DE102014105552A1 - Reference product and method for validating the damage rate of fruit pulp processing plants - Google Patents

Abstract

The invention relates to a process for process validation of treatment processes of solids-containing, z. Fruit-containing beverages in a beverage treatment plant, comprising: providing a standardized validation reference product which may include solids, for example as reference for fruit pieces contained in the beverage, having at least one reproducible characteristic (107), infusing the validation reference product into the beverage treatment plant predetermined plant operating point and / or a predetermined plant operating mode and / or a predetermined validation time, the analysis of a validation reference product sample taken after a partial and / or a complete run of the validation reference product by the beverage treatment plant, comprising a measurement of the characteristic parameter (107) of the validation reference product, for description damage caused by the beverage treatment plant to the validation reference product.

Description

State of the art

The invention relates to a method specified in the preamble of claim 1. Art and a product specified in the preamble of claim 17 Art.

In the production and treatment of solids containing, especially fruit pieces, drinks, it is problematic to find criteria that allow the quality of the solids-containing beverage z. B. with regard to a desired by the customer or the customer of a beverage treatment plant minimum level of integrity of the solids contained in the beverage to describe.

This is partly due to the fact that the fruit pieces used are not uniform and have a large variety of size, shape and weight, so there are no Produktprozessvalidierungsmethoden with which statements about the quality of the processes for the production and treatment of solids containing, especially fruitaceous , Drinks, in particular with regard to possible damage to the individual solids contained in the drinks, in particular fruit pieces, would be to meet.

task

It is therefore an object of the invention to provide a suitable process validation of treatment processes of solids containing, z. B. fruit-containing beverages in a beverage treatment plant to create, in particular with regard to the description of the effects of the treatment processes on the solids or fruit pieces contained in the beverage.

solution

This is achieved according to the invention by a method according to claim 1 and a product according to claim 17. Advantageous embodiments and further developments are the subject of the dependent claims.

An inventive method for process validation of treatment processes of solids-containing, z. B. fruit pieces, drinks in a beverage treatment plant, eg. B. a bottling plant (with cold filling and / or hot filling), a mixing plant (eg., For the addition of concentrate to water), a system suitable for double-fill aseptic Zweistromverfahren, a sterilization system, a valve, a pipe - or pipe system, can include the following steps:
First, a standardized validation reference product may contain the solids, for example, as a reference for fruit pieces contained in the beverage, e.g. As peach, cherry, strawberry, or pineapple pieces, or fruit pulp, provided with at least one reproducible characteristic parameter.

In this case, the reproducible characteristic parameter of the provided validation reference product may have a predetermined initial value and / or a predetermined output distribution of the characteristic parameter.

The term validation reference product may here be understood inter alia to include both individual and also several reference particles or reference solid particles, as well as a reference mixture of reference particles or reference solid particles with liquid.

In this case, the inoculation of the validation reference product into the beverage treatment plant can take place at a predefined plant operating point and / or a predetermined plant operating mode and / or a predetermined validation time.

Preferably, the inoculation may be done when the beverage handling equipment has reached a stable plant operating mode equal to or near the normal production cycle to enable validation under conditions as close to production as possible.

One or more validation reference product samples may be taken from said beverage treatment plant after a partial and / or a complete run of the validation reference product by the beverage treatment plant.

Preferably, a plurality of validation reference product samples may be taken at the same and / or different plant stations of the beverage treatment plant so as to advantageously increase the statistical accuracy of the validation analysis.

The analysis of a retrieved validation reference product sample may include a measurement of the characteristic of the validation reference product.

Said analysis of a validation reference product sample may include, for example, measuring a current mean value and / or measuring the current distribution of the characteristic of the validation reference product of the validation reference product sample.

Further, the analysis of a validation reference product sample may also include a determination of the number, e.g. By simply counting solids or solid particles in the validation reference product sample having a predetermined characteristic, and / or determining the number of solids in the validation reference product sample that are within a predetermined interval of a predetermined characteristic.

In addition, at least one characteristic process validation parameter can be derived.

Said characteristic process validation parameter can be derived from a measurement of the characteristic parameter of the validation reference product of the validation reference product sample.

The derivation of a characteristic process validation parameter can here be based, for example, on a measurement of a current average value and / or a measurement of the current characteristic distribution of the validation reference product of the validation reference product sample, and / or a comparison of the measured current mean value of the characteristic of the validation reference product of the validation reference product sample and / or a comparison of the measured actual distribution of the characteristic parameter of the validation reference product of the validation reference product sample with or with the predefined initial value and / or with one or the predetermined output distribution.

The use of a standardized validation reference product with one or more reproducible characteristic values thus advantageously allows a starting or comparison reference to be defined by means of which the effects of the system on the validation reference product can be described by the analysis of validation reference product samples, in particular with regard to integrity and damage Thus, in order to make more reliable predictions or assurances about the integrity of the solids or fruit pieces, or the extent of possible damage or impairment of the actual solids-containing beverage caused by the beverage treatment process.

In this case, the at least one reproducible characteristic parameter of the validation reference product can be a reproducible shape and / or a reproducible size and / or a reproducible density and / or a reproducible weight and / or a reproducible strength, for example a reproducible compressive strength and / or z. A reproducible shear strength, and / or a reproducible fiber length of the validation reference product.

The validation reference product may advantageously be spherical or cube-shaped.

The description of a reproducible characteristic parameter of the validation reference product may be the specification of a radius, for example between 3 and 10 mm, and / or one or more edge lengths, for example between 3 and 10 mm, and / or a fiber length, for example between 3 and 15 mm, and or an average Feret diameter, for example between 3 and 15 mm, and / or the indication of a sphericity and / or the specification of a convexity of the validation reference product. The dimensions given, or absolute size dimension value ranges, are exemplary because they depend on the dimensioning of the the product or the validation reference product can depend on conductive plant components.

Preferably, said radius, and / or said edge length (s), and / or said fiber length, and / or said mean ferret diameter may have mean size dimensions less than 75% or less than 60% of the inner maximum cross-section of, e.g. , B. of the smallest, to be run by the validation reference product portion of the beverage processing plant, said inner maximum cross-section may be related to the maximum space diagonal of the plant part, and said plant part may for example be a filling member of a filling system, or a plant pipe or the like.

As a result, it can be advantageously avoided that the validation reference product clogs parts of the beverage treatment plant.

Particularly preferably, the validation reference product, or the validation reference product particles, may have a cube shape, for example with typical edge lengths of about 3 × 3 × 3 mm to 5 × 5 × 5 mm, or z. B. dimensioned in response to an inner maximum cross section of a beverage treatment plant part.

The possible use of a strength as a characteristic parameter of the validation reference product is also advantageous because z. B. remain in typical beverage treatment processes usually the strongest particles and only the soft ones are damaged or destroyed and disappear.

As noted above, strength, compressive strength, and / or shear strength may be used to establish a characteristic of the validation reference product / parameter of the validation reference product particle, since validation reference product particles are truncated or simply crushed, for example, on a sharp edge or in a shear flow can be.

Among other things, the use of a shear strength for establishing a characteristic parameter of the validation reference product has proved to be preferred.

Advantageously, the validation reference product particles may thereby have a strength distribution with a narrow distribution around the mean value, preferably the strength or shear strength may follow a probability distribution whose normalized density function has a variance of less than 0.5, or less than 0.2 or less than 0.1, may have.

This allows z. Advantageously, for example, exact counting of surviving validation reference product particles, i. H. validation reference product particles that have survived a test process path through the beverage processing plant with acceptable damage.

On the other hand, advantageously, the known or specified strength distribution of the validation reference product particles before inoculating the validation reference product particles into the beverage treatment plant to be tested / validated, with the strength distribution of the validation reference product particles in a validation reference product sample, taken after a partial and / or a complete Passage of the validation reference product are compared by the beverage treatment plant and serve as a basis for the assessment of damage caused by the beverage treatment plant damage.

For this purpose, as of course also for all other characteristic parameters of a validation reference product described here, test series with validation reference products with respectively different strength distributions or shear strength distributions can be carried out.

However, a validation reference product may also comprise a combination or mixture of validation reference product particles each having different predetermined distributions of a reproducible characteristic index, i. H. a validation reference product may comprise a mixture of validation reference product particles following different well-defined probability distributions for a given reproducible characteristic, e.g. B. Probability distributions of a reproducible characteristic with different predetermined expected values, different predetermined variations or different predetermined variances.

In particular, the use of a validation reference product with a mixture of validation reference product particles having several well-defined different strength distributions or shear strength distributions, for example a mixture of validation reference product particles having 3 to 5 different strength distributions or shear strength distributions, is conceivable.

This makes it possible to evaluate a grading of the expected damage to the validation reference product particles, which makes it possible to identify and / or evaluate differently damaging components of the beverage treatment system.

The decrease in certain strength fractions of a validation reference product, after passing through the process path under test, can be analyzed and evaluated and used to describe and evaluate damage to the validation reference product particles caused by the beverage treatment facility, for example, anticipating that the softer less solid particles in the validation reference product sample are expected to disappear first ,

Preferably, the strengths, i. H. For example, the compressive strengths and / or shear strengths of validation reference products of a test series may be selected such that their shear stress limit, i. H. the transition value between pure compressive load for destructive shear stress, in the size range of about 5 to 200 N, preferably at 10 to 100 N, may be.

The already mentioned sphericity, for example, can be defined as sphericity S for a given projection view of a validation reference product particle, as the ratio of the circumference U _EQ of the area _coextensive with the projection surface A of the validation reference product particle to the actual circumference U _real validation reference product particle in the given projection:

Further, for example, the above-mentioned convexity may be defined as the convexity φ for a given projection view of a validation reference product particle, as the ratio of the projection area A of the validation reference product particle to the area A _{KH of} the convex hull of the projection area A of the validation reference product particle

Tests have shown that cube-shaped validation reference product particles may be better able to describe potential damage to the validation reference product caused by the beverage treatment facility than, for example, compared to spherical validation reference product particles.

Cube-shaped validation reference product particles may e.g. B. first fringing, which can be well described by said convexity φ.

The convexity can thus be used as a characteristic parameter of the validation reference product, which is well suited for a damage evaluation.

Tests have shown the following values of convexity, which may be suitable for describing different levels of damage. For example, validation reference product particles having a convexity value of 0.5 or less, may be evaluated as being slightly compact and damaged, while well compact, barely or acceptably damaged particles having convexity values> 0.8 may be writable.

An exemplary tolerable damage threshold may be given with a convexity value of about 0.78 +/- 0.02.

Among other things, this describes very well that, in part, the corners of particles first fray and are cut off.

The reproducible characteristic parameter of the validation reference product can advantageously follow a probability distribution whose normalized density function can have a variance of less than 0.5 or less than 0.2 or less than 0.1.

The smaller the variance or spread of the probability distribution of the reproducible characteristic parameter, the better the validation reference product is suitable as a reliable and reproducible standard, for example with a well-defined initial value and / or well-defined initial distribution or output function, for the validation of the beverage treatment process.

For example, the probability distribution of the reproducible characteristic parameter may be a particle size distribution or a strength distribution, in particular a shear strength distribution or a compressive strength distribution.

Among other things, a reproducible characteristic parameter of the validation reference product may be, in particular, the density of the validation reference product whose mean value has a tolerance of z. B. better than +/- 1% compared to the solids-containing, z. B. fruit pieces, drink and / or in comparison may have solid or fruit piece of the actual product.

The density of the validation reference product or of the validation reference particles is thus advantageously as close as possible (max +/- 1%) to the density of the continuum phase (eg beverage) surrounding the validation reference particles, since the validation reference particles can optimally follow the process flow in order to find the most suitable and easiest to simulate again adjustable test case.

In particular, when evaluating the effect of inhomogeneities in the beverage, it is advantageous that the density of the validation reference particles corresponds to the density of the real product particles.

However, it is also conceivable, for example for test purposes, to set the density of the validation reference product as different as possible from the actual product.

Said derivation of the at least one characteristic process validation parameter may, for example, be a damage rate as a function of one or more characteristic parameters of the validation reference product.

wobei z. B. die Beschädigungsrate DR(X, K) in Abhängigkeit der charakteristischen Kenngröße X für eine bestimmte Kenngrößenkategorie und/oder eine bestimmte Kenngrößenklasse und/oder einen bestimmten Kenngrößenwertebereich K, in Prozent angegeben ist, und m(X) K / 0 der Ausgangswert, beispielsweise an einem Zeitpunkt vor oder gleich dem Zeitpunkt der Einimpfung des Validierungsreferenzprodukt in die Anlage, der Anzahl oder der Menge oder der Masse der Kenngröße X für eine bestimmte Kenngrößenkategorie und/oder Kenngrößenklasse und/oder einen bestimmten Kenngrößenwertebereich K, ist, und m(X) K / t ein Messwert zum Zeitpunkt t der Anzahl oder der Menge oder der Masse der Kenngröße X für eine bestimmte Kenngrößenkategorie und/oder Kenngrößenklasse und/oder einen bestimmten Kenngrößenwertebereich K ist, wobei der Zeitpunkt t die Entnahme der Validierungsreferenzproduktprobe markiert, bei der das Validierungsreferenzprodukt wenigstens einen Teil oder einen vollständigen Produktprozessweg der Anlage durchlaufen hat.By way of example, a damage rate, also referred to as a so-called damage rate DR, can be defined as follows:

where z. B. the damage rate DR (X, K) as a function of the characteristic parameter X for a certain characteristic category and / or a certain characteristic class and / or a specific characteristic value range K, is given in percent, and m (X) K / 0 the initial value, for example, at a time before or equal to the time of inoculation of the validation reference product in the plant, the number or quantity or mass of the characteristic X for a particular characteristic category and / or characteristic class and / or a specific characteristic value range K, and m (X) K / t is a measurement at time t of the number or quantity or mass of characteristic X for a particular characteristic category and / or characteristic class and / or a particular characteristic value range K, wherein the time t marks the withdrawal of the validation reference product sample at which the validation reference product is at least a part or through a complete product process path of the plant.

Alternatively, to mark the validation reference product sample value, for example, simply use the product process path traveled at the time the validation reference product sample is taken, or simply the location / station of extraction.

A characteristic category or characteristic class can, for example, be a category or class for defined shapes, eg. Sphere, cuboid, cube, fiber, polyhedron, etc., and / or sizes and / or densities and / or weights and / or strengths and / or shear loads and / or fiber length, or also the degree of integrity of the validation reference product, or the validation reference product particle, and the mesh size of a sieve or filter for analyzing the validation reference product sample.

In addition to mathematical or geometric definitions, empirical criteria may also be used to define said characteristic category or characteristic class, wherein, for example, characteristic categories or parameter classes based on manual visual definitions for an exemplary terminology for describing the damage of the validation reference product such as "undamaged", "virtually undamaged", " slightly damaged "," badly damaged "or" badly damaged "or" extremely / unusably damaged "can be used.

Exemplary characteristic value ranges may be value ranges for radius, for example between 3 and 10 mm, and / or for one or more edge lengths, for example between 3 and 10 mm, and / or fiber length, for example between 3 and 15 mm, and / or average heel diameter, for example between 5 and 15 mm, and / or sphericity, for example between 0.6 and 1.0 and / or convexity, for example between 0.6 and 1.0, of the validation reference product or validation reference product particle.

Also, a characteristic value range may include, for example, specifying a mesh size range of a sieve or filter for analyzing the validation reference product sample, for example mesh sizes between 5 and 100.

The use of a damage rate for a standardized validation reference product advantageously makes it possible to provide an easily interpretable process validation parameter which can be used, for example, for quality control of the beverage treatment process and can serve as a parameter in the optimization of the beverage treatment process.

wobei z. B. die Beschädigungsrate DR ^(X, K₁, K₂, ..., K_n) in Abhängigkeit der charakteristischen Kenngröße X aufsummiert bzw. kumuliert ist für Anzahl i ≥ 2 von Kenngrößenkategorien und/oder Kenngrößenklassen und/oder Kenngrößenwertebereiche K_i, in Prozent angegeben ist, und

der Ausgangswert, beispielsweise an einem Zeitpunkt vor oder gleich dem Zeitpunkt der Einimpfung des Validierungsreferenzprodukt in die Anlage, der Anzahl oder der Menge oder der Masse der Kenngröße X für eine bestimmte Kenngrößenkategorie und/oder Kenngrößenklasse und/oder einen bestimmten Kenngrößenwertebereich K_i, ist, und

ein Messwert zum Zeitpunkt t der Anzahl oder der Menge oder der Masse der Kenngröße X für eine bestimmte Kenngrößenkategorie und/oder Kenngrößenklasse und/oder einen bestimmten Kenngrößenwertebereich K_i ist, wobei der Zeitpunkt t die Entnahme der Validierungsreferenzproduktprobe markiert, bei der das Validierungsreferenzprodukt wenigstens einen Teil oder einen vollständigen Produktprozessweg der Anlage durchlaufen hat.Also a damage rate accumulated or accumulated over different characteristic categories and / or different characteristic classes and / or different characteristic value ranges K, for example referred to as DR ^, can be used to describe a process validation and, for example, be defined as:

where z. B. the damage rate DR ^ (X, K ₁ , K ₂ , ..., K _n ) is added up or accumulated as a function of the characteristic parameter X for the number i ≥ 2 of characteristic categories and / or characteristic classes and / or characteristic value ranges K _i , given in percent, and

the initial value, for example at a time before or equal to the time of inoculation of the validation reference product in the plant, the number or quantity or mass of the parameter X for a particular characteristic category and / or characteristic class and / or a specific characteristic value range K _i , and

is a measurement at time t of the number or quantity or mass of characteristic X for a particular characteristic category and / or characteristic class and / or a particular characteristic value range K _i , wherein the time t marks the withdrawal of the validation reference product sample at which the validation reference product is at least one Has gone through part or a complete product process path of the plant.

Furthermore, a characteristic process validation parameter can also be described from or through the particle size distribution in the validation reference product sample, in particular by the variance of the particle size distribution and / or by the slope of the cumulative particle size distribution cumulative curve.

In order to make the validation reference product as close as possible in consistency and / or density and / or concentration to a desired product, the validation reference product, or the validation reference product particles, may be swollen in a liquid, for example in water, before being seeded into the system ,

The desired concentration for validation reference product can be set, for example, in a slurry tank, wherein z. For example, typically the mass concentration of the validation reference product may be about 30 to 50 volume percent.

Furthermore, the validation reference product may contain one or more dyes, preferably food grade inks, e.g. B. Cochenillerot A (E124), a carrot extract red (E163), yellow beta-carotene (E160a), green from a mixture of indigotine (E132) and quinoline yellow (E104), methylene blue, or even a fluorescent food coloring material which may be released upon damage to the validation reference product such that a measured color intensity of the validation reference product may be used as the basis for a process validation parameter or for describing a corruption rate, respectively.

For example, the dye (s) may be encapsulated in a validation reference product particle.

Advantageously, the color can be chosen so that the best possible contrast to the color of the continuum phase (of the beverage) can be made possible.

The removal of the validation reference product sample after a partial or complete run of the validation reference product by the system may advantageously be depressurized or near-zero pressure and / or low shear, e.g. With shear rates of less than 5N to minimize the impact of damage to the validation reference product by the sampling process itself, which could distort the results of the analysis of the validation reference product sample.

If necessary, the system can be equipped with special unpressurized reservoirs along the product process path of the system

Incidentally, validation reference product samples may be taken along the entire product process path within the plant to better and more accurately identify critical beverage treatment processes or critical beverage treatment facilities, for example.

For example, in particular, a bottle filled with the validation reference product after passing through the plant can serve as a validation reference product sample.

Preferably, a multiple pass of the same validation reference product is to be avoided by the entire process path of the system, since in normal operation, the drink to be treated also passes through the entire system only once.

For a most reliable statistical analysis of the effects of the beverage treatment process or the plant on the validation reference product, it is advantageous if the validation reference product sample number is as high as possible, for example a number of more than 3, 10, or more than 20 validation reference product samples, or for example more than 3, 10, or more than 20 bottles filled with the validation reference product after running the system.

The analysis of the validation reference product sample may include a computer-implemented image evaluation method that can image the validation reference product and derive characteristic characteristics, in particular shape data and size data, of the validation reference product from image contour data of the validation reference product, for example to generate a particle shape distribution and / or particle size distribution of the validation reference product particles in the validation reference product Validation reference product sample after at least partial passage of the product process path, for comparison with the particle shape distribution and / or particle size distribution of undamaged validation reference product particles.

One of the advantages of this computer-assisted imaging is that once the data of the validation reference product has been recorded and stored, it can be quickly analyzed with a variety of statistical evaluation methods and algorithms.

Further, the analysis of the validation reference product sample may include performing a manually and / or automatically performed screen cascade, wherein, for example, a screen cascade using mesh sizes between 5 (mesh 4.00 mm) and 100 (mesh 0.149), or using meshes between 8 mm and 0.149 mm, can be made.

An exemplary preferred suitable mesh grading or mesh grading of a z. B. five-stage screen cascade is z. Given by the mesh sizes 8.00 mm (no corresponding mesh size designation defined), 6.00 mm (no corresponding mesh size designation defined), 4.00 mm (mesh 5), 2.00 mm (mesh 10) and 0.85 mm (mesh 20).

Different stage sieve cascades, d. H. of course with a different number of sieves or screening stages and / or other mesh sizes or mesh sizes, depending on requirements.

The mesh size can serve to establish or identify a characteristic category and / or a characteristic class and / or a characteristic value range.

With this comparative sieve cascade, for example, a particle size distribution and / or particle mass distribution of the validation reference product particles which at least partially pass through the system can be established, which in turn can be compared with the particle size distribution and / or particle mass distribution of the undamaged validation reference product particles as the starting reference.

The analysis or evaluation of the validation reference product sample can essentially also be carried out manually by the plant personnel, e.g. B. based on previously agreed evaluation criteria, eg. B. defined categories or classes of characteristic characteristics or for different ranges of characteristic values, suitable for a description of damage caused by beverage treatment processes of the validation reference product.

Previously agreed rating categories or rating classes for describing the corruption of the validation reference product may, as mentioned above, e.g. For example, by agreed definitions of the terms "undamaged", "virtually undamaged", "slightly damaged", "clearly damaged" or "severely damaged" or "extremely / unusably damaged".

The analysis of the validation reference product sample may thus include a manual evaluation of the validation reference product sample particles, in particular z. For example, a manual measurement of the dimensions of the validation reference product sample for comparison with dimensions of undamaged validation reference product particles.

In an optical assessment or haptic assessment, e.g. B. by means of the human sense of sight or the human sense of touch by pressing the finger, it may be possible to dispense with a Siebkaskade. Since it may be sufficient, the samples with a sieve z. B. the mesh 20 from seven and by hand, d. H. manually, to sort and then z. B. according to specified evaluation criteria for undamaged or damaged, or as listed above, count.

In a manual analysis or evaluation of the validation reference product sample z. For example, for a touch comparison, the particles of the validation reference product sample are compared with corresponding intact comparison particles of the validation reference product.

For example, in a manual analysis of the validation reference product sample by an optical comparison, the dimensions of the particles of the validation reference product sample may be linearly measured or measured by measuring the particles of the validation reference product sample on a normalized and scaled pad , z. Millimeter paper, and the dimensions of the validation reference product sample particles on said base can be read.

The results of this manual measurement of the particles of the validation reference product sample can then be compared again with the known dimensions of the intact comparison particles of the validation reference product so as to be able to arrive at a description or damage to the validation reference product caused by a beverage treatment process.

A standardized validation reference product according to the invention for use in a process for process validation of treatment processes of solids-containing, eg. B. fruit pieces, drinks in a beverage treatment plant, thus having at least one reproducible characteristic parameter, for example, said at least one reproducible characteristic, a reproducible shape and / or a reproducible size and / or a reproducible density and / or a reproducible weight and / or a reproducible strength and / or reproducible shear resilience of the validation reference product.

Although it is self-explanatory, for the sake of completeness, it should be noted that, since this is primarily the validation of processes in the food industry, the validation reference products and / or dyes are said to be harmless to health. However, this would not necessarily be necessary for a food industry remote use of the invention.

The following figures are an example:

1a : Exemplary probability distribution of an exemplary reproducible characteristic of a standardized validation reference product.

1b : Exemplary probability or frequency distribution of a non-reproducible characteristic of an actual solids-containing beverage product.

2 Exemplary comparison of the cumulative distribution for a characteristic parameter of a standardized validation reference product between the output reference and the validation reference product sample after at least partial passage of the product process path.

3a : Exemplary description of the sphericity of a validation reference product particle.

3b : Exemplary description of the convexity of a validation reference product particle.

3c : Exemplary description of a Feret diameter of a validation reference product particle.

The 1a exemplifies a possible normalized probability or frequency distribution 100 , or an output distribution, of an exemplary reproducible characteristic parameter 107 plotted along the linear or logarithmically scaled abscissa axis 101 , a standardized validation reference product in differential as well as integral representation.

Exemplary is both the density function 103 as well as the sum function 104 depending on the exemplary characteristic parameter 107 shown.

The ordinate axis of the density function 103 is for example the axis 102 and the ordinate axis of the sum function 104 for example, the axis 105 ,

The density function 103 Among other things, it can be distinguished by the fact that, for example, it can be described well with a normal distribution, with a well-defined half-width 113 (eg definable as difference of the values 111 . 112 the characteristic parameter 107 where the density function 103 takes half the maximum value, z. B. also bezeichbar as Full width at half maximum FWHM, z. Defined as a function of the standard deviation σ over FWHM = 2√ 2ln2 σ) or well-defined variance (definable as a square of the standard deviation, ie σ ² ), the z. B. may be less than 0.5 or less than 0.2 or less than 0.1.

In other words, the characteristic parameter 107 a well-defined expectation or mean 106 having a small or small standard deviation σ deviation from said expected or average value compared to characteristics of non-standardized solids-containing products or non-standardized particles 106 ,

The sum function 104 is also characterized by a steeper slope and smaller width compared to characteristics of non-standardized solids-containing products or non-standardized particles 108 , the difference between the minimum 109 and maximum value 110 the characteristic parameter 107 , out.

By way of example, the particle size, and / or particle mass and / or fiber length as a possible characteristic parameter may be mentioned here as an example 107 called.

A validation reference product according to the invention can therefore be characterized in particular by the fact that it can be described by characteristic parameters whose density function or sum function are standardized and readily reproducible.

The 1b exemplifies a possible normalized probability or frequency distribution 200 an exemplary non-reproducible characteristic parameter 206 plotted along the linear or logarithmically scaled abscissa axis 201 , a standardized validation reference product in differential as well as integral representation analog and directly comparable to 1a represents.

Exemplary is both the density function 203 as well as the sum function 204 depending on the exemplary characteristic parameter 206 shown.

The ordinate axis of the density function 203 is for example the axis 202 and the ordinate axis of the sum function 204 for example, the axis 205 ,

For a nonstandard solids-containing product or for non-standardized particles, the values of the density function 203 the characteristic parameter 206 much wider than in the case of 1a illustrated standardized validation reference product and the density function 203 can be much more irregular and varied than the comparatively simple density function 103 the standardized validation reference product.

For example, the maximum peak value 207 peak or main peak 210 the density function 203 not necessarily representative of the distribution of the characteristic parameter 206 because the density function 203 more than one peak, sometimes of similar magnitude, e.g. B. peak or secondary peak 209 , may have.

The sum function shown as an example 204 the characteristic parameter 206 is therefore opposite to the summation function 104 greatly widened z. B. and, starting from a same normalization of the axes in 1a and 1b , the width 208 the sum function 204 many times larger than the width 108 the sum function 104 ,

Furthermore, the slope of the sum function is also 204 significantly lower than the slope of the sum function 104 ,

But above all, in a non-standard solids-containing product, the density function 203 and the sum function 204 the characteristic parameter 206 not reproducible and even exposed to a sometimes large dispersion.

The 2 exemplifies on the one hand the summation function 303 a characteristic parameter 307 a standardized validation reference product without the intervention of a treatment process or before the inoculation of the validation reference product into the system to be validated, ie an output distribution, or an output or reference sum function, and secondly a summation function 304 a validation reference product sample, taken after partial or complete run of the validation reference product by the plant, also denominated as a sample sum function.

For example, the damage to the validation reference product caused by the treatment processes of the equipment may be manifested as changes in the slope and width of the cumulative function 303 In particular, a reduction in the slope and an increase in the width 305 the sum function or sample sum function 304 compared to the output sum function 303 observable.

These changes in the slope and / or width of the sum function of a characteristic parameter of a standardized validation reference product can also be used to describe a process validation parameter or to describe damage to solids caused by the system, for example pieces of fruit, in beverages.

For completeness, it should be mentioned that reference numerals 301 and 302 the abscissa or ordinate of the illustrated probability distribution comparison 300 describe.

The 3a Illustratively and illustratively, illustrate the sphericity S for a given projection view of a particle 400 , defined as the ratio of the circumference U _EQ , 404 of the projection surface A, 401 of the particle of the same area circle 405 to the real extent U _{real of} the particle 401 in the given projection, so:

For example, if the sphericity of the validation reference product or particles of the validation reference product is known before a treatment process affects the validation reference product, it may be measured with a measured sphericity or with the measured sphericity of the particles from the validation reference product sample taken after the device has partially or completely traversed the validation reference product to be compared. A change in the sphericity of the particles of the validation reference product caused by effects of treatment processes of the plant can in turn be used as a description of a process validation parameter or to describe damage to solids, for example pieces of fruit, in beverages caused by the plant.

The 3b Illustratively and by way of illustration, illustrate the convexity φ for a given projection view of a particle 500 is, as a ratio of the projection area A, 501 of the particle to the area A _{KH of} the convex hull 504 its projection surface A, the convex hull being that of particles 500 released concave area B, 503 with, ie A _KH = A + B, ie

Analogous to the sphericity of the validation reference product or particles of the validation reference product, the convexity φ can also be used to derive a process validation parameter in which a convexity φ measured on a validation reference product sample, or the convexities measured on the particles from the validation reference product sample with a known output convexity of the Validation reference product can be compared, and so for describing caused by the treatment process damage to solids, such as fruit pieces, in drinks serve.

The 3c exemplifies for better understanding and purely illustrative the determination of a possible Feret diameter 603 of a particle 600 Defined by the distance 603 two tangents 601 . 602 to the particle contour 604 in a fixed measuring direction.

In other words, a Feret diameter can be interpreted as the result of a caliper.

As a possible characteristic parameter, a Feret diameter averaged over several measuring directions and / or a maximum or minimum Feret diameter can be used.

Also, a Feret diameter as determined above is useful for deriving a process validation characteristic in which changes in Feret diameters measured on particles of the validation reference product sample are compared to the initial Feret diameter value of the standardized validation reference product.

Incidentally, the possible characteristic parameters exemplified here are particularly well suited for being measured and analyzed by computer-implemented image acquisition and evaluation methods.

LIST OF REFERENCE NUMBERS

100

Probability or frequency distribution of an exemplary reproducible characteristic parameter of a standardized validation reference product.

101

abscissa

102

first ordinate axis

103

density function

104

sum function

105

second ordinate axis

106

Expectation or mean value of the characteristic parameter

107

characteristic parameter

108

Width of the sum function

109

minimum value of the characteristic parameter

110

maximum value of the characteristic parameter

111

first value of the characteristic characteristic at which the density function 103 takes half the maximum value.

112

second value of the characteristic characteristic at which the density function 103 takes half the maximum value.

200

Probability or frequency distribution of an exemplary non-reproducible characteristic parameter

201

abscissa

202

first ordinate axis

203

density function

204

sum function

205

second ordinate axis

206

characteristic parameter

207

maximum peak value

208

Width of the sum function

209

Peak, secondary peak

210

Peak, main peak

300

Probability distribution comparison

301

abscissa

302

axis of ordinates

303

Sum function, output or reference sum function

304

Sum function of the validation reference product sample, taken after partial or complete run of the validation reference product by the plant, also denominated as a sample sum function

305

Width of the sum function 305

306

Width of the sum function 303

307

characteristic parameter

400

Particles, validation reference product particles, validation reference product sample particles

401

Projection surface of particles

402

Projection surface of circle 405 coextensive with the projection area of particles 400

403

actual volume of particles 400 in the given projection

404

Perimeter of the projected area of particles 400 coextensive circle

405

to the projection surface of particles 400 coextensive circle

500

Particles, validation reference product particles, validation reference product sample particles

501

Projection surface of particles

502

Projection surface of particles

503

of particles 500 released concave area B

504

convex hull

600

particle

601

first tangent to particle contour

602

second tangent to particle contour

603

Feret diameter

604

particle shape

Claims (17)

Method for process validation of treatment processes of solids-containing, eg. B. fruit-containing beverages in a beverage treatment plant, comprising: providing a standardized validation reference product may contain solids, for example, as a reference for fruit pieces contained in the beverage, with at least one reproducible characteristic parameter ( 107 ), Inoculating the validation reference product into the beverage treatment plant at a predetermined plant operating point and / or a predetermined validation time, analyzing a validation reference product sample taken after a partial and / or complete run of the validation reference product by the beverage treatment plant, comprising a measurement of the characteristic Characteristic ( 107 ) of the validation reference product, and derivation of at least one characteristic process validation parameter for describing damage to the validation reference product caused by the beverage treatment facility. The method of claim 1, wherein analyzing a validation reference product sample, determining the number of solids in the validation reference product sample having a predetermined characteristic, and / or determining the number of solids in the validation reference product sample at a predetermined interval a predetermined characteristic characteristic. The method of claim 1 or 2, wherein the analysis of the validation reference product sample comprises measuring the current mean value of the current distribution of the characteristic of the validation reference product of the validation reference product sample, and / or measuring the current distribution of the characteristic of the validation reference product of the validation reference product sample. Method according to one of the preceding claims, wherein the at least one reproducible characteristic parameter ( 107 ) of the validation reference product a reproducible shape and / or a reproducible size and / or a reproducible density and / or a reproducible weight and / or a reproducible strength, for. B. a reproducible pressure resistance and / or z. A reproducible shear strength, and / or a reproducible fiber length of the validation reference product. Method according to one of the preceding claims, wherein the description of a reproducible characteristic parameter ( 107 ) of the validation reference product, the specification of a radius, for example between 3 and 10 mm, and / or one or more edge lengths, for example between 3 and 10 mm, and / or a fiber length, for example between 3 and 15 mm, and / or a medium Feret Diameter, for example between 3 and 15 mm, and / or includes the indication of a sphericity and / or the specification of a convexity of the validation reference product. Method according to one of the preceding claims, wherein the at least one reproducible characteristic parameter ( 107 ) of the validation reference product is a reproducible crush strength or a reproducible shear strength, and the validation reference product comprises a combination of validation reference product particles each having different predetermined compressive strength distributions or shear strength distributions. Method according to one of the preceding claims, wherein a reproducible characteristic parameter ( 107 ) of a probability distribution ( 100 ) whose normalized density function ( 103 ) has a variance less than 0.5 or less than 0.2 or less than 0.1. Method according to one of the preceding claims, wherein a reproducible characteristic parameter ( 107 ) of the validation reference product is the density of the validation product whose mean value has a tolerance of better than +/- 1% compared to the solids-containing, eg. B. fruit-containing, beverage. Method according to one of the preceding claims, wherein the derivation of the at least one characteristic process validation parameter a damage rate in dependence of one or more characteristic characteristics ( 107 ) of the validation reference product. Method according to one of the preceding claims, wherein the derivation of the at least one characteristic process validation parameter takes into account the particle size distribution in the validation reference product sample, in particular the variance of the particle size distribution and / or the slope of the cumulative particle size distribution curve. A method according to any one of the preceding claims wherein the validation reference product contains a dye which is released upon damage to the validation reference product. A method according to any one of the preceding claims, wherein the validation reference product is swollen in a liquid, for example in water, prior to being seeded into the plant. The method of any of the preceding claims, wherein the removal of the validation reference product sample after a partial pass of the validation reference product through the plant is unpressurized. Method according to one of the preceding claims, wherein the analysis of the validation reference product sample comprises a computer-implemented image evaluation method, which images the validation reference product and derives characteristic parameters, in particular shape data and size data, of the validation reference product, for example from image contour data of the validation reference product. The method of any preceding claim, wherein the analysis of the validation reference product sample comprises manually evaluating the validation reference product sample particles, in particular comprising manually measuring the dimensions of the validation reference product sample particles for comparison to dimensions of intact validation reference product particles. The method of any preceding claim, wherein the analysis of the validation reference product sample comprises performing a sieve cascade, wherein, for example, a sieve cascade is performed using mesh sizes 6 and / or 12 and / or 20 and / or 100. Standardized validation reference product for use in a process validation process for solids containing, e.g. B. fruit pieces, drinks in a beverage treatment plant, with at least one reproducible characteristic parameter ( 107 ), wherein, for example, said at least one reproducible characteristic parameter ( 107 ), a reproducible shape and / or a reproducible size and / or a reproducible density and / or a reproducible weight and / or a reproducible strength, for. B. a reproducible pressure resistance and / or z. And / or a reproducible shear strength of the validation reference product.

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