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US3883738A - Methods of analysis of radioactive material separated into solid and liquid phases - Google Patents

Methods of analysis of radioactive material separated into solid and liquid phases Download PDF

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Publication number
US3883738A
US3883738A US313263A US31326372A US3883738A US 3883738 A US3883738 A US 3883738A US 313263 A US313263 A US 313263A US 31326372 A US31326372 A US 31326372A US 3883738 A US3883738 A US 3883738A
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United States
Prior art keywords
phase
phases
solid
radioactivity
analysis
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Expired - Lifetime
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US313263A
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English (en)
Inventor
John Stuart Glover
Bryan Peter Shepherd
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AMERLITE DIAGNOSTICS Ltd A BRITISH Co
GE Healthcare Ltd
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Radiochemical Centre Ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
    • G01T7/00—Details of radiation-measuring instruments
    • G01T7/02—Collecting means for receiving or storing samples to be investigated and possibly directly transporting the samples to the measuring arrangement; particularly for investigating radioactive fluids

Definitions

  • C* is the labelled version of the compound R is the other reagent.
  • the amount of R is arranged to be insufficient to react with all of C C*.
  • an equilibrium is set up in which the ratio of [C*]/[C*]+[C*R] is determined by the amount of the unlabelled compound C which is present. If C* is separated from C*R and the level of activity of each separated part measured, then the value of the ratio is easily calculated.
  • the amount of the unlabelled compound C can then be determined, in relative or absolute terms, by the use of standard preparation of compound C, to generate a calibration curve.
  • Separation of C* from C*R is generally effected in two stages.
  • C* or C*-R is caused to change phase for example by being precipitated from solution, or adsorbed on to an inert carrier, or passed into a water-immiscible phase.
  • the two phase are removed from one another, e.g. by filtration, or, more usually, by centrifuging followed by decanting the supernatant liquor.
  • the present invention provides a method of performing an analysis in which a radioactive element or compound is partitioned between two phases, which method comprises measuring the level of radioactivity of at least one of the two phases while that phase is in contact with the other phase.
  • At least a part of radioactive material in one phase has to be separated from the radioactive material in the other phase in order to determine the level of activity in the one phase. It is a feature of the invention that the two phases themselves are not removed from one an other, as by removal of one phase to a different vessel,
  • This invention envisages two ways of overcoming this difficulty, which may be employed either separately or, more usually, in combination:
  • the reaction tube may be specially shaped, for example, where the radioactive element is partitioned between a liquid and a heavier solid phase, as a centrifuge tube with a thin capillary at the bottom for the solid phase, so that the solid phase is separated by an appreciable distance from the bulk of the liquid phase in the body of the tube. (In the case where the radioactive element is partitioned between two liquid phases, a corresponding design of tube may be possible).
  • the counter may be accurately collimated and carefully screened from the phase whose activity is not being measured.
  • the method of this invention is particularly applicable in those cases where the radioactive tracer element involved is a soft gamma ray emitter, so that quite a thin layer of lead can be used for the screening.
  • the commonly used tracer I is particularly suitable, as its soft gamma radiation is attenuated by 3 mm of lead to an insignificantly low level.
  • the level of activity of the solid phase can be measured by screening off the body of the reaction vessel from the counter with only a very small error resulting from contamination by a tiny amount of liquid phase in the capillary; and the level of activity of the liquid phase in the body of the reaction vessel can be measured by screening off the capillary from the counter with only a very small error resulting from the absence of a tiny amount of the liquid phase in the capillary.
  • FIG. 1 is a perspective view of a conventional centrifuge tube and containing a solid in suspension in a liquid.
  • FIG. 2 is a perspective view of the centrifuge tube after centrifuging.
  • FIG. 3 is a perspective view of a partly shielded holder, with the cavity for a centrifuge tube shown dotted;
  • FIG. 4 is a perspective view of the holder with a centrifuge tube in position in it;
  • FIG. 5 is a perspective view of a shielded counting device, partly cut away to show a tube, containing solution and solid sediment, in position therein.
  • FIG. 6 is a sectional side elevation of the centrifuge tube and holder of FIG. 4 in position in the well of a sodium iodide scintillation crystal.
  • FIG. 7 is a sectional side elevation of the shielded tube of FIG. in position in the well of a sodium iodide scintillation crystal.
  • FIG. 8 is a sectional side elevation of a modification of the apparatus of FIG. 6 designed to measure the radioactivity of the solid phase but not the liquid phase.
  • a centrifuge tube 10 is made of plastics material, has a cap 11, and contains a liquid phase 12 and a solid phase 13, either or both of which may be radioactive.
  • the solid phase 13 has been concentrated in the conical tip 14 of the tube 10 by centrifuging.
  • a partly shield holder 15 comprises a lead base 16 bonded to an annular upper portion 17 of plastics material.
  • a centifuge tube fits in the holder so that the conical tip 14, and the solid material concentracted therein, is surrounded by the lead part of the holder.
  • the complete unit (holder plus centifuge tube 10) can be accommodated in the well of a sodium iodide scintillation crystal which forms part of an instrument for the measurement of radioactivity (a well-crystal counter). Screened from the counter by the lead base 16 of the holder 15 will be the solid phase 13 and the small proportion of the liquid phase 12 which is in the tip 14 of the centrifuge tube 10.
  • the error in measurement resulting from the fact that not quite all the liquid phase is visible in the counter, can generally be neglected unless very accurate measurements are required, and is in any case unimportant where levels of radioactivity of liquids in different tubes of the same design are being compared.
  • the system described with reference to FIGS. 1 to 4 is designed to measure the radioactivity of essentially the whole liquid phase in the centrifuge tube. However, when unknown samples are being measured against calibrating standards, measurement of the whole phase is not necessary. It is sufficient to ensure that the liquid volume is the same in different tubes being used in the experiment, and to measure the radioactivity of a constant volume, of the liquid phase. This constant volume need not be known, but it must form a constant proportion of the total liquid phase, as between different tubes used in the same experiment.
  • a counting device comprises a sodium iodide scintillation crystal (not shown) into the well of which lead shielding 18, 19 has been built.
  • the upper and lower parts, 18 and 19 respectively, of the lead shielding limit the field of view of the counting device to a fixed column 25 of the liquid phase 22. Provided that the diameter of that column 25 is fixed (i.e.
  • the counter measures the radioactivity of a constant proportion of the total liquid phase, as between different tubes used in the same experiment.
  • the centrifuge tube 10 in its holder 15 is placed in the well of a sodium iodide scintillation crystal 26.
  • a scintillation counter 27 is positioned below the scintillation crystal. Radiation emitted by radioactive material in the liquid 12 passes through the plastics material 17 and gives rise to scintillations in the sodium iodide crystal 26. The scintillations are detected by the counter 27. Radiation from the solid deposit 13 is largely prevented from reaching the scintillation crystal 26 by the lead shielding 16.
  • a well-type sodium iodide scintillation crystal 29 has lead shielding l8, 19 built into it in the manner described with reference to FIG. 5. Radiation emitted by radioactive material in the liquid 22 passes through the gap 25 between lead Shielding l8 and 19 and gives rise to scintillations in the sodium iodide crystal 29. The scintillations are detected by a counter 27, positioned below the scintillation crystal. Radiation from the remainder of the liquid 22 and from the solid 24 is prevented from reaching the scintillation crystal 29 by the lead shields 18, 19.
  • the centrifuge tube 10 of FIG. 2 is placed in a holder resembling that of FIG. 3, except that in this case the base 30 is of plastics material and the annular upper part 31 is of lead.
  • the tube and holder together are positioned in the well of a sodium iodide scintillation crystal 26.
  • a scintillation counter 32 Surrounding the lower part of the scintillation crystal, on a level with the plastics base 30 of the holder, is a scintillation counter 32. Radiation emitted by radioactive material in the solid deposit 13 passes through the plastics material 30 and gives rise to scintillations in the sodium iodide crystal 26. These scintillations are detected by the counter 32. Radiation from the liquid 12 is largely prevented from reaching those parts of the scintillation crystal 26 which are observed by the counter 32 by means of the lead shielding 31.
  • Insulin standards were prepared at 250, I00, 50, 25, I25, and zero uunits/ml.
  • Triplicates at each concen tration were prepared by adding 300 pl aliquots to Eppendorf centrifuge tubes.
  • Quadruplicates of the unknown sera were prepared by adding 300 ,ul of the sera to similar tubes.
  • the nature of the analysis is not material to this invention; immunoassays and similar competitive assays, as described above. are examples of suitable forms of analysis.
  • the radioactive element involved is preferably a soft gamma ray emitter, but the nature of the two phases, and the method by which the radioactive element is partitioned between them, are not material. Likewise, any suitable means may be used for determining the level of activity in one or other (or both) of the phases.
  • a method of performing an analysis in which a radioactive element or compound is partitioned between a liquid phase and a denser solid phase comprises measuring the level of radioactivity of only one of the two phases while that phase is in contact with the other phase, wherein the measuring device is collimated and screened so as to measure the radioactivity of substantially the whole of the liquid phase but not of the solid phase.
  • a method of performing an analysis in which a radioactive element or compound is partitioned between a liquid phase and a denser solid phase comprises measuring the level of radioactivity of only one of the two phases while that phase is in contact with the other phase, wherein the measuring device is collimated and screened so as to measure the radioactivity of a selected part only of the liquid phase.
  • a method of performing an analysis in which a radioactive element or compound is partitioned between a liquid phase and a denser solid phase comprises measuring the level of radioactivity of only one of the two phases while that phase is in contact with the other phase, wherein the measuring device is collimated and screened so as to measure the radioactivity of the solid phase but not of the liquid phase.

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  • High Energy & Nuclear Physics (AREA)
  • Analytical Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Molecular Biology (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Investigating Or Analysing Biological Materials (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Measurement Of Radiation (AREA)
US313263A 1971-12-16 1972-12-08 Methods of analysis of radioactive material separated into solid and liquid phases Expired - Lifetime US3883738A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
GB5856671A GB1411382A (en) 1971-12-16 1971-12-16 Methods of analysis

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US3883738A true US3883738A (en) 1975-05-13

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US313263A Expired - Lifetime US3883738A (en) 1971-12-16 1972-12-08 Methods of analysis of radioactive material separated into solid and liquid phases

Country Status (6)

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US (1) US3883738A (de)
JP (1) JPS5229956B2 (de)
DE (1) DE2261561C3 (de)
FR (1) FR2167046A5 (de)
GB (1) GB1411382A (de)
SE (1) SE390066B (de)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4051369A (en) * 1974-02-09 1977-09-27 Japan Atomic Energy Research Institute Method for inspecting nuclear fuel rod or irradiation capsule
US4158135A (en) * 1976-08-16 1979-06-12 Thorell Jan Ivan Analysis process
US4315151A (en) * 1980-07-07 1982-02-09 Beckman Instruments, Inc. Detecting phase separation in liquid scintillation samples
US4333010A (en) * 1981-05-08 1982-06-01 Miller William H Dose calibrator linearity evaluation
US4394391A (en) * 1980-02-19 1983-07-19 Thorell Jan Ivan Radioimmunoassay reagents
EP0127169A1 (de) * 1983-05-27 1984-12-05 Fuji Photo Film Co., Ltd. Verfahren zur Messung der Strahlungsintensität
US5274239A (en) * 1992-07-23 1993-12-28 Sunol Technologies, Inc. Shielded dose calibration apparatus

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SE444989B (sv) * 1979-12-17 1986-05-20 Jan Ivan Thorell Reagenskomposition for radioimmunologiska bestemningsmetoder
US5073341A (en) * 1985-08-21 1991-12-17 Biotope, Inc. Devices for conducting specific binding assays
JP2591738B2 (ja) * 1985-08-21 1997-03-19 ベーリンガー マンヘイム コーポレイション 特異的結合アッセイにおける成分の分離，混合および検出のための方法および装置
ATE91023T1 (de) * 1987-12-01 1993-07-15 Biotope Inc Verfahren und vorrichtungen zur durchfuehrung von untersuchungen.

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2927209A (en) * 1957-07-05 1960-03-01 Jones Richard Norman Spectrometric cell structure and charging method therefor
US3050628A (en) * 1957-06-19 1962-08-21 Kartridg Pak Co Method of determining composition of an oil and water mixture
US3376114A (en) * 1960-05-02 1968-04-02 Abbott Lab Method for measuring the binding capacity of serum proteins
US3451777A (en) * 1965-08-20 1969-06-24 Walter Di Giulio Method and apparatus for determining the thyroid hormone content of blood
US3588504A (en) * 1967-09-12 1971-06-28 Atomic Energy Authority Uk Apparatus for particle size analysis utilizing beta backscattering
US3666854A (en) * 1969-07-30 1972-05-30 Nuclear Med Lab Test for thyroid hormone

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3050628A (en) * 1957-06-19 1962-08-21 Kartridg Pak Co Method of determining composition of an oil and water mixture
US2927209A (en) * 1957-07-05 1960-03-01 Jones Richard Norman Spectrometric cell structure and charging method therefor
US3376114A (en) * 1960-05-02 1968-04-02 Abbott Lab Method for measuring the binding capacity of serum proteins
US3451777A (en) * 1965-08-20 1969-06-24 Walter Di Giulio Method and apparatus for determining the thyroid hormone content of blood
US3588504A (en) * 1967-09-12 1971-06-28 Atomic Energy Authority Uk Apparatus for particle size analysis utilizing beta backscattering
US3666854A (en) * 1969-07-30 1972-05-30 Nuclear Med Lab Test for thyroid hormone

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4051369A (en) * 1974-02-09 1977-09-27 Japan Atomic Energy Research Institute Method for inspecting nuclear fuel rod or irradiation capsule
US4158135A (en) * 1976-08-16 1979-06-12 Thorell Jan Ivan Analysis process
US4394391A (en) * 1980-02-19 1983-07-19 Thorell Jan Ivan Radioimmunoassay reagents
US4315151A (en) * 1980-07-07 1982-02-09 Beckman Instruments, Inc. Detecting phase separation in liquid scintillation samples
US4333010A (en) * 1981-05-08 1982-06-01 Miller William H Dose calibrator linearity evaluation
EP0127169A1 (de) * 1983-05-27 1984-12-05 Fuji Photo Film Co., Ltd. Verfahren zur Messung der Strahlungsintensität
US5274239A (en) * 1992-07-23 1993-12-28 Sunol Technologies, Inc. Shielded dose calibration apparatus
WO1994002869A1 (en) * 1992-07-23 1994-02-03 Sunol Technologies, Inc. Shielded dose calibration apparatus

Also Published As

Publication number Publication date
JPS5229956B2 (de) 1977-08-04
SE390066B (sv) 1976-11-29
GB1411382A (en) 1975-10-22
DE2261561B2 (de) 1980-01-03
JPS4866892A (de) 1973-09-13
DE2261561C3 (de) 1980-09-04
DE2261561A1 (de) 1973-07-12
FR2167046A5 (de) 1973-08-17

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Owner name: AMERLITE DIAGNOSTICS LIMITED

Free format text: CHANGE OF NAME;ASSIGNOR:AMERSHAM INTERNATIONAL PLC, F/K/A (THE RADIOCHEMICAL CENTRE LIMITED), A BRITISH CO.;REEL/FRAME:005957/0501

Effective date: 19910617