.
Background technology
The principle of attenuated total reflection examination of infrared spectrum: ATR spectral technique is a kind of application technology very widely in examination of infrared spectrum technology, and it has become the infrared sample test means of one that Fourier turn infrared test job person often uses.
Attenuated total reflection annex is referred to as ATR annex.The ATR annex that current infrared accessory manufacturer provides is divided into four classes: infrared horizontal ATR accessory, variable angle ATR, circular pond ATR and individual reflection ATR.First three class all belongs to multiple internal reflection ATR, and last class belongs to an internal reflection ATR.The principle of work of this four class ATR annex is all the same.
Attenuated total reflectance (ATR) conventional test methodologies will facilitate, and sample preparation is fast.Its principle and traditional a little difference, utilize signal intensity when decaying in the total reflection of light to measure.
When carrying out quantitative test, according to bright vigorous Beer law, accurately need control light path, namely thickness of liquid film, the very difficult fluid sample of Attenuated Total Reflectance infrared spectrum or pulverized specimen quantitative test.Main cause be fluid sample when dropping on single total reflection crystal liquid will flow to surrounding, the liquid that simultaneously some volatile is strong will volatilize fast, and pulverized specimen exists the problem of sizing difficulty equally, causes the thickness of sample accurately to control.
Also not for the good solution of fluid sample test in prior art, and when testing powder sample, usually first powder sample being squeezed in tool given shape, determining thickness of sample by pre-set shape thicknesses.
But there is certain defect in such scheme.In test process, sample needs close contact with total reflection crystal, to ensure that incident infrared ray can through the interface being totally reflected crystal and sample, enter into the degree of depth of several microns, sample, finally be reflected back crystal again, and in order to ensure that the close contact being totally reflected crystal and sample needs to apply certain pressure to sample, when applied pressure exceedes extruded pulverized specimen, it can be loose by pressure, cause test inaccurate, and the close contact being totally reflected crystal and sample room cannot be ensured when insufficient pressure.
Summary of the invention
The object of the invention is to: a kind of attenuated total reflection infrared test approach is provided, by carrying out sizing pressurization to liquor sample or powdery samples on sample load plane, and under the state of sizing pressurization, attenuated total reflection infrared test is carried out to it, avoid sample metamorphosis to impact test result.
For reaching this object, the present invention by the following technical solutions:
A kind of attenuated total reflection infrared test approach is provided, for measuring liquor sample or powdery samples, sample load plane carries out sizing pressurization to described liquor sample or described powdery samples, and under the state of sizing pressurization, attenuated total reflection infrared test is carried out to it.
For liquor sample, carry out sizing pressurization at sample load plane to it, liquid in pressure process can be avoided to cause liquor sample height uncontrollable to surrounding diffusion, and reduce the contact area of volatile liquid and air, minimizing evaporates simultaneously.
For powdery samples, at sample load plane, sizing pressurization is carried out to it, except can avoiding directly it being carried out to pressurization and making itself and sample load plane close contact cause to spread to surrounding, can also avoid adopting independent hold down gag to shape to powdery samples before testing, decrease operation quantity, larger pressure can be applied to it simultaneously, ensure itself and sample load plane close contact.
As a kind of optimal technical scheme of attenuated total reflection infrared test approach, described sizing pressurization comprises: limit described liquor sample or described powdery samples spreads along sample load plane to surrounding, and described sample is pressed on described sample load plane, make described liquor sample or described powdery samples and described sample load plane close contact.
As a kind of optimal technical scheme of attenuated total reflection infrared test approach, in described sizing pressure process, described liquor sample or the upper surface of described powdery samples and the distance of described sample load plane are controlled, ensures the thickness of described liquor sample or described powdery samples.
Preferably, with a kind of attenuated total reflection infrared test device is provided in this method, comprise the upper fixture of test and test lower clamp, in described test, fixture is set to move towards or away from described test lower clamp direction, described test lower clamp is arranged on sample load plane, described test lower clamp has sample holding tank, the sample container cavity that in described test, fixture, described test lower clamp and described sample load plane alternative coordinates formation airtight.
Sample container cavity is formed with test lower clamp by testing upper fixture, can ensure in the process of test, tested fluid sample or pulverized specimen remain in sample container cavity and do not spread to surrounding, thus test on fixture extruding under form the controlled detected sample of thickness, make the light path when measuring controlled.
As a kind of optimal technical scheme of attenuated total reflection infrared test approach, the contact area of described liquor sample or described powdery samples and described sample load plane is greater than the area of the total reflection crystal be positioned on described sample load plane.
Make the contact area of liquor sample or powdery samples and described sample load plane be greater than the area being totally reflected crystal, total reflection crystal can be made full use of, avoid sample to be damaged by pressure by total reflection crystal simultaneously.
As a kind of optimal technical scheme of attenuated total reflection infrared test approach, specifically comprise the following steps:
Step S1, liquor sample or powdery samples be placed on there is total reflection crystal sample load plane on;
Step S2, in described sample load plane, sizing pressurized operation is carried out to sample;
Step S3, total reflection crystal away from the side of sample, Infrared irradiation is carried out to sample;
Step S4, reflects infrared light to be received;
Step S5, generation infrared spectrogram.
As a kind of optimal technical scheme of attenuated total reflection infrared test approach, described step S1 liquor sample or powdery samples are placed on have total reflection crystal sample load plane on comprise:
Step S11, described sample load plane is arranged there is the test lower clamp of cylindrical cavity mould;
Step S12, in described cylindrical cavity mould, add described liquor sample or powdery samples.
As a kind of optimal technical scheme of attenuated total reflection infrared test approach, in step S2, carry out sizing pressurized operation in described sample load plane to sample to be specially: adopt the cylindrical tack pressure contact matched with described cylindrical cavity mould, in top, described liquor sample or described powder sample are exerted pressure, make described liquor sample or described powdery samples and sample load plane close contact, simultaneously accurate Control Assay thickness.
As a kind of optimal technical scheme of attenuated total reflection infrared test approach, generate infrared spectrum described in step S5 and comprise analog to digital conversion and digital-to-analog conversion.
Beneficial effect of the present invention is: by carrying out sizing pressurization to liquor sample or powdery samples on sample load plane, and carrying out attenuated total reflection infrared test to it under the state of sizing pressurization, avoiding sample metamorphosis to impact test result.
Accompanying drawing explanation
According to drawings and embodiments the present invention is described in further detail below.
Fig. 1 is attenuated total reflection infrared test approach process flow diagram described in embodiment.
Fig. 2 is attenuated total reflection infrared test device cut-open view described in embodiment.
Fig. 3 is tack pressure structure of contact terminal schematic diagram cylindrical described in embodiment.
Fig. 4 is tack pressure contact vertical view cylindrical described in embodiment.
Fig. 5 is for testing lower clamp structural representation described in embodiment.
Fig. 6 is for testing lower clamp schematic top plan view described in embodiment.
In figure:
100, fixture in test; 101, lower clamp is tested; 102, cylindrical tack pressure contact; 103, cylindrical cavity mould; 104, crystal is totally reflected; 105, the first plane mirror; 106, the second plane mirror; 107, lower clamp stationary installation.
Embodiment
Technical scheme of the present invention is further illustrated by embodiment below in conjunction with accompanying drawing.
As shown in figs. 1 to 6, introduce a kind of attenuated total reflection infrared test approach, the method is mainly used in measuring liquor sample or powdery samples, but it can be measured the figurate sample of tool equally.
In the present embodiment, sample load plane carries out sizing pressurization to described liquor sample or described powdery samples, and under the state of sizing pressurization, attenuated total reflection infrared test is carried out to it.
For liquor sample, carry out sizing pressurization at sample load plane to it, liquid in pressure process can be avoided to cause liquor sample height uncontrollable to surrounding diffusion, and reduce the contact area of volatile liquid and air, minimizing evaporates simultaneously.
For powdery samples, at sample load plane, sizing pressurization is carried out to it, except can avoiding directly it being carried out to pressurization and making itself and sample load plane close contact cause to spread to surrounding, can also avoid adopting independent hold down gag to shape to powdery samples before testing, decrease operation quantity, larger pressure can be applied to it simultaneously, ensure itself and sample load plane close contact.
In the present embodiment, described sizing pressurization is specially: limit described liquor sample or described powdery samples spreads along sample load plane to surrounding, and described sample is pressed on described sample load plane, make described liquor sample or described powdery samples and described sample load plane close contact.In described sizing pressure process, described liquor sample or the upper surface of described powdery samples and the distance of described sample load plane are controlled, ensures the thickness of described liquor sample or described powdery samples.
The contact area of described liquor sample or described powdery samples and described sample load plane is greater than the area of the total reflection crystal 104 be positioned on described sample load plane.Make the contact area of liquor sample or powdery samples and described sample load plane be greater than the area being totally reflected crystal 104, total reflection crystal 104 can be made full use of, avoid sample to be damaged by pressure by total reflection crystal 104 simultaneously.
Attenuated total reflection infrared test approach described in the present embodiment, specifically comprises the following steps:
Step S1, sample load, liquor sample or powdery samples are placed on have total reflection crystal 104 sample load plane on;
Step S1 specifically comprises:
Step S11, test fixture are installed, and described sample load plane arranges the test lower clamp 101 with cylindrical cavity mould 103;
Step S12, sample are installed, in described cylindrical cavity mould 103, add described liquor sample or powdery samples.
Step S2, sizing pressurization, carry out sizing pressurized operation in described sample load plane to sample;
Step S2 specifically comprises: adopt the cylindrical tack pressure contact 102 matched with described cylindrical cavity mould 103, in top, described liquor sample or described powder sample are exerted pressure, make described liquor sample or described powdery samples and sample load plane close contact, simultaneously accurate Control Assay thickness
Step S3, Infrared irradiation, carry out Infrared irradiation away from the side of sample to sample at total reflection crystal 104;
Step S4, infrared light receive, and receive reflects infrared light;
Step S5, generation infrared spectrogram, be converted to infrared spectrum by analog to digital conversion and digital-to-analog conversion by Infrared.
In order to realize also providing a kind of attenuated total reflection infrared test device in above-mentioned method of testing the present embodiment, comprise the upper fixture 100 of test and test lower clamp 101, in described test, fixture 100 is set to move towards or away from described test lower clamp 101 direction, described test lower clamp 101 is arranged on sample load plane, described test lower clamp 101 has sample holding tank, the sample container cavity that in described test, fixture 100, described test lower clamp 101 and described sample load plane alternative coordinates formation airtight.
Sample container cavity is formed with test lower clamp 101 by testing upper fixture 100, can ensure in the process of test, tested fluid sample or pulverized specimen remain in sample container cavity and do not spread to surrounding, thus test on fixture 100 extruding under form the controlled detected sample of thickness, make the light path when measuring controlled.
Concrete, comprise cylindrical tack pressure contact 102 in the upper fixture 100 of test described in the present embodiment, described test lower clamp 101 comprises the cylindrical cavity mould 103 matched with described cylindrical tack pressure contact 102.
Test liquid sample or pulverized specimen is held by described cylindrical cavity mould 103, exerted pressure by the sample in cylindrical tack pressure contact 102 pairs of cylindrical cavity moulds 103 again, fluid sample is avoided to flow to surrounding, or the quick problem such as volatilization, guarantee thickness of liquid film is unified, conveniently carries out quantitative test.
Be injected into optically thinner medium by optically denser medium to realize Infrared thus can form total reflection, in described sample load plane, be provided with total reflection crystal 104, the diameter of described cylindrical tack pressure contact 102 is greater than the diameter of described total reflection crystal 104.
The too small sample cake that causes of diameter is less than normal, when the pressure that sample is subject to cylindrical tack pressure contact 102 all acts on total reflection crystal 104, easily damages total reflection crystal 104; And diameter is crossed conference and is caused sample waste.
In the process of test liquid sample or pulverized specimen, in order to ensure thickness of sample, the liquid of excess or powder is needed to discharge, the diameter of cylindrical cavity mould 103 is set to the diameter being greater than cylindrical tack pressure contact 102, make to form gap between the two, when cylindrical tack pressure contact 102 pairs of samples applying acting forces make it reach predetermined thickness, unnecessary sample can be discharged from gap.Therefore in actual use, the diameter of cylindrical cavity mould 103 is greater than diameter 0.02 ㎜ to 0.1 ㎜ of described cylindrical tack pressure contact 102.The diameter of the mould of cylindrical cavity described in the present embodiment 103 is greater than diameter 0.05 ㎜ of described cylindrical tack pressure contact 102.
In order to the thickness of effective Quality control, avoiding sample to reveal between cylindrical cavity mould 103 and sample load plane, contacting being set to seal between described cylindrical cavity mould 103 with described sample load plane.Seal between described cylindrical cavity mould 103 with described sample load plane and contact.
As a kind of optimal technical scheme of attenuated total reflection infrared test device, below described sample load plane, and be positioned at the position corresponding with described total reflection crystal 104 and be provided with the first plane mirror 105 and the second plane mirror 106.
First plane mirror 105 is for receiving infrared light supply, and the incident ray sent by infrared light supply reflexes to total reflection crystal 104.Second plane mirror 106 for receiving by the infrared light that reflects of total reflection crystal 104, and by infrared light reflection to infrared spectrum detecting device.Be fixedly connected with between first plane mirror 105 with the second plane mirror 106 in the present embodiment.And can also relative angle between the first plane mirror 105 and the second plane mirror 106 be set to adjustable in other embodiments.By the first plane mirror 105 and the second plane mirror 106 angle are set to adjustable, length or the width that can make full use of installing space under different operating environment are installed attenuated total reflection infrared test device, reduce its requirement to environment for use.
Preferably, described first plane mirror 105 is arranged with described second plane mirror 106 is mutually vertical.By arranging mutually vertical to the first plane mirror 105 and the second plane mirror 106, can ensure that the infrared ray of incident infrared ray and injection is parallel to each other, reducing the Installation and Debugging requirement to attenuated total reflection infrared test device.
The side of described first plane mirror 105 is provided with infrared light supply, and the side of described second plane mirror 106 is provided with infrared spectrum detecting device.
Described test lower clamp 101 has the lower clamp stationary installation 107 of alternative fixing described sample container cavity.
Concrete, in the second movable clamping device that the stationary installation of lower clamp described in the present embodiment 107 comprises the first movable clamping device and is oppositely arranged with described first movable clamping device, described first movable clamping device and described second movable clamping device can be movable relatively or mutually deviate from motion.
Sample holds cavity and is connected with on-fixed between sample load plane, therefore in use need locate it and clamp, lower clamp stationary installation 107 is set and can realizes clamping easily, lower clamp stationary installation 107 position can also be fixed the sample accommodation cavity of different size, structure simultaneously, increases the versatility of attenuated total reflection infrared test device.
In described test, fixture 100 also comprises fixture drive unit, and described upper fixture drive unit is connected with described cylindrical tack pressure contact 102 by Flexible Connector.By upper fixture drive unit is connected with described cylindrical tack pressure contact 102 by Flexible Connector, the Flexible Connector when pressure reaches certain value can be made to be compressed, thus no longer sample is carried out excessive extruding, avoid sample load plane bear excessive pressure and damage.
In description herein, it will be appreciated that, term " on ", the orientation such as D score or position relationship be based on orientation shown in the drawings or position relationship, only for convenience of description and simplify the operation, instead of indicate or imply that the device of indication or element must have specific orientation, with specific azimuth configuration and operation, therefore can not be interpreted as limitation of the present invention.In addition, term " first ", " second ", only for being distinguished in description, not special implication.
It is to be understood that; above-mentioned embodiment is only preferred embodiment of the present invention and institute's application technology principle; in technical scope disclosed in this invention, the change that any those skilled in the art of being familiar with easily expect or replacement, all should be encompassed in protection scope of the present invention.
Claims (8)
1. an attenuated total reflection infrared test approach, for measuring liquor sample or powdery samples, it is characterized in that, sample load plane carries out sizing pressurization to described liquor sample or described powdery samples, and under the state of sizing pressurization, attenuated total reflection infrared test is carried out to it.
2. attenuated total reflection infrared test approach according to claim 1, it is characterized in that, described sizing pressurization comprises: limit described liquor sample or described powdery samples spreads along sample load plane to surrounding, and described sample is pressed on described sample load plane, make described liquor sample or described powdery samples and described sample load plane close contact.
3. attenuated total reflection infrared test approach according to claim 2, it is characterized in that, in described sizing pressure process, described liquor sample or the upper surface of described powdery samples and the distance of described sample load plane are controlled, ensures the thickness of described liquor sample or described powdery samples.
4. attenuated total reflection infrared test approach according to claim 3, is characterized in that, the contact area of described liquor sample or described powdery samples and described sample load plane is greater than the area of the total reflection crystal be positioned on described sample load plane.
5. attenuated total reflection infrared test approach according to claim 4, is characterized in that, specifically comprise the following steps:
Step S1, liquor sample or powdery samples be placed on there is total reflection crystal sample load plane on;
Step S2, in described sample load plane, sizing pressurized operation is carried out to sample;
Step S3, total reflection crystal away from the side of sample, Infrared irradiation is carried out to sample;
Step S4, reflects infrared light to be received;
Step S5, generation infrared spectrogram.
6. attenuated total reflection infrared test approach according to claim 5, is characterized in that, described step S1 liquor sample or powdery samples are placed on have total reflection crystal sample load plane on comprise:
Step S11, described sample load plane is arranged there is the test lower clamp of cylindrical cavity mould;
Step S12, in described cylindrical cavity mould, add described liquor sample or powdery samples.
7. attenuated total reflection infrared test approach according to claim 5, it is characterized in that, in step S2, carry out sizing pressurized operation in described sample load plane to sample to be specially: adopt the cylindrical tack pressure contact matched with described cylindrical cavity mould, in top, described liquor sample or described powder sample are exerted pressure, make described liquor sample or described powdery samples and sample load plane close contact, simultaneously accurate Control Assay thickness.
8. attenuated total reflection infrared test approach according to claim 5, is characterized in that, generates infrared spectrum and comprise analog to digital conversion and digital-to-analog conversion described in step S5.
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CN110520712A (en) * | 2017-12-26 | 2019-11-29 | 株式会社Lg化学 | The method for analyzing the infrared spectroscopy of polyacrylonitrile fiber |
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