Abstract:
It is suggested to use mass spectroscopy in in-line testing of closed containers. 
     The method for evaluating a quality of a number of closed filled containers filled with a filling product comprises: 
     detecting at least one analyte by means of a mass spectroscopy technique, wherein said at least one analyte comprises at least one of
       said filling product;   one or more components of said filling product;   a decomposition product of said filling product;   one or more decomposition products of one or more components of said filling product.

Description:
TECHNICAL FIELD  
       [0001]    The invention relates to the field of quality control and in particular leak testing. It relates to methods and apparatuses according to the opening clauses of the claims. Such methods and apparatuses find application, e.g., in food industry and pharmaceutical industry. 
       BACKGROUND OF THE INVENTION 
       [0002]    Various ways of evaluating the quality of closed filled containers are known in the art. E.g., tracer gases such as Nitrogen or Argon can be filled into the containers, in addition to the filled products, and then, a leakage rate for said tracer gas is determined. From said leakage rate, a leak rate for the filled product is then estimated. 
       SUMMARY OF THE INVENTION 
       [0003]    Therefore, one object of the invention is to create an alternative way of evaluating a quality of a closed filled container, in particular a leak tightness thereof. 
         [0004]    In particular, the invention shall be applicable in-line in a production process. 
         [0005]    Further objects emerge from the description and embodiments below. 
         [0006]    At least one of these objects is at least partially achieved by apparatuses and methods and uses according to the patent claims. 
         [0007]    It is suggested to use mass spectroscopy for detecting whether or not and to which extent said filling product has escaped from a closed filled container. This method is very specific and precise and very direct, at least when compared to methods where tracer gases or other tracer materials are used. The present invention allows to dispense with tracer materials. 
         [0008]    The invention also comprises: 
         [0009]    A method for evaluating a quality of a number of closed filled containers filled with a filling product, said method comprising detecting at least one analyte by means of a mass spectroscopy technique, wherein said at least one analyte comprises at least one of
       said filling product;   one or more components of said filling product;   a decomposition product of said filling product;   one or more decomposition products of one or more components of said filling product.       
 
         [0014]    Further embodiments of this method are disclosed in the Patent Claims, particularly in the claims depending on claim  1 . 
         [0015]    The invention furthermore comprises: 
         [0016]    A method for determing a leak tightness of a number of closed filled containers filled with a filling product, said method comprising detecting at least one analyte by means of a mass spectroscopy technique, wherein said at least one analyte comprises at least one of
       said filling product;   one or more components of said filling product;   a decomposition product of said filling product;   one or more decomposition products of one or more components of said filling product;
 
in particular wherein said method comprises determing said leak tightness from a result of said detecting, and in particular wherein said method is carried out in an in-line fashion following a closing step for closing said containers.
       
 
         [0021]    And the invention also comprises further embodiments of this before-addressed method, namely those having in addition features corresponding to features of an embodiment of the first-addressed method. 
         [0022]    The invention furthermore comprises: 
         [0023]    A method for in-line leak-testing closed filled containers filled with a filling product, comprising for each of said containers the step of detecting at least one analyte by means of a mass spectroscopy technique, wherein said at least one analyte comprises at least one of
       said filling product;   one or more components of said filling product;   a decomposition product of said filling product;   one or more decomposition products of one or more components of said filling product.       
 
         [0028]    And the invention also comprises further embodiments of this before-addressed method, namely those having in addition features corresponding to features of an embodiment of one of the before-addressed methods. 
         [0029]    The invention furthermore comprises: 
         [0030]    A method for manufacturing closed filled containers filled with a filling product, comprising for each container to be manufactured the steps of
       filling the respective filling product into the respective container or into a portion thereof;   closing said respective container;   extracting material from an environment of said respective of container;   guiding said extracted material to a mass spectrometer;   detecting by means of said mass spectrometer at least one analyte in said extracted material;
 
wherein said at least one analyte comprises at least one of
   said filling product;   one or more components of said filling product;   a decomposition product of said filling product;   one or more decomposition products of one or more components of said filling product.       
 
         [0040]    And the invention also comprises further embodiments of this before-addressed method, namely those having in addition features corresponding to features of an embodiment of one of the before-addressed methods. 
         [0041]    The invention furthermore comprises: 
         [0042]    A use of a mass spectroscopy technique, namely for evaluating a quality of a number of closed filled containers filled with a filling product by detecting at least one analyte by means of said mass spectroscopy technique, wherein said at least one analyte comprises at least one of
       said filling product;   one or more components of said filling product;   a decomposition product of said filling product;   one or more decomposition products of one or more components of said filling product;
 
in particular comprising extracting material from an environment of each of said number of containers or from an environment of two or more of said number of containers, and detecting said at least one analyte in said extracted material.
       
 
         [0047]    And the invention also comprises further embodiments of this use, namely those having in addition features corresponding to features of an embodiment of one of the before-addressed methods. 
         [0048]    The invention furthermore comprises: 
         [0049]    An apparatus for evaluating a quality of closed filled containers filled with a filling product, said apparatus comprising a mass spectrometer adjusted for detecting at least one analyte, wherein said at least one analyte comprises at least one of
       said filling product;   one or more components of said filling product;   a decomposition product of said filling product;   one or more decomposition products of one or more components of said filling product.       
 
         [0054]    Further embodiments of this apparatus are disclosed in the Patent Claims, particularly in the claims depending on claim  41 . And the invention also comprises further embodiments of this apparatus, namely those which in addition have features corresponding to features of one of the before-addressed methods or of the before-addressed use. 
         [0055]    The invention furthermore comprises: 
         [0056]    A production line for producing closed filled containers, comprising at least one apparatus according to the invention. 
         [0057]    Further embodiments of this production line are disclosed in the Patent Claims, particularly in the claims depending on claim  48 . And the invention also comprises further embodiments of this production line, namely those which in addition have features corresponding to features of one of the before-addressed methods or of the before-addressed use. 
         [0058]    It is to be noted that the invention also comprises embodiments of the above-described methods and embodiments of the above-described use, namely those which have in addition features corresponding to features of one of the before-addressed apparatuses or of the before-addressed production line. 
         [0059]    The present patent application discloses all embodiments of any of the addressed methods, of the addressed use, of the addressed apparatus and of the addressed production line which have features identical with or corresponding to features of any more explicitely disclosed embodiment, irrespective of that embodiment being an embodiment of any of the addressed methods, of the addressed use, of the addressed apparatus or of the addressed production line. 
     
    
     
       BRIEF DESCRIPTION OF DRAWINGS 
         [0060]      FIG. 1  is a schematic diagram generically showing processing steps according to the present invention. 
           [0061]      FIG. 2  is a schematic diagram generically showing processing steps in the analyzing or testing step in  FIG. 1  where a pre-conditioning step of the container, COND, is performed followed by a detection step, DETECT, with a first step to determine whether the container being tested fulfills first conditions and if so followed by a second detection step. 
           [0062]      FIG. 3  is a schematic diagram of one possibility of performing the two sub-step detection steps of  FIG. 2 . 
       
    
    
     DETAILED DESCRIPTION OF THE INVENTION 
       [0063]    Although the invention being amply described and taught in the summary of the invention as well as in the claims, it shall be further exemplified with the help of figures. According to  FIG. 1  there are most generically shown processing steps according to the present invention. In a step  1  addressed by “FILLING” a container  3  is filled with the product. If the filling product is not exclusively gaseous, there may or may not remain in the container  3  a space as shown in  FIG. 1  filled with a gas. Irrespective of the fact whether the container  3  is filled with a gas, a liquid or a solid, we address the overall content of the container after the filling step as filling product P. As may be seen in  FIG. 1  a container  3  which has passed through processing according to the present invention is exploited in the step addressed by “exploit”  5 . The product P′ which is exploited from container  3  according to step  5  for a respective use is the product P which is present in the container  3  after the filling step  1  and sealing step  7 . This as if such container was not subjected to the testing step  9  according to the invention but such container was filled, sealed and then just led to exploitation as e.g. delivered to a consumer. 
         [0064]    We call such product a “consumer product”. 
         [0065]    In other words no product is added to the container  3  which would be specifically provided to perform the specific processing step  9  according to the present invention. After the container  3  has been filled with the addressed product P the container is sealed as schematically shown in  FIG. 1  by a sealing step  7 . Such sealing is maintained during the subsequent processing step  9  up to exploitation in step  5 . After performing the sealing step  7  the container is subjected to the analyzing or TESTING step  9 . In this test or analyzing step  9  there is investigated, whether product P as contained in the container after sealing step  7  or possibly a product which results from the product contained in the container  3  has an impact on the atmosphere A which surrounds the container  3  subjected to step  9 . Thus, we may address the addressed testing to be performed upon the atmosphere A which surrounds, during performing testing or analyzing, a sealed container  3  with respect to the fact whether the product P or a reaction product of product P has a material impact on atmosphere A. Such impact is dependent from product P and is thus addressed in  FIG. 1  by the function A(P). 
         [0066]    If the analyzing or testing step  9  reveals by its result that the container does not fulfill predetermined conditions with respect to leakiness, then such container is rejected as addressed in  FIG. 1  by the output arrow N for “no”. Only if the addressed container having been analyzed or tested fulfils—Y—the addressed conditions, then it is freed for exploitation in generic step  5 . 
         [0067]    As has been addressed already before, the present invention resides on analyzing presence of a potential impact on atmosphere A dependent from product P, A(P) by means of mass spectroscopy technique. Thus, the analyzing or testing step  9  of  FIG. 1  includes or comprises mass spectroscopy—MS—analyzing so as to finally conclude upon exploitability of the container—Y—. Please note that the product of the container as exploited—step  5 —needs not necessarily be equal to the product in the container as sealed—step  7 —due to possible container internal product reaction. Therefore, the product is addressed by P′ in step  5 . 
         [0068]    Nevertheless and as will be schematically and principally explained in context with  FIG. 2 , it might be that a container analyzed in step  9  of  FIG. 1  is considered not fulfilling first predetermined conditions before an analyzing step by mass spectroscopy is at all applied to check on second predetermined conditions. Let us make an example: If a container under test is heavily leaking it might be advisable not to have such container to interact with the mass spectroscopy equipment so as not to overload such equipment by extensive amount of product pouring out of the container, but to detect first, whether the container is or is not heavily leaking (first predetermined conditions) and only to activate mass spectroscopical analyzing if no large leak is detected. 
         [0069]      FIG. 2  most schematically and generically addresses such processing. After having performed the sealing step  7  as of  FIG. 1  the testing or analyzing step  9  is performed. According to  FIG. 2  this testing or analyzing step  9 , as an example, comprises pre-conditioning the container as shown in step  9   a  named “COND”. In this step e.g. in a testing chamber (not shown) the container  3  is e.g. pressurized which may e.g. be performed by mechanical pressurizing members as shown at  13 , if at least a part of the container wall is flexible. A second example of such conditioning in step  9   a  is evacuating the surrounding A(P) of the container  3  as by a vacuum pump  15 . 
         [0070]    After performing such conditioning step  9   a  the container is subjected to the detection step  9   b  of the overall testing or analyzing step  9 . Thereby, as schematically shown in  FIG. 2  as a first stage  9   ba  of the detection step  9   b  there is first detected whether the container being tested fulfils first conditions, e.g. has a large leak. If there is detected that these first conditions as preestablished are fulfilled—Ya—e.g. the container has leakage in excess of a predetermined threshold amount, then the container addressed is rejected. If the container being tested does not fulfill the addressed first condition, e.g. has no “large leak” and is thus tight within the frame of the predetermined first tightness conditions, such container—Na—is subjected to the second detection step  9   bb , which step is performed by mass spectroscopically— 10 —analyzing the surrounding A(P) of the container. Only then the mass spectroscopy is exploited for analyzing the surrounding A(P) of the container. If and only if such mass spectroscopical analysis reveals that the container fulfils the second predetermined conditions, e.g. having a leakiness below predetermined extent, such container as addressed by Y b  is freed for further exploitation according to step  5  of  FIG. 1 , otherwise as addressed by N b  it is rejected. 
         [0071]    In  FIG. 3  there is again most schematically shown one possibility of performing the two sub-step detection steps  9   b  as of  FIG. 2 . The container has been conditioned according to step  9   a  of  FIG. 2  by evacuating in a testing chamber  11 . Operationally connected to the testing chamber  11 , there is provided a pressure sensor arrangement  19  as well as the mass spectroscopic equipment  21 . The sub-detection step  9   ba  for large leak detection is performed by evaluating the pressure course in the surrounding A(P) of the container  3 . This is addressed in  FIG. 3  by pressure evaluation  23 . With respect to such pressure evaluation we e.g. refer to the U.S. Pat. No. 5,907,093 and/or U.S. Pat. No. 6,305,215, both of the same applicant as the present application, which are with respect to large leak detection of liquid-filled containers to be considered as integrated part of the present description by reference. 
         [0072]    Back to  FIG. 3 : If by pressure evaluation  23  there is detected leakiness in excess of a predetermined amount and as addressed by “LL” in  FIG. 3 , operational connection S of the test chamber  11  to the mass spectroscopical equipment  21  is disabled. Only if by pressure evaluation  23  there is detected no large leak in the sense as addressed above, then operational connection S of the test chamber  11  to the mass spectroscopical equipment  21  is enabled, i.e. S in  FIG. 3  is closed. 
         [0073]    As was addressed above, containers which are filled and sealed shall be tested or analyzed according to step  9  of  FIG. 1  in line, i.e. the containers are conveyed in a stream. This necessitates making use of a mass spectroscopical equipment, which allows short-time subsequent analyzing. At the present moment it has been found that a SIFT-mass spectrographic technique as addressed in the enclosed papers is most suited to be applied in the present invention:
   A: SIFT-MS selected ion flow tube mass spectrometry   B: voice  200 , data sheet   C: Real-time resolution of Analytes, without . . . March 5h, 2004, Syft Technologies Ltd.   D: voice  200 , SIFT-MS at its best,   E: From flowing afterglow to SIFT-MS . . . Feb. 24, 2004, Syft Technologies Ltd.   
 
         [0079]    Further, attention is drawn to the DE 33 40 353 which teaches leak detection by mass spectrography and—in opposition to the present invention—by a tracer gas, which is filled to container specifically for testing purposes.