FI122250B - Lactose-low and lactose-free milk product and process for making them - Google Patents

Description

Low lactose and lactose free milk product and process for their preparation

Field of the Invention

The invention relates to a process for separating milk components into individual components and to a low-lactose or lactose-free milk product composed of these components. The invention relates in particular to the use of nanofiltration technology for the separation of milk components.

Background of the Invention

There are several known methods based on membrane technology for the production of low-lactose and lactose-free milk. Also known in the art is the traditional enzymatic method for lactose digestion, which comprises the step of adding lactose from yeast or yeast to lactose so that more than 80% of the lactose is digested into monosaccharides, not glucose and galactose.

Several methods of strain filtration have been proposed for the removal of lactose from milk raw material. There are generally four basic types of membrane filtration methods: reverse osmosis (RO), nanofiltration (NF), ultrafiltration (UF) and microfiltration (MF). Of these, UF is mainly suitable for the separation of lactose from milk. Reverse osmosis is generally used for concentration-20, ultra- and microfiltration fractionation, and nanofiltration for both concentration and fractionation. A lactose removal method based on KaSo technology is described, for example, in WO 00/45643, in which lactose is removed by ultrafiltration and diafiltration.

It is well known in the art that membrane techniques in general also have the problem that, in addition to lactose,

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™ is also part of the minerals that have a clear bearing on the taste of milk and dairy products made from it. The management of mineral content, and in particular of divalent minerals such as calcium and magnesium, is particularly problematic in the art, and the losses in the known methods are high and often require the use of such materials. restoration or separate addition of divalent minerals.

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§ Membrane processes often also contain minerals, for example

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g side streams that cannot be efficiently utilized and which also increase wastewater load require further treatment and cost. Thus, it is hoped that there will be processes that control divalent minerals in the process in particular and recover the process more efficiently, thereby enabling the recycling of process waters without the generation of side streams, WO 03/094623 A1 discloses a method for ultrafiltration, nanofiltration and 5, after which the minerals removed by ultrafiltration are returned to the UF retentate. The residual lactose of the low-lactose milk product thus obtained is hydrolyzed by the lactase enzyme to the monosaccharides to give a substantially lactose-free milk product. The method provides lactose removed from milk without affecting the organoleptic properties of the milk product being prepared. In this process, loss of divalent minerals such as calcium and magnesium can be significant. In addition, the process also generates mineral-containing side streams that cannot be utilized in the process and require post-treatment. However, alternative and even simpler and more effective methods are needed to solve these problems.

The lactose can also be specifically separated from the milk also by chromatography. However, milk processing involves many problems other than whey, such as the delicate precipitation of casein, the preservation of the micelle structure of casein, the behavior of fat and the very high hygiene requirements. For example, EP-20 Publication 226035 S1 describes a lactose separation process in which milk is fractionated so that the lactose fraction is separated off and the minerals are in the protein fraction or the protein fat fraction. The method is characterized in that the cation exchange resin is equilibrated by matching its cation composition to the milk cation composition, and the milk is chromatographed on a column with a balanced cation exchange resin at a temperature of about 50-80 ° C using ___ water. The advantage of this method is that all the δ essential substances are retained in the milk. However, the chromatographic separation of lactose is a slow and complicated process and is not directly applicable to conventional dairies without expensive equipment investment. Another problem is the high water consumption 30 and the high amount of chemicals.

| KR20040103818 discloses a process for preparing low-lactose co-milk in which lactase-hydrolyzed milk is nanofiltered.

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S3 is partially removed to remove galactose and glucose and water is added to the nanofiltration retentate to obtain a suitable sweetness. Choi et al. (Asian-35 Aust. J. Anim. Sci. 20 (6) (2007) 989-993) describe a process for the preparation of lactose hydrolyzed milk, in which raw milk is hydrolyzed partially by β-galactosidase (5,000 lactase activity units / g, Validase, Valley Research). 3 (0.03%; 4 ° C, 24 hours) or 'completely' (0.1%; 40 h), heat treated to inactivate the enzyme (72 ° C, 5 min), cooled to 45-50 ° C and nanofiltrated -detected at about 9-10 bar (130-140 psi; concentration factor 1.6). Water was added to the NF retentate and heat treated at 65 ° C for 30 min. Lactose-5 hydrolysed milk consisted of protein (3.1%), fat (3.5%), lactose (0.06%), glucose (1.45%) and galactose (1.29%). By the methods described in said publications, which include single-stage nanofiltration, not all monovalent minerals are yet effectively returned to milk in the villages.

WO 2007/076873 describes a low-carbohydrate milk containing essentially all of the calcium and protein of the original milk and a process for preparing it. In this method, the pH of the milk is adjusted to a basic pH of 7.0-9.5, ultrafiltrated, UF permeate is nanofiltered, preferably at about 10 ° C to minimize microbiological risk, combined with NF permeate, UF retentate and water and adjusted to pH milk pH (pH 6.7) by adding acid, preferably citric acid or phosphoric acid. The energy content of the product is 90-250 kJ / 100 g. The process is multistep and requires strong chemicals to adjust pH and minimize calcium and protein losses.

WO Publication 2004/019693 describes a process for separating the various components into membrane techniques (ultrafiltration, nanofiltration and reverse osmosis) and combining these components into dairy products such as ice cream, yogurt and milk beverage.

In addition, the use of milk after lactose removal as a raw material in the manufacture of low-carbohydrate dairy products is also known. For example, WO juicing 2006/087409 A1 describes a low-energy, low-fat, non-skimmed calcium milk beverage containing a low-energy milk base consisting of skimmed milk or whey protein solution or a mixture thereof, with carbohydrates removed either wholly or partly by ultrafiltration or by chromatography previously known methods. The energy content of the product shall not exceed 20 kcal / 100 g.

cd Indeed, recent research has focused on mining milk filtration and the use of such low-carbohydrate filtered milk in dairy products such as cheese, ice cream and yogurt. One of the well known multistage membrane filtration process methods comprising nanofiltration, known in the art, for the preparation of low carbohydrate 4 dairy products is that residual lactose is only removed from the mine-filtered milk raw material.

It is very challenging to achieve products that are completely flawless in taste and structure, which satisfy consumers' expectations of a sensibly acceptable dairy product, and which are produced economically and simply without the loss of multivalent minerals.

Surprisingly, a method has now been invented for the production of low-lactose, lactose-free, milk products with absolutely no organoleptic properties, at no additional cost. The process according to the invention allows for a more efficient and simpler control of divalent monomers compared to conventional methods at no extra cost and minimizes losses. In addition, the process of the invention does not generate side streams that require post-treatment, thus making the process more efficient,

BRIEF DESCRIPTION OF THE INVENTION The present invention provides a novel solution to avoid calcium and protein losses that have been shown to be problematic in the manufacture of both low lactose and lactose free and low carbohydrate dairy products, as well as problems of organoleptic properties of such dairy products. , the resulting hydrolysed milk raw material is separated into proteins, sugars, and minerals by differentiating the nanofiltration conditions with respect to film type, temperature, pressure and / or diawash addition, and further film separation and / or chromatographic separation methods are applied. From the separated fractions, the desired milk-25 product can be suppressed.

In one aspect, the invention provides a method for separating milk components into individual components, which method is characterized in what is stated in the independent claim. Kek - 1 is also a low - lactose and lactose - free product, (3) The process according to the invention can be used to simplify and improve the production of low-lactose and lactose-free dairy products, resulting in particular in divalent minerals, especially calcium and magnesium, loss is minimized and no separate supplementation / addition of minerals 35 and / or protein is required.

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All by-products obtained in the process of the invention are normal dairy products and the side streams generated by the process can be further utilized in the process of the invention. The process does not produce products or side streams that should be treated or separated in a special abnormal manner, thus minimizing wastewater load.

In addition, the process of the invention avoids protein and mineral losses typical of lactose-free and low-lactose dairy products, and in particular enhances the recovery of divalent minerals.

The invention further provides a method which is simple, economical, large scale industrially feasible and does not involve any additional cost.

Surprisingly, it has been found that by hydrolyzing all or part of the lactose of the milk raw material and stepping the nanofiltration of the hydrolyzed milk raw material in at least two different nanofiltration ratios, such as temperature and / or pressure and / or addition of diawater and / was minimized and the calcium / protein ratio was effectively managed. The invention thus provides a method for separating the components of hydrolyzed skimmed milk milk raw material by utilizing different maturity properties and process conditions of nanofiltration membranes. The change of condition can be immediate or even or staggered at a certain rate, whereby the desired change / change of the profile of the condition can also be understood to be a single phase.

The milk product produced by the process of the invention has a desirable, low-carbohydrate, desirable, low-carbohydrate properties, δ ^ Brief Description of the Drawings 00 9 Figure 1a shows the chromatographic separation of the mineral sugar fraction at 65 ° C. (Finex CS09GC resin, flow rate 160 ml / h, feed 20mL, 2.

Ee 30 nanofiltration NF retentate, Brix 16%).

Figure 1b shows the chromatographic separation of the mineral sugar fraction at 10 ° C (Finex CS09GC resin, flow rate 160 mL / h, feed 20 mL, 2).

o Nanofiltration NF retentate, Brix 16%).

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Detailed Description of the Invention

In one aspect, the invention relates to a process for separating milk components, characterized by: a) hydrolyzing the lactose of the milk raw material to obtain a hydrolyzed milk raw material; and b) nanofiltrating the hydrolysed milk raw material in at least two a plurality of NF-retenate fractions NF Ret I, NF Ret II, NF Ret HI, etc ,, and two or more NF permeate fractions NF Perm i, NF Perm II, NF Perm ΙΠ etc. to separate proteins, sugars and minerals into these different verses.

In the context of the present invention, a milk raw acne is meant milk, whey and milk and whey combinations. The milk raw material may be supplemented with ingredients commonly used in the manufacture of dairy products such as fat, protein or sugar fractions, etc. The milk raw material may thus be e.g. 15 whole milk, cream, skimmed milk or skimmed milk, ultrafiltered milk, diafiltered milk, or by reconstituting milk, organic milk or a mixture thereof made from milk powder. Preferably, the milk raw material is skim milk.

In step a) of the process according to the invention, lactose of the milk raw material 20 is hydrolyzed to monosaccharides as is known in the art. In one embodiment of the process of the invention, the hydrolysis is carried out in its entirety (full hydrolysis) prior to the stepwise nanofiltration. In another embodiment of the process of the invention, the hydrolysis is performed partially prior to the stepwise nanofiltration and then the final lactose of the partially hydrolysed milk raw material is subsequently hydrolyzed and substantially simultaneously when the partially hydrolyzed milk raw material is nanofiltered. In a preferred embodiment of the invention, post-hydrolysis is carried out in the first sub-step of nanofiltration, whereby total hydrolysis means that the lactose content of the hydrolysed milk raw material is less than 0.5%. Partial hydrolysis means that the lactose content of the hydrolysed milk feedstock is greater than 0.5%.

§ The hydrolyzed milk raw material obtained in step b) of the process according to the invention is nanofiltered in a stepwise manner to separate proteins, sugars and minerals into different fractions. In the context of the present invention, stepwise C C \ 35 nanofiltration means that the nanofiltration comprises at least two sub-steps. Each sub-step is carried out under different process conditions and / or different types of membranes are used. The ratio to be changed may be, for example, the filtration temperature, filtration pressure, diaphragm addition and / or filtration concentration factor. The conditions can be changed for each sub-step for either one or more variables. The change of condition can be instantaneous or evenly or staggered at a certain rate, whereby the desired change / change of the profile of the condition means one sub-step. In one embodiment of the invention, the stepped nanofiltration involves a change in temperature conditions and / or film type. In another embodiment of the invention, the nanofiltration is combined with diafiltration (DF), whereby diawater is added in at least 10 nanofiltration retentates in one nanofiltration sub-step.

The stepped nanofiltration of the invention, comprising at least two partial steps, yields two or more nanofiltration or NF retentates, hereinafter designated as NF Ret I, NF Ret II, NF Ret III, etc., and two or more nanofiltration or NF permeate, denoted as NF Perm I, NF Perm IS, NF Perm II, etc. The sequence number represents the number of nanofiltration steps in the process. Thus, NF Ret I means retentate obtained in the first sub-stage of nanofiltration. 20 N N Ret Ret means retentate obtained in the second sub-stage of nanofiltration. NF Ret III means retentate obtained in the third sub-stage of nanofiltration, etc.

NF Perm I means permeate obtained in the first sub-stage of nanofiltration NF Perm II means permeate obtained in the second sub-stage of nanofiltration

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^ NF Perm III refers to the permeate obtained in the third stage of nanofiltration, etc.

In one embodiment of the invention, the phased nanofiltration NF retentate and NF permeate fractions obtained by further processing by membrane cd techniques and / or chromatographic separation of proteins, sugars and minerals.

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in order to further improve the efficiency of the process. Further treatment may be carried out on one or more NF retentate liquids or NF permeate. Among the 0X1 35 membrane techniques suitable for further processing, reverse osmosis (RO) may be mentioned in particular. Hereinafter, RO Ret means retentate from reverse osmosis, and RO Perm means permeate derived from reverse osmosis.

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The various separation methods may also be combined in one or more steps as desired. In one embodiment of the invention, the protein, sugars, and minerals of the hydrolysed milk feedstock are separated by membrane methods, preferably by nanofiltration in a first step under conditions of low retention of monosaccharides and under conditions of retention of monosaccharides. In a particular embodiment of the invention, the stepped nanofiltration is carried out in a first step at a warm temperature of about 42-51 ° C and in a second step a cold one at about 10-18 ° C. Alternatively, according to another embodiment of the invention, nanofiltration may be carried out first in the cold and then in the warm. As is known in the industrial process, the temperature of the film process is generally 10 ° C, for example, in order to avoid microbiological problems.

Suitable nanofiltration membranes are, for example, Desai 5 DL (GE Os-15 monies, USA), Desai 5 DK (GE Osmonics, USA), TFC® SR3 (Koch membrane systems, Inc., USA), FILMTEC ™ NF (Dow, USA). Suitable reverse osmosis membranes include, for example, TFC® HR (Koch membrane systems, incM USA) and FILMTEC FT30 (Dow, USA).

In one embodiment of the invention, further matrographic separation of the minerals and sugars Kro-20 is carried out on one or more NF retentants. In a preferred embodiment of the invention, the separation is performed on the retentate obtained in the second stage of nanofiltration.

The concentration factor (K) refers to the weight ratio of liquid to retentate fed to filtration and is defined by the following formula: K = feed (kg) / retentate (kg) 5 In the process of the invention, nanofiltration is performed

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preferably with a concentration factor K = 1-10, more preferably K = 2-6. If diafiltration is used in the stepped nanofiltration according to the invention, the concentration factor can be considerably higher.

| The process of the present invention can be applied to both batch and continuous production. Preferably, the inventive method is carried out in a batch process.

In a particular embodiment of the process of the invention, wherein stepwise nanofiltration of lactose hydrolyzed skim milk is performed by performing the first step in warm (K = 3) and nanofiltrating the NF permeate (NF Perm!) obtained in the first step in cold (K = 6) minerals. for recovery, the NF retentate (NF Rei!) of the first nanofiltration step contains 2.5% glucose, 2.5% galactose and 1.4% ash, and has a dry solids content of 15.5%, and the permeate of the second nanofiltration step. (NF Perm II) contains 0.2% glucose, 0.2% galactose and 0.2% ash and has a dry matter content of 0.5%. Lactose-free milk was obtained by combining this NF retentate (21.3%), said NF permeate (35.4%) and hydrolysed skim milk (43.2%) with the desired organoleptic properties. The amount of calcium was exactly the same as in the original milk (1,100 mg / kg). The milk contained 10.3% protein, 1.6% glucose, 1.6% galactose, 0.7% ash and had a dry matter content of 7.3%. This embodiment of the invention is illustrated in Example 3 and the milk composition of these fractions is shown in Example 8.

In another particular embodiment of the process of the invention, after stepwise nanofiltration and diafiltration, reverse osmosis was performed, in a second nanofiltration step, NF-permeate 11 containing 0.7% glucose, 0.7% galactose and 0.2% ash and dry content was 2.0% and NF retentate H (K-3), respectively, containing 3.1% glucose, 3.1% galactose and 1.1% ash and a dry matter content of 14.4% %. The milk composed of this hydrolysed skimmed milk NF retentate and RO retentate (50:50) otherwise corresponded to normal milk with the exception of carbohydrates (protein 3.3%, glucose 1.7%, galactose 1.6%, ash 0.7%, dry substance 7.5%, calcium 1100 mg / kg). This embodiment of the invention is described in Example 2 and the milk composition of said fractions is shown in Example 6.

From the fractions obtained by the process of the invention, lactose-free skimmed milk having the desired organoleptic properties and corresponding to the composition of the hydrolysed milk, with the exception of carbohydrates and carbohydrates, can be specifically prepared by combining a first N? , 5) (66.6%)

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£ NF permeate I of the filtration step! (27.7%) and the mineral fraction separated on the chromatography column (5.7%). The amount of calcium was exactly the same as in the original S milk (1,100 mg / kg). The drink contained 3.3% protein, 1.6% glucose, 00 g 1.6% galactose, 0.7% ash and had a dry matter content of 7.5%. The composition of the 35 milk in question is described in Example 7.

In another aspect, the invention thus relates to a lactose-free or low-lactose milk product comprising at least one NF retenate fraction NF Ret 10 !, NF Ret II, NF Ret III, etc. or NF permeate fraction NF Perm !, NF Perm II, NF Perm III, etc. obtained by nanofiltration of a hydrolysed milk feedstock comprising at least two steps.

In another embodiment of the invention, the dairy product is prepared by combining two or more fractions: NF Ret I, NF Ret II, NF Ret III, NF Perm I, NF Perm IE, NF Perm II, RO Ret, RO Perm and NF Ret 1 Chromatographically separated fraction containing minerals and / or sugars, NF Rei II, NF Ret II, etc.

The lactose-free and low-lactose-free milk product of the invention may be liquid or may be in the form of a concentrate or powder.

In another aspect, the invention relates to a process for the preparation of a lactose-free or low-lactose milk product, comprising a) hydrolyzing lactose of a milk raw material to obtain a hydrolyzed milk raw material and b) nanofiltrating the hydrolyzed milk raw material in at least two retenate fractions NF Ret I, NF Ret II, NF Ret II, etc., and two or more NF permeate fractions NF Perm I, NF Perm II, NF Perm III, etc. for separating proteins, sugars and minerals into these different fractions, c) if desired, one or more of NF Ret I, NF Ret II, NF Ret

H1 etc. and NF Perm I, NF Perm II, NF Perm lii etc. are further processed by membrane technology and / or by evaporation and / or chromatography, d) from one or more fractions obtained in step b) and, if desired, from one or more fractions obtained in step c) and optionally, the other ingredients are formulated into a product of the desired composition 5 e) if desired, concentrating the product obtained in step d) into a concentrate

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^ or powdered.

The milk product of the present invention is low-lactose or 30-lactose-free. The term low-lactose in the present invention means that | the lactose content of the milk product is not more than 1.0%. The term lactose-free means that the milk product contains lactose up to 0.5 g / portion (e.g. liquid en g for maize milk 0.5 g / 244 g with a lactose content of up to 0.21%), but not more than 0.5% . According to the invention, it is also possible to prepare ™ 35 low-carbohydrate milks which are organoleptically flawless. In addition, the loss of calcium and protein 11 in the milk raw material is minimized and no separate supplementation / addition of minerals and / or protein is required.

The following examples illustrate the invention but do not limit the invention to the embodiments described.

Reference Example 1. Nanofiltration of Hydrolysed Skimmed Milk in a Single Step with Desal 5 DL (K = 3)

Skimmed milk (20 L) was hydrolyzed (9 ° C, 18 h) with Godo YNL2 lactase (Godo Shusei Company, Japan) at a dosage of 0.08% and nano-filtered with Desal 5 DL (GE Osmonics, USA) at 10 ° C. 10-18 ° C and a pressure of 12-21 bar. The permeate flow was 5.7-9.6 l / m2h. The nanofiltration was continued at a concentration factor of 3, i.e. retentate volume was 6.7 L and permeate 13.3 L.

NF retentate and NF permeate obtained from feed containing hydrolysed skimmed milk were sampled and assayed for protein, dry matter, glucose, galactose as well as ash and calcium (Table 1).

Table 1. Compositions of nanofiltration retentate and permeate j Composition | Input j j

| j (hydrolyzed j NF retentate I NF permeate i

| | skimmed milk) i j [Protein (%) [3,4 '' '' '[[8.7 f' '0.1 |

[Ash (%) i s 0.2 J

[Calcium (mg / kg) J 1100 J 3000 23__ !:

! Dry matter (_%) _ 8.8 | 19.6 1.9 I

[Glucose (%) | 2.3 j 4.4 0.9 j ^ | Galactose (%) 2.2 j 4.5 0.8 j p ...........: ........................... .................................................. ........... ........................................ ...........! , [Ca / protein (g / kg) \ 32.5 j 34.5 j i

The results show that calcium was not lost permeate was practically absent but remained in the same fraction as the cd 20 protein (Table 1). In addition, the monosaccharides penetrate the membrane to a significant extent in o g. When the retentate was diluted to its original milk protein content, the taste was found to be "empty" or atypical of the milk. The reason is the milk minerals lost in permeate filtration by nano filtration, which give the milk taste an important salty taste. Thus, once-through nanofiltration of hydrolysed milk, lactose-free or low-lactose malt of ordinary, i.e., normal milk, cannot be produced.

Example 2, Three-Step Nano Filtration of Hydrolyzed Skimmed Milk (Well Desai DK + Diafiltration and Filmtec NF Well) Combined-5 with RO Filtration

To skimmed milk (20 L) was added 0.06% Godo YNL2-lactase (Godo Shusei Company, Japan) and hydrolyzed for 18 h at 10 ° C. In this case, the residual lactose content of the skimmed milk was 0.03%. The hydrolyzed skimmed milk thus obtained was nanofiltered at 10-15 ° C, with Desai 5 DK 10 (GE Osmonics, USA) as the filtration membrane and a pressure of 13-19 bar with a permeate flow of 8.4-10.5 l / m 2, hydrolysed fat-free the milk was initially filtered with a concentration factor of 2, i.e. a total of 10 l of permeate was removed from the apparatus. Thereafter, dlofluorization (5 l) was added to the NF retentate f (10 l) at the same rate as NF permeate II was generated. The permeate of the first nanofiltration step 15 and the permeate obtained by diafiltration were collected for art and combined. This combined permeate fraction is hereinafter referred to as NF permeate IL

The feed containing hydrolysed skimmed milk, NF permeate II and the retentate obtained by diafiltration, hereinafter referred to as NF retentate II, were sampled and assayed for protein, dry matter, glucose, galactose, and ash and calcium (Table 2). The lactose content of the NF retentate was <0.01% after 4 h, i.e. hydrolysis continued during and after nanofiltration, δ

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Table 2, 1st Nanofiltration of Hydrolysed Skimmed Milk with Diafiltration, Composition of Feed, Retentate and Permeate. For the volumes of the table, the Si filter was fed to the filter.

I I Input | } j (hydrolysed NF retentate II] NF permeate skim milk) ___ j_ | Volume (I) 20 10! 15 | Composition \

Protein (%) 3.4 6.5 j 0.1

Ash (%) 0.7 1.1 [0.2 |

Calcium (mg / kg) 1100 j 2100 30 |

Magnesium (mg / kg) 110 | 200 I <10 j

Dry matter (%) 9.0 [14.4 2.0]

Glucose (%) 2.3 f 3.1 0.7 [

Galactose (%) 2.2 J 3.1 J 0.7 |

Ca / protein (g / kg) 32.5 [33.0 [| The experiment was continued in the third sub-step by nanofiltration of NF permeate II with a factor of 10 on Filmtec NF films (Dow, USA) and a filtration temperature of 10-20 ° C. The permeate flow rate was 5.3-9.4 l / m2h and the pressure was 10-21 bar.

The resulting NF-permeate was further concentrated by reverse osmosis (10? La (Filmtec RO-390-FF, Dow, USA) at room temperature (ca. 25 ° G) with a concentration factor of 1.35.

Dry matter, glucose, galactose and ash were determined from NF-permeate III and NF-retentate III and RO-retentate I. The results are shown in Table 3.

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Table 3, Hydrolyzed Skimmed Milk 2, namofiltration, and concentration by reverse osmosis. Composition of feed, ratate and permeate.

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Input NF- NF »RO-

(NF-permeate II) and retentate ill

Volume (I) _15 j 1.5 13.5__10 {

Composition j ......... L "................" ...................

Dry matter (%) i 2.0 j 15.3 0.5 0.7

Glucose (%) j ......... 0.7 6.9 0.1 ...... + ..... 0.2

Glycose (%) j 0.7 | ___________ 6.4 _J 0.1 j; 0.2 _______________ I'The Ash (%) ____________ | 0.2 0.7 | 0.2 "| 0.2 ...........

The second stage retentate (NF retentate II; Table 2) and RO retentate (Table 3) were used in milk formulation (Example 6). RO permeate can also be used in the formulation of milk.

Example 3. Two-Stage Nano Filtration of Hydrolyzed Skim Milk (Wells Desal 5 DL (K-3) and Fiimtec NF (K '6)) 10 Phase Nanofiltration of Lactose Hydrolyzed Skim Milk Permeate I in a second step in the cold to recover minerals,

According to the procedure described for Edei, skimmed milk (40 L) was hydrolyzed (9 ° C for 18 h) at a dosage of 0.08% by Godo YNL2 lactase (Godo Shusei Company, Japan). The hydrolysed skimmed milk was nanofiltered at a temperature of 47-51 ° C. The nanofiltration well was Desal 5 DL (GE Osmonics, o ™ USA). The pressure was increased to keep the flux constant. The permeate flow was 8.1-9.6 l / m2h and the pressure was 4-6.4 bar. Filtration was continued until the concentration factor was 20.

x Samples were taken from feed, retentate, and permeate and analyzed for protein, dry matter, glucose, galactose, ash, and calcium (Table

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Table 4, 1st nanofiltration of hydrolysed skim milk.

Composition of feed, retentate and permeate, 15

Composition Feed (hydrolyzed NF retentate I NF permeate I greasy mast) j

Protein (%) 3.4 8.5 _________________ 0.2 ___________]

Ash (%) 0.8 1.4 J 0.3

Calcium (mg / kg) 1200 2900 T 40

Dry matter (%) 8.9 15.7 j 4.6

Glucose (%) 1 2.3 J 2.5 [1.8 J

Galactose (%) 2.2 2.5] 1.7 |

Ca / protein (g / kg) _35.1 34.2 µl

The NF-permeate I (20 L) of hydrolyzed skim milk was further nanofiltered with a concentration multiplier 8 to give NF-retentate II and NF-permeate II. The nanofiltration membrane was Filmtec NF (Dow, USA) and the filtration temperature was 10-25 ° C. The permeate flow oil is 4.3-9.6 l / m2h and the filtration pressure is 10-26 bar.

Samples were taken from feed (NF permeate I), NF retentate E1 and 10 NF permeate II and assayed for protein, dry matter, glucose, galactose and ash (Table 5).

Table 5. 2nd nanofiltration of hydrolysed skim milk.

Composition of feed, retentate and permeate.

I Composition Supply i NF-Retentate H NF-Permeate! j (NF-permeate I), o j Solid (%)! 4.6 15.9 0.5 ab j Glucose (%) "" 8 1.8 7.5 0.2 ^ j Galactose (%) | _1.7 7.1 _ 0.2 ___ ^ [Ash (% ) I 0.3 0.6 f 0.2_

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o First stage retentate (NF retentate I; Table 4) and 00 g of second stage permeate (NF permeate II; Table 5) were used in milk o formulation (Example 8). NF-Retentate I was also used in the formulation of whey protein milk (Example 10).

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Example 4. Two-step Nano Filtration of Hydrolyzed Skimmed Milk (Wells Desal 5 DL {K-1,5} and Fiimtec NF (K = 6)}

The hydrolysis of the lactose in the skimmed milk was done in the same manner as in Example 3. The first step of the stepwise nanofiltration of the hydrolyzed skimmed milk was carried out at 50 ° C as described in Example 3 except that the concentration factor was 1.5. The NF permeate obtained in the first step! nanofiltrated to recover the minerals in a second step at 10-25 ° C with a concentration factor of 6 as described in Example 3.

10 From the feed of the first nanofiltration step (hydrolysed skim milk), NF retentate! and NF-permeate I were assayed for protein, dry matter, glucose, galactose, and ash and calcium (Table 6). From the feed of the second nanofiltration step (NF permeate I), NF retentate S! and NF permeate Π were assayed for dry matter, glucose, galactose and ash (Table 7).

The sugars and minerals were further chromatographically separated from the NF retentate II as described in Example 5.

Table 6. First nanofiltration of hydrolysed skim milk.

Composition of feed, retantate and permeate.

j Composition Feed j I (Hydrolysed NF Retentate S NF Penmeate I J Skimmed Milk) {j [Protein (%) 3.4 5.0 G, 1 j | Ash (%) ........................................... 0.7 .......................................... 1.0 0.3 | | Calcium (mg / kg) 1100 1700 38 |

Dry matter (%) 8.9 '11.1 .............. 4.3 [% glucose (%) 2.3] 2.3 1.8 µg Galactose (%) 2.2 | 2.3 1.7 µCa / protein (g / kg) 35.1 | 34.3 |

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Table 7. Hydrolysed skimmed milk 2 = nanofiltration.

Composition of feed, retentate and permeate.

17 | Composition Feed j NF retentate H j NF permeate l! j I (NF-permeate I) | I___ j | Dry matter (%) 4.3 j -16.1 j 0.5 j

Glucose (%) ______________________ 1.8 ............................. 7-.6 [0.2 |

Galactose (%) 1.7 7.1 0.2

Ash (%)] 0,3 0,6 0,2]

First stage retentate (NF retentate!) (Table 6) and 5 second stage permeate (NF permeate II) were used in milk formulation (Example 7).

Example 5. Mineral Recovery from Concentrated Nanofiltration Permeate

Concentrated NF permeate of hydrolyzed skimmed milk, i.e. 10 second nanofiltration retentates (NF retentate II), were further processed on a Krom matrix column to separate the mineral and sugar fractions.

The cation exchange resin (Finex CS 09 GC, Finex Oy, Finland, Na form) was equilibrated with skim milk (1 liter / 50 ml resin) for 30 minutes. Skimmed milk was rinsed from the resin with deionized water. The equilibrated 15 resin (180-200 ml) was packed in a jacketed 65 ° C column (height 100 cm, diameter 1.5 cm). 20 ml of NF retentate concentrate (NF retentate II) (Brix about 16; Example 4) was fed to the column. The flow rate was 160 ml / h, the temperature was 65 ° C and tap water was used as eluent. Fractions of 5 ml were collected and combined into two fractions, a mineral fraction and a sugar fraction. A similar difference of ε 20 was also made at 10 ° C.

The fractions were determined ash, galactose and glucose.

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In practice, milk minerals and monosaccharides were completely separated from NF permeate (NF-

Retentate H) (Tables 8 and 9). The separation of sugars was more effective at 65 ° C

g at 25 ° C.

The mineral fraction separated at 65 ° C (fractions 0-50; ref. 8) was used to form lactose-free milk (Example 7).

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Table 8. Fractions and conductivity of fractions separated from condensed skimmed milk NIF permeation chromatography.

Input ° Brix {%) j High temperature f C) Fractionate (ml) | ° Brix (%) Conductivity (mS / cm) I 0-50 | 0.6 2.98 16 | 65 - 1 --------------------------------------------- - - s 50--100 | 6.4 ___ 0.236 ____________________ 1 0-50! 1.6 2.98 16 I 10 r .................................. I ...... .................................................. ............................

j 50-100 | 5.5 (0.159

Break © 9. Galactose, glucose, and ash content of fractions chromatographically separated from condensed skimmed milk NF permeate.

Feed ° Brix i High Temperature Fractions j Galactose Glucose Ash __ (%) ............. J ................. CC) ... ............................ (ml) ............. | ______________ (%) ________ (%) (%) 16 | 65 0-50 j 0.02 ...................... 0.13 0.22 16 | 10 0-50 | 0.28 0.78 ........... 0.23 ...........

Example 6. Composition of lactose-free milk from nanofiltration retentate of hydrolysed skimmed milk and RO retentate

The lactose-free milk was composed of the NF retentate II and RO retentate I of the hydrolysed skimmed milk 10 of Example 2.

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Table 10, Composition of lactose-free skim milk with NF retentate and RO retentate of hydrolysed skim milk, NF retentate il j RO retentate I | Lactose free fat free (Example 2) (Example 2) scale i

Proportion (%) 50 50 i j

Composition ___ j

Protein (%} 6.4 0.2 j 3.3 j

Glucose (%) 3.1 0.2 j 1.7 j

Glycose (%) 3.1 0.2 | 1.6 |

Ash (%) 11 _______________________________________ 0.2 j 0.7!

Dry matter (%} 14.4 0.7 i 7.5 i --------------------------------- -------------- 1 ----------------------------— "" —'— - ---------------------— ---------- "-" "I ----------! Calcium ( mg / kg) | 2100 - | 1100 ij Magnesium (mg / kg) | 200 <10 j 100 |

Example 7, Preparation of Lactose-Free Milk from Nanofiltration and Chromatography Fractions of Hydrolysed Fat-5 Milk

Lactose-free milk was composed of the fractions of Examples 4 and 5, i.e. retentate (NF retentate I) from the first nanofiltration step of hydrolysed skimmed milk, NF permeate from the second nanofiltration step from NF and from the second NF permeate from NF permeate. retenate from a chromatographically separated mineral fraction. The composition of the fractions as well as the proportions in the compound milk are shown in Table 11 as well as the composition of the compound product. (The liquid contained in the lactose-free milk is from the pro-T process and no separate addition of water is required.) £ 3 In addition, lactose-free milk was prepared as above, except that water was added to the chromatographically separated mineral fraction (Table 12).

The RO permeate fraction from reverse osmosis can be used in place of water.

x The composition of the milk was identical to that of the hydrolysed milk, with the exception of black carbohydrates. The amount of calcium (1100 mg / kg) was almost the same as in the original milk. The products were also evaluated organoleptically and found to have good properties and taste like normal skim milk.

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Table 11. Composition of lactose-free milk from NF retentate I, NF »permeate II and the mineral fraction of the chromatograph. Composition of fractions and product and proportion of fractions.

| NF-r @ tannate f NF-primer i \ Chromafogra-Lactose-free j (Example 4) (Example 4) fian mineral-free | \ | Isjae milk and milk (example 5) | Share (%) 66.8 I 27.7 _ ^ 5.7 | Composition It Protein (%) 5.0 - 0 3.3 L Glucose (%) 2.3 0.2 0.1 1.6 S 2.3 0.2 <01_ 1.6 ___ 1.0 0.2 0.2 0.7 8.8_ 0.5 7.5 1700 12 - 1140 5 Table 12. Preparation of lactose-free milk from NF-retentate, NF »permeate II and water. The composition of the products and the proportion of the products.

NF retentate NF permeate Water Lactose-free (Example 4) (Example 4) skimmed milk

Proportion (%) - 88.8 27.7 5.7

Composition x- Protein (%) 5.0 - 0 3.3 § Glucose (%} 2.3 0.2 0 1.6 § Galactose (%) 2.3 0.2 _____0 ___ 1.6 - Ash (%) ) ........................... 1.0 0.2 I 0 0.7! Solid (%} 8.8 0 , 5 0 7.5 * Calcium (mg / kg) 1700 12 0 1100 CD "''

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Example 8. Composition of Low Lactose, Lactose-Free and Low Carbohydrate Milk from Nanofiltration Fractions of Hydrolysed Skimmed Milk

The lactose-free, lactose-free and low-carbohydrate milk according to the invention was composed of the fractions of Example 3, i.e. NF retentate I and NF permeate IL. Hydrolysed skimmed milk 14), Low-carbohydrate lactose-free milk was composed solely of those NF-10 fractions (Table 15). The composition of the fractions and their proportions in the compounded milk are given in Tables 13-15 as well as the composition of the product.

Table 13. Composition of lactose-free milk from nanofiltration fractions having the same product composition as normal milk.

| NF Retentate I Hydrolyzed! NF permeate il Lactose free (Example 3) skimmed milk i (Example 3) fat free | scale I Proportion _ (%). I 21.3 43.2 [35.4 j Composition [il ^ Protein (%) J__ 8.5 ___ j 3.3_ j __ - 3.3

Glucose (%) 2.5 | 2.3 [0.2 1.6]

Glycose (%) J 2.5 | 2.2 | 0.2 1.6

Ash (%) I 1.4 | 0.7 0.2 0.7

Dry matter (%) | 15.7 j8.8 .......... 0.5 N7.3

Calcium (mg / kg) 2900 I 1100 10 f 1100 ^ 15 The composition of the lactose-free skimmed milk described in Table 13 was identical to that of completely hydrolysed milk, except for carbohydrates. Note that the amount of calcium was exactly the same as in the a! ~ X original milk. The product was also evaluated organoleptically and was found to taste good and to taste normal skim milk.

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Table 14, Preparation of Low Lactose Protein and Caffeine Enriched Milk.

| | MF-ret @? Itaatt81 Fat-free NF-permattl 11 ProteHmpitoirssrs, j | | (example 3} mast (example 3) rimsaskatssumsners j | | j | milk | I Proportion _ (%) 47.0 12.2 | 40.8 _ j Composition j I | | Protein (%) 8.5 | 3 , 3} - 4.4] [Lactose (%) <0.01 4.7 |, <0.01 0.6__ | | Glucose (%) 2.5 Q j 0.2 1.3 [... ......___________ 0 ^ .................................. 1.3 ..... ..................

Ash <%) 1.4 0.7 L 0.2 0.8 [Dry matter (%) 15.7 8.8 0.5 8.6 [Calcium (mg / kg) 2900 and 1100 10 1500

The milk depicted in Table 14 has a significantly higher protein content than normal milk but with a level of monosaccharides at a level similar to that of normal milk. In an organoleptic test, milk was found to be fuller than ordinary skimmed milk but otherwise tastes like ordinary milk.

Table 15. Preparation of Lactose-Free Milk-Low Hydrate, N-Retentate NF-Permeate 11 1 Low-Hydrate (Example 3) j (Example 3) j Lactose-Free | j | minced T- Share (%) | 38.9 I 61.1 j ^ Compositions | | | § Protein (%) 8.5 _L i 3.3 ^ Glucose (%) 1 2.5j 0.2 [_1.1 i x Galactose (%) [2.5 | 0.2 "ash 1.1% ash (%) '1.4 t 0.2 f 0.7 io Solid (%) 15.7 0.5 f 6.4 £ Calcium (mg / kg) 2900 [_10 | ________ 1100_____________________j

The product described in Table 15, by the way, had the same composition of ordinary milk but no lactose and very low glucose and galactose levels of 10 ° C to 23, despite its surprisingly full-bodied taste despite its sweetness compared to normal milk,

Example 9, Hydrolyzed Whey Sulfur Filtration in One Layer from Desal 5 OL Film (K-7) 5 Peeled whey (40 L) was hydrolyzed (9 ° C, 20 h) by Godo YNL 2 -actase (Godo Shusei Company> Japan) at a dosage of 0.1 % and nano-filtered with a Desal 5 DL well (GE Osmonics, USA) at a temperature of 46-51 ° C and a pressure of 3-6.5 bar. The permeate flow was 10.0-13.5 i / m2h. The Na-filtration was continued at a concentration factor of 7, i.e. the volume of retentate was 5.5 L and 34.5 L of permeate.

Feed (hydrolyzed whey), retentate, and permeate were sampled and analyzed for protein, dry matter, glucose, galactose, and ash and calcium (Table 16),

Table 16. First Nanofiltration of Hydrolyzed Whey, Compositions of Feed, Retentate 15 and Permeate

Composition Input I

, i NF retentate S NF permeate | (hydrolysed whey) _______

Protein (%) 0.6 4.6 _

Ash (%) __ 0.3 T5 0.3

Calcium (mg / kg) 4,000 2700 80

Dry matter (%) 5.0 10.2 4.1

Glucose (%) 2.2 2.7 2.0 |

Galactose (%) 1.9 2.7 ^ ___ 1.8 1

Ca / protein (g / kg) ______ 59.0 58.8 _j δ ^ NF permeate I separated from the hydrolysed whey corresponded to NF permeate extracted from the hydrolysed skimmed milk under similar conditions (Example 3, Table 4). | The filtration can be continued in the second step in the same manner as described in Example 3.

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Example 10. Composition of lactose-free whey protein-containing milk from nanofiltration fractions of hydrolyzed whey and skimmed milk

Lactose-free whey protein-containing milk was composed of the NF retentate I of hydrolyzed whey of Example 9, NF-lentate I of hydrolysed skimmed milk of Example 3, the hydrolysed skimmed milk and the RO permeate obtained in Example 2. Whey protein-containing milk contained less carbohydrates and more calcium than normal milk and whey protein, 10% of the milk protein.

Table 17. Composition of lactose-free whey protein-containing milk of nanofiltration fractions and skimmed milk.

NF-Reterostats I MF-Rechatate I Hydrply »RO-Permeatsts Lactose-free (milk, (whey, whey fat-free example 3} example 9) non-fat foeroprotein-milk-plain _ ________________ mast

Proportion (%) 12.7 18.7 40.2 28.4

Composition

Protein (%) 8.5 4.6 3.4 <0.1 3.3

Glucose (%) 2.5 2.0 2.3 <0.1 _ 1.6

Glycose (%) 2.5 1.8 2.2 <0.1__1.6

Ash (%) 1,4__1.5__0.8 | <0.1 0.8

Calcium (mg / kg) 2900 2700 1100 - 1300

Solids (%) c 15.7 10.2 8.8 <0.1 7.4 δ

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Claims (16)

1. Separation of milk components, characterized in that a) the lactic acid of the soft powder is hydrolyzed, whereby the hydrolyzed soft powder is obtained and b) the hydrolyzed soft powder is nanofitrated divided into phases in at least two part steps and at least one of the The nanofiltration permeate NF Perm I obtained in the first step is brought to a second nanofiltration step, whereby the second 10-step nanofiltration retentate NF Ret H and the nanofiltration permeate NF Perm I1 are obtained, and any detachable nanofiltration and / or deletion deletion deletion regeneration steps are made at least permeate or combinations thereof, whereby the following deisteg nanofitration retentate fractions NF Ret III are obtained, etc. and on the corresponding sets of nanofitration penmeat fractions NF Perm III, etc., for separating proteins, sugars and minerals in these different fractions. 2. A process according to claim 1, characterized in that the lactose of the milk powder is partially hydrolyzed. 3. A process according to claim 2, characterized in that the partially hydrolyzed milk powder's final lactose is post-hydrolyzed at the same time as the partially hydrolyzed milk powder is nanofitrated in phases. Process according to any of claims 1-3, characterized in that the nanofiltration is divided into phases by changing the process conditions, such as temperature and / or pressure and / or adding a diafiltration step and / or changing the membrane type of the filtration and / or concentration factor. 5. A process according to claim 4, characterized in that the third nanofiltration is conducted in hot, about 42-51 ° C, and the second nanofiltration in potassium, about 5-25 ° C. § 6. Process according to any of claims 1-5, characterized in that at least some of the NF retentate fractions NF Ret I, NF Ret II, NF Ret II and so on. and the NF permeate fractions NF Perm I, NF Perm II, NF Perm 35 III etc. or combinations of them are further processed with membrane technology and / or evaporation and / or chromatographically. 7. A process according to claim 6, characterized by reduced nutrient fraction of the NF retentate fractions NF Ret 1, NF Ret II, NF Ret III, etc., preferably NF Ret II, chromatographically van / id various fractions containing minerals are obtained. sugar. 8. Lakiosin or lactose-low milk product, characterized in that it comprises at least one NF retentate fraction NF Ret II, NF Ret III, etc., or NF permeate fraction NF perm II, NF Perm III, etc., obtained from non-filtration of hydrolyzed milk powder. , which nanofiltration involves less than two steps, Milk product according to Patent Claim 8, characterized in that it has been prepared by combining two or more of the following fractions: the retentate and permeate fractions of the first nanofiltration step NF Ret I and the corresponding seeding NF Perm I, the second and subsequent nanofiltration filter retentate fractions. NF Ret M, NF Ret III, etc., the second and subsequent nanofiltration step permeate fractions NF Perm II, NF Perm III, etc., from any permeation fraction permeate fraction or a combination of these reverse osmosis-derived retentate fraction RO Ret and permeate fraction RP Perm, and the NF Ret I, NF Ret II, NF Ret III, etc. chromatographically separated fractions containing minerals and sugars. Milk product according to claim 9, characterized in that the RO Ret and the RO Perm originate from the reverse osmosis of the permeate fraction N F Perm II of the nanofiltration step. Milk product according to claim 9, characterized in that the fractions containing minerals and sugars originate from the chromatographic separation of the nanofiltration step retentate fraction NF Ret II. Milk product according to claim 10, characterized in that it has been produced by combining NF Ret II, RO Ret and optional (M 2 other manufacturing substances). ° Milk product according to claim 11, characterized in that it has been prepared by combining NF Ret I, NF Perm II, a fraction which | contains minerals and possibly other manufacturing substances. to A process for producing a lakiosin or lactose-deficient milk product, characterized in that oa) the lactose of the milk powder is hydrolyzed, the hydrolyzed milk powder is obtained and b) the hydrolyzed milk powder is nanofitrified, at least one of which is divided into phases. the nanofiltration retentate NF Ret I and / or the nanofiltration permeate NF Perm I obtained in the first step is brought to a second nanofiltration step, the second nanofiltration retentate NF Ret II and the nanofiltration permeation NF Perm II are obtained and any subsequent nitrate permeation NF Perm II of any of the preceding sub-steps nanofiltration retentate and / or permeate or a combination thereof, whereby the following sub-step nanofiltration retentate fractions NF Ret II etc. are obtained. and on the corresponding site 10 nanofliteration permeate fractions NF Perm III, etc., for separating proteins, sugars and minerals into these various fractions, c) if desired. one or more of the NF retentate fractions NF Ret I, NF Ret II, NF Ret III, etc., and of the NF permeate fractions NF Perm I, NF Perm II, NF Perm lii, etc. are processed. or a combination thereof with membrane technology and / or evaporation and / or chromatographic, d) one or more retentate and permeate fractions obtained from nanofiltration comprising at least two part steps and, if desired, of a retentate and / or permeate fraction obtained from the first nanofiltration sub-step, which fractions obtained in step b), and if desired by one or more fractions obtained from step c) and optionally of other preparations, a product of the desired composition is prepared, e. ) if desired, concentrate the product obtained in step d) into a concentrate or powder. 15. A process according to claim 14, characterized in that the milk lactose lactose is partially hydrolyzed. 16. A process according to claim 15, characterized in that the partially partially hydrolyzed milk lactose is post-hydrolyzed and at the same time the C1 as the partially hydrolyzed milk powder is nanofitrated in phases. o X Χ CL CD O 00 tn oo o o CM