Chemistry: analytical and immunological testing – Including chromatography
Reexamination Certificate
2002-02-20
2003-11-11
Ludlow, Jan (Department: 1743)
Chemistry: analytical and immunological testing
Including chromatography
C073S023350, C073S052000, C095S082000, C374S142000, C374S159000
Reexamination Certificate
active
06645773
ABSTRACT:
FIELD OF THE INVENTION
The present invention relates to a method of analyzing materials, and more particularly, to a method of accurately measuring the effective temperature inside a sealed container, such as a headspace vial.
BACKGROUND OF THE INVENTION
The technique of equilibrium headspace extraction involves placing a liquid or solid sample into a suitable sealed vial and allowing volatile analytes within the sample to reach equilibration in concentration between the sample matrix and the vapor above it (i.e., the headspace). A fixed volume of the vapor is then transferred to a gas chromatograph for analysis. At equilibration, the concentration of each analyte in the headspace is defined by the amount of the analyte present, the volumes of the two phases and the partition coefficient for that analyte between the two phases. The partition coefficient, which is a thermodynamic property, is highly dependent on temperature and so must be carefully controlled within the instrumentation if good analytical precision is to be achieved.
Current state-of-the-art headspace samplers, such as the model TurboMatrix Automatic Headspace Sampler distributed by PerkinElmer Instruments LLC, are designed to maintain a very stable vial temperature by making use of a large thermostatted metal oven block. However, despite the fact that stable vial temperatures can be maintained, a number of issues regarding temperature control remain.
For example, the true temperature of the vial may not be accurately measured. The electronic sensor used to monitor temperature is typically located within a heating belt that surrounds the oven block and is remote from the vial. As such, the temperature reading may not reflect the true vial temperature at all settings. Moreover, it is possible that all vial positions may not be at the same temperature.
Another issue may arise when a new (cold) vial is inserted into the oven block. In such a case, there may be a drop in temperature in one or more of the other vials which cannot be readily detected using known methods. Furthermore, known methods of temperature measurement may not take into account the fact that the vial temperature may change over time.
Another potential issue is that certain requirements, such as GLP (Good Laboratory Practices) certification standards and FDA (Food and Drug Administration) approval requirements, may require that the vial temperature be monitored and/or calibrated.
In addition, some instruments which are not state-of-the-art may be weak in the area of vial temperature control. As such, it may be desirable to evaluate the performance of such instruments using a simple method for temperature measurement.
Traditionally, a thermocouple or similar temperature-measuring probe would be inserted into the vial. However, this technique is tedious to perform, interrupts the normal operation of the instrument, and requires special tools. Moreover, taking a reading from a single point inside the vial may not truly reflect the “effective” temperature of the whole vial. Instead, it would be more desirable to make use of a suitable sample in a vial and use chromatography to determine temperature—after all, it is this process for which standardization is being attempted.
What is desired, therefore, is a method of measuring the effective temperature inside a sealed container which accurately reflects the true container temperature at all instrument settings, which takes into account temperature variations across various container positions, which measures the temperature of each container separately from other containers when a plurality of containers are used, which takes into account the fact that the container temperature may change over time, which allows for temperature calibration, which can be used to evaluate the temperature control performance of an instrument, which is easy to perform, which does not interrupt the normal operation of the instrument, which does not require special tools, and which uses chromatography to determine temperature.
SUMMARY OF THE INVENTION
Accordingly, it is an object of the present invention to provide a method of measuring the effective temperature inside a sealed container which accurately reflects the true container temperature at all instrument settings.
Another object of the present invention is to provide a method of measuring the effective temperature inside a sealed container having the above characteristics and which takes into account temperature variations across various container positions.
A further object of the present invention is to provide a method of measuring the effective temperature inside a sealed container having the above characteristics and which measures the temperature of each container separately from other containers when a plurality of containers are used.
Still another object of the present invention is to provide a method of measuring the effective temperature inside a sealed container having the above characteristics and which takes into account the fact that the container temperature may change over time.
Yet a further object of the present invention is to provide a method of measuring the effective temperature inside a sealed container having the above characteristics and which allows for temperature calibration.
Still a further object of the present invention is to provide a method of measuring the effective temperature inside a sealed container having the above characteristics and which can be used to evaluate the temperature control performance of an instrument.
Still a further object of the present invention is to provide a method of measuring the effective temperature inside a sealed container having the above characteristics and which is easy to perform.
Yet another object of the present invention is to provide a method of measuring the effective temperature inside a sealed container having the above characteristics and which does not interrupt the normal operation of the instrument.
Still a further object of the present invention is to provide a method of measuring the effective temperature inside a sealed container having the above characteristics and which does not require special tools.
Yet still a further object of the present invention is to provide a method of measuring the effective temperature inside a sealed container having the above characteristics and which uses chromatography to determine temperature.
These and other objects of the present invention are achieved by provision of method of measuring the effective temperature inside a sealed container having a headspace. A liquid solvent is added to the container, and a solid compound is added to the liquid solvent to create a saturated solution. Vapor of the saturated solution is allowed to equilibrate in the headspace of the sealed container, and a volume thereof is transferred to a chromatographic column, where chromatographic readings of the equilibrated vapor are taken. A temperature within the sealed container is then calculated based upon the chromatographic readings of the equilibrated vapor, wherein the temperature calculation is based upon the concentrations of the liquid solvent and the solid compound in the equilibrated vapor.
Preferably, the chromatographic readings comprise readings of peak areas of the liquid solvent and the solid compound. Most preferably, the calculating step comprises the step of calculating a temperature within the sealed container based upon a ratio of the readings of peak areas of the liquid solvent and the solid compound.
In one preferred embodiment, the liquid solvent comprises n-dodecane and the solid compound comprises naphthalene. In another embodiment, the liquid solvent comprises n-octadecane and the solid compound comprises anthracene.
REFERENCES:
patent: 5431023 (1995-07-01), Howard et al.
patent: 5441700 (1995-08-01), Markelov
patent: 5792423 (1998-08-01), Markelov
patent: 5932482 (1999-08-01), Markelov
patent: 6146895 (2000-11-01), Green et al.
Chickos et al, Thermochimica Acta 313 (1998) 101-110.
Ludlow Jan
PerkinElmer Instruments LLC
St. Onge Steward Johnston & Reens LLC
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