CN101097182B - Dynamic rotating sample pool and infrared spectrum analysis general purpose accessory - Google Patents

Dynamic rotating sample pool and infrared spectrum analysis general purpose accessory Download PDF

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Publication number
CN101097182B
CN101097182B CN 200610090580 CN200610090580A CN101097182B CN 101097182 B CN101097182 B CN 101097182B CN 200610090580 CN200610090580 CN 200610090580 CN 200610090580 A CN200610090580 A CN 200610090580A CN 101097182 B CN101097182 B CN 101097182B
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sample cell
sample
turning axle
box body
framework
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CN101097182A (en
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孙岩峰
陆婉珍
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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Abstract

A kind of dynamic rotating sample pool includes rotating shaft (2)which passes through the sample pool, direction of said rotating shaft (2)is level, and the sample pool includes sample pool frame (3)and sample pool window (4)which is at two sides of the sample pool frame (3). The dynamic rotating sample pool fits for detecting near infrared spectrum of solid sample; the sample pool rotates vertically, the stack state of the sample changes continuously during course of detecting spectrum, repetition of spectrum is well, the precision of near infrared spectrum testing can be increased effectively.

Description

A kind of dynamic rotating sample pool and infrared spectrum analysis general purpose accessory
Technical field
The present invention relates to a kind of rotating sample pool and infrared spectrum analysis general purpose accessory, in particular, is a kind of dynamic rotating sample pool and general-purpose accessory that near-infrared diffuse reflectance and diffuse transmission mode are gathered solid sample spectrum that be used for.
Background technology
Near-infrared spectrum technique as a kind of fast, Dynamic Non-Destruction Measurement obtains attention more and more widely at agricultural, medicine, food, clinical medicine, environment, chemical field.In recent years, computing machine and multivariate statistical analysis The Application of Technology, and the release of the modern near infrared spectrometer of high s/n ratio make near infrared spectroscopy obtain more deep research and application in the solid sample non-destructive analysis.
The influence that existing mensuration solid particle sample, the particularly near-infrared spectrum method of bulky grain sample are subjected to sample form, bulk density is very big.The stacking states of sample in analytic process do not change, adorn sample again after, therefore the spectrum poor repeatability adopts traditional diffuse reflection and transmission method to be difficult to obtain ideal results.
CN2285895Y discloses a kind of near infrared petroleum composition analyser.This instrument adopts the fixed light path structure, and linear charge-coupled array CCD is as photoelectric signal converter.Sample cell is fixed between light source and the detecting device, by the near infrared spectrum of transmission mode collected specimens.The sample cell of this instrument is suitable for measuring fluid sample, if be used to test the solid particle sample, then Gu Ding sample cell only can obtain the spectrum of a position of sample.Because the particle diameter of solid particle sample is bigger, skewness, the SPECTRAL DIVERSITY that different stowed locations records is bigger, therefore, when using this instrument test solid sample, can not be reflected the spectrum solid particle sample, good reproducibility comprehensively.
CN2697642Y discloses the special-purpose testing table of a kind of near infrared spectrometer, is provided with the horizontal rotating table of a carry sample groove.In measuring process, adopted the dynamic acquisition signal, sample cell is done at 0.3~0.5 millimeter place of measurement mouth of distance near infrared spectrometer and is horizontally rotated, so just enlarged the signals collecting area of near infrared spectrometer, increase the quantity of information of sample collecting, reduced the personal error that dress sample process brings and the systematic error of the inhomogeneous generation of sample itself.
CN2615660Y discloses a kind of near infrared grain quality analyser diffuse transmission determinator.This device receives optical fiber, coaxial sampling thief and circular transparent rotary container by light source input optical fibre, signal and forms, circular transparent rotary container receives between the signal receiving plane of optical fiber with signal at the light source input face that is the light source input optical fibre that subtend is provided with, and characteristics are fan-shaped diaphragm to be set in the transparent rotary container of circle and to be located at that the circular fixed attenuation corresponding to the light source input face compares light damping plate on the fan-shaped diaphragm.The bottom surface and the end face of the transparent rotary container of described circle are respectively Transparent frame, place tested cereal in Transparent frame.The transparent rotary container of described circle horizontally rotates when test, passes the near infrared diffuse transmission spectrum of transparent rotary container by the transmission mode collection.
The above-mentioned instrument that horizontally rotates sample cell that is provided with can not change the stacking states of sample in gatherer process, and the sample spectra that obtains in the mensuration process still can be subjected to the influence of sample stacking states and can't obtain desirable analysis result.
Summary of the invention
The purpose of this invention is to provide a kind of dynamic rotating sample pool, this sample cell is used for the Infrared spectroscopy of solid sample, has spectrum repeatability preferably.
Another object of the present invention provides a kind of infrared spectrum Gneral analysis annex that comprises described dynamic rotating sample pool, and this annex is easy to carry and operates.
Dynamic rotating sample pool provided by the invention comprises turning axle, sample cell framework that passes the sample cell center and the sample cell window that places sample cell framework both sides, and the axial of described turning axle is level.
Infrared spectrum analysis general purpose accessory provided by the invention, comprise dynamic rotating sample pool and place its outer annex box body, be respectively equipped with on the wall of the described box body left and right sides and detect light entrance and detect light exit, be respectively equipped with charging aperture and discharging opening on the wall at two ends about the box body, described dynamic rotating sample pool comprises turning axle, sample cell framework that passes the sample cell center and the sample cell window that places sample cell framework both sides, the axial of described turning axle is level, and link to each other with drive motor in placing the annex box body, the sample cell framework is provided with injection port.
Dynamic rotating sample pool of the present invention, turning axle is passed the sample cell center, and make it axially be horizontal direction, sample cell changes at the sagging direct rotary of the drive of turning axle during use, the illumination that light source sends is mapped to the solid sample that continuously changes stacking states in the sample cell, make the spectrum of collection can fully reflect the feature of solid particle sample, effectively improve the spectrum repeatability of measuring solid sample, reduce to adorn in the sample process because of the solid particle sample is in the influence that different stacking states brings spectrum repeatability at every turn, and then improve the accuracy of measuring.Infrared spectrum analysis general purpose accessory provided by the invention described dynamic rotating sample pool is easy to carry and with the supporting use of near-infrared analyzer, mix the operation of being more convenient for behind the turnover sample funnel.
Description of drawings
Fig. 1 is the structural representation of a kind of dynamic rotating sample pool provided by the invention.
Fig. 2 is the sectional view of D-D face among Fig. 1.
Fig. 3 is the structural representation of another kind of dynamic rotating sample pool provided by the invention.
Fig. 4 is the sectional view of E-E face among Fig. 2.
Fig. 5 is the structural representation of infrared spectrum Gneral analysis annex provided by the invention.
Fig. 6 gathers the principle of work synoptic diagram of spectrum for using dynamic rotating sample pool provided by the present invention by the diffuse transmission mode.
Fig. 7 is the near infrared diffuse transmission spectrum of the polypropylene granules sample of use dynamic rotating sample pool collection provided by the present invention.
Fig. 8 is the near-infrared diffuse reflection spectrum of the polypropylene powder sample of use dynamic rotating sample pool collection provided by the present invention.
Embodiment
Dynamic rotating sample pool provided by the invention passes the center of sample cell with turning axle, and turning axle is a level axially, drives sample cell during rotation and vertically rotates.When carrying out near-infrared analysis, the solid sample that is placed in the sample cell moves up from the sample cell bottom with the sample cell rotation, behind the arrival certain altitude, slides into the sample cell bottom under action of gravity, again after piling up, lower floor's sample no longer slides under the restriction of upper strata sample.In the spectroscopic assay process, solid sample is constantly piled up again.Solid sample in the light transmission sample cell that light source sends is at sample surfaces and inner can reflect, refraction, diffraction and transmission, make gained spectrum can reflect the feature of sample under different stacking states, improve the repeatability of spectrum greatly.
For ease of the dissimilar sample of filling in sample cell, sample cell of the present invention has two kinds of different structures.A kind of is the both sides formation sample cell that two sample cell windows is fixed in the sample cell framework, is provided with injection port on the sample cell framework.Another kind is at the fixing a slice sample cell window of a side of sample cell framework, another sheet is movable sample cell window, be fixed on the sample cell framework during use again, preferable methods is to be provided with screw thread on the turning axle of sample cell framework opposite side, during use movable sample cell window is fixed on the sample cell framework by nut and forms sample cell.
Described turning axle is preferably multidiameter shaft, and it is big that its diameter that is positioned at sample cell is positioned at the outer diameter of sample cell.
Described sample cell framework preferably drum shape, the sample cell window preferably is annular.The sample cell window places the both sides of sample cell framework to form the cylindrical vessel of sealing.
The material of described sample cell window is any glass that sees through near infrared light.
Preferred sliding bearing of described turning axle or rolling bearing.Turning axle can manually be grasped and do, and preferably links to each other with drive motor and by its driving, to carry out uniform rotation.Preferred stepper motor of described drive motor or direct current generator.Described drive motor can directly link to each other with turning axle and drive the sample cell rotation, also can adopt gear, tooth bar or belt etc. to link to each other with turning axle, drives sample cell indirectly and rotates.
Infrared spectrum analysis general purpose accessory of the present invention is that dynamic rotating sample pool of the present invention is placed in the box body, sets up separately on the wall of box body both sides and detects light entrance and detect light exit, and the detection optical channel promptly is set.Described annex box body upper and lower side sets up charging aperture and discharging opening separately, is beneficial to sample and passes in and out from sample cell.
The charging aperture place of described box body upper end preferably is provided with loading hopper, and the discharging opening place of box body lower end preferably sets out funnel.
Preferably be provided with integrating sphere in the described box body, the incident light passage of described integrating sphere links to each other with detection light entrance on the box body, and the integrating sphere sidewall is provided with the photoelectric detector interface.
Describe the present invention in detail below in conjunction with accompanying drawing, but the present invention is not limited to this.
Fig. 1 is a kind of dynamic rotating sample pool structural representation of the present invention.As shown in Figure 1, this dynamic rotating sample pool is made up of the turning axle 2 and the sample cell that pass the sample cell center, and described sample cell is made up of sample cell framework 3 and sample cell window 4, and the upper end of sample cell framework 3 is provided with injection port 1, and sample cell window 4 is annular.By the sectional view in D-D cross section among Fig. 1 shown in Figure 2 as can be known, described sample cell window 4 is fixed on the both sides of sample cell framework 3, turning axle 2 passes sample cell center and horizontal positioned, and it axially is a level, and turning axle 2 is positioned at the diameter of sample cell greater than being positioned at the outer diameter of sample cell.
By another kind of dynamic rotating sample pool of the present invention shown in Figure 3 as can be known, this dynamic rotating sample pool is made up of the turning axle 2 and the sample cell that pass the sample cell center, and described sample cell is made up of sample cell framework 3 and sample cell window 4.By the sectional view in E-E cross section among Fig. 3 shown in Figure 4 as can be known, a slice of described sample cell window 4 is fixed on a side of sample cell framework 3, and turning axle 2 horizontal positioned are also passed the sample cell center, and it axially is a level.The diameter that turning axle 2 is positioned at sample cell is greater than being positioned at the outer diameter of sample cell, and the turning axle 2 that is positioned at the outer end of sample cell is provided with screw thread 5.Another sheet sample cell window then is fixed on the opposite side of sample cell framework 3 with nut 16 by screw thread.
As shown in Figure 5, infrared spectrum analysis general purpose accessory provided by the invention comprises box body 10 and places its interior dynamic rotating sample pool.The left and right sides of described box body 10 is respectively equipped with to be detected light entrance 6 and detects light exit 7, and the two ends up and down of box body 10 are respectively equipped with charging aperture 8 and discharging opening 9.Described dynamic rotating sample pool is made up of the turning axle 2 and the sample cell that pass the sample cell center, and sample cell is made up of sample cell framework 3 and the sample cell window 4 that is fixed on its both sides, and the upper end of sample cell framework 3 is provided with injection port 1.An end that places the interior turning axle 2 of box body to stretch out sample cell links to each other with drive motor 15.Integrating sphere 13 is positioned at turning axle 2 belows, the incident light passage of integrating sphere one side links to each other with detection light entrance 6 on the box body, the opposite side of integrating sphere 13 places the window place of sample cell towards integrating sphere one side, and the photoelectric detector interface 14 of integrating sphere is positioned on the sidewall of integrating sphere.Charging aperture 8 places of described box body 10 upper ends are provided with loading hopper 12, and discharging opening 8 places of box body 10 lower ends are provided with out funnel 11.
Dynamic rotating sample pool provided by the invention and general-purpose accessory have the acquisition method of two kinds of sample spectra in use, and a kind of is the diffuse transmission spectrum of gathering sample, and another kind is a diffuse reflection spectrum of gathering sample.
The method of gathering the diffuse transmission spectrum of sample is: with the tested solid sample sample cell of packing into, the charge weight of sample is 30~70% of a sample cell volume, preferred 45~55%.Rotate sample cell behind the dress sample.Along with the rotation of sample cell, sample constantly changes stacking states in the latter half of sample cell.Light source is placed the side of sample cell the latter half, detect optical receiver and place the opposite side relative with light source.Sample in the rayed sample cell that light source sends, the detection optical receiver promptly receives the diffuse transmission light through sample, and by minute optical detecting unit the diffuse transmission light that receives is carried out converting electric signal to after the beam split and output to data processing unit, data processing unit carries out the diffuse transmission spectrum that data processing promptly obtains sample to the electric signal that receives.
The method of gathering the diffuse reflection spectrum of sample is: with the tested solid sample sample cell of packing into, sample cell sample-loading amount and rotating manner are identical with first method.Light source is placed the side of sample cell the latter half, detect the homonymy that optical receiver places light source.Sample in the rayed sample cell that light source sends, diffusing enters detecting device and converts electric signal to and output to data processing unit, promptly obtains the diffuse reflection spectrum of sample through data processing.
Described light source can be pointolite, also can be area source.Owing to need more powerful light source during the solid particle test analysis, preferred area source, more preferably with the halogen tungsten lamp of reflector as light source.
The using method of dynamic rotating sample pool shown in Figure 1 provided by the invention is: tested solid sample by injection port 1 sample cell of packing into, is sealed injection port 1 then.When unloading sample, again injection port 1 is opened, poured out sample.The using method of the dynamic rotating sample pool of structure shown in Figure 3 provided by the invention is: tested solid sample is put into sample cell, again the sample cell window of activity is placed a side of sample cell framework 3, be fixed on sample cell framework 3 and the turning axle 2 with nut 16, form closed system.When unloading sample, open movable sample cell window, sample is taken out.
The place that Fig. 1 or dynamic rotating sample pool shown in Figure 3 below is held sample places infrared spectrometer light source irradiation place, opening drive motor rotates turning axle 2 average rates that are attached thereto, sample rotates constantly with sample cell and piles up in the dynamic rotating sample pool, the diffuse transmission light that test sample is sent or the signal that diffuses can obtain the diffuse transmission spectrum or the diffuse reflection spectrum of sample through data processing.
The using method of infrared spectrum analysis general purpose accessory shown in Figure 5 provided by the invention is: with the tested solid sample loading hopper 12 of packing into, the injection port 1 of adjusting dynamic rotating sample pool is positioned at the below of loading hopper 12, open injection port 1, sample is then entered in the sample cell by injection port 1.Close injection port 1 behind the sample introduction, start drive motor, turning axle 2 is rotated in the vertical plane direction, sample is promptly constantly piled up with the rotation of sample cell.The light that light source sends then enters in the box body 10 of annex by detecting light entrance 6, sample in the irradiation sample cell, the diffuse transmission light of sample is derived by detecting light exit 7, import the branch optical detecting unit into and convert electric signal to and output to data processing unit, after data processing, obtain the diffuse transmission spectrum of sample.Test finishes, and control injection port 1 is in the top of funnel 11, opens injection port 1, and sample is promptly discharged along going out funnel 9.The integrating sphere 13 that is provided with in the described general-purpose accessory is more suitable for measuring the diffuse reflection spectrum of sample.
Dynamic rotating sample pool provided by the invention and general-purpose accessory are applicable to the analysis of near infrared spectrum of composition, molecular structure and other relevant information of solid sample, be particularly useful for the analysis of the near infrared spectrum of high molecular polymer, as measure polyolefinic melt flow rate, tensile yield strength, isotacticity etc.
Following example further specifies the application of the present invention in the near infrared ray of solid sample.
Example 1
Adopt dynamic rotating sample pool of the present invention shown in Figure 1, by the injection port 1 of sample cell polypropylene granules sample 50 gram of in sample cell, packing into.The light path that dynamic rotating sample pool is placed infrared spectrometer as shown in Figure 6.Among Fig. 6, the bottom of dynamic rotating sample pool places between light source 17 and the lens combination 18, and lens combination 18 is linked to each other by optical fiber 19 with lens combination 21.Divide optical detecting unit to form by grating 23, catoptron 24 and photodiode alignment detecting device 25.
With rated power be 50 watts, the band reflector halogen tungsten lamp be near-infrared light source 17, polypropylene granules in the irradiation sample cell, the diffuse transmission light that penetrates sample is collected by lens combination 18, offer grating 23 through optical fiber 19, lens combination 21 and slit 22, enter photodiode alignment detecting device 25 by the monochromatic light behind the grating beam splitting through catoptron 24 and convert electric signal to and output to computing machine 26 and carry out data processing, the diffuse transmission spectrum of the polypropylene granules sample that obtains as shown in Figure 7.
120 millimeters of described sample cell framework diameters, 25 millimeters of window thickness, turning axle 2 adopts rolling bearing.30 millimeters of convex lens group 18 diameters.Optical fiber 19 is SMA905 standard interface optical fiber.Grating is the transmission hologram grating; Slit width is 50 microns.Photodiode alignment detecting device 25 is an InGaAs photodiode alignment, and the pixel number is 512, wavelength coverage 900~1700 nanometers.Spectroscopic data is according to pixel sequential scheduling interval value.
Example 2
Adopt dynamic rotating sample pool shown in Figure 3,10 millimeters of its sample cell window thickness, 120 millimeters of sample cell framework diameters, turning axle adopts rolling bearing.Earlier 20 gram polypropylene powder samples are packed in the sample cell, again another sheet sample cell window is passed turning axle 2, cover back nut 16 fixing seals on sample cell framework 3.
With rated power is that 20 watts halogen tungsten lamp is a near infrared light light source irradiation polypropylene powder sample, reflected light is collected the back with lens combination and is introduced photodiode alignment detecting device by optical fiber by light path shown in Figure 6, light signal is converted to the laggard line data of electric signal handles.Used spectral detection parts are all with example 1, and the diffuse reflection spectrum of the polypropylene granules sample that obtains as shown in Figure 8.

Claims (9)

1. dynamic rotating sample pool of measuring solid particle, comprise turning axle (2), sample cell framework (3) that passes the sample cell center and the sample cell window (4) that places sample cell framework (3) both sides, the axial of described turning axle (2) is level, described sample cell framework (3) is a cylindrical shape, sample cell window (4) is annular, sample cell window (4) places the both sides of sample cell framework (3) to form the cylindrical vessel of sealing, and sample cell framework (3) is provided with injection port (1).
2. according to the described sample cell of claim 1, it is characterized in that the described outer turning axle (2) of sample cell that is positioned at is provided with screw thread (5).
3. according to the described sample cell of claim 1, it is characterized in that described turning axle (2) is a multidiameter shaft, it is big that its diameter that is positioned at sample cell is positioned at the outer diameter of sample cell.
4. according to the described sample cell of claim 1, it is characterized in that described turning axle (2) is sliding bearing or rolling bearing.
5. according to the described sample cell of claim 1, it is characterized in that described turning axle (2) links to each other with drive motor and by its driving.
6. according to the described sample cell of claim 5, it is characterized in that described drive motor is stepper motor or direct current generator.
7. infrared spectrum analysis general purpose accessory, comprise dynamic rotating sample pool and place its outer box body (10), be respectively equipped with on the wall of described box body (10) left and right sides and detect light entrance (6) and detect light exit (7), be respectively equipped with charging aperture (8) and discharging opening (9) on the wall at two ends about the box body, described dynamic rotating sample pool comprises the turning axle (2) that passes the sample cell center, sample cell framework (3) and place the sample cell window (4) of sample cell framework (3) both sides, the axial of described turning axle (2) is level, and link to each other with drive motor (15) in placing the annex box body, described sample cell framework (3) is a cylindrical shape, sample cell window (4) is annular, sample cell window (4) places the both sides of sample cell framework (3) to form the cylindrical vessel of sealing, and sample cell framework (3) is provided with injection port (1).
8. according to the described annex of claim 7, it is characterized in that the charging aperture (8) of described box body upper end locates to be provided with loading hopper (12), the discharging opening of box body lower end (12) locates to be provided with out funnel (11).
9. according to the described annex of claim 7, it is characterized in that also being provided with in the described box body integrating sphere (13), the incident light passage of described integrating sphere links to each other with detection light entrance (6) on the box body (10), and the integrating sphere sidewall is provided with photoelectric detector interface (14).
CN 200610090580 2006-06-29 2006-06-29 Dynamic rotating sample pool and infrared spectrum analysis general purpose accessory Active CN101097182B (en)

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CN103808660B (en) * 2014-03-12 2017-02-15 大连民族学院 Gas cell for ultraviolet-visible spectrum analysis
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