CN105527253B - Decay Total Reflection Infrared test method - Google Patents
Decay Total Reflection Infrared test method Download PDFInfo
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- CN105527253B CN105527253B CN201510873304.3A CN201510873304A CN105527253B CN 105527253 B CN105527253 B CN 105527253B CN 201510873304 A CN201510873304 A CN 201510873304A CN 105527253 B CN105527253 B CN 105527253B
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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 present invention discloses a kind of decay Total Reflection Infrared test method, for measuring liquor sample or powdery samples, sizing pressurization is carried out to the liquor sample or the powdery samples on sample load plane, and carries out decay Total Reflection Infrared test to it in the state of sizing is pressurizeed；The present invention provides a kind of decay Total Reflection Infrared test method, by carrying out sizing pressurization to liquor sample or powdery samples on sample load plane, and decay Total Reflection Infrared test is carried out to it in the state of sizing is pressurizeed, avoid sample form change from impacting test result.
Description
Technical field
The present invention relates to decay Total Reflection Infrared technical field of measurement and test, more particularly to a kind of decay Total Reflection Infrared test side
Method.
Background technology
Decay the principle that In situ ATR-FTIR is tested：ATR spectral techniques are a kind of applications in examination of infrared spectrum technology
Quite varied technology, it has become a kind of infrared sample that Fourier turn infrared test job person is commonly used
Product means of testing.
Decay total reflection annex is referred to as ATR annexes.The ATR annexes that current infrared accessory manufacturer provides are divided into four classes：
Infrared horizontal ATR accessory, variable angle ATR, circle pond ATR and individual reflection ATR.Preceding three classes belong to multiple internal reflection ATR, last
Class belongs to an internal reflection ATR.What the operation principle of this four classes ATR annex was just as.
Attenuated total reflectance (ATR) conventional test methodologies will facilitate, and sample preparation is fast.Its principle and traditional a little difference, utilize light
Signal intensity when decaying in total reflection measures.
When carrying out quantitative test, according to bright vigorous Beer law, light path, that is, thickness of liquid film need to be accurately controlled, is decayed
Total reflection method infrared spectrum is difficult to use fluid sample or pulverized specimen quantitative analysis.It is complete that main cause is that fluid sample drops in single
Liquid will flow around when on reflection crystal, while the liquid of part high volatility will quickly volatilize, and pulverized specimen is equally deposited
In the problem of difficult of shaping, causing the thickness of sample can not accurately control.
In the prior art also not for the good solution of fluid sample test, and when testing powder sample, lead to
Powder sample is first often squeezed into given shape in gauge, thickness of sample is determined by pre-set shape thicknesses.
But there are certain defect for such scheme.Sample needs to be in close contact with total reflection crystal during the test, with
Ensure that incident infrared ray can pass through the interface of total reflection crystal and sample, enter the depth of several microns of sample, finally
Crystal is reflected back again, and in order to ensure that the close contact for being totally reflected crystal and sample needs to apply sample certain pressure, when
When the pressure of application exceedes the pulverized specimen of extrusion forming, it can be dissipated by pressure, cause test inaccurate, and when insufficient pressure without
Method ensures the close contact of total reflection crystal and sample room.
The content of the invention
It is an object of the invention to：A kind of decay Total Reflection Infrared test method is provided, by sample load plane
Sizing pressurization is carried out to liquor sample or powdery samples, and decay Total Reflection Infrared is carried out to it in the state of sizing is pressurizeed and is surveyed
Examination, avoids sample form change from impacting test result.
For this purpose, the present invention uses following technical scheme：
A kind of decay Total Reflection Infrared test method is provided, for measuring liquor sample or powdery samples, is carried in sample
Sizing pressurization is carried out in plane to the liquor sample or the powdery samples, and is declined in the state of sizing is pressurizeed to it
Subtract Total Reflection Infrared test.
For liquor sample, sizing pressurization is carried out to it in sample load plane, can be avoided in pressure process
Liquid is spread around causes liquor sample highly uncontrollable, while reduces the contact area of volatile liquid and air, reduces
Evaporate.
For powdery samples, sizing pressurization is carried out to it in sample load plane, except can avoid directly pressurizeing to it
Make it be in close contact with sample load plane to cause to spread around outside, can also avoid using independent pressing device before testing
Shape to powdery samples, reduce operation quantity, while the pressure of bigger can be applied to it, ensure that it is carried with sample
Plane is in close contact.
As a kind of optimal technical scheme of decay Total Reflection Infrared test method, the sizing pressurization includes：Limitation institute
State liquor sample or the powdery samples are spread around along sample load plane, and the sample is pressed on the sample
On load plane, the liquor sample or the powdery samples are made to be in close contact with the sample load plane.
It is right in the sizing pressure process as a kind of optimal technical scheme of decay Total Reflection Infrared test method
The upper surface of the liquor sample or the powdery samples and the distance of the sample load plane are controlled, and ensure the liquid
The thickness of body sample or the powdery samples.
Preferably, with providing a kind of decay Total Reflection Infrared test device, including test upper fixture and survey in this method
The lower fixture of examination, the test upper fixture are arranged to move towards or away from fixture direction under the test, are pressed from both sides under the test
Tool is arranged on sample load plane, and fixture has sample holding tank under the test, under the test upper fixture, the test
Fixture and the sample load plane alternative cooperatively form closed sample accommodating chamber.
Sample accommodating chamber is formed by testing the lower fixture of upper fixture and test, can ensure during test, be tested
The fluid sample or pulverized specimen of examination are maintained in sample accommodating chamber not to spread around, so that under the extruding of test upper fixture
Form the controllable detected sample of thickness so that light path is controllable when measuring.
As a kind of optimal technical scheme of decay Total Reflection Infrared test method, the liquor sample or powdery examination
The contact area of sample and the sample load plane is more than the area of the total reflection crystal on the sample load plane.
The contact area of liquor sample or powdery samples and the sample load plane is set to be more than the area of total reflection crystal,
Total reflection crystal can be made full use of, while avoids sample from being damaged by pressure crystal is totally reflected.
As a kind of optimal technical scheme of decay Total Reflection Infrared test method, following steps are specifically included：
Step S1, liquor sample or powdery samples are placed on the sample load plane with total reflection crystal；
Step S2, sizing pressurized operation is carried out to sample in the sample load plane；
Step S3, Infrared irradiation is carried out to sample in total reflection side of the crystal away from sample；
Step S4, reflection infrared light is received；
Step S5, infrared spectrogram is generated.
As a kind of optimal technical scheme of decay Total Reflection Infrared test method, the step S1 is by liquor sample or powder
Shape sample, which is placed on the sample load plane with total reflection crystal, to be included：
Fixture under test with cylindrical cavity mould is set step S11, on the sample load plane；
Step S12, the liquor sample or powdery samples are added in the cylindrical empty cavity mould.
As a kind of optimal technical scheme of decay Total Reflection Infrared test method, in step S2, carried in the sample
Plane carries out sample sizing pressurized operation：Using with the matched cylindrical tack pressure of the cylindrical cavity mould
Contact, presses the liquor sample or the powder sample in top, makes the liquor sample or the powdery samples and examination
Sample load plane is in close contact, while accurate Control Assay thickness.
As a kind of optimal technical scheme of decay Total Reflection Infrared test method, infrared spectrum bag is generated described in step S5
Include analog-to-digital conversion and digital-to-analogue conversion.
Beneficial effects of the present invention are：Added by carrying out sizing to liquor sample or powdery samples on sample load plane
Pressure, and decay Total Reflection Infrared test is carried out to it in the state of sizing is pressurizeed, sample form change is avoided to test result
Impact.
Brief description of the drawings
The present invention is described in further detail below according to drawings and examples.
Fig. 1 is Total Reflection Infrared test method flow chart of decaying described in embodiment.
Fig. 2 is Total Reflection Infrared test device sectional view of decaying described in embodiment.
Fig. 3 is cylindrical tack pressure structure of contact terminal schematic diagram described in embodiment.
Fig. 4 is cylindrical tack pressure contact top view described in embodiment.
Fig. 5 is the lower clamp structure schematic diagram of test described in embodiment.
Fig. 6 is the lower fixture schematic top plan view of test described in embodiment.
In figure：
100th, upper fixture is tested；101st, lower fixture is tested；102nd, cylindrical tack pressure contact；103rd, cylindrical empty cavity mold
Tool；104th, it is totally reflected crystal；105th, the first plane mirror；106th, the second plane mirror；107th, lower fixture fixing device.
Embodiment
Further illustrate technical scheme below with reference to the accompanying drawings and specific embodiments.
As shown in figs. 1 to 6, a kind of decay Total Reflection Infrared test method is introduced, this method is mainly used for measuring liquid examination
Sample or powdery samples, but it can equally be measured to having figurate sample.
In this present embodiment, sizing is carried out to the liquor sample or the powdery samples on sample load plane to add
Pressure, and decay Total Reflection Infrared test is carried out to it in the state of sizing is pressurizeed.
For liquor sample, sizing pressurization is carried out to it in sample load plane, can be avoided in pressure process
Liquid is spread around causes liquor sample highly uncontrollable, while reduces the contact area of volatile liquid and air, reduces
Evaporate.
For powdery samples, sizing pressurization is carried out to it in sample load plane, except can avoid directly pressurizeing to it
Make it be in close contact with sample load plane to cause to spread around outside, can also avoid using independent pressing device before testing
Shape to powdery samples, reduce operation quantity, while the pressure of bigger can be applied to it, ensure that it is carried with sample
Plane is in close contact.
In this present embodiment, it is described sizing pressurization be specially：The liquor sample or the powdery samples are limited along sample
Load plane is spread around, and the sample is pressed on the sample load plane, makes the liquor sample or institute
Powdery samples are stated to be in close contact with the sample load plane.In the sizing pressure process, to the liquor sample or institute
The upper surface and the distance of the sample load plane for stating powdery samples are controlled, and ensure the liquor sample or the powdery
The thickness of sample.
The contact area of the liquor sample or the powdery samples and the sample load plane, which is more than, is located at the examination
The area of total reflection crystal 104 on sample load plane.Make connecing for liquor sample or powdery samples and the sample load plane
Contacting surface product is more than the area of total reflection crystal 104, can make full use of total reflection crystal 104, while avoids sample from being totally reflected
Crystal 104 damages by pressure.
Decay Total Reflection Infrared test method described in the present embodiment, specifically includes following steps：
Step S1, sample loads, and liquor sample or powdery samples are placed on the sample with total reflection crystal 104 carries
In plane；
Step S1 is specifically included：
Step S11, test fixture is installed, and is set on the sample load plane with cylindrical empty cavity mould 103
The lower fixture 101 of test；
Step S12, sample is installed, and the liquor sample or powdery samples are added in the cylindrical empty cavity mould 103.
Step S2, sizing pressurization, sizing pressurized operation is carried out in the sample load plane to sample；
Step S2 is specifically included：Using with the matched cylindrical tack pressure contact of the cylindrical empty cavity mould 103
102, press in top to the liquor sample or the powder sample, make the liquor sample or the powdery samples and sample
Load plane is in close contact, while accurate Control Assay thickness
Step S3, Infrared irradiation, Infrared irradiation is carried out in total reflection side of the crystal 104 away from sample to sample；
Step S4, infrared light-receiving, receives reflection infrared light；
Step S5, infrared spectrogram is generated, infrared light is converted to by infrared light by analog-to-digital conversion and digital-to-analogue conversion
Spectrum.
A kind of decay Total Reflection Infrared test device is also provided in above-mentioned test method the present embodiment in order to realize, including is surveyed
Try upper fixture 100 and the lower fixture 101 of test, the test upper fixture 100 is arranged to can be towards or away from pressing from both sides under the test
Has the movement of 101 directions, fixture 101 is arranged on sample load plane under the test, and fixture 101 has sample under the test
Holding tank, fixture 101 and the alternative cooperation shape of the sample load plane under the test upper fixture 100, the test
Into closed sample accommodating chamber.
Sample accommodating chamber is formed by testing the lower fixture 101 of upper fixture 100 and test, can ensure the process in test
In, tested fluid sample or pulverized specimen are maintained in sample accommodating chamber and do not spread around, so that in test upper fixture
The controllable detected sample of thickness is formed under 100 extruding so that light path is controllable when measuring.
Specifically, the test upper fixture 100 includes cylindrical tack pressure contact 102, the survey in this present embodiment
The lower fixture 101 of examination includes and the cylindrical 102 matched cylindrical empty cavity mould 103 of tack pressure contact.
Test liquid sample or pulverized specimen are held by the cylindrical empty cavity mould 103, then pass through cylindrical tack
Pressure contact 102 presses the sample in cylindrical empty cavity mould 103, avoids fluid sample from flowing around, or quickly
The problems such as volatilization, ensure that thickness of liquid film is unified, convenient to carry out quantitative test.
Optically thinner medium is injected into so as to form total reflection, in the sample in order to realize infrared light by optically denser medium
Total reflection crystal 104 is provided with load plane, the diameter of the cylinder tack pressure contact 102 is more than the total reflection crystalline substance
The diameter of body 104.
Diameter is too small to cause sample cake less than normal, when sample is subject to the pressure of cylindrical tack pressure contact 102 all to act on
When crystal 104 is totally reflected, total reflection crystal 104 is easily damaged；And diameter crosses conference causes sample waste.
During test liquid sample or pulverized specimen, in order to ensure thickness of sample, it is necessary to the liquid or powder of excess
Body is discharged, and the diameter of cylindrical empty cavity mould 103 is set greater than to the diameter of cylindrical tack pressure contact 102, makes both
Between form gap, cylindrical tack pressure contact 102 to sample apply active force reach predetermined thickness when, it is unnecessary
Sample can be discharged from gap.Therefore in actual use, the diameter of cylindrical empty cavity mould 103 is more than the cylinder
0.02 ㎜ of diameter to 0.1 ㎜ of shape tack pressure contact 102.The diameter of cylindrical empty cavity mould described in the present embodiment 103 is big
In 0.05 ㎜ of diameter of the cylindrical tack pressure contact 102.
In order to effectively control the thickness of sample, avoid sample from cylindrical empty cavity mould 103 and sample load plane it
Between reveal, will be arranged in sealing contact between the cylindrical empty cavity mould 103 and the sample load plane.The cylinder
It is in sealing contact between cavity mould 103 and the sample load plane.
As a kind of optimal technical scheme of decay Total Reflection Infrared test device, below the sample load plane, and
The first plane mirror 105 and the second plane mirror are provided with positioned at 104 corresponding position of the total reflection crystal
106。
First plane mirror 105 is used to receive infrared light supply, and the incident ray that infrared light supply is sent reflexes to entirely
Reflection crystal 104.Second plane mirror 106 is used to receiving the infrared light that is reflected by total reflection crystal 104, and by infrared light
Reflex to infrared spectrum detector.It is fixed between first plane mirror 105 and the second plane mirror 106 in this present embodiment
Connection.And in other embodiments can also be by relative angle between the first plane mirror 105 and the second plane mirror 106
It is arranged to adjustable.By the way that the first plane mirror 105 and 106 angle of the second plane mirror are arranged to adjustable, in different works
Make to make full use of the length of installation space or width that decay Total Reflection Infrared test device to be installed under environment, reduce it
Requirement to use environment.
Preferably, first plane mirror 105 is arranged in a mutually vertical manner with second plane mirror 106.Pass through
First plane mirror 105 and the second plane mirror 106 are arranged in a mutually vertical manner, can ensure infrared ray and the injection of incidence
Infrared ray be parallel to each other, reduce to decay Total Reflection Infrared test device installation and debugging requirement.
The side of first plane mirror 105 is provided with infrared light supply, the side of second plane mirror 106
It is provided with infrared spectrum detector.
Fixture 101 has the lower fixture fixing device 107 of the alternative fixed sample accommodating chamber under the test.
Specifically, in this present embodiment the lower fixture fixing device 107 include the first movable clamping device and with institute
The second movable clamping device that the first movable clamping device is oppositely arranged is stated, the first movable clamping device is lived with described second
Dynamic clamping device can be movable relatively or mutually away from movement.
On-fixed connects between sample accommodating cavity and sample load plane, therefore needs to position it in use
And clamp, set lower fixture fixing device 107 easily to realize clamping, may be used also with 107 position of fixture fixing device at present
Different sizes, the sample accommodating cavity of structure to be fixed, the versatility of increase decay Total Reflection Infrared test device.
The test upper fixture 100 further includes upper fixture driving device, and the upper fixture driving device passes through elastic connection
Part is connected with the cylindrical tack pressure contact 102.By the way that upper fixture driving device is passed through flexible connector and the circle
Cylindricality tack pressure contact 102 connects, and enables to the flexible connector in the case where pressure reaches certain value to be compressed, so that
Sample is no longer subjected to excessive extruding, avoids sample load plane from bearing excessive pressure and damage.
In description herein, it is to be understood that the orientation such as term " on ", " under " or position relationship is based on attached drawing institutes
The orientation or position relationship shown, is for only for ease of description and simplifies operation, rather than instruction or the device or member that imply meaning
Part must have specific orientation, with specific azimuth configuration and operation, therefore be not considered as limiting the invention.This
Outside, term " first ", " second ", are used only for being distinguish between in description, not special implication.
It is to be understood that above-mentioned embodiment is only that presently preferred embodiments of the present invention and institute's application technology are former
Reason, in technical scope disclosed in this invention, change that any one skilled in the art is readily apparent that or
Replace, should all cover within the scope of the present invention.
Claims (8)
1. one kind decay Total Reflection Infrared test method, for measuring liquor sample or powdery samples, it is characterised in that in sample
Carry out sizing pressurization on load plane to the liquor sample or the powdery samples, and in the state of sizing is pressurizeed to its into
Row decay Total Reflection Infrared test, the sizing are forced through decay Total Reflection Infrared test device and carry out, and the decay is all-trans
Penetrating infrared test device includes test upper fixture and the lower fixture of test, and the test upper fixture is arranged to can be towards or away from institute
The lower fixture direction movement of test is stated, fixture is arranged on the sample load plane under the test, and fixture has under the test
There is sample holding tank, fixture and the alternative cooperation shape of the sample load plane under the test upper fixture, the test
Into closed sample accommodating chamber, the test upper fixture includes cylindrical tack pressure contact, under the test fixture include with
The cylinder tack pressure contact matched cylindrical empty cavity mould, it is brilliant to be provided with total reflection in the sample load plane
Body, the diameter of the cylinder tack pressure contact are more than the diameter of the total reflection crystal.
2. decay Total Reflection Infrared test method according to claim 1, it is characterised in that the sizing pressurization includes：
Limit the liquor sample or the powdery samples are spread around along sample load plane, and the sample is pressed on institute
State on sample load plane, the liquor sample or the powdery samples is in close contact with the sample load plane.
3. decay Total Reflection Infrared test method according to claim 2, it is characterised in that in the sizing pressure process
In, the upper surface and the distance of the sample load plane of the liquor sample or the powdery samples are controlled, ensured
The thickness of the liquor sample or the powdery samples.
4. decay Total Reflection Infrared test method according to claim 3, it is characterised in that the liquor sample is described
The contact area of powdery samples and the sample load plane is more than the total reflection crystal on the sample load plane
Area.
5. decay Total Reflection Infrared test method according to claim 4, it is characterised in that specifically include following steps：
Step S1, liquor sample or powdery samples are placed on the sample load plane with total reflection crystal；
Step S2, sizing pressurized operation is carried out to sample in the sample load plane；
Step S3, Infrared irradiation is carried out to sample in total reflection side of the crystal away from sample；
Step S4, reflection infrared light is received；
Step S5, infrared spectrogram is generated.
6. decay Total Reflection Infrared test method according to claim 5, it is characterised in that the step S1 tries liquid
Sample or powdery samples, which are placed on the sample load plane with total reflection crystal, to be included：
Fixture under test with cylindrical cavity mould is set step S11, on the sample load plane；
Step S12, the liquor sample or powdery samples are added in the cylindrical empty cavity mould.
7. decay Total Reflection Infrared test method according to claim 5, it is characterised in that in step S2, in the examination
Sample load plane carries out sample sizing pressurized operation：Using flat with the matched cylinder of the cylindrical cavity mould
Head pressure contact, presses the liquor sample or the powder sample in top, tries the liquor sample or the powdery
Sample is in close contact with sample load plane, while accurate Control Assay thickness.
8. decay Total Reflection Infrared test method according to claim 5, it is characterised in that generation is infrared described in step S5
Spectrum includes analog-to-digital conversion and digital-to-analogue conversion.
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| CN106596454B (en) * | 2016-12-19 | 2019-04-02 | 扬州大学 | A kind of starch Fourier transform decaying In situ ATR-FTIR sample preparation apparatus and application method |
| KR102109834B1 (en) * | 2017-12-26 | 2020-05-12 | 주식회사 엘지화학 | Method for infrared spectroscopy analysis of polyacrylonitrile based fiber |
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