Device for photometric analysis of liquid in centrifuge
专利摘要:
1520918 Rotary photometric analyzers F HOFFMANN-LA ROCHE & CO AG 26 Nov 1975 [29 Nov 1974] 48679/75 Heading G1A In a rotary photometric analyzer, tubular sample holders can be inserted into radial apertures in the rotor, and are investigated by light which passes along the holders to a detector on the rotor axis. The holders are shown in Fig. 7, and comprise a body 24 with a removable cap 25. A reagent can be placed in the body before the cap is attached, and then a sample is placed in the cap using a hollow needle; surface tension prevents contact between the sample and the reagent at this time. The holders are then inserted into the rotor 11, Fig. 2, and the rotor is attached to the analyzer by clips 10. Following rotation to cause preliminary mixing, the rotor is oscillated to produce thorough mixing; the rotor is then rotated, the caps are removed by raising a disc 26, and a lamp 10 is activated. A photo-multiplier 23 is lowered to an axial position, and with the aid of rotor timing signals a photometric measurement is made on each holder. A thermostatically controlled reservoir of water is provided, and on rotation some of the water is forced to occupy a region 16 around the bodies of the holders. 公开号:SU873896A3 申请号:SU752193204 申请日:1975-11-27 公开日:1981-10-15 发明作者:Ревиллет Жорж;Занц Мануель;Фаркас Рудольф 申请人:Ф.Гоффманн-Ля Рош И Ко Аг(Фирма); IPC主号:
专利说明:
a permeable material, the open and closed ends of the container thus forming the translucent windows of the cuvette. In addition, the device for temperature stabilization includes a bath for receiving liquid with a given temperature, located under the rotor, and a separator immersed in the liquid and having side walls extending upward, and the rotor is fixed on the separator and contains at least one thermally stabilized chamber in which there are cuvettes having an opening for draining the liquid into the bath. FIG. 1 shows the device a general view; in fig. 2 is a block diagram of a control device; 3 a device in the analysis phase, partial view; in fig. 4-10 - operation of the device. one. , . The device has a housing 1, subdivided into two chambers 2, nd 3, one above the other, with a horizontal pier 4. The upper chamber is a bathroom chamber, the lower chamber 3 includes a constant-current electric motor 5 with a tubing 1 "(shaft 6 passing through the pier 4. Shaft b / lits in sleeve 7, attached to wall 4, with the upper end of the sleeve equipped with a bearing 8 for shaft 6. The upper end of shaft b extends beyond sleeve 7 and is flow-through connected to the shaft by a curved coaxial shaft, b separator i with a circular cross-section or a single whole, the separator 9 extending towards the bottom of the bath and having the shape of a truncated cone, the truncated end of which is directed downwards. The upper edge of the separator 9 is surrounded by a series of elastic upwardly shaped brackets formed by elastic levers 10 that press radially towards the axis of the separator 9. These elastic skins are designed to fix the rotor 11, which serves for analysis. For this purpose, the rotor 11 is equipped with a mounting flange 12, which goes into the bias, pushing the levers 10, so that The axial pressure of the rotor 11 is pressed against the separator 9. This mounting flange 12 has an outside thickening that engages under the internal thickening 13 of each lever 10. The cover of the separator 9 connected to the shaft 6 is equipped with a number of holes 14, and its bottom forms a 7 with a sleeve 7: oz. hole 15. From the flange 12, the rotor 11 expands. This expansion part ends with a vertical annular wall, followed by a horizontal and Ytora vertical annular walls, so that an annular chamber 1 is formed 6 for receiving the cuvette 17.. Ring section 18, stretching from. parallel to the rotor 11 above the expanding part of the latter, forms together with this expanding part a channel between the openings 14 of the separator 9 and the annular chamber 16. The annular part 18 is attached to the rotor 11 by means of vertical pipes 19 passing through the expanding part of the rotor 11. The housing 1 is equipped with a window 20, the axis of which is coplanar with the longitudinal axis of the cuvette 17. Outside the housing 1, a light source 21 is installed, which includes a glow lamp and a lens, so that the output light beam passes coaxially with the window axis 20. Photomultiplier (PMT) 22 y mounted on the end of a lever 23 installed in a vertical plane with the possibility of rotation around an axis located Vertically on the axis of the window 20. Each cell 17 for loading and measuring the transmission is delivered in two parts. One part is an analysis tank 24, the other is a cover 25. The analysis device is also equipped with a mechanism for ejecting covers 25. This mechanism has a plate 26 which is integral with the rod 27 passing through the axial hole of the shaft 6. The rod 27 projects from under dvigated 5 and bears 28c outer ring groove. One end of the lever 29 extends into the groove of the washer 28, while the other end of the lever 29 is mounted in the bearings of the electromagnet core 30. Moreover, the lever 29 is supported by bearings between the two cylinders on a horizontal axis firmly connected to the housing 1. In a resting state ( figure 1 is shown by the dotted line) plate. 26 forms a support plane for the covers 25, while in the ejection position (indicated by dotted lines) the plate 26 separates the covers 25 and the analysis tanks 24. The bottom of the bath is equipped with a heater 31, while the side wall is equipped with a cooling jacket 32 connected for example, to a source of cold water (not shown). Two temperature probes 33 and 34 are provided in the bath and at the exit of pipes 19. The possibility of rotating the photomultiplier 22 allows the lever 23 to be driven into two fixed positions: lowered, with which the photomultiplier 22 is on the axis of the light beam, and photomultiplier 22 is removed from the rotor 11 (figure 1). For this purpose, the lever 23 osngide gear sector 35, which is engaged with the screw 36, provided on the shaft, driven by the engine 37, Monitoring and adjusting temperatures located in or in the fluid chamber, as well as controlling various mechanisms, we offer carried out using a control device (Fig. 2). The block diagram is equipped with an automatic tracking control circuit 38 of the analysis process, input 39 of which is connected to a switch of type of work (not shown), and outputs 40-45 of which are provided for controlling individual organs and devices. Output 40 is provided at the input of the recorder of measurement results 46 , outputs 41 and 42 at regulator amplifier 47 for engine 5, with output 41 supplying constant current 47 to regulator 47, and output 42 giving alternating current to amplifier. The output 44 controls the amplification element 48 connected to the electromagnet 30, the output 43 of the amplifier 49 for the engine 37, the output 45 controls the control unit 50 of the fluid temperature in chamber 2. The control unit 50 receives from the amplifier 51 a signal corresponding to the average value temperatures recorded by the probes 33 and 34, and in accordance with the temperature control circuit 35 installed or shown at the output of the temperature control, the heating amplifier 52 for the heater (radiator) 31 or the cooling amplifier 53 for the jacket 32 so that the average value eratur recorded by the probes 33 and 34, stabilize to a value appropriate illustrated servo control circuit 38 temperature. The rotor shaft 6, which is at the same time the driving shaft of the engine 5, is firmly connected to two lanes 54 and 55, which serve to generate pulses in two photodetectors. 56 and 57, located at the inputs of the amplifier 58, the outputs of which lead to the recorder of measurement results 46 These photodetectors 56 and 57 send synchronization signals to the recorder of measurement results 46. For this, the first track interacting with the photodetector 56 has a mark for each cuvette 17, while the second track interacting with the photo detector 57 has a mark for each rotation of the rotor 11, as a result of which the first cuvette 17 and the others can be identified . This identification is carried out using measurement results set in the recorder 46, which after each rotation returns via track 55 to the zero position and then counting each pulse Formed during the passage of each mark track 54 past the photo detector 56. A stabilized source is provided for the incandescent light source 21 current 59. Power 22 is provided by high voltage source 60. Additionally, the PMT 22 is connected to the input of the amplifier 61, the output of which is connected to the recorder input of measurement results 46. Based on the synchronization signals from the photo detector 56, the output 62 of the recorder of measurement results 46 at the time of each sample passes the PMT 22, only results related to individual samples are issued measurements, with each measurement result being related to an exactly determined sample; the second track 55 in this way gives a signal that the first sample passes at each turn of the rotor 11. In FIG. 4 shows a front view of the rotor removed from the device in the load phase. FIG. Figure 5 shows a cuvette 17 containing a container for analysis 24 formed by a cylindrical pipe, bent and closed at one end with a flat bottom arranged vertically on the longitudinal axis of the pipe. The container for analysis is made of a light transmitting material, such as glass or transparent synthetic material. Vos1 “{Augene is also an option in which only the bottom passes the light, and which is connected to the pipe. In any case, the bottom is preferably offset relative to the end of the pipe back. The other part of the cuvette 17 is a cover 25 formed by a second pipe closed at one end, the other end of which has an end section with an outer diameter, corresponding to the inside diameter of the open end of the first pipe or accordingly, an analysis tank 24 (Fig. 7). The end portion that enters the first pipe ends with a collar (Fig. 7), which limits the opening of the cover 25 into the tank 24 for ana. Liza. The cap is made of a soft material through which a metal needle, such as an injection needle, can pass through the floor. The cover should not be transparent. Capacity 24 for analysis and cover. 25 is about the same. Figure 6 shows an assay tank 24, on the bottom of which with a pipette, reactants are applied if it is a liquid (only the end of the pipette is shown, which gives the reagent). It is also possible to use solid reagents, for example, in. lyophilized form. The cuvettes can be prepared for delivery together with the necessary reagent filled in them already in the manufacture of the latter. In this case, when the reagent is already contained in the cuvette 17 in one form or another, the lid 25 is inserted into the opening of the analysis tank 24. Thereafter, the rotor 11 is loaded by inserting the cuvette 17 outside and then pressing them towards the axis of the rotor 11 in the position shown in FIG. Seal 63 is used to seal chamber 16. When the cuvette 17 is inserted and properly positioned, the previously used test container 24 is pushed out (Fig. 4). The arrangement of the cuvette 17 on the rotor 11 is preferably carried out before the rotor 11 is mounted on the separator 9. Which is an advantage, since several rotors can be prepared in advance without decommissioning the entire analyzing device. When loading samples, the rotor can be mounted on the separator 9. In the case of mounting the rotor 11 on the separator 9, the cover 25 is supported on the plate 26 (Fig.7). Thus, it is possible to pierce the caps 25 with two hollow needles 64 and 65, with the needle 64 being the end of a pipette (not shown) giving out the reagent, while the pipette 65 is only an outlet. A sample of the liquid 66 to be analyzed is introduced through a needle and then with a certain amount of water for dilution. The insertion of the sample with a needle, which pierces the wall of the lid 25, is characterized in that the tip of the needle is cleaned from the outside, and internal cleaning occurs when water is introduced for dilution. In this case, the water ensures that the sample does not flow to the cuvette 17. The inner diameter of the cap 25 is chosen so that, due to the surface tension of the injected fluid, a meniscus is formed, which prevents the ingress of fluid into the analysis tank 24. Thus, all the sample and all the water is in the cap 25, so that the volume of this tank is generally 24 dl analysis. Immediately upon loading all the samples into the cuvettes 17, the liquids are overloaded by short centrifugation into the analysis tank 24, where they come in contact with liquid or lyophilized reagents (Fig. 9). Then the solution is mixed and homogenized. For this, the following control circuit 38 (Fig. 2) sends a signal to Eochrd 42, so that the amplifier / regulator 47 begins to feed the motor 5 with alternating currents. Since motor 5 is a direct current motor, its picking with alternating current causes the shaft b to oscillate at a frequency corresponding to the frequency of the alternating current fed by the motor -5. Oscillatory the movement of the rotor 11 causes a strong disturbance of liquids or liquids and solid reagents inside the cuvette 17 (FIG. 9). Because of this disturbance, the liquids are mixed and / or the solid reagent is dissolved in the liquid. After that, the motor 5 is supplied with a constant current for centrifuging the solution, and the rotor rotates at a speed of about 10QO rpm. Centrifugation is intended to degass the solution by removing bubbles that are lighter than liquid. Bubbles cause perturbation of the fluid. Centrifugation also serves to transfer the entire volume of the solution to the test container 24. The covers 25 are then discharged by activating the electromagnet 30, which raises the plate 26 with the lever 29. The analysis tank 24 is prepared for carrying out the process of optical analysis of the solution contained therein. For this, a water circulation system is provided for adjusting the temperature, so that during the measurement process the temperature of the solution can be maintained at a certain value. A certain amount of water is introduced into chamber 2 or, respectively, a bath. Through the annular opening 15 (Fig. 1 and 2) this water penetrates into the separator 9. Centrifugal force acts on the water in separator 9. during its rotation, so that due to the curved taper of this separator and its internal truncated conical form, a layer is formed water. This water is discharged through the holes 14, entering the rotor channel 11, which is formed between the expanding part of the latter and the ring part 18, and then enters the annular chamber 16, through which the containers 24 pass for analysis. Excess water is continuously fed into chamber 1b and fed back into chamber 2 through branch pipes 19. Due to the centrifugal force that causes circulation in this circle, water is thrown out of the outlet of these pipes 19 to the outside. Thus, the temperature probe 34, which is attached outside the outlet end of the pipes 19 and below it, receives a flow of water from these pipes, so that the probe can measure the temperature of the water flow. Temperature-controlled circulation of water can be used for other areas, besides centrifugation, a rotor must be available.
权利要求:
Claims (3) [1] For photometric analysis of the liquids contained in each of the containers 24 for analyzing fluids, the following control circuit 38 sends to the amplifier 49, which drives the motor 37, a signal so that the screw 36 of the motor 37 is lowered, the lever 47 with the photomultiplier tube 22 reaches the device shown in FIG. . 3 positions Each mark of the first detector of the photodetector 54 causes the formation of a fixed sign at the output of the recorder 46 of measurement results. The width and position of the marks on the first track 54 of the photodetector are chosen so that the measured value is given at the moment when the longitudinal axis of the tube-shaped capacitance 24 for analysis coincides with the axis of the light beam emanating from the light source 21 and entering into the photomultiplier 22 V proposed the device for analyzing the length of the liquid layer through which the light beam passes is proportional to the volume of this solution in the tank 24 –dl of analysis. Accuracy is no longer dependent on the amount of reagents contained in the liquid. Accuracy now depends only on the amount of sample and the diameter of the tubular container 24 for analysis. The distance between the incandescent light source 21 and the PMT 22 in the lowered position of the latter is significantly reduced relative to the total length of the cuvette 17 due to the ejection of the cover 25. The rotor 11 can be reused for loading purposes from the device. For each individual analysis, only the cuvettes 17 are replaced. Since they are closed, they can preferably be additionally loaded with lyophilized reagents or fluids suitable for this analysis. The operator performing the analysis, no longer has to perform the techniques of FIGS. 5 and 6, he can (FIG. 4) load the rotor directly and then work in accordance with FIG. 7-10. The operator can install several rotors 11 on the same device for analysis, which means that he can pre-charge several rotors without taking the entire installation out of operation. In addition, an advantage of the proposed device is a method of stabilizing the temperature with a water bath, surrounding the container 24 for analysis during the analysis process and continuously renewable. The temperature of this bath is constantly monitored, updated. occurs at each turn of the rotor 11. The concept of the cuvette 17 for loading and for analysis plays an important role; The cuvette 17 is so cheap that it can be thrown away after use. In this case, it is possible to pierce the cover 25, which is a storage tank before mixing the sample with the reagent. In addition, the cover prevents leakage of fluid during the oscillatory movement of the rotor 11 (Fig.9). It is easy to remove the cap when the mixing and homogenization of the solution is completed. Due to the displacement of the bottom of the container 24 for analysis, relative to the end of the tube, the window formed by the bottom, through which the light beam enters or leaves (depending on whether the light source is inside or outside the rotor), is protected from dirt and traces during operations and cause a decrease in light transmission and thereby measurement accuracy. Claim 1. A device for photometric analysis of liquids in a centrifuge, comprising a housing, a rotor with a rotating drive, provided with openings with cuvettes in them having two translucent windows arranged radially to the rotor axis on the same angular angle. spaced from each other, and clamps, a light source and a photodetector, characterized in that, in order to improve the accuracy of the analysis, the device is equipped with a rotor angular oscillation drive, a drive switch and a device located under the rotor mperaturnoy stabilization, and the optical axis of the light beam emitted by the source of light is directed radially to the rotor axis of rotation and lying in the path described by the longitudinal axis of each cell. 2. A device according to Claim 1, characterized in that one window of each cell is located vertically to its radially oriented longitudinal axis. 3. The device according to Claim 1, about T l is implied by the fact that each cuvette contains a tubular container, one end of which is open and the other is covered with a transparent material, with the container open and closed thus forming the transparent windows of the cuvette. 4. The device according to claim 1, wherein the device for temperature stabilization includes a bath for receiving a liquid with a predetermined temperature, located under the rotor, and a separator immersed in the liquid and having side walls extending upwards, and the rotor is fixed on the separator and contains at least one thermally stabilized chamber, in which there are cuvettes having an opening for draining the liquid into the bath. Sources of information taken into account in the examination 1. Application 2257069, cl. 42 e 3/08, published, 1973. [2] 2. Forward Germany No. 2336619, cl. 42 e 3/08, publ. 21.02.74, [3] 3. The patent of Great Britain 1357231, cl. 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同族专利:
公开号 | 公开日 SE7513329L|1976-05-30| FR2292973A1|1976-06-25| CH589319A5|1977-06-30| JPS552579B2|1980-01-21| NL7513944A|1976-06-01| DK145729B|1983-02-07| NL173889C|1984-03-16| DK536075A|1976-05-29| DE2560001B1|1979-03-29| AU8690275A|1977-06-02| DK145729C|1983-07-25| NL173889B|1983-10-17| CA1048294A|1979-02-13| GB1520918A|1978-08-09| FR2292973B1|1980-09-19| DE2552833A1|1976-08-12| JPS5178287A|1976-07-07| SE414551B|1980-08-04| DE2552833B2|1979-02-22| US3999862A|1976-12-28| IT1049794B|1981-02-10| DE2552833C3|1979-10-18| DE2560001C2|1979-11-22| DD122723A5|1976-10-20|
引用文献:
公开号 | 申请日 | 公开日 | 申请人 | 专利标题 EA002403B1|1997-02-28|2002-04-25|Бурштейн Текнолоджис, Инк.|Laboratory in a disk|NL109202C|1959-11-20| CH552208A|1971-04-27|1974-07-31|Max Planck Gesellschaft|DEVICE FOR OPTICAL EVALUATION OF SEVERAL LIQUID SAMPLES ACCUMULATING AT THE SAME TIME| US3844662A|1971-07-13|1974-10-29|Froreich A Von|Sedimentation instrument for body fluids and method of microscopic examination of the sediment|WO1982000360A1|1980-07-24|1982-02-04|Oy Labsystems|Method and equipment for the measurement of properties of aliquid| JPH0115012B2|1981-02-10|1989-03-15|Olympus Optical Co| US4452902A|1981-11-19|1984-06-05|Labsystems Oy|Method and equipment for the measurement of properties of a liquid| IT1151524B|1982-03-25|1986-12-24|Dideco Spa|DEVICE TO OBTAIN PLASMAPHERESIS BY CENTRIFUGATION| JPS5930923A|1982-08-12|1984-02-18|Toyoda Autom Loom Works Ltd|Ending in open end fine spinning frame| US4632908A|1984-05-03|1986-12-30|Abbott Laboratories|Heating system for rotating members|
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申请号 | 申请日 | 专利标题 CH1585974A|CH589319A5|1974-11-29|1974-11-29| 相关专利
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