CN87103339A - The online spectrophotometric chemical analysis method and the device of material in process of flowing stream - Google Patents
The online spectrophotometric chemical analysis method and the device of material in process of flowing stream Download PDFInfo
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- CN87103339A CN87103339A CN 87103339 CN87103339A CN87103339A CN 87103339 A CN87103339 A CN 87103339A CN 87103339 CN87103339 CN 87103339 CN 87103339 A CN87103339 A CN 87103339A CN 87103339 A CN87103339 A CN 87103339A
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- 238000002329 infrared spectrum Methods 0.000 description 6
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- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
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- 239000010951 brass Substances 0.000 description 1
- HGAZMNJKRQFZKS-UHFFFAOYSA-N chloroethene;ethenyl acetate Chemical compound ClC=C.CC(=O)OC=C HGAZMNJKRQFZKS-UHFFFAOYSA-N 0.000 description 1
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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
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3577—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
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- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
Spectrophotometer (10) utilizes sample box (14) to carry out containing for example ir spectrophotometry analysis of the process of flowing stream (11) of polymkeric substance melt.Analyzed material in sight chamber (42) two intervals very close to crystal (40) between flow through.Infrared radiation is from the emission of a side of this material, penetrates out from its opposite side.Crystal (40) is contained in and is positioned within the threaded window frame (38) and (39) in the hole.Threaded window frame (38) and (39) can be by moving the distance change between them, thereby change the absorptivity of this material.
Description
The present invention relates to be included in the spectrophotometric chemical analysis method and the device of the material in the mobile steady-state process stream.The invention that the application introduces is intended to special-purpose production or the on line operation of other processing occasion, at this moment, the economic quality management in order to realize effectively, it is very crucial that the chemical analysis of material in the process of flowing stream is analyzed rapidly.The application's invention disclosed scope of application is very wide.For the ease of introducing and explanation, this spectrophotometer utilizes the infrared radiation form to produce infrared spectrum and analyzes.
Although the present invention can carry out chemical analysis to various types of materials,, for convenience of explanation, with only relating to the chemical analysis that is comprised in the polymkeric substance melt that flows in the process stream, such as the material in picture polymkeric substance or the synthon production process stream.
Utilizing wavelength is that 2.5 to 50 microns or wave number (Wave numbers) are that 4800 to 200 infrared frequency scope is carried out infrared spectrum measurement and phase of history arranged.Utilizing infrared radiation why to be popularized as analysis means, be because infrared spectrum can provide considerable information, and infrared spectrum production method and analytical approach is also many.Infrared radiation is used most widely for differentiating all organic compounds and many mineral compounds, so this method is so useful, is because no matter sample is solid-state, fused solution or gaseous state, and no matter material is pure or impure, all can analyze.Take different analytical approachs, qualitative or quantitative results can both obtain.The analysis of infrared radiation output data is quite fast, the theoretical analysis when therefore being suitable on line operation at least.But the practical problems relevant with testing of materials is very difficult under online situation.So most of infrared analysiss always, also will remain under laboratory condition and carry out.Under above-mentioned polymer production and processing situation, the typical method that the polymkeric substance melt is carried out qualitative analysis is to take a sample from powdery or granular finished product, sample is delivered to the laboratory again and is carried out infrared analysis.This program is not suitable for the characteristics of production processes of polyalcohol especially.Polypropylene, tygon, polymkeric substance such as nylon are at nearly 527 (300 ℃) and 2500 pounds/inch
2(1757750 kilograms/meter
2) generate by various organic compound reactions under the high-temperature and high-pressure conditions of magnitude.It is very important keeping this temperature and pressure in whole process stream, this be because polymkeric substance when cooling very rapid hardening be very firm material.Owing to this reason, polymer production equipment all is a Zhou Qitian, one day twenty four hours some months that ceaselessly turns round continuously usually.Therefore, general medium-sized polymer production factory output is all quite high.Because the purposes of polymkeric substance varies, this produces according to the prescription of various variations with regard to requiring factory.Typical polymkeric substance generally contains several main compositions and multiple less important, the adjuvant of minute quantity normally, but these adjuvants are for but important influence of the character of product.For example, add adjuvant in the compound of polyester and nylon polymer, can reduce by these polymkeric substance is the raw material gauze produced
Wipe coefficient, thereby make guiding mechanism that those and the gauze that moves rapidly be in contact with one another, ring wheel etc. be not easy rapidly
Decrease.Other adjuvant in the polymkeric substance and form end group and be used to control polymkeric substance to the speed of the absorption of dyestuff and coloring reaction and degree etc.Also have some adjuvants can intensity, extensibility, washing shrinkage and many other performances of polymkeric substance be exerted an influence.The infrared analysis of polymkeric substance normally becomes polymer powder or particle and carries out after film or the melt.If analyze, need film or melt cooling are analyzed under its cold state in the laboratory.The polymkeric substance at room temperature the possibility of result that provides of infrared analysis and same material is analyzed the result who provides sizable difference is arranged under process stream temperature.This has just limited the validity of resulting information.Even the polymkeric substance melt reheated analyzes, its result still can not fully accurately reflection process stream in the actual composition of polymkeric substance melt.Because the polymkeric substance melt is whenever heating, cooling, when heating again, because the hot correlated response of polymkeric substance composition and because the volatilization loss that heating causes, its chemical analysis more or less changes.Move back it, even if lab analysis can access quite accurate result, because sampling, finish lab analysis and modification prescription etc. and need occupy a very long time, the number of polymers that might cause producing during it can not be qualified, need do over again, or become waste product, or become substandard products.
Therefore, urgent hope can be carried out online direct sample and infrared radiation analysis to the materials such as polymkeric substance in the process stream.The online infrared analysis of some material widely known to.According to circulation internal reflection (circular internal reflection) principle water is carried out infrared analysis, the content of definite wherein sugar and/or carbon dioxide is exactly an example.In a saturating ultrared cylindrical crystal material Feng Jinyi container, sample flow is by beverage production line this container of flowing through.Infrared radiation is focused on an end of cylinder crystal, reflex to the other end by crystals again, when infrared radiation brought out thus, because the selection filtering of infrared spectrum, radial fission became three sections.One is by the absorption band of sugar, and another is by the absorption band of carbon dioxide, and the 3rd is reference wavelength.In this operational version, the cylinder crystal is taken as detector, the flow through liquid of detector outside surface of radiation samples.
There is certain application in this system when analyzing such as more runny non-viscous liquid such as water and beverage, but utilizes the detector can not be to carrying out infrared analysis as the less opaque viscous mass of this analogy of polymkeric substance melt.Its reason is many-sided.At first, crystal is difficult to be heated to equably the temperature of process stream.Under quite high temperature scenario (at this moment, the temperature of polymkeric substance melt must be kept with process stream temperature and equate), even the polymerization logistics with such as detector like this moment between the colder comparatively speaking object contact, all can on detector, be stained with the quite thick polymer film of one deck.After this, infrared radiation is only sampled and is bonded at thickness on the detector is 4 to 8 microns constant material, but not the material in the process of flowing stream.
Polymkeric substance melt in the process of flowing stream is carried out online chemico-analytic sample box succeed in developing, make sampling be achieved, and can go out the variation of properties of samples, so just can before producing a large amount of waste products or substandard products, be corrected with quickish speed detection.And this sample box can continuous sampling polymkeric substance melt.Utilize this continuous process can set up the limiting alarm system, in case the standard of the chemical analysis overshoot of polymkeric substance melt, will automatically remind producers, underproof polymkeric substance melt migrated out again from process stream process, perhaps adopt suitable servo control mechanism, and then controlled in " upstream " of process stream, make chemical analysis results satisfy specified standard again.
The present invention in fact is resolved this problem by following method: flow " thin slice " that will contain such as the polymkeric substance melt strictly maintains under the temperature and pressure condition of process stream, makes infrared radiation pass through to its opposite side from a side of thin slice again.
Therefore, one of purpose of the present invention is carried out chemico-analytic sample box with regard to providing a kind of spectrophotometer that utilizes to the material in the process of flowing stream.
Another object of the present invention just provides a kind of sample box, utilizes it can make a side of the material of radiation from process of flowing stream pass through to opposite side, so that it is carried out chemical analysis and it is not made a difference.
The 3rd purpose of the present invention just provides a kind of sample box, and it can make material keep same temperature and pressure with process stream during the Emanations Analysis process.
The 4th purpose of the present invention just provides a kind of sample box, and it can perhaps abandon material after analyzing, and perhaps material refilled among the process of flowing stream.
The 5th purpose of the present invention just provides a kind of sample box, and it can carry out the infrared radiation chemical analysis by the flow process stream to the polymkeric substance melt under the temperature and pressure condition of process stream.
The 6th purpose of the present invention utilizes full scan (2.5 microns to 50 microns) spectrophotometer that the material in the process of flowing stream is carried out chemico-analytic method with regard to providing, to realize all above-mentioned purposes.
Enumerated some purpose of the present invention above.Other purpose of the present invention and advantage will embody when in conjunction with the following drawings the result who invents being described.In the accompanying drawing,
Fig. 1 is the sketch of spectrophotometric spectra meter, and it comprises getting in touch of the invention that will apply for and it and process stream;
Fig. 2 is the spectrometer shown in Figure 1 and the skeleton view of sample box;
Fig. 3 is the skeleton view of heat insulating reflecting plate washer, and this plate washer is used to prevent be heated owing to the sample box heat release makes spectrometer;
Fig. 4 be the Fourier Transform Infrared spectrometer of band michelson interferometer with according to the sample box of the present invention sketch of coupling mutually;
Fig. 5 is the decomposition diagram of the sample box of the embodiment of the invention;
Fig. 6 is the skeleton view of a kind of embodiment of window-frame of the present invention;
Fig. 7 is the skeleton view that window-frame shown in Figure 6 is looked from opposite end;
Fig. 8 is the sectional view of Fig. 7 and window-frame shown in Figure 6;
Fig. 9 is the valve mechanism of sample box and the vertical cross-section diagram of sight chamber, has for the sake of clarity omitted some parts;
Figure 10 is the horizontal sectional view of the sample box of expression valve mechanism of the present invention shown in Figure 9 and sight chamber, has for the sake of clarity omitted some parts.
Most preferred embodiment
Now, specifically with reference to each accompanying drawing, spectrophotometric spectra meter of the present invention obviously illustrates, and represents with numeral 10 at this.The material that device 10 samplings are flowed in process stream 11.For the ease of the present invention is introduced, regard the material in the process stream as the polymkeric substance melt, it is flowed out by the retort 12 that is known as source of polymer, and polymkeric substance produces in retort.Certainly, in other occasion, the source of process stream upstream can be a heating tank, the sheet that it will make elsewhere, and graininess or pulverous polymkeric substance reheat to molten state, so that further processing.By the polymkeric substance melt that 11 shuntings of process stream are come out, the supply line 13 of flowing through, supply line 13 are positioned at jacket 13A the inside, make the polymkeric substance melt keep and the identical temperature of process stream.The polymkeric substance melt that flows into supply line 13 can be controlled by charging pump 13B and valve 15.According to the present invention, the polymkeric substance melt flows into sample box 14 by supply line 13.Utilize spectrometer 50 sample to be analyzed again by means of infrared radiation.Analytic process is controlled by computing machine 60, and computing machine also demonstrates the infrared spectrum that is produced by the analysis of polymkeric substance melt.The analysis result of representing on computing machine 60 display terminals can utilize draught machine 70 to provide with the hard copy form.The temperature of sample box 14 interpolymer melts will be described in further detail below by thermostat 80 controls.
Referring now to Fig. 2,, spectrometer 50 places guard shield 51, and guard shield also has a groove 52 for 51 li, and sample box 14 just is placed in the groove.
Spectrometer 50 describes in detail in Fig. 4, and infrared origin 90 is after the reflection of level crossing 91 right angles, through beam splitter 92.So 50 percent infrared light reflection is to fixing level crossing 93, other 50 percent infrared transmission is to removable level crossing 94.Fixing level crossing 93 reflects back into infrared radiation on the beam splitter along changeless light path by reflection.When removable level crossing 94 reflected radiation, its optical path length changed, therefore may be different with the light path of the radiation of returning from fixing flat mirror reflects.The light beam that reflects reconfigures on beam splitter 92 again, a part of directive condenser lens 95 of combination back light beam.Lens 95 project the infrared beam of assembling on the focus that is arranged in sample box 14, and then, infrared beam is dispersed once more.The light beam of dispersing is reflexed on the infrared eye 97 by condenser lens 96 again.Utilize the variation of optical path difference in the laser instrument 98 measure spectrum meters 50.Laser instrument 98 is launched has the very accurately light beam of interference pattern, and this interference pattern produces the interferogram of cosine wave (CW).This cosine wave (CW) has triggered digitized signal at detector.Spectrometer 50 also comprises a laser detector 99 and a white light detector 100.
Spectrometer 50 is very responsive for thermal effect.As following described, because the polymkeric substance melt must be kept same temperature with its process stream, therefore, in groove 52, place a L shaped heat insulation plate washer 54, prevent to damage spectrometer 50 from the heat of sample box 14.Be easy to find out that plate washer 54 is structure of right angle tyoe of being made by thermal insulation material 54 by Fig. 3, thermal insulation material can be the product as Mick Nuo Feierte (Microfelt), pastes press polished reflective aluminum skin of one deck or stainless steel sheet| 55 in the above.Sample box 14 is placed in the groove 52 through inlet 56.
Referring now to Fig. 5,, sample box 14 is described in detail.The core of sample box 14 is blooms 18, and a duct 19 is arranged in the bloom.In fact duct 19 takes the shape of the letter U, and top is threaded inlet 20, is used for linking to each other with supply line 13, and end is outlet 21, just in time be positioned at inlet 20 below, by outlet 21 the polymkeric substance melt is discharged into stockline 16.
The hole 22 and 23 that two longitudinal extensions are arranged in bloom 18 is used for placing elongated resistor-type heater 24 and 25.Heater 24 with 25 with duct 19 parallel and close proximity, be used for making the polymkeric substance of bloom 18 and its process stream to keep equal temperature.Also have two additional holes 26 and 28 that are placed with elongated resistance wire heater 29 and 30 in addition, as described below, they are to be used for making near the polymkeric substance melt of sight chamber and its process stream to keep equal temperature.Thermocouple 31 is used to monitor heater 29 and near 30 temperature.Same thermocouple 32 is used for monitoring bloom 18 heaters 24 and near 25 temperature.Heater 24,25,26 and 28 and thermocouple 31 and 32 by thermostat 80 control with monitor.
A threaded temperature sample valve inlet 33 is arranged on bloom 18, and it communicates with duct 19.In sample valve inlet 33 a latch valve 34 that has adaptive screw thread is arranged, its position can change, and when being shown in an open position, the polymkeric substance melt can flow into the area of observation coverage, when in the closed position, does not then allow the polymkeric substance melt to flow into the area of observation coverage.Also have a bypass valve inlet 35 on bloom 18, it also communicates with duct 19.A bypass plug valve 36 that has adaptive screw thread is arranged in bypass inlet 35, and it also can move between the opening and closing position.The function of these valves will be described further with reference to Fig. 9 and Figure 10 below.Also opened a threaded window frame hole 37 on the bloom 18, it passes straight through to opposite side from a side one of bloom.One side in hole 37 has a threaded window frame 38, and opposite side has a same threaded window frame 39.
Referring now to Fig. 6, Fig. 7 and Fig. 8 double thread window- frame 38 and 39 are done an explanation.Be easy to find out that window- frame 38 and 39 each has a bellmouth 38A and 39A by Fig. 8, lead to opposite side from a side of window-frame.End at window-frame 38 has the recessed rafter 38B of a ring-type, at an end of window-frame 39 the recessed rafter 39B of a ring-type is arranged also.The high-temperature agglomerant that utilizes epoxy resin and so on adheres to the disc crystal 40 of the ir transmitting material of zinc selenide (ZnSe) and so on recessed rafter 38B and the 39B securely.Crystal has formed saturating infrared radiation " window ".Should see, for example the diameter of crystal 40 is 0.72 inch (18 millimeters), and thickness is 0.16 inch (4 millimeters), so, in fact whole area is all respectively by window- frame 38 and 39 supports, has only the exposed aperture of center diameter 0.32 inch (8 millimeters) to allow to penetrate and sees through.This makes crystal 4 .0 can stand very high temperature and pressure.
As shown in Figure 6, window-frame 38 has a square groove 41 at its end relative with crystal 40, is used for accepting impact wrench.This is that many kinds are regulated window- frames 38 and 39 both or one of them, a kind of with in the method for controlling relative position between them.
As Fig. 9 and shown in Figure 10, intersect with duct 19 after sampling valve inlet 33 in hole 37.Window- frame 38 and 39 is placed very close to ground in hole 37.Clearance gauge in the window- frame 38 and 39 between the crystal 40 is made the space of sight chamber 42.When the polymkeric substance melt is flowed into by duct 19 and during through sight chamber 42, melt just is exposed to by sight chamber one side and wears the chamber and cross among the infrared radiation of directive opposite side.
When sampling valve 34 was shown in an open position, the space of polymkeric substance flow of melt between the crystal 40 of window- frame 38 and 39 formed one deck polymer samples as thin as a wafer, and infrared radiation is transmitted to opposite side from sample one side.The polymkeric substance melt continues to flow in duct 19 backward, and arranges to unloading stockline 16 through discharging outlet 21.Unloading stockline 16 has an operation valve 17, and by means of it, the polymkeric substance melt can perhaps abandon as required, perhaps flows back to again in the process stream 11.
If sampling is not carried out continuously, sampling valve 34 and bypass valve 36 are closed respectively and are opened at interval according to preset time so.In this case, the polymkeric substance melt can not enter sight chamber 42, but flows in the duct 19 of sight chamber 42 fronts by bypass valve inlet 35, and is top for another example described by discharging outlet 21 discharges.
The polymkeric substance melt also has the possible approach of the third bloom 18 of flowing through.Here it is all is opened to predetermined degree with sampling valve 34 and bypass valve 36.When continuous sampling is carried out in hope, take this mode mostly.At this moment, sampling valve 34 leaves enough greatly, and making for example has about 10 polymkeric substance flow of melt over-sampling valve 34 in the duct 19, enters sight chamber 42.Bypass valve 36 leaves to such an extent that more strengthen, and makes to export all the other polymkeric substance melt bypass sight chambers 42 of 90 percent 21 by discharging and discharge.
By regulating the relative openings of sizes of sampling valve 34 and bypass valve 36, can change the percent quantities that the polymkeric substance melt is sampled and analyzes in the duct 19 in sight chamber 42, thereby obtain sampled result quickly.
Return Fig. 5, the remaining part of sample box 14 is done simple introduction.Bloom 18 is positioned at adiabatic outer cover 43 inside.Relevant parts have many corresponding holes on the outer cover 43, so that can install on the bloom 18.Bloom 18 is subjected to the fixing of its thermal insulation material and a pair of bearing 44 and 45 in outer cover 43 inside, this a pair of bearing is screwed on the outer cover 43.Bloom 18 and outer cover 43 are fixed to by means of convex fixed head 46 in the groove 52 of spectrometer 50, and this convex fixed head 46 utilizes screw 47 and bearing 48 to pass outer cover 43 and is fastened on the bloom 18.Fig. 5 shows in the middle of these two kinds other parts (referring to: screw 47 and bearing 48).Spill fixed mount 49 engagements in convex fixed head 46 and the groove 52 that is fixed on spectrometer 50.Have hole 46A and 49A on fixed head 46 and the fixed mount 49, infrared beam two holes thus passes.Two axial adjustable taper pipes 101 and 102 and window- frame 38 and 39 match, therefore when infrared beam passes sample box 14, can fully light beam be surrounded.Usually, pipe 101 and 102 all will purify, to prevent the interference to infrared radiation of water steam and carbon dioxide.
Referring to Fig. 8, regulate window- frame 38 and 39 once more, can make the focus of infrared beam be arranged in sight chamber 42.By regulating the distance between window-frame 38 and 39 a little, just can obtain to obtaining the desirable absorbance log of the most accurate result.Can expect that window- frame 38 and 39 controls by graduation apparatus make that the predetermined gap between them will finally form corresponding relation with the expectation absorptivity of specific tested material.Otherwise, can determine the optimum width of sight chamber 42 with experimental technique, method is that two crystal 4s 0 are contacted with each other, and then window- frame 38 and 39 both or one of them direction outside hole 37 are moved, and observe owing to increase optical length to the corresponding influence that brings of absorbed rate.As far as is known, the maximum effectively optical length of sampling polymkeric substance melt roughly is no more than 1/30th inch (0.76 millimeter).
Utilize above-mentioned sample box 14 to carry out accurate spectrophotometric analysis to the material in the process stream.Except using infrared radiation, can also use visible light, ultraviolet and other spectrum segment radiation.A major advantage of sample box 14 is that sample is sampled under nondestructive state and analyzed, this with prior art in to diminish check be different.
For accommodate sample box 14 bears the requirement of High Temperature High Pressure, the critical piece of sample box all adopts the high-quality stainless steel to make.All ducts and mechanical whorl all polish.In addition, the also available teflon belt of screw thread looping is got up.Brass, copper or other material that may react with analyzed material all will not adopt.
At last, a pressure transducer (not shown) can be housed also, the pressure in the duct 19 is monitored.
More than introduced and utilized spectrophotometer that the material in the process of flowing stream is carried out the used sample box of chemical analysis.Each details of the present invention may change, but does not break away from scope of invention.And previously described most preferred embodiment according to sample box of the present invention only provides in order to say something, and-scope of the present invention is limited by claim.
Claims (32)
1, a kind of spectrophotometer that adopts carries out chemico-analytic sample box to the material in the process of flowing stream, it is characterized in that this sample box is by forming with the lower part:
A) determine the guard shield in one-piece construction duct, this duct is linked up with process stream therein by the inlet on the guard shield;
B) whole sight chamber in above-mentioned guard shield, that link up with above-mentioned duct;
C) first saturating rediation aperture on first threaded engagement hole that sealing and fixing is linked up with above-mentioned sight chamber in above-mentioned guard shield in the threaded adjusting mode;
D) be fixed on second transmission window on second threaded engagement hole in the above-mentioned guard shield in the threaded adjusting mode, this window is relative with above-mentioned first transmission window and place with interval, and has determined flow through therebetween optical length of material in the process stream.
E) above-mentioned first window and second window can relatively move by the threaded adjusting mode in described guard shield, maintenance simultaneously and guard shield and the sealing of above-mentioned sight chamber, change by the determined optical length of above-mentioned sight chamber spacing with this, and the sealing relationship of maintenance and above-mentioned guard shield;
F) the first above-mentioned window is used to receive predetermined spectral radiance, and will import above-mentioned sight chamber through the radiation of this window, pass described material, thereby produce the spectroscopic data of representing this material chemical analysis result, the second above-mentioned window is used to receive the radiation that contains spectroscopic data from sight chamber, and this radiation transmission is gone out so that handle;
G) there is discharging outlet in the described duct in the above-mentioned guard shield.
2, according to the sample box of claim 1, it is characterized in that having valve and described duct links, be used for optionally
A) material is imported and the described sight chamber of flowing through, or
B) with the material exit, and not earlier through described sight chamber.
3, according to the sample box of claim 1, it is characterized in that having valve and described duct links, be used for optionally
A) material is imported and the described sight chamber of flowing through, or
B) with the material exit, and not earlier through described sight chamber, or
C) first predetermined portions with described material imports described sight chamber; Simultaneously, with the second predetermined portions exit of described material, and at first do not pass through described sight chamber.
4, according to the sample box of claim 1, it is characterized in that, wherein comprise infrared radiation by spectrophotometric spectra meter radiation emitted, the described first and second saturating rediation aperture materials comprise ir transmitting material.
5, according to the sample box of claim 1, it is characterized in that, have at least one can move with respect to another among the first wherein above-mentioned window and second window, so that change the space between first window and second window, that is material flows through interval optical length in the change sight chamber.
6, according to the sample box of claim 1, it is characterized in that wherein first window and the second window both can relatively move, so that change the distance between them, that is material flows through interval optical length in the sight chamber.
7, according to the sample box of claim 5 and 6, it is characterized in that including first and second threaded window frames, have radiation channel in the window-frame, the first above-mentioned window and second window just are fixed on these two window-frames, are used for seeing through radiation; Also include an adaptive threaded hole in above-mentioned guard shield, be used to support above-mentioned threaded window frame, between threaded hole and sight chamber, radiation can be passed through.
8, according to the sample box of claim 7, the width that it is characterized in that observation ward wherein zero to variable between the usable range of a thirtieth inch (0.76 millimeter).
9, carry out in the chemico-analytic spectrophotometer at the material that is used for process stream flows, the sample box that the material stream that it is characterized in that and flow keeps dynamically linking up combines with the spectrophotometric spectra meter, material sampling in the process stream is sent in the sight chamber, utilizes ray to be transmitted through opposite side from material one side and carries out the spectrophotometric spectra analysis.
10, in spectrophotometer, it is characterized in that sample box includes to send the sampling material back in the process of flowing stream device according to claim 9.
11, in spectrophotometer, it is characterized in that described spectrophotometer comprises an infrared radiation transmitter and an infrared radiation detector according to claim 9.
12, in the spectrophotometer according to claim 9,10 or 11, the structure that it is characterized in that described sight chamber is variable, can change with what of material sample so pass the radiation optical length of specimen material, thereby regulate the absorption of material to radiation.
13, in spectrophotometric spectra meter, it is characterized in that including valving, be used for optionally according to claim 12
A) material is imported and the described sight chamber of flowing through, or
B) material the is led outlet of described sample box, and earlier through described sight chamber.
14, in the spectrophotometric spectra meter according to claim 12, it is characterized in that containing valving, it is used for optionally with described sample box
A) material is imported and the described sight chamber of flowing through, or
B) material is led outside the described sample box, and not earlier through described observation ward, or
C) first of material is imported and the described sight chamber of flowing through, simultaneously, second portion is led outside the described sample box, and not earlier through described sight chamber.
15, in spectrophotometric spectra meter according to claim 9, it is characterized in that above-mentioned material comprises the polymkeric substance melt, above-mentioned sample box contains heating arrangement, is used for making described polymkeric substance melt and process stream keep equal temperature and pressure in analytic process.
16, a kind of spectrophotometer that adopts carries out chemico-analytic sample box to the polymkeric substance melt in the process of flowing stream, it is characterized in that this sample box is by forming with the lower part:
A) determine the guard shield in duct, this duct is linked up by inlet on the guard shield and process stream;
B) in described guard shield, make polymkeric substance melt and process stream keep the heating arrangement of equal temperature;
The sight chamber of the sealing of linking up with described duct that c) in described guard shield, forms, this sight chamber is limited by following each one:
(1) first transmission window;
(2) with spaced second transmission window of above-mentioned first transmission window, between these two transmission window is the place of process stream polymkeric substance flow of melt warp at interval, and it has determined optical path length;
(3) above-mentioned first window that is used to receive the spectral radiance of being scheduled to transmission, radiation is injected in the described observation ward through this window, and the focus of passing through the polymkeric substance flow of melt inside that is arranged in sight chamber, thereby produce the spectroscopic data of representing polymkeric substance melt chemical analysis results, and
(4) above-mentioned second window that is used to receive from the radiation that contains spectroscopic data of sight chamber, and this radiation sent out handle;
D) outlet that the polymkeric substance melt is emitted is contained in the duct in the above-mentioned guard shield from this guard shield.
17, according to the sample box of claim 16, it is characterized in that containing valving, it is used for optionally with described duct
A) the polymkeric substance melt is imported and the above-mentioned sight chamber of flowing through, or
B) with polymkeric substance melt exit, and the above-mentioned sight chamber of not flowing through earlier.
18, according to the sample box of claim 16, it is characterized in that containing valving, it is used for optionally with described duct
A) the polymkeric substance melt is imported and the above-mentioned sight chamber of flowing through, or
B) with polymkeric substance melt exit, and the above-mentioned sight chamber of not flowing through earlier, or
C) first predetermined portions with the polymkeric substance melt imports and the above-mentioned sight chamber of flowing through, with constantly, and with the second portion exit of polymkeric substance melt, and the above-mentioned sight chamber of not flowing through earlier.
19, according to the sample box of claim 16, it is characterized in that the radiation of wherein being launched by spectrophotometric degree meter comprises infrared radiation, the material of the first and second above-mentioned transmission window comprises infrared transmission material.
20, according to the sample box of claim 16, it is characterized in that in wherein said first window and second window, have at least one can move with respect to another, be used to change the interval between described first window and second window, that is change in the sight chamber polymkeric substance flow of melt through the optical path length in interval.
21, according to the sample box of claim 16, it is characterized in that wherein said first window and the second window both can relatively move, be used to change spacing between the two, that is change in the sight chamber polymkeric substance flow of melt through the optical path length in interval.
22, according to the sample box of claim 20 or 21, it is characterized in that wherein said two windows respectively are fixed on the threaded window frame, radiation channel is arranged in the threaded window frame, link up by radiation and window, adaptive screw is arranged in above-mentioned guard shield, be used to support above-mentioned threaded window frame.
23, according to the sample box of claim 16, the optical path length that it is characterized in that observation ward wherein infinitely small to variable between the usable range of a thirtieth inch (0.76 millimeter).
24, according to claim 16,17,18,19,20,21 or 23 sample box, it is characterized in that an adiabatic outer cover is arranged on described guard shield, be used to aid in the described guard shield polymkeric substance melt and process stream are maintained equal temperature.
25, utilize spectrophotometer that the material in the process of flowing stream is carried out chemico-analytic method, it is characterized in that may further comprise the steps:
A) material sample is branched to the area of observation coverage from process stream;
B) employing is carried out spectral analysis with radiation by the method for the side permeable material arrival opposite side of material; And
C) material is discharged by the area of observation coverage.
26,, it is characterized in that comprising that further adjusting radiation passes the optical path length of material, so that change the absorptivity of material to radiation according to the method for claim 25.
27,, it is characterized in that comprising the step that the material after area of observation coverage analysis is discharged as waste material according to the method for claim 25.
28,, it is characterized in that comprising the material after above-mentioned area of observation coverage analysis is refilled step among the process of flowing stream according to the method for claim 25.
29,, it is characterized in that may further comprise the steps according to the method for claim 25:
D) from process of flowing stream, tell first, inject the above-mentioned area of observation coverage, carry out the spectrophotometric spectra analysis by the method that allows radiation pass material; And
E), just do not get rid of by analysis or refill during process of flowing flows as waste material from the other second portion material of telling of the area of observation coverage.
30, according to the method for claim 25, it is characterized in that wherein above-mentioned material comprises the polymkeric substance melt, above-mentioned method may further comprise the steps:
F) in order in analytic process, to make polymkeric substance melt and process stream keep equal temperature, when the polymkeric substance melt branches to the area of observation coverage and flow back in the process of flowing stream again, it is heated.
31, according to claim 25,26,27,28 or 29 method, it is characterized in that above-mentioned radiation comprises infrared radiation.
32, according to claim 25,26,27,28 or 29 method, it is characterized in that wherein adopting spectrophotometric method to analyze the step of described material, comprise the step that makes above-mentioned radiation see through first transmission window and enter the area of observation coverage; The step of first transmission window and the radiation afterwards of described material is passed in reception, and the above-mentioned radiation that contains the spectroscopic data relevant with material is sent out the step of handling.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 87103339 CN87103339A (en) | 1986-02-20 | 1987-05-06 | The online spectrophotometric chemical analysis method and the device of material in process of flowing stream |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US06/831,296 US4717827A (en) | 1986-02-20 | 1986-02-20 | Apparatus for on-line spectrophotometric chemical analysis of material in moving process stream |
| CN 87103339 CN87103339A (en) | 1986-02-20 | 1987-05-06 | The online spectrophotometric chemical analysis method and the device of material in process of flowing stream |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN87103339A true CN87103339A (en) | 1988-11-16 |
Family
ID=25742316
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 87103339 Pending CN87103339A (en) | 1986-02-20 | 1987-05-06 | The online spectrophotometric chemical analysis method and the device of material in process of flowing stream |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN87103339A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106908533A (en) * | 2016-12-14 | 2017-06-30 | 宁海德宝立新材料有限公司 | A kind of application of metal oxide |
-
1987
- 1987-05-06 CN CN 87103339 patent/CN87103339A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106908533A (en) * | 2016-12-14 | 2017-06-30 | 宁海德宝立新材料有限公司 | A kind of application of metal oxide |
| CN106908533B (en) * | 2016-12-14 | 2019-11-12 | 宁海德宝立新材料有限公司 | A kind of application of metal oxide |
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