|Title of Invention||
ICE CONTAINING PRODUCT HAVING BIMODAL FROZEN PARTICLE DISTRIBUTION FOR IMPROVED FLOW/SOFTNESS CHARACTERISTICS
THE PATENTS ACT, 1970
(39 of 1970)
The Patents Rules, 2003
(See Section 10 and Rule 13)
HINDUSTAN LEVER LIMITED, a company incorporated under the Indian Companies Act, 1913 and having its registered office at Hindustan Lever House, 165/166, Backbay Reclamation, Mumbai -400 020, Maharashtra, India
The following specification particularly describes the invention and the manner in which it is to be performed
Field of the invention
The invention relates to ice-containing products with inclusions, which have a
5 particular bimodal frozen particle distribution that gives improved product flow/softness characteristics and a process for production of such products.
Summary of the invention
We have developed novel frozen compositions comprising inclusions, typically
10 frozen food products, that are softer than the equivalent products having the
same ingredients and ice content and made by conventional processes. The
process used to make such products involves manipulating the ice phase by
substituting some of the ice present in the final product with frozen particle
inclusions in the mm size range (as compared with the typical ice crystal size of
15 less than 0.1 mm and the typical inclusion size of greater than 5mm). We have
found that not only is it important that the larger frozen particle inclusions are in a
particular size range, but also that the ratio of the weight of the population of large
frozen particle inclusions to the weight of the population of small ice crystals
formed when the remainder of the product is frozen is important in providing an
20 optimum product.
The resulting bimodal ice distribution where the sizes of the ice crystals in one population and the frozen particles in the other population are within certain size ranges and the two populations are present in certain proportions, leads to
25 products which are softer, for example having improved spoonability and/or scoopability when taken straight from the freezer, i.e. at about -18°C. It is also possible to produce frozen products, such as ice confections, that are squeezable when taken straight from the freezer.
30 An additional advantage of adding inclusions in this way is that where the inclusions are fruit pieces or the like, it is possible to maintain the desirable properties of the fruit, such as flavour and texture, through the reduced heat
F3389 (c) com
processing of the fruit ingredients i.e. direct addition of frozen fruit eliminates the need to thaw the fruit and heat it during mixing and pasteurization.
Accordingly, in a first aspect, the present invention provides an ice-containing
5 product, such as a frozen food product, which comprises at -18°C, (i) a first population of frozen particles, which first population comprises frozen edible particles having a particle size of greater than 1 mm and less than 5mm; and (ii) a second population of ice particles having a mean particle size such that the ratio of the mean particle size for the first population to the mean particle size for the
10 second population is greater than 9, preferably 10, wherein the ratio of the weight of the first population of particles to the weight of the second population is from 2:3 to 9:1, preferably 2:3 to 4:1 or 3:1, and the first population and second population together provide at least 90%, preferably at least 95%, of the frozen particles present in the ice-containing product.
Preferably the ice-containing product is an ice confection.
In a second aspect, the present invention provides a method for producing an ice-containing product, such as a frozen food product, which method comprises in the
20 following order.
(i) cooling a product concentrate to a temperature of below -4°C; (ii) combining the cooled concentrate with frozen particles, a substantial proportion of which have a particle size of greater than 5 mm, said particles comprising frozen edible particles; and
25 (iii) mechanically reducing the size of the frozen particles such that substantially all of the resulting frozen particles have a size of greater than 0.5 mm and less than 5 mm; and optionally
(iv) lowering the temperature of the product obtained in step (iii) to a temperature of-18°C or lower.
Preferably the ice-containing product is an ice confection.
Preferably the concentrate is a frozen confectionery premix concentrate.
In one embodiment, the method further comprises a step (v) of adding an aqueous liquid to the product obtained in step (iii) or step (iv).
In a related aspect the present invention provides an ice-containing product obtainable by the method of invention. Also provided is an ice-containing product obtained by the method of invention.
10 Detailed description of the invention
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art (e.g. in frozen confectionery manufacture). Definitions and descriptions of various terms and techniques used in frozen confectionery manufacture are found in Ice Cream,
15 4th Edition, Arbuckle (1986), Van Nostrand Reinhold Company, New York, NY.
Tests and Definitions
20 Ice-containing products of the invention can be aerated or unaerated. The term "aerated" means that gas has been intentionally incorporated into the product, such as by mechanical means. The gas can be any food-grade gas such as air, nitrogen or carbon dioxide. The extent of aeration is typically defined in terms of "overrun". In the context of the present invention, %overrun is defined in volume
25 terms (measured at atmospheric pressure) as:
The amount of overrun present in the product will vary depending on the desired 30 product characteristics. For example, the level of overrun in ice cream is typically
from about 70 to 100%, whereas the overrun In water ices is typically less than 20%.
An unaerated Ice-containing product preferably has an overrun of less then 20%,
5 more preferably less than 10%. An unaerated frozen food product is not subjected to deliberate steps such as whipping to increase the gas content. Nonetheless, it will be appreciated that during the preparation of unaerated frozen food products, low levels of gas, such as air, may be incorporated in the product.
10 Ice Content
Ice content is measured by adiabatic calorimetry as described by de Cindio and Correra in the Journal of Food Engineering (1995) 24 pp.405-415. Calorimetric techniques, particularly adiabatic calorimetry, have proved to be the most suitable, since they can be used on complex food systems, and do not require
15 any other information about the food, such as composition data, unlike some of the other techniques. The larger measured sample size (80g) allows measurement of heterogeneous samples such as those claimed with varied ice particle sizes.
20 Size, Area Size and Volume
Frozen particles are 3-dimensional objects, often of an irregular shape. However, methods for viewing and measuring such particles are often 2-dimensional (see below). Consequently, measurements are often made solely in one or two dimensions and converted to the required measurement.
By "area size", we mean the maximum area as seen in the image plane (i.e. when viewed using optical imaging). Typically at least 500 particles should be measured.
30 The size and volume of a particle can be calculated from an area size
measurement by assuming a regular shape for the particle and calculating the size or volume on that basis. Typically, the assumed regular shape is a sphere
and therefore the size is 2 X the square root of (the area size/pi). This is described in detail below.
Measurements are made at -10°C or -18°C. However, size, area and volume
5 measurements made at -10°C, whilst easier to perform, will need to be converted to an equivalent at -18°C as described below. Measurements are made at standard pressure.
Frozen Particle Size Distribution
10 The frozen particle size distribution of a frozen product can be measured as follows.
All equipment, reagents and products used in sample preparation are equilibrated 15 to the measurement temperature (-10°C) for at least 10 hours prior to use.
A 10 gm sample of the frozen product is taken and added to 50 cm3 of dispersing solution (20% ethanol in aqueous solution) and gently agitated for 30s or until the sample has completely dispersed into single particles. The whole ice / ethanol /
20 water mix is then gently poured into a 14 cm diameter petri dish - ensuring complete transfer and again gently agitated to ensure even dispersal of the ice particles in the dish. After 2 s (to allow for cessation of particle movement) an image is captured of the full dish.
25 Ten replicate samples are taken for each product.
The aqueous ethanol dispersing solution can be designed to match the
measurement conditions of the experimental system - see 'Concentration properties of Aqueous solutions: conversion tables' in "Handbook of Chemistry
30 and Physics", CRC Press, Boca Raton, Florida, USA.
Images can be acquired using a domestic digital camera (e.g. JVC KY55B) with its macro-lens assembly as supplied. The camera is selected to provide sufficient magnification to reliably image particles with an area size from 0.5 mm2 to greater
5 than 50 mm2. For imaging, the petri dish containing the sample was placed on a black background and illuminated at low angle (Schott KL2500 LCD) to enable the ice to be easily visualised as bright objects.
10 Image analysis was conducted using the Carl Zeiss Vision KS400 Image analysis software (Imaging Associates Ltd, 6 Avonbury Business Park, Howes Lane, Bicester, 0X26 2UA) with a macro programme specifically developed to determine the area size of each particle in the image. User intervention is required to remove from the image: the edge of the petri dish, air bubbles,
15 coincidentally connected ice particles and any residual undispersed material. Of these features, only the apparent connection between ice particles is relatively frequent.
The 10 samples taken allow for the sizing of at least 500, and typically several
20 thousand, particles for each product characterised. From this image analysis it is
possible to calculate two defining characteristics of the frozen edible particles (above 0.5mm2) that are structuring these systems:
(i) the range and mean of the diameters of the larger included frozen edible particles.
25 (ii) the volume and hence weight that the larger included frozen edible particles made to the original 10gm sample.
The estimate of volume of the frozen edible particles is made by converting the two-dimensional area analysis into a calculated volume, fL. This is done
30 according to the measured diameter of each particle. Hence:
1. For spherical particles (such as particles smaller than the gap size 'd' of the
cutting blades of the crushing pump of Figure 1) where the particles are assumed
to be spherical) the measured area is converted to an equivalent circle area with
associated, diameter and radius. This equivalent radius is then used to calculate
5 the equivalent volume sphere (mm3). The diameter represents the particle "size" in terms of length.
2. For non-spherical particles, the calculations will depend on the shape. For
example those larger than the gap size 'd' of the cutting blades of the crushing
10 pump of Figure 1, the particles are assumed to be planar disks with area as measured and a thickness given by the cutting blades 'd' to yield the particle volume (mm3).
Additionally, the temperature at which measurements are made (-10°C) could be
15 different from the production or storage temperature of the product. In this case it is necessary to estimate the 'difference* in the amount of ice from the original system (where appropriate). This estimate can be made using the methodology described in WO98/41109 or by direct calorimetric measurement as described in de Cindio and Correra (ibid). The 'difference' amount is then attributed back
20 each measured frozen particle on a basis linearly proportionate to its measured volume to provide the final estimate of the volume and the volume size distribution in the original sample.
The estimated volume of the frozen edible particles measured by this image
25 analysis procedure therefore also yields the weight of frozen edible particles fL in initial products by multiplying the estimated volume by the known density of the particles.
Proportion of frozen particles and small ice crystals
30 The amount by weight of small ice crystals fs can be measured using adiabatic calorimetry (described above) on a sample of the frozen concentrate to which no
large frozen edible particles have been added, or on a sample of the product from which large frozen edible particles have been removed.
From this and the weight of larger added frozen edible particles (fL), calculated in
5 the preceding section,
the ratio of larger frozen edible particles to smaller ice is then calculated as fL / fs
Scanning Electron Microscopy
The microstructure of samples was visualised by Low Temperature Scanning 10 Electron Microscopy (LTSEM).
The samples were cooled to -80°C on dry ice prior to SEM sample preparation. A sample section was cut (6mm x 6mm x 10mm) and mounted on a modified sample holder using a compound: OCT ™ at the point of freezing. OCT is an
15 aqueous embedding medium used primarily for cryotome preparation of material for light microscopy. It is also called 'tissue tek' and is supplied by Agar Scientific. The advantage of using OCT rather than water to mount the samples for electron microscopy is that when OCT changes from liquid to solid i.e. freezes it changes to opaque from transparent allowing visual identification of the freezing point.
20 Identification of this point allows the sample to be mounted using a liquid at its coldest just prior to solidifying which will give strong support during rapid cooling. The sample including the holder was plunged into liquid nitrogen slush and transferred to a low temperature preparation chamber: Oxford Inst. CT1500HF (Oxford Instruments, Old station way, Eynsham Whitney, Oxon, 0X29 4TL, UK).
25 The chamber is under vacuum, approximately 10"4 -10'5 mbar, and the sample is warmed to -90°C. Ice is slowly etched to reveal surface details not caused by the ice itself, so water is removed at this temperature under constant vacuum for 2-3 minutes. Once etched, the sample is cooled to -110°C to prevent further sublimation, and coated with gold using argon plasma. This process also takes
30 place under vacuum with an applied pressure of 10"1 millibars and current of 5 milliamps for 30 sec. The sample is then transferred to a conventional Scanning Electron Microscope (JSM 5600 - Jeol UK Ltd, Jeol House, Silvercourt
Watchmead, Welwyn Garden City, Herts, AL7 1LT, UK)), fitted with an Oxford Instruments cold stage at a temperature of -150°C. The sample is examined and areas of interest captured via digital image acquisition software.
5 From these digital images it is possible to visualise the smaller ice particles (less than 0.5 mm2) and the mean particle size diameters can be calculated.
Particle size ratio
The ratio of mean particle sizes of the smaller and larger ice distributions can be
10 calculated from the LT SEM and optical microscopy analysis, respectively. This ratio is expressed as
0Ll 0s - Mean Larger Particle Distribution / Mean Smaller Particle Distribution
15 The dry weight of the system as measured by the oven drying method as described in Ice Cream 6th Edition, Marshall et al. (2003), p296.
Hardness Test (Vickers)
The Vickers hardness test is an indentation test that involves pushing a pyramid
20 shaped indentor into the surface of a material and recording the force applied as a function of tip displacement. Force and displacement are measured during the indentation loading cycle and the unloading cycle.
The Vickers pyramid geometry is an engineering industry standard (Bsi
25 427,1990). It has an apex angle at the tip of 136°. Hardness is determined as Hv = Fmax/ A where Hv is the Vickers Hardness, Fmax is the maximum applied force (see Fig.) and A is the projected area of the indentation left in the material surface. The area A is determined by assuming the indentation has the same geometry as the indentor that formed it and therefore the projected area can be
30 determined from the indent depth given by di (Fig) then A = 24.5 di2. The Vickers Hardness of a material is a measure of the material's resistance to plastic deformation.
The test samples were collected in small pots and after hardening (-25°C) equilibrated at the test temperature (-10°C or -18°C) overnight beforehand. Measurements were conducted on a universal testing machine made by Instron
5 (Code 4500) within a temperature controlled cabinet at -18°C. The crosshead speed was 2mm/min. The maximum load was 95 N. The pyramid tip was pushed into the surface of the material to a depth of 1.5 mm for a water ice or sorbet and 2.5 mm for an ice cream.
10 Except in the examples, including any comparative examples, or where otherwise ( explicitly indicated, all numbers in the description and claims should be understood as modified by the word "about".
15 Ice-containing products of the invention, such as ice confections, are characterised by a particular bimodal distribution of frozen particles, which give a softer, more flowable rheology than the equivalent product made with a unimodal ice distribution. The bimodal distribution is made up of two distinct populations of frozen particles. The first population (frozen edible particles) has a relatively
20 large particle size and the second population (ice crystals) has a small particle size, of the order that would be obtained using standard methods for freezing ice confections in a slush freezer, i.e. less than 100 //m.
Preferably the products have a Vickers Hardness of less than 4 MPa at -18°C, 25 more preferably less than 3 or 2 MPa at -18°C.
Importantly, the weight of the first population of frozen edible particles is equal to or greater than 40% of the total weight of frozen particles, preferably greater than 50%, 60% or 65%. The weight of the first population of frozen edible particles
30 should also be equal to or less than 90% of the total weight of frozen particles. In one embodiment it is preferred that the weight of the first population of frozen particles is equal to or less than 85% or 80%, such as less than or equal to 75% of the total weight of frozen particles.
It is also important that the weight of the second population of frozen particles (ice crystals) is equal to or less than 60% of the total weight of frozen particles, preferably less than 40% or 35%. The weight of the second population of frozen
5 particles should also be equal to or greater than 10% of the total weight of frozen particles. In one embodiment it is preferred that the weight of the second population of frozen particles is equal to or greater than 15% or 20%, such as greater than or equal to 25% of the total weight of frozen particles.
10 Expressed as ratios, the ratio of the weight of the first population to the second population of frozen particles is from 2:3 to 9:1 such as from 2:3 to 4:1,1:1 to 9:1, 1:1 to 4:1,1:1 to 3:1,2:1 to 9:1,2:1 to 4:1 or 2:1 to 3:1.
The frozen particles in the first population have a particle size of greater than
15 0.5 mm, more preferably greater than 0.75, 0.9, 1 or 1.5 mm. The frozen particles in the first population preferably have a particle size of equal to or less than 5 mm, such as less than 4 mm or 3.5 mm.
The ice particles in the second population typically have a particle size such that
20 the ratio of the mean particle size in the first population to the ratio of the mean particle size in the first population is greater than 9, more preferably greater than 10. In one embodiment, the ratio is greater than 20. Typically, the ratio is less than 100, such as less than 50.
25 In a preferred embodiment, the ice particles in the second population have a particle size of less than 100 mm, preferably less than 90 or 80 mm.
It will be appreciated that in a bimodal product, some frozen particles will have sizes that fall between the two populations. However, these particles should
30 make up 10% or less of the total weight of frozen particles in the ice-containing product, more preferably less than 5%.
WO 2006/007924 PCT/EP2005/006700
The frozen edible particles include materials with a range of water contents from relatively high (such as fruit) to little or none (such as chocolate). Thus, in the context of the present invention frozen edible particles means particles of solid edible material at a temperature below 0°C, preferably below -4°C regardless of
5 whether the particles themselves contain ice. Example of suitable frozen edible particles include fruit pieces, fruit juice, vegetable pieces, chocolate or couvertures, dairy products such as milk and yoghurt, sauces, spreads and food emulsions, confectionery pieces (e.g. candy, marshmallow, fudge) or caramel. The term "frozen edible particles" does not include ice per se or ice that only
10 contains traces of solutes such as flavourings or colour such that the total solids content is, for example, less than 1 wt%.
The frozen particles in the second population are essentially ice formed during the freezing process. However the frozen particles in the first population can be a
15 frozen edible material or a combination of frozen edible material and ice. In the later case, it is preferred that at least 20 wt% of the frozen particles in the first population, more preferably at least 30,40 or 50 wt%, are frozen edible particles.
In one embodiment, the ice-containing products of the invention are ice
20 confections and include confections that typically contain milk or milk solids, such as ice cream, milk ice, frozen yoghurt, sherbet and frozen custard, as well as frozen confections that do not contain milk or milk solids, such as water ice, sorbet, granitas and frozen purees. Ice confections of the invention also include frozen drinks, such as milkshakes and smoothies, particularly frozen drinks that
25 can be consumed at -10°C.
Ice-containing products of the invention may be in the form of concentrates, i.e. having a lower ice/water content (and therefore a higher solids content by wt%) than an equivalent normal strength product. Such concentrates can, for example,
30 be diluted with an aqueous liquid, such as milk or water, to provide a refreshing drink.
WO 2006/007924 PCT/EP2005/006700
Process for manufacturing ice-containing products
The process of the invention involves generating some of the ice by normal freezing of one portion of the product, which contains a lower percentage of water/ice than the final product, and substituting the remainder of the ice with
5 relatively large frozen edible particles (optionally mixed with relatively large pieces of ice) in the mm range. The large particles are then added to the frozen concentrate, mixed, and the size of the large particles mechanically reduced to the desired size of 0.5 mm or above. The advantage of this process is that it is possible to reduce the weight of smaller ice produced because fewer ice crystals
10 form in the frozen concentrate than would be the case with the normal strength formulation. This then allows a substantial amount of larger frozen particles made separately to be added and the mixture processed to generate the desired bimodal population with the desired ratio of small ice to large frozen particles.
15 Concentrates typically have total solids contents of at least 35% by weight, preferably at least 40% or 45% by weight. The total solids content is typically at most 65%, preferably at most 60%, since it is difficult to process very high solids content concentrates. In contrast, end products typically have a total solids content of 30% or less.
The concentrate is cooled to a temperature of below -4°C, preferably below -6°C, -6°C or -10°C. Typically, this is achieved by freezing the concentrate in an ice cream freezer or similar (e.g. scraped surface heat exchanger).
25 The large frozen particles, a substantial proportion of which have a size of at least 5 mm, e.g. greater than 5 mm, can for example be generated as follows. Large frozen particles containing up to 12% solids are produced in a fragmented ice maker such as that described in US Patent No. 4,569,209 fed from a feed tank containing unfrozen particle mix. The refrigeration capacity required is larger than
30 when pure water is frozen in such a machine because the solids depress the freezing point. Large frozen particles comprising of higher levels of solids can be produced by dropping unfrozen particle mix into liquid nitrogen through a suitable
sized nozzle, as described in US 5,126,156. Other large frozen particles, such as chocolate are frozen fruit pieces can be obtained from suppliers in suitable sized pieces, or by cutting up chocolate bars or whole frozen fruit It will be appreciated that when making the large frozen particles for inclusion in the mix, a
5 small proportion may have particles of a size of less than 5 mm. According the phrase "a substantial proportion" means that at least 90%, more preferably at least 95%, of the particles have a size equal to or greater than 5 mm.
The large frozen particles are then mixed in with the cooled/frozen concentrate.
10 This can for example be achieved by feeding the large frozen particles through a fruit feeder into the cooled/frozen concentrate exiting the ice cream freezer.
The amount of frozen particles (wt% of the final product) that is added is preferably at least 22 wt%, more preferably at least 25, 30 or 35 wt%. Typically
15 the amount of frozen particles added is less than 80, 70 or 60 wt%. It is preferred, where a mixture of ice and frozen edible particles are added, that at least 20 wt%, more preferably at least 30, 40 or 50 wt%, of the added frozen particles are frozen edible particles.
20 The particle size reduction step involves mechanically reducing the size of the added large frozen particles to the desired size. In a preferred embodiment, this can performed by passing the mix through a constriction of a size, d, less than 5 mm, preferably of from greater than 0.5 to 4 mm, more preferably greater than 0.75, 0.9 or 1 mm and less than 3.5 mm. This allows for in-line reduction of
25 particle size and may comprise, for example, passing the mix through a pump comprising an outlet of size d, and/or passing the slush between parallel plates separated by a distance of and wherein one of the plates rotates relative to the
other. An example of a suitable device is shown in Figure 1 and described in the Examples.
The mechanical size reduction step should be adjusted such that a substantial proportion (i.e. at least 90%, more preferably at least 95%) of the resulting particles
will have a size of greater than 0.5 mm and less than 5 mm, preferably greater than 0.75,0.9 or 1 mm and less than 4 or 3.5 mm.
The resulting product will then typically be subject to further treatment to lower its
5 temperature to typical storage temperatures, such as -18°C or less, e.g. -25°C. The product may also, optionally, be subject to a hardening step, such as blast freezing (e.g. -35°C), prior to storage. Before serving, the product is generally tempered back to at least -18°C. In one embodiment, the product is warmed up to -10°C and served as a drink.
The present invention will now be further described with reference to the following examples, which are illustrative only and non-limiting. The examples refer to Figures:
15 Figure 1 - is a drawing of an example of a size reduction device for use in the method of the invention.
Figure 2 - is a chart showing the effect of ice size/addition on product hardness in a model system.
Figure 3 - is an electron micrograph of a product of the invention. Size bar = 1mm.
Process for manufacture
Preparation of Concentrate
All ingredients except for the flavour and acids were combined in an agitated heated mix tank and subjected to high shear mixing at a temperature of 65°C for
30 2 minutes. The resulting mix was then passed through an homogeniser at 150 bar and 70°C followed by pasteurisation at 83°C for 20 s and rapid cooling to 4°C using a plate heat exchanger. The flavour and acids were then added to the mix
and the resulting syrup held at 4°C in an agitated tank for a period of around 4 hours prior to freezing.
Preparation of Ice Particles
5 A Ziegra Ice machine UBE 1500 (ZIEGRA-Eismaschinen GmbH, Isernhagen, Germany) was used to manufacture ice particles measuring approximately 5 x 5 x 5-7 mm.
Preparation of Frozen Edible Particles
10 An adapted Ziegra Ice machine UBE 1500 (ZIEGRA-Eismaschinen GmbH, Isernhagen, Germany) with increased refrigeration capacity, and fed from a feed tank (rather than a water supply) was used to manufacture the frozen edible particles. The Ziegra ice machine freezes the mix to form particles measuring approximately 5x5x5-7 mm. The particles were 'dry', i.e. no accompanying
15 unfrozen mix emerged from the machine.
Preparation of Frozen Fruit Particles
The mix for the frozen edible particles in the case of the cordial was pre-diluted with chilled water (+5°C) in a sterilised mix vessel with water in a ratio of 1 part
20 cordial to 3 parts water. This was then transferred to the feed tank of the Ziegra machine and processed as described above to produce frozen particles.
In the case of directly usable ingredients (fruit juice , milk and puree) the ingredients were placed directly from chill (+2 to +5°C) into the feed tank.
Pre-frozen cubes measuring approximately 10mm x 10mm x 10mm of IQF (Individually Quick Frozen) fruit were obtained directly from the supplier (SVZ, Royal Cosun Group). These were not passed through the Ziegra machine but added in to the frozen concentrate directly using the vane type feeder (Hoyer FF)
30 before subsequent size reduction as described.
Preparation of Chocolate Particles
The low solids chocolate mix was prepared by mixing the component ingredients into an agitated heated mix tank and subjecting to high shear mixing at a temperature of 65°C for 2 minutes. The resulting mix was then passed through an
5 homogeniser at 150 bar and 70°C followed by pasteurisation at 83°C for 20 s and rapid cooling to 4°C using a plate heat exchanger. This was then transferred to a cooled feed tank to hold the mix at +4°C prior to freezing through the Ziegra machine.
10 The chocolate pieces used in the frozen drinkable product were obtained directly from the supplier (Barry Callebaut) and were pre-frozen to -2°C. These did not pass through the Ziegra machine but were added directly into the frozen concentrate mix using a vane style-feeder (Hoyer FF).
15 Freezing of Concentrate
The concentrate was frozen using a typical ice cream freezer Crepaco W04 (scraped surface heat exchanger) operating with an open dasher (series 80), a mix flow rate of 120 I / hour, an extrusion temperature of -10 to -14°C and an overrun at the freezer outlet of 0 to 100%. Immediately upon exit from the freezer,
20 the frozen particles were fed into the stream of frozen concentrate using a fruit feeder Hoyer FF (vane type) to form a slush. The flow rates of the concentrate from the freezer and the flow rate of ice addition were controlled to give the desired ice inclusion level.
25 The resulting slush was then passed through a size-reduction device. The size-reduction device (10) is schematically illustrated in Figures 1a to 1c and comprises the drive (20) and casing (11) of a centrifugal pump (APV Puma pump)
The generally cylindrical casing (11) has a tubular outlet (13) disposed at its edge
30 and has a tubular inlet (12) located centrally in its base. Opposite the inlet (12)
and located in the centre of the top of the casing (11) is an aperture (14) for
receiving the drive shaft (20) of the centrifugal pump. The drive shaft (20) is in
sealing engagement with the casing (11) owing to the presence of an annular seal (14a) located there between.
Located within the casing (11) is a pair of parallel plates (15, 25), being coaxially
5 aligned with the casing (11) and spaced longitudinally from each other by a distance, d. The lower plate (15) is fixedly attached to the base of the casing (11) whilst the upper plate (25) is fixedly attached to the drive shaft (20). By means of its attachment to the drive shaft (20) the upper plate (25) is rotatable relative to the casing (11). In contrast, the lower plate (15) is stationary owing to its
10 attachment to the casing (11).
The lower plate (15) comprises a disc (16) having an central aperture (18) there through which is in fluid communication with the inlet (12) of the casing (11). The whole of the bottom surface of the disc (16) is flat and in contact with the base of
15 the casing (11). The top surface of the disc (16) tapers radially inwards towards the central aperture (18). Projecting upwards from the top surface of the disc (16) are a plurality, for example four, fins (17) spaced regularly around the circumference of the plate (15). Each fin (17) has an upper surface that extends radially inward from, and remains at a height level with, the outer edge of the top
20 surface of the disc (16).
The upper plate (25) is similar to the lower plate (15) but inverted such that it is the top surface of the disc (26) that is flat and the bottom surface tapered. The central aperture of the disc (26) of the upper plate receives the drive shaft (20)
25 and the top surface of the disc (26) is slightly spaced longitudinally from the top of the casing (11) to allow the plate (25) to rotate freely. The top plate (25) may be provided with a different arrangement of fins to the lower plate (15) and in this case the upper plate (25) has three fins (27) whilst the lower (15) has four fins (17).
The size-reduction device (10) is arranged such that slush pumped in through the inlet (12) is required to pass between the parallel plates (15, 25) before it can exit
WO 2006/007924 PCT/EP2005/006700
through the outlet (13). The narrow spacing (d) of the plates along with the grinding action of the fins (27) on the rotating top plate (25) against the fins (17) of the bottom plate (15) ensures that the ice particles passing through the device have a maximum length of less than d in at least one dimension. This constriction
5 size, d, can be varied from 0.1 to 5mm depending on product requirements.
Experiments 1-3 establish proof of principle in systems where large ice particles are used instead of frozen edible particles. The process described in experiments
10 1 to 3 was then used in examples 1 to 4 to produce inclusion-containing products according to the invention where frozen inclusions are added in place of all or some of the Ziegra ice.
15 Experiment 1 - Squeezeable Iced Drink Concentrates
The process of the invention was used to make a drinks product concentrate which is squeezeable. The concentrate can be squeezed from the container straight after being taken out of a freezer at -18°C and added to milk or water to give an iced drink. A lower amount of water is included in the formulation to
20 create a concentrated mix. The remaining water (50%) is then added as ice from a Ziegra machine. A control sample was made where the formulation contains the usual amount of water no ice was added during processing.
WO 2006/007924 PCT/EP2005/006700
Experiment 1: The ice cream freezer was run with the following settings: Mix flow of 65l/hour, overrun of 7%, barrel pressure of 2.5 bar, motor load of 110%, and an extrusion temperature of-13.1°C.
The size reduction device was run at a speed of 520rpm with a 1.5mm gap size setting. The in-line.pressure was 1 Bar. The ice particles produced using the Ziegra machine were added at a rate of 1400g/min.
10 Comparative Experiment 1: The freezer was run with the following settings: Mix flow of 1001/hour, overrun of 7%, barrel pressure of 2.5 bar, motor load of 100%, and an extrusion temperature of -6.2°C9
The size reduction device was run at a speed of 520rpm with a 1.5mm gap size 15 setting. The in-line pressure was 2-3 Bar.
Both samples were collected and hardened in a blast freezer before being stored at -25°C. Samples were analysed by using the Vickers Hardness test The Vickers Hardness test is an indentation test that involves pushing a pyramid
20 shaped indentor into the surface of material and recording the force applied as a function of tip displacement. Force and displacement are measured during the
indentation loading cycle and the unloading cycle. For water ices, the pyramid tip pushes into the surface of the material to a depth of 1.5mm, before it is pulled out.
5 The total solids of the concentrated mix with the addition of 50% ice from the
Ziegra machine was measured to be 23.31%. The total solids of the mix with no added ice was measured to be 22.47%. Therefore both products were similar in total solids (and in agreement, within experimental error, with the value of 22.75% calculated from the solids contents of each of the ingredients).
The Instron Hardness test results were as follows:
Example 1 (Product with added ice) 3.02±0.24MPa
Comp. Example 1 (Product without added ice) 7.37±0.92MPa
The Hardness test results show that by manipulation of the ice phase, products can be made softer for the equivalent solids level. The data show the significant reduction in hardness between the sample solely processed through the ice cream freezer and that with ice particles added and the size reduced after the
20 freezer. The sample containing the ice particulate inclusion can be squeezed from a sachet by hand at -18°C whereas the product without the added particles cannot be squeezed out without product warming or manipulation.
This product has the added consumer advantage that it is a frozen concentrate 25 which can be added to water or milk or other diluent to create a drink containing
ice. The softer frozen system containing the ice particulates can be stirred into the
diluent and dispersed readily to create the drink whereas the control requires
considerable physical disruption to allow its break up and subsequent dilution.
Once diluted the larger particulate ice remains to give a cool, flavoured and 30 refreshing drink that can be consumed directly or sucked up through a straw.
Other examples include those containing fruit concentrates and purees, flavoured
ice teas and frozen milk shakes.
WO 2006/007924 PCT/EP2005/006700
Experiment 2 - Soft Water-ices
This set of experiments describes frozen water ice products (Concentrates A to D) that are made with various proportions of Ziegra ice added into a concentrated
5 mix frozen through a standard ice cream freezer (Crepaco W04), the combination then being subjected to ice particle size reduction as described above.
Hardness testing (see method) of these samples shows a three-fold difference
10 between the control sample with no post-added ice and those with added ice at
WO 2006/007924 PCT/EP2005/006700
various levels. This shows the benefit of the addition of larger ice and its subsequent size control over just freezing through the ice cream freezer alone.
Comparison of the samples containing added ice shows that the hardness is
5 reduced still further for particulate ice added: (1) at a proportion of the total ice of from 40 to 70%; and (2) with a particle size diameter of 1.5 to 3mm (see Figure 2).
In each of the above the hardness can be halved so further optimising the benefit
10 of a softer frozen product to the consumer. This 'softness' can be shown across a range of product formats and the following experiments illustrate this:
Experiment 3 - Squeezable Ice Products
Experiment 3 shows a product that is made by addition of 33% ice to a cooled concentrate mix and subsequent size reduction of the ice using a crushing pump
WO 2006/007924 PCT/EP2005/006700
with gap sizes from 1 to 3mm. The product is extruded at -6°C, then blast frozen (-35°C for 2 hours) and subsequently stored at -25°C. Before serving the product is tempered back to -18°C. It is found that the product at -18°C can be squeezed directly, by hand, from the pack (see photograph in Figure 3) which is of
5 advantage to the consumer as it allows immediate consumption.
This can be compared with the control product which is frozen directly from the ice cream freezer and has no subsequently post-added ice. After equivalent hardening, storage and tempering it is found that the product at -18°C is very hard
10 and cannot be squeezed directly from the pack without significant warming or kneading of the product surface through the pack.
Example 1 - Spoonable Ice Cream Products
This set of experiments describes spoonable ice cream products that are made
15 by adding frozen edible particles to ice cream mix. Frozen edible particles were produced in the Ziegra ice machine from four liquid mixes: full fat milk, orange juice (10% solids), low solids chocolate mix (5% whole milk powder, 3% sucrose, 3% cocoa powder 10/12, 0.05% flavour and 89% water) and diluted peach cordial comprising 1 part cordial (Robinsons High Juice, consisting of 50% orange juice
20 from concentrate, 44% carbohydrate) to 3 parts water. The frozen particles were added to an ice cream concentrate mix frozen to 100% overrun through a standard ice cream freezer (Crepaco W04) to form the small ice crystals. The combination was then subjected to ice particle size reduction as described above, using two different gap sizes in each case.
WO 2006/007924 PCT/EP2005/006700
Sucrose 20.00 13.00 13.00 13.00 13.00
Low fructose 15.00 9.75 9.75 9.75 9.75
glucose syrup (78%
LBG 0.25 0.16 0.16 0.16 0.16
K-Carrageenan 0.04 0.03 0.03 0.03 0.03
MGP 0.30 0.20 0.20 0.20 0.20
Flavour 0.10 0.07 0.07 0.07 0.07
Colour 0.01 0.01 0.01 0.01 0.01
Added Particles % 35 35 35 35
Amount of small ice 35 35 35 35
Ratio of large to — 11 11
Gap size of crushing — 1.0,3.0 1.0,3.0 1.0,3.0 1.0,3.0
Ratio of large to 10,30 10,30 10,30 10,30
small particle sizes
By use of the post addition of frozen particles, the ice cream has a soft and flowable texture that allows the product to be spoonable directly from the tub at -18°C.
Example 2 - Scoopable Fruit Ice Products
Example 1 was repeated, using a fruit ice (aerated to 10% and 60% overrun) instead of the ice cream. Frozen particles made from orange juice and peach cordial (as described above) and also strawberry puree (10 Brix single strength
10 from supplier SVZ) were added.
Concentrate Product 1 Product 2 Product 3
Orange Juice Strawberry Peach Cordial
Frozen Puree Frozen Frozen
Particles Particles Particles
Water 49.66 32.28 32.28 32.28
Sucrose 23.30 15.15 15.15 15.15
Low fructose glucose syrup 22.50 14.63 14.63 14.63
WO 2006/007924 PCT/EP2005/006700
LBG 0.23 0.15 0.15 0.15
Guar 0.08 0.05 0.05 0.05
Hygel8293 0.23 0.15 0.15 0.15
Lemon cone x5 4.00 2.60 2.60 2.60
Added particles % 35 35 35
Amount of small ice 35 35 35
Ratio of large to small 1 to 1 1 to 1 1 to 1
Gap size of crushing pump 1.0,4.0 1.0,4.0 1.0,4.0
Ratio of large to small 10,40 10,40 10,40
By use of the post addition of frozen particles, the product is scoopable directly from the tub at -18°C.
5 Example 3 - Water Ice Product with added Frozen Fruit Particles
Aerated water ice products with added frozen fruit pieces were produced as follows. Approximately 10mm cubes of frozen fruit (strawberry or mango) were added to a water ice mix that had been frozen to 10% or 60% overrun in a standard ice cream freezer (Crepaco W04). The combination was then subjected
10 to particle size reduction as described above.
Concentrate Product 1 Product 2
Frozen strawberry Frozen mango
Water 64 41.60 41.6
Sucrose 9.23 6.00 6
Low fructose glucose 19.62 12.75 12.75
syrup (78% solids)
Dextrose 6.22 4.04 4.04
Guar 0.23 0.15 0.15
Citric Acid 0.6 0.39 0.39
Flavour 0.1 0.07 0.07
Added particles % 35 35
Amount of small ice 35 35
particles at -18°C %
Ratio of large to — 1 to 1 1 to 1
Gap size of crushing — 1.0,3.0 1.0,3.0
Ratio of large to — 10,30 10,30
small particle sizes
The addition of the frozen particles within the product creates a spoonable water ice that would be difficult to spoon otherwise. The inclusion of frozen fruit pieces within the water ice also creates a refreshing product with novel texture contast
5 and flavour delivery.
Example 4 - Frozen Drinkable Product with Added Chocolate Particles
By the use of this technology, products can be made that are distributed at colder than -18°C and then, by tempering back to -10°C, the products become drinkable.
10 A chocolate drink product with added chocolate pieces was produced as follows. Approximately 5-7mm size pre-frozen (-2°C) chocolate pieces were added to a chocolate ice cream mix frozen to 30% overrun through a standard ice cream freezer (Crepaco W04). The pieces were controllably dosed into the frozen concentrate using a vane type feeder (Hoyer FF4000). The combination was
15 then subjected to particle size reduction as described above.
Low fructose glucose syrup (78% solids)
Whey concentrate 4.3 2.15
Cocoa Powder 10/12 2 1
Chocolate Dark White 3 1.5
Chocolate particles 0 20
Added large ice particles 0 30
Total added frozen edible particles % — 50
(ice + chocolate)
Amount of small ice particles at -18°C — 23
Ratio of large to small particle amounts — 2.2 to 1
Gap size of crushing pump (mm) — 1.75
Ratio of large to small particle sizes — 17
Without the inclusion of the frozen particles these systems would be very hard and would require high levels of sugar to make them drinkable at -10°C but this would then also make them intensely sweet. These examples are suckable up a
5 straw at -10°C and do not require high sugar levels to make them so. For the consumer this allows the delivery of a product that is directly consumable as a drink containing ice at -10°C. The large ice and chocolate particles remain in the drink to provide the consumer with a novel and refreshing ice sensation.
10 The various features and embodiments of the present invention, referred to in
individual sections above apply, as appropriate, to other sections, mutatis mutandis. Consequently features specified in one section may be combined with features specified in other sections, as appropriate.
15 All publications mentioned in the above specification are herein incorporated by reference. Various modifications and variations of the described methods and products of the invention will be apparent to those skilled in the art without departing from the scope of the invention. Although the invention has been described in connection with specific preferred embodiments, it should be
20 understood that the invention as claimed should not be unduly limited to such specific embodiments. Indeed, various modifications of the described modes for
carrying out the invention which are apparent to those skilled in the relevant fields are intended to be within the scope of the following claims.
F3389 (c) com
1. An ice-containing product comprising at -18°C,
(i) a first population of frozen particles, which first population consists
5 essentially of frozen edible particles, or a mixture of frozen edible particles and
ice particles, having a particle size of greater than t mm and less than 5mm; and
(ii) a second population of ice particles having a mean particle size such
that the ratio of the mean particle size for the first population to the mean particle
size for the second population is greater than 10 and less than 100,
10 wherein the ratio of the weight of the first population of particles to the
weight of the second population is from 2:3 to 9:1 and the first population and second population together provide at least 90% of the frozen particles present in the product.
15 2. A product according to claim 1 wherein the first population and second population of particles provide at least 95 wt% of the frozen particles present in the product.
3. A product according to claim 1 or claim 2 wherein the first population of
20 frozen particles consists essentially of frozen edible food particles.
4. A product according to any one of the preceding claims wherein the ratio of
the amount of the first population of frozen particles to the amount of the second
population of ice particles is from 1:1 to 4:1.
5. A product according to any one of the preceding claims which has a
Vickers Hardness of less than 4 MPa at -18°C.
6. A product according to any one of the preceding claims which is an ice
30 confectionery product.
F3389 (c) com
7. A method of producing an ice-containing product which method comprises in the following order
(i) cooling a product concentrate to a temperature of below -4°C;
(ii) combining the cooled concentrate with frozen particles, a
5 substantial proportion of which have a particle size of greater than 5 mm,
said particles consisting essentially of frozen edible particles or a mixture
of frozen edible particles and ice particles; and
(iii) mechanically reducing the size of the frozen particles such that
substantially all of the resulting frozen particles have a size of greater than
10 0.5 mm and less than 5 mm.
8. A method according to claim 7 wherein the concentrate is a frozen confectionery premix concentrate.
15 9. A method according to claim 7 wherein the concentrate is a milk shake concentrate.
10. A method according to any one of claims 7 to 9 wherein in step (iii)
substantially all of the resulting frozen edible particles have a size of greater than
20 1 mm.
11. A method according to any one of claims 7 to 10 which further comprises a
step (iv) of lowering the temperature of the product obtained in step (iii) to a
temperature of-18°C or lower.
12. An ice-containing product obtained by the method of any one of claims 7
|Indian Patent Application Number||84/MUMNP/2007|
|PG Journal Number||28/2009|
|Date of Filing||18-Jan-2007|
|Name of Patentee||HINDUSTAN UNILEVER LIMITED|
|Applicant Address||Hindustan Lever House 165-166 Backbay Reclamation, Mumbai|
|PCT International Classification Number||A23G9/02|
|PCT International Application Number||PCT/EP2005/006700|
|PCT International Filing date||2005-06-20|