CN1062490C - Apparatus for mixing and detecting on-line homogeneity - Google Patents
Apparatus for mixing and detecting on-line homogeneity Download PDFInfo
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- CN1062490C CN1062490C CN94107246A CN94107246A CN1062490C CN 1062490 C CN1062490 C CN 1062490C CN 94107246 A CN94107246 A CN 94107246A CN 94107246 A CN94107246 A CN 94107246A CN 1062490 C CN1062490 C CN 1062490C
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F29/00—Mixers with rotating receptacles
- B01F29/20—Mixers with rotating receptacles with receptacles rotating about an axis at an angle to their longitudinal axis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61J—CONTAINERS SPECIALLY ADAPTED FOR MEDICAL OR PHARMACEUTICAL PURPOSES; DEVICES OR METHODS SPECIALLY ADAPTED FOR BRINGING PHARMACEUTICAL PRODUCTS INTO PARTICULAR PHYSICAL OR ADMINISTERING FORMS; DEVICES FOR ADMINISTERING FOOD OR MEDICINES ORALLY; BABY COMFORTERS; DEVICES FOR RECEIVING SPITTLE
- A61J3/00—Devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F29/00—Mixers with rotating receptacles
- B01F29/40—Parts or components, e.g. receptacles, feeding or discharging means
- B01F29/401—Receptacles, e.g. provided with liners
- B01F29/4011—Receptacles, e.g. provided with liners characterised by the shape or cross-section of the receptacle, e.g. of Y-, Z -, S -, or X shape
- B01F29/40118—V or W shapes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F29/00—Mixers with rotating receptacles
- B01F29/40—Parts or components, e.g. receptacles, feeding or discharging means
- B01F29/403—Disposition of the rotor axis
- B01F29/4036—Disposition of the rotor axis with a plurality of rotating receptacles
- B01F29/40363—Disposition of the rotor axis with a plurality of rotating receptacles having perpendicular axes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F29/00—Mixers with rotating receptacles
- B01F29/60—Mixers with rotating receptacles rotating about a horizontal or inclined axis, e.g. drum mixers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F29/00—Mixers with rotating receptacles
- B01F29/60—Mixers with rotating receptacles rotating about a horizontal or inclined axis, e.g. drum mixers
- B01F29/62—Mixers with rotating receptacles rotating about a horizontal or inclined axis, e.g. drum mixers without bars, i.e. without mixing elements; characterised by the shape or cross section of the receptacle, e.g. of Y-, Z-, S- or X- shape; with cylindrical receptacles rotating about an axis at an angle to their longitudinal axis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/20—Measuring; Control or regulation
- B01F35/21—Measuring
- B01F35/213—Measuring of the properties of the mixtures, e.g. temperature, density or colour
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/71—Feed mechanisms
- B01F35/717—Feed mechanisms characterised by the means for feeding the components to the mixer
- B01F35/71705—Feed mechanisms characterised by the means for feeding the components to the mixer using belts
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/75—Discharge mechanisms
- B01F35/754—Discharge mechanisms characterised by the means for discharging the components from the mixer
- B01F35/7547—Discharge mechanisms characterised by the means for discharging the components from the mixer using valves, gates, orifices or openings
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/71—Feed mechanisms
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
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- Geometry (AREA)
- Veterinary Medicine (AREA)
- Accessories For Mixers (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
- Medical Preparation Storing Or Oral Administration Devices (AREA)
- Mixers With Rotating Receptacles And Mixers With Vibration Mechanisms (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Continuous Casting (AREA)
Abstract
This invention relates to an apparatus for mixing compositions of matter into a homogeneous mixture and detecting on-line the homogeneity and potency of the mixture, and a method for using the same. More particularly, this invention relates to an apparatus for mixing the components of a pharmaceutical composition into a homogeneous mixture and detecting on-line the homogeneity and potency of said pharmaceutical composition.
Description
The present invention relates to a kind of equipment, material composition is mixed into uniform mixture with this equipment, and the uniformity coefficient of online detection mixture and effectiveness, and the method for using this equipment.More particularly, the present invention relates to a kind of equipment, each composition of composite medicine is mixed into uniform mixture with this equipment, and the mixability and the effectiveness of the described composite medicine of online detection.
In active agents being processed into the medicine process that the recipient can take, mixing composite medicine is committed step.Usually, composite medicine is made of five kinds or multiple different composition, and comprising active agents, these composite medicines must be mixed into uniform mixture.Determine that the concentration of active agents in medicinal mixture is vital.The concentration of determining other nonactive medicine components in the mixture that finally mixes also is very important.In order to guarantee that the active agents that offers the recipient has proper dosage, must guarantee the uniformity of composite medicine.
In medicinal mixture, the concentration of nonactive medicine component also is very important, because it has determined the physical property of mixture.For example, nonactive medicine component is the excipient class in the known composite medicine.An example of excipient is a distintegrant.The dissolution velocity of this distintegrant decision tablet in recipient's stomach.Therefore, if distintegrant is not to be evenly distributed in the medicinal mixture, so consequently tablet can not dissolve with uniform rate.This may produce harmful effect to drug quality, dosage and bioavailability.
Usually, the distribution situation of the uniformity of composite medicine explanation active agents in composite medicine.The quantity of effectiveness explanation active agents in composite medicine of composite medicine.Under regular situation, measure the effectiveness and the uniformity of medicinal mixture and want elapsed time.In addition, in traditional measuring method, only survey effectiveness and the uniformity of active agents composition in composite medicine, and do not relate to the uniformity of nonactive medicine component.
Traditional method uses conventional mixer (for example core pattern mixer, spiral blade stirrer, " V " type mixer, and like product) to mix each composition of composite medicine usually.When thinking that hybrid process is finished, mixer is shut down, and common sample at nine parts of the different location of conventional mixer taking-ups or more parts of mixtures.When sample being sent to laboratory and analyzing it and render a service, mixer keeps the state that shuts down.Usually adopt high-performance liquid chromatography (HPLC) to analyze.The analysis result of HPLC only can be determined the concentration of active agents composition in each sample.This measurement determines whether the active agents composition is dispersed in the mixture, and whether reaches suitable concentration level.These message reflections the effectiveness of mixture, and, if the effectiveness of each sample is identical, so just think that mixture mixes.The HPLC analytical method be can not determine the concentration of non-active ingredient in the mixture.The uniformity of all the components is very important in the medicinal mixture, because quite the distribution situation of some drug ingredients influences the physical property of the last form of composite medicine the most at last, as mentioned above.Traditional analytical method will spend 24～48 hours usually and just can finish.
In traditional method, another time consuming factor is to determine that mixture reaches or do not reach to mix a little.Usually, mixer turns round according to predetermined amount of time.Just taking out sample after mixer shuts down tests.If it is inhomogeneous that mixture mixes, mixer remains in operation so, and continues repeated test.In addition, mixture may just mix before reaching predetermined incorporation time.Under first kind of situation, the test number (TN) of execution under second kind of situation, in surpassing the hybrid process process that mixes a little, has been wasted the time again more than predetermined times.Incorporation time is long, may cause once more that the drug ingredient that mixes produces separation.Therefore, the effectiveness of online detection medicinal mixture and the equipment of uniformity coefficient can be avoided losing time in the above two kinds of cases, and can reduce because the long and issuable separation of incorporation time is dangerous.Term " online " meaning is in order to test with the uniformity coefficient of determining mixture and when rendeing a service sample thief, mixer to be shut down.
Because above-mentioned reason, just to feel for a long time to need a kind of equipment in this professional domain, this equipment can mix each composition of medicinal mixture, and all effectiveness and the uniformity coefficient of compositions in can online detection medicinal mixture.But, before this,, there is not a kind of equipment can mix composite medicine in the art, and the uniformity coefficient and the effectiveness of the online detection medicinal mixture of energy.
The present invention aims to provide a kind of equipment, with this equipment composition of matter is mixed into uniform mixture, and can online detection uniformity of mixture and effectiveness during hybrid process.This equipment comprises the mixing arrangement of compounding substances composition.Said mixing arrangement has the container that holds material composition to be mixed, and is best, and during hybrid process, described container rotates around rotation, and container has the hole that hides and seal with transparent locking device.Sniffer and transparent locking device are very approaching, preferably by thereon, so that the spectral characteristic of online detecting material mixture of ingredients.
In a preferred embodiment of the invention, seal described hole with axle (hollow shaft).The sniffer of the spectral characteristic of online detecting material mixture of ingredients is rotatably installed by described axle.The device of surveying the position of rotation of described container is connected on the mixing arrangement.The device of surveying position of rotation makes the rotation of described container or the data of angle position be delivered to data acquisition and control computer.Data acquisition and control computer are gathered spectroscopic data by sniffer synchronously on the single position of rotation of the described container of predetermined mixing arrangement or a plurality of position of rotation.During container rotates, gather spectroscopic data at a certain predetermined point always, guarantee that mixed uniformity of mixture reaches the quite high degree of accuracy.
Another aspect of the present invention aims to provide a kind of method, in this way material composition is mixed into uniform mixture, and meanwhile, the uniformity coefficient of online detecting material mixture of ingredients and effectiveness.The step of this method is: one matter composition that will the be mixed mixing arrangement of packing into; The compounding substances composition is meanwhile by the spectral characteristic of the online detection mixture of sniffer; Can be selectively, the single or multiple turned position of in the container of the mixing arrangement that rotates around rotation, being scheduled to, utilize the sniffer spectral characteristic of online detection mixture simultaneously, by comparing, when the spectral characteristic of described mixture reaches the spectrum of all even effectiveness points of predetermined known homogeneous mixture, perhaps when the difference of spectral characteristic disappears, can close equipment of the present invention artificially, perhaps utilize data acquisition and control computer to close equipment of the present invention automatically.
So the present invention can gather the spectrum of mixture in the mixing arrangement motion, thereby avoids shutting down.Long or the mixing time of mixing time is not enough to be distinctive defective when determining in traditional hybrid process method that mixture is renderd a service.
By specification and claims, and the some embodiments of the present invention of describing in the accompanying drawing, can see other features and advantages of the present invention.
Fig. 1 represents the side view of a demonstration equipment of the present invention, also shown is container 101 and first 125 section.
The vertical view of Fig. 2 presentation graphs 1 apparatus shown.
The enlarged drawing of Fig. 3 presentation graphs 1 illustrates the part of container and the syndeton of container and light-dividing device.
Fig. 4 represents to be connected the side view of autoregistration reflection (transflectance) probe on the axle.
Fig. 5 represent a side view with traditional mixer of mixing arrangement in the machine (as, spiral blade stirrer or core pattern mixer).
Fig. 6 a to 6d is the profile along 6a-6a hatching line among Fig. 5, shows the perforate on the mixer and sniffer is connected to different device on the mixer.
Fig. 7 represents container, axle and inserts the amplification profile of an embodiment of the insert in the axle.
Fig. 8 represents another embodiment of equipment of the present invention, and this embodiment has a device that is used for the position of rotation of exploration vessel.
In the technology of mixing composite medicine, adopt dissimilar mixers usually.For example, the mixer that has a type is " V " type mixer, with its compounding substances composition, for example mixes powder or liquid.This " V " type mixer makes the container that material composition is housed produce rotation around axis.Therefore, one of embodiments of the invention are improved " V " type mixers, and it is represented by Fig. 1.
According to Fig. 1 and Fig. 2, in container 101, be equipped with and want mixed material composition.Container 101 has common " V " shape shape, and described container 101 is made of second hollow pipe 204 of first hollow pipe 201 and connection with it, and described hollow pipe is gathered together with forming angle mutually, thereby forms " V " shape shape.Container 101 has the opposed walls 104 of flare, and it is the outer surface of the long part of container 101 hollow core barrels 201 and 204.Hole 107 is provided with by wall 104.The position in hole is determined following will describe with second with the position that is connected of second hollow pipe by second 111.
Opening 115 at container 101 tops is used to load the independent composition of the various materials that will mix in container 101, perhaps draw off the mixture that has mixed.Hide and sealed open 115 during hybrid process with top cover 207.With top locking button 208 top cover 207 is fixed on the container 101.Opening 119 in container 101 bottoms is used for perhaps drawing off the mixture that mixes to pack into the independent composition of various materials that will be mixed of container 101.Hide and sealed open 119 in the hybrid process process with bottom 122.With bottom locking button 123 bottom 122 is fixed on the container 101.
In the pillow block 210 of first ball bearing lateral opening that passes pillow block is arranged, preferably the hole is in pillow block central authorities.The pillow block of ball bearing is well known in the prior art, is provided with bearing in pillow block, and these bearings can make the axle that is arranged in the hole freely rotate, and supporting role is arranged.The feature of the pillow block of these ball bearings will be described below more fully.In first bearing 128 transverse holes of passing it is arranged, this hole is arranged on the bearing top.The pillow block 210 of first ball bearing is arranged between the container 101 and first bearing 128, and usually with the side of bolting to first bearing 128, so that the hole of the pillow block 210 of first ball bearing is aimed at the hole of first bearing 128.
The pillow block 213 of second ball bearing has the transverse holes of perforation, and preferably the hole is positioned at pillow block central authorities.The top of second bearing 131 is provided with the transverse holes of perforation.The pillow block 213 of second ball bearing is arranged between the container 101 and second bearing 131, and with bolt pillow block is fixed to the side of second bearing 131 usually, so that the hole of pillow block 213 of second ball bearing and the hole of second bearing 131 are aimed at.
First end and second end are arranged for second 111.Second 111 first end is connected with container 101.Second 111 second end is rotatably installed in the cross through hole of the pillow block 213 of second ball bearing of aligning and second bearing 131, and is connected with tumbler 216.Described tumbler 216 can be a motor.Motor can directly be connected with second, perhaps is connected with second 111 by transmission mechanism 219.Transmission mechanism can be chain-drive mechanism or belt gear.Motor 216 rotates container 101, thereby makes the independent composition of various materials be mixed into uniform mixture.
With reference to Fig. 3, first 125 has first end and second end.First 125 first end passes hole 107 and links to each other with container 101.In this case, first 125 first end has part to insert in the container 101.It is enough dark that first 125 first end inserts container 101, so that want mixed material composition can to contact with first 125 the above-mentioned part of first end in the hybrid process process.First 125 second end is rotatably installed in the cross through hole of the pillow block 210 of first ball bearing that aligns and first bearing 128, makes first 125 and aims at mutually with second 111, forms the rotation of level.Horizontal axis of rotation must have enough height corresponding to the hollow pipe of container 101, can be around freely turning round 360 ° by first and second pivot centers that form with Bedpan 101.
As shown in Figure 1, first 125 has through hole 134.With the first end cover apertures 134 of transparent locking device 137 at first 125.Transparent locking device 137 can be transparency window or autoregistration reflection probe.Wave-length coverage according to the radius that sends from light-dividing device (below grade describe in detail) can be made described transparency window with glass, crystal (quartz) or sapphire.In the present embodiment, the most handy transparency window is as transparent locking device, and suggestion adopts crystal material to make transparency window 137.
In addition, as shown in Figure 4, with the first end covering through hole 134 of autoregistration reflection probe 400 at first 125.Comprise housing 405 with reference to Fig. 4 autoregistration reflection probe 400, lens 410, reflector 415, and be provided with space 420.
For example, the conduction device 140 of conduction irradiation light is a light pipe, light path and fibre-optic bundle.In the present embodiment, fibre-optic bundle is preferred conduction device.With reference to Fig. 1 and 3, fibre-optic bundle 140 has first end and second end.First end of fibre-optic bundle 140 passes through cover 141, and is hidden by cover 141.The cover 141 that covers fibre-optic bundle 140 is arranged on the inboard in hole 134 removedly, first end that makes fibre-optic bundle 140 is closely near transparency window 137, so that the radius that sends from described fibre-optic bundle roughly along continuous straight runs passes transparency window 137, and not can owing to may to the influential external light source of radiation source interference change.Best described fibre-optic bundle leans on mutually with described transparency window.The opening 147 that second end of fibre-optic bundle 140 passes light-dividing device 143 removably is fixed on the light-dividing device 143.Send radius from opening 147 punishment electro-optical devices 143, and admit by fibre-optic bundle 140 and carry the mixture diffuse light or the reverberation of coming.It is the example of preferred light-dividing device below: IR spectrophotometer; Visible ultraviolet spectrophotometer, the near infrared ray spectrophotometer; The IR spectrophotometer of intermediate range and Raman (raman) spectrophotometer.
Fibre-optic bundle 140 comprises two groups of optical fibers.First group of optical fiber propagated the radiant light that sends from the mixture of light-dividing device 143 in container 101.Transparency window 137 guarantees not change when the radius that fibre-optic bundle 140 sends passes transparency window 137 arrival mixtures.
If mixture is a solid, so just according to reflectance factor analyzing radiation signal.When radius shone solid mixture, light was by diffuse reflection.Second group of optical fiber collected by the next radius of mixture diffuse reflection, and reflection ray is passed because of light-dividing device 143.
If mixture is a liquid, so just according to refraction coefficient analyzing radiation light.Autoregistration reflection probe 400 with liquid mixture replaces transparency window 137, autoregistration reflection probe 400 is installed in first end of axle 125.The radiant light of launching from first group of optical fiber of fibre-optic bundle 140 passes transparent lens 410, passes the liquid mixture in the space 420 then, and described space 420 is between reflector 415 and housing 405.The material type of manufacturing lens 410 is identical with the material type that manufacturing transparency window 137 is enumerated, and its function is identical with transparency window 137.Liquid mixture makes radius produce deviation, and the radiant light back into light guide fibre bundle 140 that will be changed by reflector 415 is collected radiation reflected light by second group of optical fiber then, hands over it is propagated into light-dividing device 143.
Store and analysis diffuses or reverberation by light-dividing device 143; Perhaps light-dividing device 143 is transferred to computer with spectroscopic data again, by computer spectroscopic data is analyzed.
Particularly preferred light-dividing device is NIRSystems 6500 type spectrophotometers (a kind of near infrared ray spectrophotometers), and this photometer can be from NIRSystems Inc., 12101Tech Road, and Silver Spring, MD, 20904 buy.The computer of analyzing spectroscopic data can be any personal computer, for example has the Zeos 33MHz 80846DX PC of 8Mb random access device.Gather spectroscopic data with near-infrared spectrum analysis software (NSAS) in computer, this software is the control software kit that is located at spectroscopic instruments that is provided by NIR Systems.Analyze spectroscopic data then in Matlab (software kit), this software kit can be from The Mathworks Inc.Cochituate Place, 24 Prime Park way, and Natick, MA, 01760 buys.
Fig. 5 is used for the common expression-form of another kind of type of conventional mixer of compounding substances composition.Such conventional mixer mixes the independent composition of various materials, when making it become uniform mixture, does not need around pivot center the container of mixer to be rotated.And such conventional mixer relies on the agitator in the container, and for example blade or blender make material composition be mixed into uniform mixture.Screw mixer is the example that utilizes the conventional mixer of blade.The core pattern mixer is the example that utilizes the conventional mixer of blender.In addition, these mixers that mix powder and liquid also can mix paste and milky substance composition.
With reference to Fig. 5, represent any fixing conventional mixer with the rectangular box that label 500 is represented, it relies on inner agitator to make material composition be mixed into uniform mixture.Has hole 502 in one of wall 501 of mixer 500.But, can in any one or more mixer walls, more than one hole be set.The internal tank of mixer 500 must be led in the hole, so that on sniffer can be delivered to mixture in the container of mixer from light-dividing device with radiant light, and can gather and analyze reflection or autoregistration radiation reflected light.
An embodiment of Fig. 6 a indication window 502, mixer wall 501 and conduction device 140, wherein mixer wall 501 inwardly concaves the container inside of mixer 500.Hide and seal the hole 502 of mixer wall 501 with transparent block 503.The material type of making transparent block 503 is with to make the material type that transparency window 137 enumerates identical, and its function is identical with the function of transparency window 137.First end of conduction device 140 is closely close, preferably leans against on the transparent block 503, be used for second end of conduction device of conduct radiation light removably to be connected on the light-dividing device 143, as shown in Figure 1, and as described above.
Another embodiment of Fig. 6 b indication window 502, mixer wall 501 and conduction device 140.The conduction device 140 that is connected on the mixer wall 501 with passing hole 502 hides and blind hole 502.Conduction device 140 inserts in the container of mixer 100.Hide the end of inserting the conduction device 140 in the container with transparent block 503.In addition, can adopt autoregistration reflection probe 400 recited above to replace transparent block 503.
The embodiment of Fig. 6 c indication window 502, mixer wall 501 and light-dividing device 143.In this embodiment, hide and be enclosed in hole 502 on the mixer wall 501 with transparent block 503.The position of light-dividing device 143 is adjacent to mixer wall 501, makes preferably to lean against emitted radiation light and admit catoptrical opening 147 closely close on the transparent block 503.
Fig. 6 d is an indication window 502, another embodiment of mixer wall 501 and conduction device 140.In this embodiment, with the hole 502 on transparent block 503 coverings and the sealing mixer wall 501.Make the position of first end of conduction device 140 closely close, preferably lean against on the transparent block 503.
Certainly, Fig. 6 a, 6b and 6d represent preferred embodiment, obtain mixed spectral mixture data for online, and conduction device 140 is combined with mixer 500, so that determine the effectiveness and the uniformity of medicinal mixture.The acquisition mode of spectrum with above-described, be identical in the exemplary embodiments of representative by improved V-mixer.
In one embodiment, as Fig. 6 a, the described conduction device of describing among 6b and the 6d 140 is fibre-optic bundles 140, and it comprises two groups of optical fibers.First group of optical fiber falls radiant light and is transferred to mixture from light-dividing device 143.The radiant light that transparent block 503 can make first group of optical fiber in the fiber illuminated 140 send passes, and there is no the mixture that deviation ground arrives material composition.The radiant light that touches mixture produces diffuse reflection under the situation of solid mixture, and produces reflection under the liquid mixture situation.Second group of optical fiber collected from the diffusing of mixture, and passes radiant light back light-dividing device 143.Light-dividing device 143 analyzing radiation light perhaps further transmit computer with data, by these data of Computer Analysis.
The embodiments of the invention that Fig. 6 c represents do not need conduction device 140, but it is adjacent with mixer 500 that light-dividing device 143 directly is set.Pass opening 147 from the radiant light of light-dividing device 143 with from the diffuse reflection radiant light of mixture is round, do not need the help of conduction device 140.
In a preferred embodiment, with reference to Fig. 7, with axle 180 closed holes 107.Axle 180 has cavity 182 and first end and second end.Hollow pipe 151 has first end and second end; With first end of sealing device 152 closed hollow pipes that can printing opacity, for example with lens or autoregistration reflection probe 400.As printing opacity locking device 152, the material of manufacturing lens is identical with the material that the transparent locking device 137 of manufacturing is enumerated with lens.The internal diameter of axle 180 is greater than the external diameter of hollow pipe 151, thereby described hollow pipe is removably disposed in the described axle.First end of axle 180 stretches into container 101, and first end that makes axle 180 contacts with mixed material composition at internal tank.Second end of axle 180 is rotatably installed in the pillow block 210 of first ball bearing of aligning and first 's 128 the cross through hole, so axle 180 is aimed at second 111, forms the rotation of level.Horizontal axis of rotation should have enough height corresponding to the hollow pipe of container 101, so that container 101 can be around freely turning round 360 ° by axle 180 and second 111 rotation that forms.Described fibre-optic bundle 140 is arranged in the hollow pipe 151.First end of described fibre-optic bundle 140 is adjacent with lens 152, and perhaps, if with first end of autoregistration reflection probe 400 closed hollow pipes 151, first end of fibre-optic bundle 140 is adjacent with lens 410 so.Hollow pipe 151 removably is arranged in the cavity 182 of axle 180, preferably makes first end of hollow pipe 151 stretch out first end of axle 180, but must not be provided with like this.In order to prevent the bleed cavity 182 of axle 180 of material mixed in container 101, self-lubricating seal 185, for example TEFLON are set sealing between first end of first end of hollow pipe 151 and axle 180
(this is the registration mark of E.I.DuPont de Nemours and Co.).Seal 185 is self lubrication parts, and it can be along with axle 180 revolution, so seal 185 can be around first end revolution of hollow pipe 151, thereby hollow pipe 151 is maintained fixed.
In another preferred embodiment of the present invention,, in this mixing arrangement, also combine and be used for the device 150 of rotary angle position of exploration vessel 101 with reference to Fig. 8.The part example that is used for surveying the device of position of rotation is pure digi-tal formula shaft encoder, pulse coder, optical encoder and analog encoder.The device that last ordered series of numbers is lifted is not exhaustive, and does not get rid of the device that any other may be used for surveying position of rotation.Support 155 and totally be " U " shape, it has first supporting leg and second supporting leg.First supporting leg of support 155 is connected on the device 150 of surveying position of rotation.Second supporting leg of support 155 is connected on second bearing 131.And Fig. 8 has represented the first connecting axle 160a and the second connecting axle 160b.The first connecting axle 160a has first end and second end.The second connecting axle 160b also has first end and second end.The first end level of the first connecting axle 160a and linking to each other with second 111 as the crow flies, thereby the first connecting axle 160a rotates along with second 111.Second end of the first connecting axle 160a is fixedly attached on the shaft coupling 165 flexibly.First end of the second connecting axle 160b also is fixedly attached on the shaft coupling 165 flexibly, and the first end end face of second end of the first connecting axle 160a and the second connecting axle 160b is relative with end face, but is not in contact with one another.Second end of the second connecting axle 160b is connected on the device 150 of surveying position of rotation.Shaft coupling 165 is delivered to the second connecting axle 160b from the first connecting axle 160a with revolving force, thereby makes the first connecting axle 160a and the second connecting axle 160b simultaneously along with second 111 rotation.And, for during second 111 rotation, between the first connecting axle 160a and the second connecting axle 160b, reducing to rotate stress, shaft coupling 165 keeps the first connecting axle 160a and the second connecting axle 160b flexibly and regularly.The device 150 that to survey position of rotation with first group of communication line 170 is connected on the interconnecting device (relay box), makes described interconnecting device and data acquisition and control computer 163 carry out interface with second group of communication line.Second group of communication line is delivered to data acquisition and control computer 163 with information from interconnecting device.In one embodiment, the device 150 of surveying position of rotation is pure digi-tal encoders, by interconnecting device the data signal of pure digi-tal encoder is translated into ASC II number.ASC II number is represented the position of rotation of each device 101 with angle.With second group of communication line ASC II number is sent to data acquisition and control computer 163.With the 3rd group of communication line 173 data acquisition and control computer 163 are connected to light-dividing device 143.When container 101 rotates, survey the rotation of the second connecting axle 160b with the device 150 of surveying position of rotation, device 150 conveys to interconnecting device by first group of communication line 170 with the turned position of container 101.Interconnecting device communicates information to data acquisition and control computer 163 by second group of communication line then.Data acquisition and control computer 163 use control software, for example use Labview
(can be from National Instruments, Austin, Texas 78730 buys), computer makes light-dividing device 143 spectrum data gatherings and surveys a precalculated position synchronised of the device 150 of position of rotation, be converted into data by device 150 position of rotation, collect spectroscopy data so that can connect in the predetermined rotational positions of said container 101 with container 101.Can select the predetermined turned position of one or more containers 101 in order to collect spectroscopic data.By software program, Microsoft Windows for example
(3.1 can buy), and WINSAS in the most computers shop
(from NIRSystems Inc.Silver springs, Maryland buys) makes light-dividing device 143 collect spectroscopic data.By control software program, for example Labview
(DDE is MicrosoftWindow to via Dynamic data Exchange
3.1 intrinsic feature), notice WINSAS
When program begins to collect spectroscopic data.And data acquisition links to each other with described interconnecting device by the 4th group of communication line with control computer 163.Tumbler 216 can artificially be controlled or be controlled by described interconnecting device.When determining that after data acquisition and computer are by the following mathematical analysis that will describe mixed material composition reaches even mixing point, with data acquisition with control the interconnecting device that computer 163 links to each other and make data acquisition control computer 163 open or close tumbler 216.Use WINSAS
The spectroscopic data that software is collected is sent to another software program, for example Instep by DDE software
(can be from Infometrix Inc., Seattle, Washington buys) determines and mixes a little, and with calculating good model analysis spectroscopic data in advance, this model is by the software program that uses, for example Pirouette then
(can be from Infometrin Inc., Seattle, Washington buys) development is come out.Mixed material composition arrive mix a little before, whirligig 216 is stopped at interval in desired time analyze so that from container 101, take out sample, perhaps other any reasons according to user's requirement stop tumbler 216.Recited abovely respectively organize the equipment that communication line is any transmission light or the signal of telecommunication.
Data acquisition of Shi Yonging and control computer are the Toshiba T6400DX with 16Mb random access memory in an embodiment of the present invention, 33MHz, the 486DX machine, still, data acquisition can be any computer with identical or higher function with the control computer.
The initial spectrum of mixture approaches the spectrum of each separate constituent in the mixture most.Along with mixing arrangement begins the compounding substances composition, the spectrum of mixture will not too resemble the spectrum of separate constituent, and more and more be same as the spectrum of the mixture that mixes.Final spectrum will be aggregated to the spectrum of the mixture that mixes.Utilize this analytical method, can measure the various compositions that in mixture, distribute, measure active drug ingredient and nonactive drug ingredient.Therefore, equipment of the present invention can be determined the distributing homogeneity that mixture is total.
As time goes on, by measuring spectrum change in groups, estimate by calculating whether all the components mixes in the mixture.For example, obtained one group of 50 spectrum at interval at one minute.Calculate spectrum 1-5, then 2-6, and 3-7 ... Deng the standard deviation of wavelength.It is maximum that the standard deviation of the spectrum that produces represents which spectral region changes.Along with the prolongation of time, the calculating of the spectrum deviation changing value that each is independent will provide the value of total variation of mixture.When total variation is reduced to constant, think to mix to reach uniformity coefficient.In addition, can work out out computer program with a known homogeneous mixture spectrum.When the spectral mixture that is mixing when known homogeneous mixture spectrum conforms to, finish hybrid process.
In Fig. 1～4,5,6a～6d, the various embodiments of the present invention of expression can be gathered the spectral mixture of material composition in the mixer motion in 7 and 8.Therefore, equipment of the present invention has been cancelled downtime, and shutdown is the major defect that exists in the traditional process.Equipment of the present invention can online detection mixture uniformity coefficient and effectiveness, this feature does not exist in legacy equipment.
Equipment of the present invention can further improve, and to adapt to the situation more than a sniffer, wherein said sniffer is a light-dividing device, but the device of leaded light is housed on it, and is as described above.Equipment of the present invention has a plurality of light-dividing devices, can link to each other with the light-dividing device of same-type, perhaps links to each other with dissimilar light-dividing device.It is improved " V " shape mixer that the typical case who invents is provided with, and by using second hollow shaft, can further improve this mixer, makes it be adapted to two light-dividing devices.As previously described, identical with first the method in described hole that fibre-optic bundle is packed into, second hollow shaft of a conduction device can being packed into.
The conventional mixer 500 of general type can further be improved, and by any position that needs in the mixer wall, a plurality of holes is set, and makes mixer be equipped with a plurality of light-dividing devices.Then, conduction device can be equipped with in each hole in a plurality of holes, and conduction device is connected on the light-dividing device, as Fig. 6 a, and shown in 6b and the 6d, and as mentioned above; Perhaps each hole can be leaned on mutually with light-dividing device, shown in Fig. 6 c, and as mentioned above, or as shown in Fig. 6 a～6d the combining form of embodiment.
Adopting the advantage more than a sniffer of the same type in equipment of the present invention is that the two or more positions in equipment of the present invention obtain the spectral signature of mixture.Embodiments of the invention will guarantee further that the mixture that comes from container mixes.
Can see, under the situation below, be provided with dissimilar sniffers in the equipment of the present invention, in composite medicine, exist various compositions, as mentioned above.Some composition only can enough a kind of types radiant light, as near-infrared radiation light, survey, and other compositions of described composite medicine can only be by the radiant light of another kind of type, rather than infrared light, for example be that visible light detects.In this case, two kinds of light-dividing devices are connected to have lot of advantages on the mixing arrangement.First light-dividing device is a near infrared spectrometer.And second light-dividing device is a visible spectrophotometer.Then, each spectrophotometer will detect the spectral signature of each composition in the composite medicine that it can detect.
In equipment of the present invention, buzzer can also be installed, reach with convenient mixture and mix and effectively during the force, buzzer will send signal to the operator of present device.In addition, when arriving, mixture mixes and effectively during the force, this system can trigger shutdown automatically.
Be appreciated that to the invention is not restricted to previously described embodiment, but under the situation of inventive concept that does not break away from new ideas of the present invention and scope, can produce various as the described changes and improvements form of claims.
Claims (19)
1. a mixing apparatus uses this equipment that material composition is mixed into uniform mixture, and the described compounding substances uniformity coefficient of online detection, and it comprises:
(a) mixing arrangement of the described material composition of mixing; It is characterized in that:
(b) sniffer of the uniformity coefficient of the described mixture of online detection; Described sniffer comprises:
(1) light-dividing device is measured the spectral characteristic of described mixtures of materials with it, and this device has opening, and radiant light can transmit and receive by opening;
(2) conduction device, it is delivered to described mixture with radiant light from described light-dividing device, will reflect then or autoregistration radiation reflected light is delivered to described light-dividing device, and described conduction device is connected on the opening of described light-dividing device;
(c) described mixing arrangement has first bearing and second bearing, and described first bearing has cross through hole, and described second bearing also has cross through hole;
(d) described container is formed by first hollow pipe and second hollow pipe that are communicated with, and described first hollow pipe and second hollow pipe is angled is gathered together makes container V-shaped, and first hollow pipe and second hollow pipe respectively have the wall of flare;
(e) described container is provided with the hole, and the flare wall of described first hollow pipe is passed in this hole;
(f) be provided with the pillow block of first ball bearing of cross through hole, the pillow block of described first ball bearing is arranged between described container and described first bearing, and be connected on described first bearing, the hole of the pillow block of wherein said first ball bearing is aimed at the hole of described first bearing;
(g) be provided with the pillow block of second ball bearing of cross through hole, the pillow block of described second ball bearing is arranged between described container and described second bearing, and be connected on described second bearing, the hole of the pillow block of wherein said second ball bearing is aimed at the hole of described second bearing;
(h) first, first end and second end are arranged, and have through hole;
(i) described transparent sealing device can be selected from transparent window and autoregistration reflection probe, and described transparent sealing device hides and seal the hole of first first end;
(j) second, first end and second end are arranged;
(k) described second first end connects the flare wall of second hollow pipe of described container;
(l) described second second end is rotatably installed in the hole of pillow block of second bearing of aligning and second ball bearing, and second described second end is connected with described whirligig;
(m) described first first end matches with through hole in the described container, and described transparent sealing device inserts in first hollow pipe of described container;
(n) described first second end is rotatably installed in the through hole in the pillow block of first bearing of aligning and first ball bearing, and aims at described second;
(o) described conduction device has first end and second end; And
(p) described conduction device is removably disposed in first the hole, and first end of described conduction device leans against on the described transparent window, and second end of described conduction device is connected on the opening of described light-dividing device.
2. according to the described equipment of claim 1, it is characterized in that:
(a) described mixing arrangement has container;
(b) described container has the hole; And
(c) the transparent sealing device in the described hole of sealing, described sealing device is arranged between described hole and the described sniffer.
3. according to the described equipment of claim 1, it is characterized in that:
(a) described container has rotating shaft;
(b) tumbler, it makes container center on described rotating shaft and rotates, and described whirligig links to each other with the fan of institute container;
(c) on turning cylinder, be provided with the hole;
(d) described conduction device is inserted in the described hole.
4. according to the described equipment of claim 1, it is characterized in that:
(a) described container has a plurality of openings to be used for packing into mixed material composition and draws off the mixture that mixes;
(b) described conduction device is a fibre-optic bundle;
(c) described tumbler is a motor.
5. according to the described equipment of claim 3, it is characterized in that: described mixing arrangement is a V-mixer, spiral blade stirrer or core pattern mixer.
6. according to the described equipment of claim 5, it is characterized in that: described sniffer is near infrared ray spectrophotometer, ultraviolet spectrophotometer, visible spectrophotometer, Raman spectrophotometer or middle infrared (Mid-IR) spectrophotometer.
7. according to the described equipment of claim 1, it is characterized in that:
(a) described mixing arrangement has container;
(b) be provided with the hole in the described container;
(c) axle seals the hole of described container, and axle is a turning cylinder.
8. according to the described equipment of claim 7, it is characterized in that: described sniffer comprises:
(a) light-dividing device is measured the spectral characteristic of described material composition with it, is provided with opening in this device, can transmit and receive radiant light from opening;
(b) conduction device is delivered to mixture with radiant light from light-dividing device with it, then, will reflect or autoregistration radiation reflected light is transmitted to described light-dividing device, and described conduction device is connected with the opening of light-dividing device.
9. according to the described equipment of claim 8, it is characterized in that:
(a) whirligig rotates the axle of container, and described whirligig is connected with container;
(b) described axle is provided with the cavity of perforation;
(c) described conduction device removably inserts in the described cavity.
10. according to the described equipment of claim 9, it is characterized in that:
(a) described mixing arrangement has first bearing and second bearing, and described first bearing has cross through hole, and described second bearing also has cross through hole;
(b) described container is formed by first hollow pipe and second hollow pipe that are communicated with, and described first hollow pipe and second hollow pipe is angled is gathered together makes container V-shaped, and first hollow pipe and second hollow pipe respectively have the wall of flare;
(c) described container is provided with the hole, and the flare wall of described first hollow pipe is passed in this hole;
(d) be provided with the pillow block of first ball bearing of cross through hole, the pillow block of described first ball bearing is arranged between the described container and first bearing, and is connected on first bearing, and the hole of the pillow block of wherein said first ball bearing is aimed at the hole of described first bearing;
(e) be provided with the pillow block of second ball bearing of cross through hole, the pillow block of described second ball bearing is arranged between described container and described second bearing, and be connected on described second bearing, the hole of the pillow block of wherein said second ball bearing is aimed at the hole of described second bearing;
(f) described axle has first end and second end, and is provided with the cavity of perforation;
(g) second, first end and second end are arranged, first described second end connects the flare wall of second hollow pipe in the container, second described second end is installed in the through hole in the pillow block of second bearing of aligning and second ball bearing rotatably, and second described second end connects described tumbler;
(h) first end of described axle matches with the through hole of described container, first end of described axle inserts in first hollow pipe of container, second end of described axle is installed in the hole in the pillow block of first bearing of aligning and first ball bearing rotatably, and aims at second;
(i) hollow pipe has first end and second openend, seals first end with the locking device of light-permeable, and locking device can be selected a kind of from lens and autoregistration reflection probe;
(j) described conduction device has first end and second end, and conduction device is removably disposed in the hollow pipe, and first end of described conduction device leans against on the locking device of described printing opacity, and second end of described conduction device is connected to the opening of described light-dividing device;
(k) described hollow pipe is removably disposed in the cavity of axle, and first end of hollow pipe stretches out from first end of axle;
(l) seal is arranged between hollow pipe and the axle hermetically;
(m) bracing or strutting arrangement has first supporting leg and second supporting leg, and first supporting leg of described bracing or strutting arrangement is connected with second bearing, and second supporting leg of described bracing or strutting arrangement is connected with the device of surveying position of rotation;
(n) first connecting axle has first end and second end, and first end flatly and as the crow flies links to each other with second, and described second end connects shaft coupling regularly and flexibly;
(o) second connecting axle, first end and second end are arranged, first end of described second connecting axle links to each other with shaft coupling regularly and flexibly, and relative with second end of first connecting axle, and second end of described second connecting axle is connected with the device of surveying position of rotation.
11., it is characterized in that according to the described equipment of claim 10:
(a) device of described detection turned position is connected with interconnecting device by first group of communications line;
(b) described interconnecting device is connected with the control computer with data acquisition by second group of communication line;
(c) described data acquisition is connected with described light-dividing device by the 3rd group of communication line with the control computer.
12., it is characterized in that according to the described equipment of claim 11:
(a) in the described container a plurality of openings are arranged so that filling is wanted mixed material composition and drawn off the mixture that mixes;
(b) described conduction device is a fibre-optic bundle;
(c) described tumbler is a motor;
(d) described seal is by TEFLON
Make.
13., it is characterized in that according to the described equipment of claim 12:
(a) described data acquisition is connected with described interconnecting device by the 4th group of communication line with the control computer;
(b) described tumbler is controlled by described relay box.
14. according to the described equipment of claim 9, it is characterized in that: described mixing arrangement is a V-mixer, spiral blade stirrer, or core pattern mixer.
15. according to the described equipment of claim 14, it is characterized in that: described sniffer is near infrared spectrometer, ultraviolet spectrophotometer, visible spectrophotometer, Raman spectrophotometer or middle infrared (Mid-IR) spectrophotometer.
16. one kind is mixed into uniform mixture with material composition, and the method for the described mixture uniformity coefficient of online detection, it comprises:
(a) will mixed material composition pack in the container of mixing apparatus with hole;
(b) mixed material composition;
(c) during hybrid process, spectral characteristic with the online detection mixture of sniffer, so that detect the uniformity coefficient and the effectiveness of described mixture, reach predetermined even mixing point up to the spectral characteristic of homogeneous mixture, perhaps when predetermined spectral characteristic overlaps till.
17. in accordance with the method for claim 16, it is characterized in that: during hybrid process, the online detection of the spectral characteristic of mixture is carried out the detection of the position of rotation of described container synchronously with adopting the device of surveying position of rotation with described sniffer.
18. in accordance with the method for claim 16, it is characterized in that: described sniffer comprises light-dividing device, on light-dividing device, be provided with an opening, radiant light can transmit and receive from opening, one conduction device is delivered to mixture with radiant light from described light-dividing device, and will reflect or autoregistration radiation reflected light is passed light-dividing device back, described conduction device has first end and second end, first end of described conduction device links to each other with the opening of light-dividing device, and its second end links to each other with hole in the described container.
19. it is characterized in that in accordance with the method for claim 16; Described sniffer comprises light-dividing device, is provided with an opening on light-dividing device, and radiant light can be launched from opening, and can receive from opening from mixture reflection or autoregistration radiation reflected light, and the opening of described sniffer leans on mutually with the hole of container.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US8523093A | 1993-06-29 | 1993-06-29 | |
| US085,230 | 1993-06-29 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1100002A CN1100002A (en) | 1995-03-15 |
| CN1062490C true CN1062490C (en) | 2001-02-28 |
Family
ID=22190294
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN94107246A Expired - Fee Related CN1062490C (en) | 1993-06-29 | 1994-06-28 | Apparatus for mixing and detecting on-line homogeneity |
Country Status (12)
| Country | Link |
|---|---|
| EP (1) | EP0631810B1 (en) |
| JP (1) | JP2650619B2 (en) |
| KR (1) | KR0162110B1 (en) |
| CN (1) | CN1062490C (en) |
| AT (1) | ATE157905T1 (en) |
| AU (1) | AU660875B2 (en) |
| BR (1) | BR9402570A (en) |
| CA (1) | CA2126826C (en) |
| DE (1) | DE69405483T2 (en) |
| DK (1) | DK0631810T3 (en) |
| ES (1) | ES2106449T3 (en) |
| GR (1) | GR3025143T3 (en) |
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| CN114471275A (en) * | 2021-12-30 | 2022-05-13 | 西安近代化学研究所 | Mixing roller, medicine mixing detection equipment, medicine mixing detection method and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US2514126A (en) * | 1949-12-08 | 1950-07-04 | Patterson Kelley Co | Blending or mixing apparatus |
| SU1402856A1 (en) * | 1985-12-13 | 1988-06-15 | Ивановский государственный университет | Apparatus for preparing thermochromatic compounds and for measuring chromatotemperature characteristics thereof |
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| US4361404A (en) * | 1981-04-06 | 1982-11-30 | Pettibone Corporation | Mixing equipment and agitator therefor for use with granular material and method of producing prepared granular material |
| DE3337403A1 (en) * | 1983-10-14 | 1985-05-02 | Seyd Fertigbeton Berlin, Zweigniederlassung der Readymix Transportbeton GmbH, 4030 Ratingen | Process and apparatus for preparing mixtures |
| DE3412620A1 (en) * | 1984-04-04 | 1985-10-17 | Basf Ag, 6700 Ludwigshafen | LASER OPTICAL ARRANGEMENT FOR MEASURING THE DEGREE OF DISPERSION IN FLOWING SYSTEMS |
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1994
- 1994-06-03 EP EP94304010A patent/EP0631810B1/en not_active Expired - Lifetime
- 1994-06-03 ES ES94304010T patent/ES2106449T3/en not_active Expired - Lifetime
- 1994-06-03 DE DE69405483T patent/DE69405483T2/en not_active Expired - Fee Related
- 1994-06-03 DK DK94304010.5T patent/DK0631810T3/en active
- 1994-06-03 AT AT94304010T patent/ATE157905T1/en not_active IP Right Cessation
- 1994-06-23 JP JP6141356A patent/JP2650619B2/en not_active Expired - Fee Related
- 1994-06-27 AU AU65997/94A patent/AU660875B2/en not_active Ceased
- 1994-06-27 CA CA002126826A patent/CA2126826C/en not_active Expired - Fee Related
- 1994-06-28 BR BR9402570A patent/BR9402570A/en not_active Application Discontinuation
- 1994-06-28 KR KR1019940014952A patent/KR0162110B1/en not_active IP Right Cessation
- 1994-06-28 CN CN94107246A patent/CN1062490C/en not_active Expired - Fee Related
-
1997
- 1997-10-22 GR GR970402775T patent/GR3025143T3/en unknown
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2514126A (en) * | 1949-12-08 | 1950-07-04 | Patterson Kelley Co | Blending or mixing apparatus |
| SU1402856A1 (en) * | 1985-12-13 | 1988-06-15 | Ивановский государственный университет | Apparatus for preparing thermochromatic compounds and for measuring chromatotemperature characteristics thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0768146A (en) | 1995-03-14 |
| ATE157905T1 (en) | 1997-09-15 |
| DK0631810T3 (en) | 1997-10-20 |
| DE69405483T2 (en) | 1998-01-15 |
| GR3025143T3 (en) | 1998-02-27 |
| JP2650619B2 (en) | 1997-09-03 |
| EP0631810A1 (en) | 1995-01-04 |
| EP0631810B1 (en) | 1997-09-10 |
| CA2126826A1 (en) | 1994-12-30 |
| AU6599794A (en) | 1995-01-27 |
| CN1100002A (en) | 1995-03-15 |
| ES2106449T3 (en) | 1997-11-01 |
| KR950001299A (en) | 1995-01-03 |
| AU660875B2 (en) | 1995-07-06 |
| BR9402570A (en) | 1995-04-11 |
| DE69405483D1 (en) | 1997-10-16 |
| KR0162110B1 (en) | 1998-11-16 |
| CA2126826C (en) | 1999-02-23 |
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