SE1530046A1 - System and method for determining the integrity of containers by optical measurement - Google Patents

System and method for determining the integrity of containers by optical measurement

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Publication number
SE1530046A1
SE1530046A1 SE1530046A SE1530046A SE1530046A1 SE 1530046 A1 SE1530046 A1 SE 1530046A1 SE 1530046 A SE1530046 A SE 1530046A SE 1530046 A SE1530046 A SE 1530046A SE 1530046 A1 SE1530046 A1 SE 1530046A1
Authority
SE
Sweden
Prior art keywords
gas
container
signal
optical
optical sensor
Prior art date
Application number
SE1530046A
Other languages
English (en)
Other versions
SE538814C2 (sv
Inventor
Dillner Joachim
Karlsson Daniel
Lewander Xu Märta
Lundin Patrik
Swartling Johannes
Original Assignee
Gasporox Ab
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Gasporox Ab filed Critical Gasporox Ab
Priority to SE1530046A priority Critical patent/SE538814C2/sv
Priority to US15/563,255 priority patent/US10101239B2/en
Priority to EP16713925.2A priority patent/EP3278074B1/en
Priority to JP2017550746A priority patent/JP2018510346A/ja
Priority to PCT/EP2016/057382 priority patent/WO2016156622A1/en
Publication of SE1530046A1 publication Critical patent/SE1530046A1/sv
Publication of SE538814C2 publication Critical patent/SE538814C2/sv
Priority to JP2021177371A priority patent/JP7300490B2/ja

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
    • G01M3/00—Investigating fluid-tightness of structures
    • G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
    • G01M3/04—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point
    • G01M3/20—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point using special tracer materials, e.g. dye, fluorescent material, radioactive material
    • G01M3/22—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point using special tracer materials, e.g. dye, fluorescent material, radioactive material for pipes, cables or tubes; for pipe joints or seals; for valves; for welds; for containers, e.g. radiators
    • G01M3/226—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point using special tracer materials, e.g. dye, fluorescent material, radioactive material for pipes, cables or tubes; for pipe joints or seals; for valves; for welds; for containers, e.g. radiators for containers, e.g. radiators
    • G01M3/229—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point using special tracer materials, e.g. dye, fluorescent material, radioactive material for pipes, cables or tubes; for pipe joints or seals; for valves; for welds; for containers, e.g. radiators for containers, e.g. radiators removably mounted in a test cell
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
    • G01M3/00—Investigating fluid-tightness of structures
    • G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
    • G01L11/00—Measuring steady or quasi-steady pressure of a fluid or a fluent solid material by means not provided for in group G01L7/00 or G01L9/00
    • G01L11/02—Measuring steady or quasi-steady pressure of a fluid or a fluent solid material by means not provided for in group G01L7/00 or G01L9/00 by optical means
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
    • G01M3/00—Investigating fluid-tightness of structures
    • G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
    • G01M3/26—Investigating fluid-tightness of structures by using fluid or vacuum by measuring rate of loss or gain of fluid, e.g. by pressure-responsive devices, by flow detectors
    • G01M3/32—Investigating fluid-tightness of structures by using fluid or vacuum by measuring rate of loss or gain of fluid, e.g. by pressure-responsive devices, by flow detectors for containers, e.g. radiators
    • G01M3/3281—Investigating fluid-tightness of structures by using fluid or vacuum by measuring rate of loss or gain of fluid, e.g. by pressure-responsive devices, by flow detectors for containers, e.g. radiators removably mounted in a test cell
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
    • G01M3/00—Investigating fluid-tightness of structures
    • G01M3/38—Investigating fluid-tightness of structures by using light
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01—Arrangements or apparatus for facilitating the optical investigation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/1717—Systems in which incident light is modified in accordance with the properties of the material investigated with a modulation of one or more physical properties of the sample during the optical investigation, e.g. electro-reflectance
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3504—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/39—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using tunable lasers
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
    • G01N21/718—Laser microanalysis, i.e. with formation of sample plasma
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/39—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using tunable lasers
    • G01N2021/396—Type of laser source
    • G01N2021/399—Diode laser
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65—Raman scattering
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications
    • G01N21/88—Investigating the presence of flaws or contamination
    • G01N21/90—Investigating the presence of flaws or contamination in a container or its contents
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00

Description

lO l5 20 25 30 35 40 systems to detect anomalies, detect small leaks, and the method is limited to certain kinds of containers. Small leaks can be detected by penetration tests using dyes or trace gases such as Another method is to subject the container to external variations e.g., or exerting overpressure on the but again this may not helium, but such tests are often destructive. in the outside atmosphere, by placing it in a (partial) vacuum chamber, container with atmospheric air or other gases, or With this method, additional means to detect a leak of a container is combinations of these techniques. some required, i.e., by controlling or measuring one or more parameters that will change as consequence of the variation in outside pressure or gas composition, if a leak is present. Several such techniques are known in the art. For example, transient pressure variation in the chamber may be recorded, and its behaviour may be indicative of a leak in the sample. As another example, if the container contains a gas species that is not present in normal air at significant concentrations, a gas detector may be placed in the test chamber (or at the outlet) to detect the presence of that gas species, indicating a leak.
Non-intrusive optical detection of gases inside packages for the purpose of quality control is disclosed in patent EP lO720l5l.9 detection of the gas in the headspace of packages for the This method is based on that the gas inside the package will (Svanberg et al.). The principle of optical purpose of indicating leaks is known in the art. deviate from an assumed gas composition due to interaction with the surrounding atmosphere through the leak. However, in normal atmosphere, for small leaks, it may take a very long time before there is a detectable deviation of the gas composition inside a package, which makes the method impractical in many situations.
There are situations where none of the methods previously described in the art are suitable for detecting a leak. when the volume Examples include, but are not limited to, of gas inside the container is very small, or in certain cases where the gas inside the container is normal air. lO 15 20 25 30 35 40 Hence, new improved apparatus and methods for detecting leaks in such containers would be advantageous.
Summary of the invention Accordingly, embodiments of the present disclosure preferably seek to mitigate, alleviate or eliminate one or more deficiencies, disadvantages or issues in the art, such as the above-identified, singly or in any combination by providing a device, system or method according to the appended patent claims for non- destructively determining the integrity of sealed containers, by subjecting said containers to variations in outside atmosphere and performing optical measurements on the container.
The disclosure generally comprises the combination of two parts, where the first part consists of subjecting the container to variations in outside pressure or gas composition, such as by placing it in a (partial) vacuum or underpressure, or exerting overpressure on the container with atmospheric air or other gases, or combinations of these steps. The purpose of this first part is to impose change to the concentration, or composition, or pressure, of the gas or gases inside the container as result of any leaks in the container. The second part consists of subjecting the container to optical spectroscopic measurement of the gas or gases inside the container, with the purpose of detecting any variation in the optical signal arising as consequence of the leak as opposed to the signal where no leak is but a decreased concentration of the gas present. Such difference in signal could be due to, is not limited to, inside the container as result of the leak, or a variation in the gas pressure inside the container, or the introduction of a new gas species inside the container due to the leak.
It should be noted that the use of the terms “first part” and “second part” in the previous description must not be interpreted as meaning that these two steps must be carried out in sequential order. The actions described in the second part can in some situations be carried out lO 15 20 25 30 35 40 before, simultaneously with, or after the actions described in the first part, or combinations of these.
It should be emphasized that the term “comprises/comprising” when used in this specification is taken to specify the presence of stated features, integers, steps or components but does not preclude the presence or addition of one or more other features, steps, integers, components or groups thereof.
Description of the drawings These and other aspects, features and advantages of which examples of the disclosure are capable of will be apparent and elucidated from the following description of examples of the present disclosure, reference being made to the accompanying drawings, in which Fig. l is illustrating an example of a system and method to determine the integrity of a sealed container; Fig. 2 is illustrating an example of a plastic pharmaceutical bottle that is subjected to a spectroscopic measurement; Fig. 3 is illustrating an example of the spectroscopic signal from oxygen gas inside a pharmaceutical bottle as it is subjected to external partial vacuum.
Description of embodiments The following disclosure focuses on examples of the present disclosure applicable to determining the integrity of containers, by subjecting said containers to Variations in outside atmosphere and performing optical this is measurements on the container. For example, advantageous for detecting leaks in a package. However, it will be appreciated that the description is not limited to this application but may be applied to many other systems where the integrity of containers needs to be determined. lO 15 20 25 30 35 40 In an example (Figure 1), a container ll that has a certain amount of gas is subjected to an integrity test in the system 100, wherein it is placed inside an enclosure 12, and the air in said enclosure is at least partially evacuated by a pump 13. In case there is a leak in the container, the gas inside the container will leak out into the enclosure and the absolute concentration of as will the An optical sensor 14 is the gas inside the container will decrease, pressure inside the container. applied to the outside of the container, said sensor consisting of a light source 15 and a light detector l6.
Preferably, the sensor is designed or adjusted to detect the spectroscopic signal of at least one of the gases that are present inside the container. at least partly, least partly transmits light at a wavelength suitable for If there is a leak in the this is indicated by a difference in signal The container must, be made of a material that at detection of said gas or gases. container, from the sensor for the leaking container compared to a similar container with no leak, or simply indicated by a difference in signal before and after the container is the signal from the sensor can be used to determine the subjected to the partial vacuum. Alternatively, absolute concentration or pressure of the gas inside the container, and that information is used to determine whether a leak is present or not.
Depending on the size of the leak one intends to detect, it may be preferable to wait some time after the enclosure has been evacuated of air before performing the sensor measurement, to allow a sufficient amount of gas to leak out of the container. be advantageous to allow the optical sensor to measure continuously and analyse the rate of change of the In some situations it may signal, since this rate of change is a measure of the size of the leak.
In a particular example, an experiment was carried out where the method outlined in the previous sections was applied to pharmaceutical plastic bottles. A test bottle made of white plastic was prepared to have a leak with a capillary tube with a The specific characteristics: diameter of 30 um was inserted through the cap. 10 15 20 25 30 35 40 bottle was subjected to a measurement using a tunable diode-laser absorption spectroscopy sensor at 760 nm, to detect oxygen gas non-intrusively inside the bottle. The optical measurement provided a baseline signal of the oxygen gas inside the bottle. Figure 2 depicts the measurement situation, bottle, 22 shows the laser transmitter, light detector. where 21 shows the pharmaceutical and 23 shows the The bottle was then subjected to partial vacuum for 10 The which shows the seconds, and then the optical measurement resumed. effect of this is depicted in Figure 3, spectroscopic oxygen signal (%meter) as a function of (seconds). At the point 31, took place. After the 10-second vacuum, time the 10-second vacuum there was an increase in the spectroscopic oxygen signal of 0.4%. The despite the fact that the oxygen pressure inside the bottle decreased as result reason for the signal increasing, of the surrounding vacuum, is that the decreased pressure causes a spectroscopic line-narrowing, which in turn causes an increase in the peak value of the line.
The bottle was subjected to vacuum again at point 32 in there The Figure 3, this time for 30 seconds. At this point, was a 1.2% increase in the spectroscopic signal. experiment shows that the method of subjecting a pharmaceutical bottle to vacuum, in combination with a spectroscopic technique to detect the signal from oxygen gas inside the bottle, can be used to determine the presence of a leak in the bottle.
In another example, or mix of gases, the gas concentration inside the container is performed a container containing a gas, is placed in an enclosure, and a measurement of using an optical sensor consisting of a light source and a light detector. Said measurement provides a baseline recording of the gas concentration inside the container.
Then, air. said enclosure is at least partially evacuated of The enclosure is then filled with a gas composition Then, concentration is again measured using the optical sensor. different from air, such as nitrogen. the gas A lower reading compared to the baseline is indicative of a leak. An advantage of this example compared to lO 15 20 25 30 35 40 performing the optical measurement in vacuum, or near vacuum, is that the spectroscopic linewidth of the gas inside the container is essentially the same, regardless of whether a leak is present or not, Thus, correction is required due to differences in pressure. because the pressure is essentially the same. no spectroscopic linewidth In another example, a container containing a gas, or mix Then, is at least partially evacuated of air. then filled with a different gas (or gases) initially present inside the container, Then, the concentration of said different gas inside the of gases is placed in an enclosure. said enclosure The enclosure is that is not or which is present at a known concentration. a measurement of container is performed using an optical sensor consisting of a light source and a light detector. The presence of, or increased concentration of, said different gas inside the container is indicative of a leak. In some examples, said different gas may consist of carbon dioxide.
It should be noted that in the examples described above, it is not necessary to measure the gas concentration in absolute values. In some examples it is sufficient to measure a signal that is related to the gas concentration.
In some examples, the spectroscopic signal is related to the gas pressure.
In some examples, at least one reference container is used, said reference container having no leaks, or having leaks with known characteristics. The measurement on the reference container provides a baseline signal which is used for comparison with the measured signals on subsequent containers.
In some examples, the optical sensor consists of a sensor based on tunable diode-laser absorption spectroscopy (TDLAS).
In some examples, the optical sensor consists of a sensor for gas in scattering media absorption spectroscopy (GASMAS), such as disclosed in EP lO720l5l.9 al.).
(Svanberg et lO 15 20 25 30 35 40 In some examples, the optical sensor consists of an LED light source and a photodetector. sensor consists of a sensor In some examples, the optical for photoacoustical detection. sensor consists of a sensor In some examples, the optical for Raman spectroscopy of the gas inside the container. sensor consists of a broad In some examples, the optical wavelength light source and a spectrometer.
In some examples, the optical sensor consists of a sensor for laser-induced breakdown spectroscopy of the gas inside the container. the optical sensor is working in the light transmitter is located and the light detector is located on the opposite side of the container, In some examples, transmission mode, i.e., on one side of the container, and a light beam is transmitted from the light transmitter through the container to the light detector.
In some examples, the optical sensor is working in reflection mode, on the same side of the container as the light detector, i.e., the light transmitter is located and the light detector records back-scattered light from the container. the light transmitter and the light detector are positioned in arbitrary positions in and the light detector records scattered light from the container.
In some examples, relation to each other on the container, In some examples, the light is guided to and/or from the container by means of optical fibres. In some examples, the light is guided to and/or from the container via windows, or optical components including lenses, mirrors, other means of guiding and directing light.

Claims (26)

Claims l. A method of determining the integrity of a closed container, said method comprising: - positioning said container in a surrounding; - changing gas pressure, or gas composition, or a combination of gas pressure and gas composition, in said surrounding; - subjecting said container to an optical sensor, non- intrusively, said sensor sensitive to at least one said gas, and said sensor capable of detecting said gas inside said container; - reading a signal from said optical sensor related to gas pressure, or gas concentration, or any combination of gas pressure, gas concentration, and gas composition, inside said container; the behaviour of said signal being indicative of breach in integrity of said container. 2. The method according to claim l, in which a vacuum or underpressure is applied in said surrounding. 3. The method according to claim l, in which overpressure is applied in said surrounding. 4. The method according to claim l, in which a gas or mix of gases is applied in said surrounding. 5. The method according to claim l, in which any combination of claims 2-4 is applied. 6. The method of any of claims l-5, in which said optical sensor is based on any spectroscopic or optical means of gas detection. 7. The method of any of claims l-5, in which said optical sensor is based on tunable diode laser absorption spectroscopy (TDLAS). 8. The method of any of claims l-5, in which said optical sensor is based on gas in scattering media absorption spectroscopy (GASMAS). 9. The method of any of claims l-8, in which a reference container which is known not to have leaks, or to have leaks of known characteristics, is used to provide a baseline signal, and the difference in optical signal compared to said baseline signal is used to detect leaks in subsequent containers. 10. The method of any of claims 1-8, in which the variation in optical signal from one time to another on the same container is used to detect a leak. 11. The method of any of claims 1-8 and either of claims 9 or 10, in which the concentration of gas inside the container is determined. 12. The method of any of claims 1-8 and either of claims 9 or 10, in which the absolute or relative pressure of gas inside the container is determined. 13. The method of any of claims 1-8, in which a measure of the size of a leak is determined by measuring continuously or repeatedly an optical signal and determining the rate of change of said signal. 14. A system for determining the integrity of a sealed container, said system comprising: - a surrounding where said container can be positioned, where gas pressure, or gas composition, or a combination of gas pressure and gas composition, can be changed; - a non-intrusive optical sensor sensitive to at least one said gas, and said sensor capable of detecting said gas inside said container; - a means to read a signal from said optical sensor related to gas pressure, or gas concentration, or any combination of gas pressure, gas concentration, and gas composition, inside said container; the behaviour of said signal being indicative of breach in integrity of said container. 15. The system according to claim 14, in which a vacuum or underpressure is applied in said surrounding. 16. The system according to claim 14, in which overpressure is applied in said surrounding. 17. The system according to claim 14, in which a gas or mix of gases is applied in said surrounding. 18. The system according to claim 14, in which any combination of claims 15-17 is applied. 19. The system of any of claims 14-18, in which said optical sensor is based on any spectroscopic or optical means of gas detection. 20. The system of any of claims 14-18, in which said optical sensor is based on tunable diode laser absorption spectroscopy (TDLAS). 21. The system of any of claims 14-18, in which said optical sensor is based on gas in scattering media absorption spectroscopy (GASMAS). 22. The system of any of claims 14-21, in which a reference container which is known not to have leaks, or to have leaks of known characteristics, is used to provide a baseline signal, and the difference in optical signal compared to said baseline signal is used to detect leaks in subsequent containers. 23. The system of any of claims 14-21, in which the variation in optical signal from one time to another on the same container is used to detect a leak. 24. The system of any of claims 14-21 and either of claims 22 or 23, in which the concentration of gas inside the container is determined. 25. The system of any of claims 14-21 and either of claims 22 or 23, in which the absolute or relative pressure of gas inside the container is determined. 26. The system of any of claims 14-21, in which a measure of the size of a leak is determined by measuring continuously or repeatedly an optical signal and determining the rate of change of said signal. Patentansökan nr/ Patent application No: 1530046-0 I följande bilaga finns en översättning av patentkraven till svenska. Observera att det är patentkravens lydelse på engelska som gäller. A Swedish translation of the patent claims is enclosed. Please note that only the English elaims have legal effect. 10 15 20 25 30 PATENTKRAV
1. Förfarande för fastställande av integriteten för en sluten behållare (l 1), varvid nämnda förfarande innefattar: - placering av nämnda behållare (11) i en omgivning; - förändring av gastryck, eller gassammansättning, eller en kombination av gastryck och gassammansättning, i nämnda omgivning; - att låta nämnda behållare (11) undergå en optisk givare (14), på ett icke- inkräktande sätt, varvid nämnda givare (14) är känslig för minst en nämnd gas, och varvid nämnda givare (14) är i stånd att detektera nämnda gas inuti nämnda behållare (1 1); - avläsning av en signal från nämnda optiska givare (14) avseende gastryck, eller gaskoncentration, eller någon kombination av gastryck, gaskoncentration, och gassammansättning, inuti nämnda behållare (11); varvid reaktionen hos nämnda signal är indikativ om åsidosättande av integritet för nämnda behållare (1 l).
2. Förfarande enligt krav 1, i vilket ett vakuum eller undertryck tillämpas i nämnda omgivning.
3. Förfarande enligt krav 1, i vilket övertryck tillämpas i nämnda omgivning.
4. Förfarande enligt krav l, i vilket en gas eller blandning av gaser tillämpas i nämnda omgivning.
5. Förfarande enligt krav 1, i vilket någon kombination av stegen enligt krav 2 till 4 tillämpas i sekvens.
6. Förfarande enligt något av krav 1 till 5, i vilket nämnda optiska givare (14) baseras på något medel av spektroskopisk eller optisk gasdetektering.
7. Förfarande enligt något av krav 1 till 5, i vilket nämnda optiska givare (14) baseras på avstämbar diodlaserabsorptionsspektroskopi (TDLAS).
8. Förfarande enligt något av krav 1 till 5, i vilket nämnda optiska givare (14) baseras på absorptionsspektroskopi av gas i spridande medium (GASMAS).
9. Förfarande enligt något av krav l till 8, i vilket en referensbehållare vilken är känd att inte ha något läckage, eller att ha läckage enligt kända särdrag, används för att tillhandahålla en baslinjesignal, och varvid skillnaden i optisk signal 10 15 20 25 30 _2_ j ämförd med nämnda baslinjesignal används för att detektera läckage i efterföljande behållare.
10. Förfarande enligt något av krav l till 8, i vilket variationen i optisk signal från en gång till en annan på samma behållare (11) används för att detektera ett läckage.
11. Förfarande enligt något av krav 1 till 8, och antingen krav 9 eller 10, i vilket koncentrationen gas inuti behållaren (l 1) fastställs.
12. Förfarande enligt något av krav 1 till 8, och antingen krav 9 eller 10, i vilket det absoluta eller relativa gastrycket inuti behållaren (11) fastställs.
13. Förfarande enligt något av krav 1 till 8, i vilket ett mått av storleken på ett läckage fastställs genom kontinuerlig eller upprepad mätning av en optisk signal och fastställande av förändringshastigheten hos nämnda signal.
14. System för fastställande av integriteten för en tätad behållare (ll), varvid nämnda system innefattar: - en omgivning där nämnda behållare (1 1) kan placeras, där gastryck, eller gassammansättning, eller en kombination av gastryck och gassammansättning, kan förändras; - en icke-inkräktande optisk givare (14) som är känslig för minst en nämnd gas, och varvid nämnda givare (14) är i stånd att detektera nämnda gas inuti nämnda behållare (11); - ett organ för avläsning av en signal från nämnda optiska givare (14) avseende gastryck, eller gaskoncentration, eller någon kombination av gastryck, gaskoncentration, och gassammansättning, inuti nämnda behållare (l1); varvid reaktionen hos nämnda signal är indikativ om åsidosättande av integritet för nämnda behållare (1 1).
15. System enligt krav 14, i vilket ett vakuum eller undertryck tillämpas i nämnda omgivning.
16. System enligt krav 14, i vilket övertryck tillämpas i nämnda omgivning.
17. System enligt krav 14, i vilket en gas eller blandning av gaser tillämpas i nämnda omgivning.
18. System enligt krav 14, i vilket någon kombination av stegen enligt krav 15 till 17 tillämpas i sekvens. 10 15 20 _3_
19. System enligt något av krav 14 till 18, i Vilket nämnda optiska givare (14) baseras på något medel av spektroskopisk eller optisk gasdetektering.
20. System enligt något av krav 14 till 18, i vilket nämnda optiska givare baseras på avstämbar diodlaserabsorptionsspektroskopi (TDLAS).
21. System enligt något av krav 14 till 18, i vilket nämnda optiska givare baseras på absorptionsspektroskopi av gas i spridande medium (GASMAS).
22. System enligt något av krav 14 till 21, i vilket en referensbehållare vilken är känd att inte ha något läckage, eller att ha läckage enligt kända särdrag, används för att tillhandahålla en baslinjesignal, och varvid skillnaden i optisk signal j ämförd med nämnda baslinjesignal används för att detektera läckage i efterföljande behållare.
23. System enligt något av krav 14 till 21, i vilket variationen i optisk signal från en gång till en annan på samma behållare (11) används för att detektera ett läckage.
24. System enligt något av krav 14 till 21, och antingen krav 22 eller 23, i vilket koncentrationen gas inuti behållaren (11) fastställs.
25. System enligt något av krav 14 till 21, och antingen krav 22 eller 23, i vilket det absoluta eller relativa gastrycket inuti behållaren (11) fastställs.
26. System enligt något av krav 14 till 21, i vilket ett mått av storleken på ett läckage fastställs genom kontinuerlig eller upprepad mätning av en optisk signal och fastställande av förändringshastigheten hos nämnda signal.
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