US3798459A - Compact dynamic multistation photometer utilizing disposable cuvette rotor - Google Patents

Abstract

A compact analytical photometer of the rotary cuvette type designed to use small disposable cuvette rotors. A power driven cuvette rotor holder having a generally flat, circular configuration is provided with an integral, upstanding, annular lip for receiving, in an easily insertable and removable fashion, small disposable cuvette rotors. A series of axially extending apertures are disposed in a circular array through the rotor holder in axial alignment with respective cuvettes in the rotor to permit light to be transmitted through the cuvettes as the rotor holder and cuvette rotor rotate between a stationary light source and photodetector. Additional apertures extend through the rotor holder near its periphery to permit light passage through the rotor holder for rotor and cuvette synchronization purposes. Movable rotor and cuvette synchronization detectors are positioned along the periphery of the rotor holder for generating signals which are used to synchronize the photometer output with a computer and to provide rotor speed control. Rapid deceleration of the rotor holder and rotor for sample mixing purposes is accomplished by braking means engaging the rotor holder drive shaft.

Description

United StatesPatent 1 Anderson et, al. v

[ 1 COMPACT DYNAMIC MULTISTATION PHOTOMETER UTILIZING DISPOSABLE CUVETTE ROTOR [75] Inventors: Norman G. Anderson, Oak Ridge;

Carl A. Burtis, Knoxville; Wayne F. Johnson, Loudon; James C. Mailen; Charles D. Scott, both of Oak Ridge, all of Tenn.

[73] Assignee: The United States of America as represented by the United States Atomic Energy Commission, Washington, DC.

22 Filed: Oct. 6,1972

[21] Appl. No.: 295,780

52 us. Cl. 250/218, 250/106 R 3.215.849 11/1965 Golden 250/218 Primary Examiner-Harold A. Dixon Attorney, Agent, or Firm-John A. I-Ioran 1 1 Mar. 19, 1974 57 ABSTRACT A compact analytical photometer of the rotary cuvette type designed to use small disposable cuvette rotors. A power driven cuvette rotor holder having a generally flat, circular configuration is provided with an integral, upstanding, annular lip for receiving, in an easily insertable and removable fashion. small disposable cuvette rotors. A series of axially extending apertures are disposed in a circular array through the rotor holder in axial alignment with respective cuvettes in the rotor to permit light to be transmitted through the cuvettes as the rotor holder and cuvette rotor rotate between a stationary light source and photodetector. Additional apertures extend through the rotor holder near its periphery to permit light passage through the rotor holder for rotor and cuvette synchronization purposes. Movable rotor and cuvette synchronization detectors are positioned along the periphery of the rotor holder for generating signals which are used to synchronize the photometer output with a computer and to provide rotor speed control. Rapid deceleration of the rotor holder and rotor for sample mixing purposes is accomplished by braking means engaging the rotor holder drive shaft.

9 Claims, 6 Drawing Figures PATENTEUMR 1 9 i974 SHEET 2 [IF 4 PATENTEDHAR 1 9 m4 3798.459

v sum u 0F 4 52wxwmmw 51 wi 11 BACKGROUND OF THE INVENTION The invention described herein relates generally to photometers of the rotary cuvette type and more particularly to a compact photometer utilizing disposable cuvette rotors. It was made in the course of, or under, a contract with the U. S. Atomic Energy Commission.

A representative fast photometric analyzerof the rotary cuvette type is described in U. S. Pat. No. 3,555,284, issued to common assignee on Jan. 12, 1971. In the fast analyzer described in that patent, centrifugal force is used to transfer and mix samples and reagents in a mul ti-cuvette rotor. A stationary photometer scans the cuvettes during rotationsThe signals thus generated are evaluated by a computer, allowing the reactions taking placein'the respective cuvettes to be observed as they occur. Since all reactions are initiated simultaneously and are coupled with the continuous referencing of the spectrophotometric system of the analyzer, errors due to the electronic, mechanical, or chemical drift are minimized.

Although analyzers built in accordance with the aforementioned patent have been highly successful in that they operate with relatively low sample and reagent volume requirements, have demonstrated a high sample analysis rate, and are subject to automated operation, further improvement isdesirable. For example, the cuvette rotor described in that patent is a relatively large and complex structure of glass and polytetrafluorethylene rings sandwiched together and secured between a steel rotorbody and bolted flange ring. Such rotors are expensive and must be cleaned between analytical runs to avoid contamination of subsequent samples. correspondingly large cabinetry, drive motors, etc., must be used with the rotor with the result that the fast analyzer is not truly portable and requires a rela tively large amountof valuable laboratory space.

A further reduction in sample and reagent volume requirements is also desirable. Savings of expensive reagents would result from such a reduction in volume requirements. Also, the analyzer could be used in testing applications where it is difficult to obtain a sufficient volume of sample for analysis. For example, a greatly reduced sample volume requirement would facilitate operation in a pediatric laboratory where several analyses could be performed on the small volume of blood obtained from the finger or toe-prick of a newborn infant.

It is also desirable to make the cuvette rotors disposable to avoid the possibility of sample contamination and to permit preloading of standardized reagents. Such disposability would require the cuvette rotor to be simple and inexpensive to construct and easily inserted Other objects of the invention will be apparent upon examination of the following description of the invention and the appended drawings.

SUMMARY OF THE INVENTION In accordance with the invention, a compact analytical photometer of the rotary cuvette type is provided which is especially designed to use small disposable cuvette rotors. A power driven cuvette rotor holder having a generally flat, circular configuration is provided with an integral, upstanding, annular lip for receiving, in an easily insertable and removable fashion, small disposable cuvette rotors. A circular array of axially extending apertures extend through the rotor holder in axial alignment with respective cuvettes in the rotor to permit light to be transmitted axially through the cuvettes as the cuvette rotor and rotor holder rotate between a stationary light source and photodetector. Synchronization apertures extend through the rotor holder near its periphery to permit light passage through the holder and rotor for sample mixing purposes is accomplished by braking means engaging the rotor holder drive'shaft.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a top plan view, partially cut away, of a photometer made in accordance wtih the invention.

FIG. 2 is a vertical section view of the photometer of FIG. 1.

FIG. 3 is an enlarged plan view showing the static loading side of a disposable cuvette rotor for use in the photometer of FIGS. 1 and 2. l

FIG. 4 is an enlarged isometric view, sectioned and partially cut away, further illustrating the static loading side of the cuvette rotor of FIG. 3.

FIG. 5 is an enlarged plan view, showing the dynamic loading side of the cuvette rotor of FIGS. 3 and 4.

FIG. 6 is anenlarged isometric view, sectioned and DETAILED DESCRIPTION OF PREFERRED EMBODIMENT Referring now to the drawings, initially to FIGS. 1 and 2, a compact photometric analyzer is shown in a top plan view and in vertical section, respectively. Rotatably mounted on top of a small, generally rectangular, sheet metal cabinet I is a power-drivencuvette rotor holder 2 having a flat, plate-like, circular base 3 with an integral, upstanding, annular lip or rim 4 for receiving and retaining adisposable cuvette rotor 5. Two or more retaining pins 6 (only one shown) are fixed torotor holder 2 within the confines of lip 4 and engage mating recesses incuvette rotor 5.Pins 6 prevent relative rotation of the cuvette rotor and rotor holder during operation of the analyzer under conditions of high rotary acceleration, while permitting relatively effortless manual insertion or removal of the cuvette rotor under static conditions. A circular array of apertures 7 extends through base 3 of the rotorholder in axial register with respectivesample analysis cuvettes 8 withincuvette rotor 5.

A movable photometric light source 9 provides a light beam of constant intensity interesectingrotor 5 at a point corresponding to the radial positions ofsample analysis cuvettes 8. The light beam from source 9, indicated by a broken line in FIG. 2, is aligned in such a manner so as to be transmitted through each aperture 7 andcuvette 8 as they are rotated through the beam. Light source 9 includes a quartz-iodineincandescent lamp 10, a finned lamp housing 11, and a set of focusing lenses l2.Knob 14 is attached to housing 11 to facilitate positioning of the lamp housing during or immediately following analyzer operation when the housing is at an elevated temperature due to the heat generated bylamp 10.

Anelectronic photodetector 15 is disposed belowrotor holder 2 and the top ofcabinet 1 where it is positioned to receive light transmitted throughsample analysis cuvettes 8 as they pass between the photodetector and light source 9.Photodetector 15 comprises a photomultiplier tube which provides an output signal proportional to the intensity of the light which it receives.

lnterposed between photodetector l5 androtor holder 2 is amovable filter holder 16 which permits the selective positioning of one of a plurality of interference filters 17 in the path of the light transmitted throughcuvettes 8.Filter holder 16 is fixed, by means of a set screw, to vertically extending shaft 18 which is rotatably supported by a roller thrust bearing 19 fixed within the base offixture 20.Fixture 20, which is rigidly fixed tocabinet 1, is slotted to permit angular displacement offilter holder 16 within the limits necessary to align any of filters 17 abovephotodetector 15. Afilter selector knob 22 is fixed to the top end of shaft 18 to enable an operator to manually select the filter desired.

As shown in FIG. 2, a thin-walled tube 23 serve as a mounting post for movable light source 9. Tube 23 is attached to and supported within fixture by means of a set screw and extends coaxially with shaft 18. R0- tatably engagingtube 23 immediately abovefixture 20 is afirst sleeve 24. Asecond sleeve 25, which serves as a mounting fixture for lamp housing 11, is fixed tofirst sleeve 24 by set screw means and is rotatable therewith.First sleeve 24 is provided with depressions 26 (only one shown) which are engaged by spring loadeddetent 27 when the light source is in operating position as shown or swung away 90 for rotor replacement as indicated in phantom in FIG. 1. Radial adjustment of the light source to align it with the cuvettes is accomplished by loosening set screw 28 and sliding adjustment sleeve 29 within opening 30 insecond sleeve 25. Anindicator plate 32, which together withfilter selector knob 22 shows the position offilter holder 16, is fixed to the top oftube 23 by set screw means. A spring loaded detent inknob 22 engages depressions inindicator plate 32 to provide positive positioning of the filter holder.

Fixed to the bottom of shaft 18 is anindex wheel 33 engaging amicro switch 34. Rotation of shaft 13 during a filter selection operation causes a corresponding rotation of the index wheel and activation of the micro switch. This causes a different preset potentiometer to be connected into the photodetector high voltage supply circuit in order to maintain a constant signal from a reference cuvette filled with a water blank. A different preset potentiometer is used for each interference filter 17 infilter holder 16.

An alternative method for maintaininga constant output from the photodetector is described in copending application of common assignee Ser. No. 289,906 filed Sept. 18, 1972. According to that method, the signal level from the reference cuvette is compared with a preset desired level and adjustments to the high voltage photodetector supply made as needed by appropriate control circuitry to maintain the desired output. Drift in the photomultiplier tube and associated circuitry is also compensated for.

The rotor holder and cuvette rotor are rotatably driven by a combination servomotor-tachometer generator 35. Amagnetic brake 36 acts on the rotor holder drive shaft 37 to provide rapid braking action to the cuvette rotor to enhance sample and reagent mixing in the cuvettes. Braking from a rotor speed of about 2,000 rpm to a standstill in less than 1 second has been achieved usingmagnetic brake 36.

Synchronization signals are provided by rotor andcuvette synchronization detectors 38 and 39, respectively. A similarly constructeddetector 40 provides a signal for activating the automatic photomultiplier voltage control (not shown). Signals are generated when appropriately spaced apertures in the rotor holder pass through the detectors and allow light from a small tungstenincandescent lamp 41 disposed in the detector above the rotor holder to reach aphotodiode 42 disposed in the detector below the cuvette holder.Detector 39, shown in section in FIG. 2, is representative of all three detectors. Acircular track 44 for positioning the detectors partially encirclescuvette holder 2. Synchronization may be adjusted by moving the detectors alongtrack 44 until proper synchronization is obtained and then securing them to the cabinet with locking screws.

As shown in FIG. 1, a circular array ofsynchronization apertures 45 is provided inrotor holder 2 to generate a signal indetector 39 just after each cuvette passes between light source 9 andphotodetector 15.Single apertures 46 and 47 cause signals to be generated indetectors 38 and 40, respectively, on each revolution of the rotor holder.

The temperature ofcuvette rotor 5 is monitored by means of a thermistor within retainingpin 6 which is positioned to extend between two cuvettes on a common radius with the circular array of cuvettes. The thermistor is further positioned withinpin 6 so as to be axially centered withinrotor 5. Such positioning provides a close correlation between the output of the thermistor and the temperature of the cuvettes. Slip rings 48 in electrical communication with the thermistor are provided on' the rotor holder for reading the signal from the thermistor. The rotor temperature and speed are both read from onemeter 49 mounted on top of the analyzer cabinet.

Referring now to FIGS. 3 and 4, the static loading side of thedisposable cuvette rotor 5 used in the analyzer of FIGS. 1 and 2 is illustrated in plan and sectioned isometric views, respectively. In construction, the rotor is of laminated design with a central, preferably opaque,plastic disk 51 sandwiched between outertransparent disks 52 and 53. A circular array of axially extending apertures are provided indisk 51 to serve assample analysis cuvettes 8. Concentric annular arrays of sample andreagent loading cavities 54 and 55 are disposed on a one-to one basis along radii passing through each cuvette. As shown in FIG. 4,loading cavities 54 and 55 are formed fromdepressions incentral disk 51 and are closed byouter disk 52.Loading apertures 56 and 57 are provided indisk 52 in register with each cavity in the respective arrays of loading cavities. Static loading of reagents and samples through the loading apertures is possible using a hypodermic syringe or automated dispensing equipment. Radial liquid communication is provided by means of small connectingpassageways 58 and 59 between respective sets of loading cavities and cuvettes. Acentral loading port 60 extends throughdisks 51 and 52 to permit dynamic loading of liquids using the dynamic loading side of the rotor described below in reference to FIGS. 5 and 6.

Plan and perspective views of the dynamic loading side ofrotor 5 are shown in FIGS. 5 and 6, respectively.

Loadingport 60 terminates in a distribution chamber provides a substantially equal distribution of liquid into 2 the respective passageways whenrotor 5 is rotating and liquid is injected throughport 60 into the distribution chamber.

Several methods of loading sample and reagent liquids inrotor 5 arepossible. One method involves static loading of individual samples and reagents inrespective loading cavities 54 and 55. This is accomplished by inserting the sample and reagent volumes through respective loading apertures "56 and 57. Great flexibility is possible using this method since different combinations of samples and reagents are possible in each set of loading cavities. Rotation of the rotor following static loading effects transfer of the sample and reagent liquids into respective cuvettes for photometric analysis.

Another method of loading may be used where it is desired to either react a plurality of reagents with a single sample or a single reagent with a plurality of samples. ln that case, the single sample or reagent is injected through loading-port 60 into. the spinning. rotor and distributed equally to the cuvettes. The rotor is then brought to a standstill and individual sample or reagent loadings are made from the static loading side of the rotor.

Still another method of loading involves the preloading and lyophilization of different reagents in the respective cuvettes. When a photometric analysis is to be made, the lyophilized reagents are solubilized by injecting water or buffer into the spinning rotor in the manner described above. Sample fluid may be likewise dynamically loaded to obtain multiple chemical analyses on a single blood sample.

The above description of one embodiment of the invention should not be interpreted in a limiting sense. For example, the rotor may have a different number of sample analysis cuvettes than the 17 shown. Also, the particular arrangement of passageways for static and dynamic loading could be modified and/or omitted in part so that only static or dynamic loading would be possible. It is intended, rather, that the invention be limited only by the scope of the appended claims.

What is claimed is:

1. A compact fast analyzer of the rotory cuvette type comprising:

a. a power-driven cuvette rotor holder comprising a flat circular base, an annular, upstanding retaining rim integrally fixed to said base, and an axially extending upstanding pin fixed to said base within the radial confine of said rim; said base defining:

i. a first series of axially extending apertures disposed in a circular array through said base within the radialconfine of said rim.

ii. a second series of axially extending apertures disposed in a circular array through said base without the radial confine of said rim, said aper tures in said second series of apertures being equal in number to said apertures in said first series of apertures;

b. a removable cuvette rotor having a circular platelike configuration disposed on said base within the confine of said rim, said rotor having an opening for receiving said pin and, defining a circular array of sample analysis cuvettes in axial register with respective apertures in said first series of apertures;

c. a adjustable light source disposed above said cuvette rotor for providing a beam of light incident on said rotor assembly at a point corresponding to the radial position of said sample analysis cuvettes;

d. means for detecting light from said light source I after it has passed through 'said sample analysis cuvettes, said means for detecting light generating an output signal proportional to .the intensity of light detected; and

e. signal generating means disposed adjacent said rotor holder for detecting the passage of apertures in said second series of apertures.

2. The fast analyzer ofclaim 1 wherein an adjustable filterholder containing a plurality of absorbance filters extends between said base and said means for detecting light from said light source after it has passed through said sample analysis cuvettes.

3. The fast analyzer ofclaim 1 further including means for rapidly braking rotation of said rotor holder and rotor.

4. The fast analyzer ofclaim 1 further including a thermistor mounted within said upstanding pin for measuring the temper'ature'of said cuvette rotor, and electrical slip rings in electrical communication with said thermistor affixed to said rotor holder.

5. The fast analyzer of claim 4 wherein said upstanding pin is located at a radial position corresponding to the radius of said first series of axially extending apertures and said sample analysis cuvettes, and wherein said thermistor is within said pin so as to be axially centered within said removable cuvette rotor when said rotor is disposed on said base within the confine of said rim.

6. The fast analyzer ofclaim 1 wherein said removable cuvette rotor defines:

a. first and second sets of radially oriented loading cavities disposed in concentric annular arrays; and

b. means for effecting centrifugal passage of fluid from said first and second sets of loading cavities to respective cuvettes in said circular array of sample analysis cuvettes.

7. The fast analyzer ofclaim 6 wherein said cuvette rotor is of laminated construction with a central opaque disk sandwiched between first and second transparent disks, said sets of first and second cavities between said distribution chamber and respective cuvettes in said circular array of sample analysis cuvettes.

9. The fast analyzer ofclaim 8 wherein each of said distribution passageways intersects with adjacent distribution passageways at an acute angle so as to form a serrated periphery about said distribution chamber.

10K 1K 1' l

Claims (9)

1. A compact fast analyzer of the rotory cuvette type comprising: a. a power-driven cuvette rotor holder comprising a flat circular base, an annular, upstanding retaining rim integrally fixed to said base, and an axially extending upstanding pin fixed to said base within the radial confine of said rim; said base defining: i. a first series of axially extending apertures disposed in a circular array through said base within the radial confine of said rim. ii. a second series of axially extending apertures disposed in a circular array through said base without the radial confine of said rim, said apertures in said second series of apertures being equal in number to said apertures in said first series of apertures; b. a removable cuvette rotor having a circular plate-like configuration disposed on said base within the confine of said rim, said rotor having an opening for receiving said pin and, defining a circular array of sample analysis cuvettes in axial register with respective apertures in said first series of apertures; c. a adjustable light source disposed above said cuvette rotor for providing a beam of light incident on said rotor assembly at a point corresponding to the radial position of said sample analysis cuvettes; d. means for detecting light from said light source after it has passed through said sample analysis cuvettes, said means for detecting light generating an output Signal proportional to the intensity of light detected; and e. signal generating means disposed adjacent said rotor holder for detecting the passage of apertures in said second series of apertures.

2. The fast analyzer of claim 1 wherein an adjustable filter holder containing a plurality of absorbance filters extends between said base and said means for detecting light from said light source after it has passed through said sample analysis cuvettes.

3. The fast analyzer of claim 1 further including means for rapidly braking rotation of said rotor holder and rotor.

4. The fast analyzer of claim 1 further including a thermistor mounted within said upstanding pin for measuring the temperature of said cuvette rotor, and electrical slip rings in electrical communication with said thermistor affixed to said rotor holder.

5. The fast analyzer of claim 4 wherein said upstanding pin is located at a radial position corresponding to the radius of said first series of axially extending apertures and said sample analysis cuvettes, and wherein said thermistor is within said pin so as to be axially centered within said removable cuvette rotor when said rotor is disposed on said base within the confine of said rim.

6. The fast analyzer of claim 1 wherein said removable cuvette rotor defines: a. first and second sets of radially oriented loading cavities disposed in concentric annular arrays; and b. means for effecting centrifugal passage of fluid from said first and second sets of loading cavities to respective cuvettes in said circular array of sample analysis cuvettes.

7. The fast analyzer of claim 6 wherein said cuvette rotor is of laminated construction with a central opaque disk sandwiched between first and second transparent disks, said sets of first and second cavities comprising depressions in said opaque disk, and loading apertures being provided through said first transparent disk in axial register with respective cavities in said first and second sets of loading cavities.

8. The fast analyzer of claim 6 wherein said cuvette rotor further defines a central distribution chamber and a plurality of distribution passageways communicating between said distribution chamber and respective cuvettes in said circular array of sample analysis cuvettes.

9. The fast analyzer of claim 8 wherein each of said distribution passageways intersects with adjacent distribution passageways at an acute angle so as to form a serrated periphery about said distribution chamber.

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