It is necessary to bring the Spanish legislation into line with the provisions of Council Directive 83/417 of the European Economic Community on the approximation of the laws of the Member States relating to certain lactoproteins (caseins and caseinates) intended for human consumption, as well as Commission Directives 85/503 and 86/424 concerning methods of analysis and Community procedures for sampling for analysis Chemicals for caseins and caseinates, it seems appropriate to issue these General Quality Standards for Food caseins and caseinates.

In its virtue, the sectors affected, prior to the mandatory report of the Inter-Ministerial Commission for Food Management, and on the proposal of the Ministers of Economy and Finance, Agriculture, Fisheries and Food, and Health and Consumer Affairs, this Ministry of Relations with the Courts and the Government Secretariat has:

First.

The General Quality Standards for Food Caseins and Caseinates are approved for the internal market, which are collected, respectively, in Annex 1 and 2 of this Order.

Second.

The sampling and analytical determinations shall be performed in accordance with the methods set out in the notes 3 and 4 of this Order.

Third.

The competent departments shall ensure compliance with the provisions of this Order through their administrative bodies, which shall coordinate their actions, in any event, without prejudice to the powers conferred upon them. correspond to the Autonomous Communities and Local Corporations.

Fourth.

This Order shall enter into force on the day following that of its publication in the "Official State Gazette".

Madrid, March 28, 1988.

ZAPATERO GOMEZ

Excms. Mr Ministers for Economic Affairs and Finance, Agriculture, Fisheries and Food and Health and Consumer Affairs.

ATTACHED 1

General quality standard for food caseins destined for the internal market

1. Name of the rule.

General quality standard for food caseins.

2. Object of the rule.

The purpose of this standard is to define the conditions and characteristics to be met by food caseins for marketing and use in the internal market.

3. Scope of application.

This general rule covers all food caseins intended for placing on the market in the internal market for use in the food industry.

Products defined in this standard can only be marketed if they conform to the definitions and requirements laid down in it.

4. Definitions.

4.1 Casein: For the purposes of this standard "caseins" means the main protein component of milk, insoluble in water obtained by washing, pressing and drying the clot obtained from skimmed milk by the addition of acid, or by microbial acidification (acid casein), or by means of rennet or other milk coagulant enzymes (casein al rennet), without prejudice to a possible prior application of ion and ion exchange procedures concentration.

4.2 Food Caseins: These are the caseins for which the processing of the skimmed milk used, the clot obtained from the same, or the aqueous suspension of the casein is compulsorily subjected to a pasteurization process.

5. Denominations.

The names listed below are reserved for the products covered by the standard and must be used in the industrialization and marketing of these products.

5.1 Food acid casein: This is called the food casein for which the processing aids and/or bacterial cultures listed in section 6.3.1 have been used, which meets the requirements set out in paragraph 6.

5.2 Casein the food cutout: This is called the food casein for which the processing aids listed in paragraph 6.3.2 have been used, which complies with the requirements laid down in paragraph 6.3.2. 6.

6. Essential factors of composition and quality.

6.1 Essential ingredients: Skimmed milk.

6.2 Physical-chemical characteristics:

	Food Acid Casein - Percentage	Casein the food bowl - Percentage
moisture content	10 m/m	10 m/m
Minimum milk protein content calculated on dry extract	90 m/m	84 m/m
Minimum caseins for dairy proteins	95 m/m	95 m/m
Maximum milk fat content on dry extract	2,25 m/m	2 m/m
titratable acidity expressed in ml of decitnormal sodium hydroxide solution per gram	0.27 ml/g
content (P2OR5 included)	(max) 2.5 m/m	(min) 7.5 m/m
anhydrous lactose content	1 m/m	1 m/m
Maximum sediment content (burned particles)	22.5 mg in 25 g	22.5 mg in 25 g
Testing the phosphatase	Negative	Negative

6.3 Technology aids:

6.3.1 For food-acid casein:

Lactic acid (E 270).

Hydrochloric acid.

Sulfuric acid.

Citric acid (E 330).

acetic acid (E 260).

Orthophosphoric acid (E 338).

Lactoserum.

Bacterial cultures that produce lactic acid (lactic ferments).

6.3.2 For casein food cutout:

Cover.

Other milk coagulant enzymes.

6.4 Organoleptic Characters: Olor: Absence of Strange Smells.

Appearance: Color of white to white cream; the product must be free of clumps that resist light pressure.

7. Contaminants.

The maximum levels of pollutants and toxic substances must not exceed the limits set out in paragraphs 7.1 and 7.2 and in the legislation in force and, failing that, in international standards accepted by the Spanish State, which shall ensure its compliance as a guarantor of the same, with the determination and requirement of responsibility at this point by the body of the State concerned.

7.1 Pollutants: Maximum lead content: 1 mg/kg.

7.2 Impurities: Strange materials (particles of wood, metal, hairs or fragments of insects, etc.): Absence in 25 g.

8. Prohibitions.

It is expressly prohibited:

8.1 Use for the manufacture of food caseins raw materials that are adulterated or altered, as well as those considered strange to their composition.

8.2 The presence in the food caseins of proteins and/or fats other than those of the milk itself.

8.3 The marketing and sale of products that do not comply with this standard include in their denomination the words "food acid casein" or "casein in the food bowl".

8.4 The sale of adulterated, altered, contaminated or parasitic caseins.

9. Hygiene.

9.1 The skimmed milk, the clot of the milk obtained or the aqueous suspension of casein must be subjected to a heat treatment equivalent to at least the pasteurisation. That is, that the phosphatase test must be negative.

9.2 The manufacturer shall be responsible for the controls of the raw material and other ingredients, unless otherwise tested, by checking the conditions of purity at the time of receipt or use, by examination and normal analyses in good industrial practice or through the necessary certifications provided by the supplier.

9.3 The preservation of the finished product shall be carried out in such a way as to ensure total protection against contaminants, moisture absorption or action of light.

10. Packaging.

Food caseins for industrial use shall be presented in due hygiene and cleaning conditions, either in containers or in industrial containers for food use, conveniently closed.

11. Tagged.

Mandatory data on the labelling of packaging must be easily understood and must be entered in a prominent place in such a way as to be easily visible, clearly legible and indelible. This information should not be masked by drawings or any text or image, written, printed or graphic.

Mandatory data on the labelling of food products placed on the market in Spain will necessarily be expressed at least in the official Spanish language of the State.

The information on the labelling of the packaging of food caseins subject to this quality standard shall be mandatory for the following specifications:

11.1 Product Naming:

a) It shall be indicated in accordance with paragraph 5 of this standard.

(b) Where food caseins are marketed in a simple mixture with other products, the name shall be:

The mention "Mix of ......................." followed by the names of the different products which constitute the mixture, in order of decreasing weight.

The indication of the cations or cations for the caseinates.

The proportion of proteins for mixtures containing caseinates.

11.2 Net content: The net content, expressed in grams or kilograms, shall be indicated.

11.3 Identification of the Company: The name or the name and the name and address of the manufacturer, packer or seller established in the European Economic Community, as well as the other specifications set out in paragraphs 13.2 and 13.3 of Article 13 of Royal Decree 2058/1982.

11.4 Identification of the manufacturing batch: Any packaging must bear an indication to identify the batch of manufacture, with the form of such identification at the discretion of the manufacturer. This indication shall be required only for the products covered by this Regulation, manufactured or packaged in Spain. The documentation in which the data necessary for the identification of each batch of manufacture shall be made available to the competent authorities of the Administration shall be made available.

11.5 Country of origin: In the case of products imported from third countries.

11.6 The indications provided for in the third indent of paragraph 11.1 (b) and in paragraphs 11.2, 11.3 and 11.5 may appear, instead of the packages, in a document accompanying the goods.

In the case of bulk transport in containers, this derogation may be extended to the second indent of paragraph 11.1 (b) and to paragraph 11.4.

12. Tag out.

The labels of the packages shall include:

Denomination of the product or brand.

Number and net contents of containers.

Company name or reason or Company name.

Instructions for conservation, if necessary.

It will not be mandatory to mention these indications as long as they can be clearly and easily determined on the labelling of packaging without the need to open the packaging.

13. Responsibilities.

Responsibilities will be established in accordance with the following assumptions:

(a) The responsibility inherent in the identity of the product contained in non-open containers, integrated, corresponds to the manufacturer or packer of the packaged food product or, where appropriate, to the importer.

(b) The responsibility inherent in the identity of the food products contained in open containers corresponds to the product holder.

(c) The inherent responsibility for the poor preservation of the product in packaging, whether open or not, or unpackaged, corresponds to the product holder.

In any case, such liability assumptions will fail in those assumptions where the liability of the previous holder or supplier of the product can be identified and tested.

14. Sanctioning regime.

The infringements of the provisions of this Regulation shall be sanctioned in each case by the competent authorities in accordance with the laws in force and with the provisions of Royal Decree 1945/1983 of 22 June 1983. (a) the rules governing infringements and penalties in the field of consumer protection and agri-food production, subject to the instruction of the relevant administrative file. In any event, the following information shall be immediately available to the health authorities concerned by the instructor of the file, where health offences are detected.

ATTACHED 2

General quality standard for food caseinates destined for the internal market

1. Name of the rule

General quality standard for food caseinates.

2. Object of the rule

The purpose of this standard is to define the conditions and characteristics to be met by the food caseinates for marketing and use in the internal market.

3. Scope of application

This general rule covers all food caseinates intended for placing on the market within the internal market for use in the food industry.

Products defined in this standard can only be marketed if they conform to the definitions and requirements laid down in it.

4. Definitions

4.1 Caseinates: caseinates are understood to mean products obtained by drying casein in aqueous suspension treated with one or more neutralized agents.

4.2 Food caseinates: Food caseinates obtained from edible caseins in aqueous suspension, treated with one or more of the processing aids listed in the paragraph, are understood as food caseinates. 6.3 and which meet the requirements set out in paragraph 6.

5. Denominations

Food caseinates will be called "Caseinato de ... alimentary", including the name of the cation or cations, in the latter case separated by a "y", or "Caseinato ... food", including the name of the cation or cations.

These names are reserved for the products covered by this standard and must be used in the industrialization and marketing of these products.

6. Essential factors of composition and quality

6.1 Essential ingredients: Food caseins.

6.2 Physical-chemical characteristics:

Maximum moisture content: 8% m/m.

Minimum protein casein content of milk, calculated on dry extract: 88% m/m.

Maximum fat content of milk calculated on dry extract: 2% m/m.

Maximum anhydrous lactose content: 1% m/m.

pH: 6 to 8.

Maximum sediment content (burnt particles): 22.5 mg in 25 g.

phosphatase test: Negative.

Caseinates are almost totally soluble in distilled water, except for calcium caseinate that may present different degrees of solubility.

6.3 Food quality processing aids: The following neutralising agents and optional tampons can be used:

Sodium hydroxides.

Potassium carbonates.

Calcium Phosphates.

Ammonium Phosphates.

Magnesium citrates.

6.4 Organoleptic characters:

Smell: Aroma and light foreign odors.

Appearance: Color of white to white cream; the product must be free of clumps that resist light pressure.

7. Pollutants

The maximum levels of pollutants and toxic substances must not exceed the limits set out in paragraphs 7.1 and 7.2 and in the legislation in force and, failing that, in international standards accepted by the Spanish State, which shall ensure its compliance as a guarantor of the same, with the determination and requirement of responsibility at this point by the body of the State concerned.

7.1 Pollutants: Maximum lead content: 1 mg/kg.

7.2 Impurities: Strange materials (particles of wood, metal, hairs or fragments of insects, etc.), ...................... absence in 25 g.

8. Bans

It is expressly prohibited:

8.1 Use for the manufacture of food caseinates raw materials that are adulterated or altered, as well as those considered to be foreign to their composition.

8.2 The presence in the food caseinates of proteins and/or fats other than those of the milk itself.

8.3 The marketing and sale of products that do not comply with this standard include in their denomination the words "food casework".

8.4 The sale of adulterated, altered, contaminated or parasitic caseinates.

9. Hygiene

9.1 The manufacturer shall be responsible for the controls of the raw material and other ingredients, unless otherwise tested, by checking the conditions of purity at the time of receipt or use, by examination and normal analyses in good industrial practice or through the necessary certifications provided by the supplier.

9.2 The preservation of the finished product shall be carried out in such a way as to ensure total protection against contaminants, moisture absorption or action of light.

10. Packaging

Food caseinates for industrial use shall be presented in due hygiene and cleaning conditions, either in containers or in industrial containers for food use, conveniently closed.

11. Labelling

Mandatory data on the labelling of packaging must be easily understood and must be entered in a prominent place in such a way as to be easily visible, clearly legible and indelible. This information should not be masked by drawings, or by any text or image, written, printed or graphic.

Mandatory data on the labelling of food products placed on the market in Spain will necessarily be expressed at least in the official Spanish language of the State.

The information on the labelling of the packaging of food caseinates subject to this quality standard shall be mandatory for the following specifications:

11.1 Product Naming:

a) It shall be indicated in accordance with paragraph 5 of this standard.

(b) Where food caseinates are marketed in a simple mixture with other products, the name shall be:

The mention "Mix of ........" followed by the denominations of the different products that constitute the mixture, in descending order of weight.

The indication of the cations or cations for the caseinates.

The proportion of proteins.

11.2 Net content: The net content, expressed in grams or kilograms, shall be indicated.

11.3 Identification of the Company: The name or the name and the name and address of the manufacturer, packer or seller established in the European Economic Community, as well as the other specifications set out in paragraphs 13.2 and 13.3 of Article 13 of Royal Decree 2058/1982.

11.4 Identification of the batch of manufacture: Any packaging must bear an indication to identify the manufacturing batch, with the form of such identification at the discretion of the manufacturer. This indication shall be required only for the products covered by this Regulation, manufactured or packaged in Spain. The documentation in which the data necessary for the identification of each batch of manufacture shall be made available to the competent authorities of the Administration shall be made available.

11.5 Country of origin: In the case of products imported from third countries.

11.6 The indications provided for in the third indent of paragraph 11.1 (b) and in paragraphs 11.2, 11.3 and 11.5 may appear, rather than on packaging, in a document accompanying the goods.

In the case of bulk transport in containers, this derogation may be extended to the second indent of paragraph 11.1 (b) and to paragraph 11.4.

12. Tag Out

The labels of the packages shall include:

Denomination of the product or brand.

Number and net contents of containers.

Company name or reason or Company name.

Instructions for conservation, if necessary.

It will not be mandatory to mention these indications as long as they can be clearly and easily determined on the labelling of packaging without the need to open the packaging.

13. Responsibilities

Responsibilities will be established in accordance with the following assumptions:

(a) The responsibility inherent in the identity of the product contained in non-open containers, integrated, corresponds to the manufacturer or packer of the packaged food product or, where appropriate, to the importer.

b) The responsibility inherent in the identity of the food products contained in open containers corresponds to the product holder.

(c) The inherent responsibility for the poor preservation of the product in packaging, whether open or not, or unpackaged, corresponds to the product holder.

In any case, such liability assumptions will fail in those assumptions where the liability of the previous holder or supplier of the product can be identified and tested.

14. Sanctioning regime

The infringements of the provisions of this Regulation shall be sanctioned in each case by the competent authorities in accordance with the laws in force and with the provisions of Royal Decree 1945/1983 of 22 June 1983. (a) the rules governing infringements and penalties in the field of consumer protection and agri-food production, subject to the instruction of the relevant administrative file. In any event, the following information shall be immediately available to the health authorities concerned by the instructor of the file, where health offences are detected.

ATTACHED 3

Sampling procedure for the analytical control of certain edible caseins and caseinates intended for human consumption

I. GENERAL PROVISIONS

1. Administrative prescriptions

1.1 Personnel: The taking of samples shall be carried out by an authorised and qualified person, as laid down in the provisions in force in the Member States.

1.2 Sellading and labelling of samples: Each official sample shall be closed, sealed at the site of the taking and shall be identified in accordance with the provisions in force in the Member States.

1.3 Duplicate samples: At least two equivalent and representative samples shall be prepared for the analysis. Without prejudice to the Community provisions which may be adopted, the number of samples to be taken shall be in accordance with the applicable national legislation in each Member State. Once the intake has been made, the samples will be sent to the laboratory as soon as possible.

1.4 Report: The samples will be accompanied by a report, which will be produced according to the legislation of the Member States.

2. Sampling equipment

Features:

The sampling equipment shall not cause any change in the sample that could alter the results of the analyses and shall be sufficiently resistant in order to avoid any distortion of the results. It is recommended to use stainless steel material.

All surfaces of the material must be polished and free of cracks, and all angles rounded. The sampling equipment shall comply with the requirements laid down in respect of the products from which samples are to be taken.

3. Sample intake vessels

Features:

The samples and closures for samples shall be of a suitable material and structure that adequately protect the sample, and which do not cause changes that may alter the result of the analyses or examinations. Suitable materials include glass, some metals and some plastics. The containers shall preferably be opaque. If they are transparent or translucent, the samples containing samples shall be placed in a dark place.

The containers and their closures must be clean and dry.

The shape and capacity of the container will be suitable to meet the requirements for the product to be taken.

Single-use plastic containers, allumunium sheets or adapted plastic bags may be used, provided with appropriate closure systems.

Containers other than plastic bags shall be closed hermetically either by means of a suitable stopper or by a metal or plastic screw cap, if necessary; a plastic seal, Insoluble, non-absorbent and impermeable to fats, and which does not alter the smell, taste, properties or composition of the sample.

In case plugs are used, these must be made or coated with non-absorbent materials and toilets.

4. Sampling techniques

The sample collection container will be closed immediately after the takeover.

5. Storage of the samples

The recommended sample storage temperatures for the various caseins and caseinates will not exceed 25 ° C.

6. Transport of samples

The samples will be sent to the laboratory responsible for testing as soon as possible (preferably before 24 hours after the taking). During transport, precautions must be taken to prevent samples from being exposed to pollutants, direct sunlight and temperatures above 25 ° C.

II. METHOD: SAMPLING OF EDIBLE CASEINS AND CASEINATES

1. Object and scope of application

This method describes sampling for chemical analysis of:

Edible acid cases.

Caseins to edible rennet.

Edible Caseinates.

2. Team

See section 2. of the general provisions.

2.1 Long enough probes to reach the bottom of the product canister. The probes corresponding to the description given in Part III of Annex 3 to this Order are suitable.

2.2 Spoon, spatula or spoon. Wide-leaf.

2.3 Sample Receipts. See section 3 of the general provisions.

3. Procedure

3.1 Generalities: Care will be taken to minimize the absorption of atmospheric humidity by the product contained in the container during or before the sampling for analytical purposes. The container shall be resealed hermetically after the sampling has been carried out.

3.2 For chemical analysis.

3.2.1 Sampling (in general). A sample of not less than 200 grams shall be taken. Insert a clean, dry probe into the product if necessary with the container tilted or lying laterally. The slot shall be oriented downwards and a uniform rate of penetration shall be adopted. When the probe reaches the bottom of the container it shall be rotated 180 degrees, the contents shall be removed and the contents of the sample container discharged. For a sample not less than 200 grams one or more takes shall be made. The container shall be closed immediately after the taking. This takes place in the same batch or consignment.

3.2.2 Taking samples of packaged products in small packages for retail sale.

The sample may consist of the contents of an unopened and unopened container. Where possible, to constitute a sample of not less than 200 grams one or more packages of the same consignment or lot shall be taken.

If this is not possible, use another method to obtain a representative sample.

3.2.3 Conservation, storage, and transport of samples.

See sections 5 and 6 of the general provisions.

III. PROBES FOR THE SAMPLING OF CASEINS AND CASEINATES

1. Types of probes

Type A: Long (see figure).

Type B: Short (see figure).

2. Materials

The blade and the shaft must be polished metal, preferably made of stainless steel.

The long-type handle should preferably be made of stainless steel.

The short-type probe will hold a removable wooden or plastic handle, fixed to the blade with a bayonet junction.

3. Construction

3.1 The shape, material and finish must be such that they can easily be cleaned.

3.2 The outstanding edge of the type A sheet must be sharp enough so that it can be scratched with it.

3.3 The tip of the sheet must be sharp enough to facilitate the sampling.

4. Main dimensions

The probes must present the dimensions given in the bottom frame (with a tolerance of 10 per 100).

	Type A Long (in mm)	Type B Short (in mm)
Length	800	400
thickness of the metal leaf	From 1 to 2	From 1 to 2
sheet diameter at tip	18	32
sheet diameter on the handle or axis	22	28
Width slot in the tip	4	20
Width of the slot in the handle or axis	14	14

5. Warning about the use of probes

5.1 With more or less loose dust, the probes may be introduced vertically. The type A probes will be fully filled with spin, and then vertically removed. Type B probes shall be fully filled as they are being introduced, but must be removed in an oblique position in order to avoid losses at the lower end.

5.2 In the case of loose powders, the containers must be tilted, the probes being inserted in almost horizontal position, with the groove down, to be removed after the groove upwards.

ATTACHED 4

Methods of analysis of the composition of food caseins and caseinates

GENERAL PROVISIONS

1. Preparing the analysis sample

1.1 General observation: The mass of the sample presented to the laboratory for analysis must be at least 200 grams.

1.2 Sample preparation for laboratory analysis.

1.2.1 Homogenise carefully the laboratory sample, crush the possible lumps, shake and rotate the container frequently (if necessary, after transferring the entire sample to an air-tight container). of the sample volume double capacity to be able to perform this operation.)

1.2.2 Verter in the sieve 3.3 a most representative part of the carefully homogenized sample (about 50 grams).

1.2.3 If the entire 50 grams completely or almost completely crosses the sieve (at least 95 per 100 by weight), use for the determination of the prepared sample according to 1.2.1.

1.2.4 If not, grind the 50 grams using the grinding device (3.4) until they meet the sifting criterion (1.2.3). Immediately pass the entire sample to an air-tight container of double capacity of the sample volume, and homogenise carefully stirring and rotating continuously. During these operations, take precautions to prevent any modification of the water content of the product.

1.2.5 After preparing the sample for the test, proceed as quickly as possible to the determination.

1.3 Startups: The sample should always be kept in an air-tight container and moisture.

2. Reagents

2.1 Water.

2.1.1 Water used for the preparation of solution, dilution or washing solution shall be distilled water or demineralised water of purity at least equivalent.

2.1.2 Each time a "solution" or "dilution" is referred to without another indication, it will be an "aqueous solution" or a "water dilution".

2.2 Chemicals: Except where otherwise indicated, all chemical substances must be of recognised analytical quality.

3. Material

3.1 Material List: Material lists will only comprise items that have a particular job and that respond to particular characteristics.

3.2 Analytical balance: An analytical balance shall mean a balance with a heavy precision of at least 0,1 milligrams.

3.3 Tamiz: The sieve must have a diameter of 200 millimeters and be provided with a lid and a collector container. The metal fabric of the sieve must have a nominal opening of 500 µ m. The opening tolerances and the diameter of the metal wire shall correspond to the values set out in ISO/3310/1 (Tamiz for testing-technical standards and verification-Part One: Metal Tela ISO/3310/1 -1975, or the last edition of this rule).

3.4 Molder device: Allows, if necessary, to grind the laboratory sample without causing excessive heat and without modifying the humidity (1.2.4). A hammer mill must not be used.

4. Expression of the results

4.1 Results: If the reproducibility conditions applicable to a method are met, the arithmetic mean of two determinations will be taken as a result.

4.2 Percentage Calculation: Except where otherwise indicated, the results must be calculated as the percentage by mass of the sample.

5. Test minutes

The test report shall specify the analytical method used and the results obtained. It shall also include all the details of the procedure not provided for in the analytical or optional method, as well as all the circumstances which have been able to influence the results obtained. The test report shall give all the information necessary for the complete identification of the sample.

METHOD 1

Determining moisture content

1. Object and scope of application

This method allows you to determine the moisture content of:

Acidic caseins.

The caseinates.

The caseinates.

2. Definition

By moisture content of caseins and caseinates the loss of mass is entered by applying the method described below.

3. Principle

Drying at atmospheric pressure, in a stove at 102nd C ± 1º C, of a test sample until a constant mass is obtained, the mass loss is calculated as a percentage of the sample mass.

4. Team

4.1 Analytical Balance.

4.2 Capsules: Flat background and unalterable material under test conditions (e.g. nickel, aluminium, stainless steel or glass). They must be fitted with lids which fit perfectly but which can be removed quickly. Suitable dimensions: Dieter of 60 to 80 millimeters and depth of about 20 millimeters.

4.3 Atmospheric pressure: Well ventilated and equipped with a thermoregulation device (temperature: 102nd C ± 1º C). The temperature must be uniform throughout the inside of the stove.

4.4 Decker: It should contain recently activated silica gel, provided with a hydrometric indicator, or an equivalent desiccation device.

4.5 Instrument for handling capsules: For example, laboratory tweezers.

5. Procedure

5.1 Preparation of the sample for the test: See paragraph 1.2 of the general provisions.

5.2 Preparation of the capsules.

5.2.1 Place the uncovered capsule and its lid (4.2) on the stove (4.3), regulated at 102nd C ± 1º C, for at least one hour.

5.2.2 Place the cap on the capsule, insert the cap so plugged into the desiccator (4.4), allow to cool to room temperature and weigh with precision of 0.1 milligrams (m₀).

5.3 Test Sample: Introduce 3 to 5 grams of the sample for test (5.1) in the capsule, cap it, and weigh it with precision of 0.1 milligrams (m₁).

5.4 Determination.

5.4.1 Highlight the capsule and place it along with the lid on the stove, regulated at 102nd C ± 1º C; leave it there for four hours.

5.4.2 Place the cap on the capsule, insert it into the desiccator, allow to cool to room temperature and weigh to the nearest 0.1 milligrams.

5.4.3 Highlight the capsule and place it along with the lid on the stove for an hour. Repeat the operation described in 5.4.2 below.

5.4.4 If the mass obtained according to 5.4.3 is less than one milligram to that obtained according to 5.4.2, repeat the operation described in 5.4.3.

If you get an increase in the mass, use for the calculation the lowest number recorded (6.1).

The total length of drying does not usually run for six hours.

We designate as m₂ the final mass recorded, in grams.

6. Expression of the results

6.1 Method of calculation: The mass loss of the test sample, expressed as a percentage of mass, is given by the following formula:

		μ1 -μ2	× 100
	1 -μ0

where:

m₀ = Mass in grams of the capsule and its cap after operation 5.2.

m₁ = Mass in grams of the capsule, its cap, and the test sample before drying (5.3).

m₂ = Mass in grams of the capsule, its cap, and the test sample after drying (5.4.3 or 5.4.4).

Express the final result with precision of 0.01 per 110.

6.2 Reproducibility: The difference between the results of two determinations made simultaneously with a brief interval on the same sample, under the same conditions and by the same analyst, should not exceed 0.1 grams of moisture per 100 grams of product.

The probability of not exceeding this value is 95 per 100 of the cases.

METHOD 2

Determining protein content

1. Object and scope of application

This method allows you to determine the protein content of:

Acidic caseins, caseinates and caseinates.

With the exception of caseinates containing ammonium and other ammonium or non-protein nitrogen compounds.

2. Definition

Protein content: nitrogen content determined by the method described here, multiplied by 6,38 and expressed as a percentage by mass.

3. Principle

A test sample is attacked with a mixture of potassium sulphate and sulphuric acid in the presence of copper sulphate (II) as a catalyst, in order to transform the organic nitrogen into ammoniacal nitrogen. Ammonia is distilled and absorbed in a boric acid solution.

It is valued by a standard hydrochloric acid solution. The protein content is obtained by multiplying the nitrogen content by 6,38.

4. Reagents

4.1 Concentrated sulphuric acid D₂₀, 1.84 g/ml.

4.2 anhydrous potassium sulphate (K₂SO₄).

4.3 Copper (II) sulphate pentahydrate (CuSO₄-5H₂O).

4.4 Sucrose (C₁₂H₂₂Or₁₁).

4.5 Boric acid, 40 g/l solution.

4.6 Sodium Hydroxide, concentrated solution at 30 per 100 by mass, free of carbonate.

4.7 Hydrochloric acid: Standard solution at 0.1 mol/l.

4.8 Mixed indicator: Mix to equal volumes a 2 g/l methyl red solution in ethanol, at least 95 per 100 (in volume), and a 1 g/l methylene blue solution in ethanol, at least 95 per 100 (in volume).

5. Team

5.1 Analytical Balance.

5.2 Kjeldahl Mataz, 500 millilitres.

5.3 Protein decomposition apparatus. It should allow the Kjeldahl flask (5.2) to be maintained and provided with a heating system that prevents heating of the part of the flask above the level of the liquid.

5.4 Rectilinear Inner Tube Condenser.

5.5 Output Tube. With a safety ampoule attached to the lower end of the condenser (5.4) by a connection in frosted glass or a rubber tube. In the latter case, the glass ends must be close to each other.

5.6 Deflegmator. Attached to the Kjeldahl flask (5.2) and to the condenser (5.4) by means of well-adjusted rubber plugs.

5.7 Matraz Erlenmeyer, 500 millilitres.

5.8 Graduates, 50 millilitres, and 100 millilitres.

5.9 50 milliliter Bureta, 0.1 milliliter graduations.

5.10 Boiling Regulators.

5.10.1 For protein decomposition: Small porcelain or glass balls.

5.10.2 For distillation: Small granules of pumice stone.

6. Procedure

6.1 Preparing the sample for testing. See point 1.2 of the general provisions.

6.2 Demonstration of ammoniacal nitrogen. If the presence of ammonium caseinate or other ammoniacal compounds is assumed, the following test shall be carried out: In a small flask Erlenmeyer, add to 1 gram of sample 10 millilitres of water and 100 milligrams of magnesium oxide. Rinse the oxide adhered to the glass wall, cover the flask with a cork stopper, tucking between the cap and the neck of the flask a strip of wetted paper. Carefully mix the contents of the flask and heat it in a bath at about 60 ° C. If the paper turns blue in the next fifteen minutes, this reveals the presence of ammonia; in this case, the method is not applicable (see point 1).

6.3 Test blank. Simultaneously with the determination of the nitrogen content of the test, perform a blank test by replacing the test sample with 0,5 grams of sucrose (4.4) and using the same equipment, the same reagent quantities and the same the procedure described in point 6.5. If the measurement exceeds 0,5 millilitres of the 0,1 mol/l acid solution in the blank test, the reagents must be checked and the reagent or the impure reagents replaced or replaced.

6.4 Test Sample. Enter the Kjeldahl flask (5.2) from 0.3 to 0.4 grams of the sample (6.1), heavy with precision of 0.1 milligrams.

6.5 Determination.

6.5.1 Introduce some pieces of porcelain or some glass balls (5.10.1) into the flask and approximately 10 grams of anhydrous potassium sulphate (4.2).

Add 0.2 grams of copper sulphate (II) (4.3) and rinse the neck of the flask with some water. Add 20 millilitres of concentrated sulphuric acid (4.1) and mix the contents of the flask.

Heat gently on the decomposition apparatus (5.3) until the foam disappears. Gently swirl until the solution is clear and the pale green colour persists. Shake the flask of time in time during heating.

Continue the boil by regulating the heating, so that the vapors are condensed in the center of the neck of the flask. Continue heating for ninety minutes, avoiding all over local heating.

Let cool at room temperature. Add with caution about 200 millilitres of water and some grains of pumice stone (5.10.2). Mix and let cool again.

6.5.2 Introduce in the flask Erlenmeyer (5.7) 50 millilitres of the boric acid solution (4.5) and four drops of the indicator (4.8). Mix. Place the Erlenmeyer flask under the condenser (5.4) so that the end of the outlet tube (5.5) is submerged in the boric acid solution. Using a graduated test tube (5.8) to enter the Kjeldahl flask 80 millilitres of the sodium hydroxide solution (4.6). During this operation the inclined flask must be maintained so that the sodium hydroxide solution flows along the wall and forms a layer at the bottom of the flask.

Re-attach the Kjeldahl flask to the capacitor immediately via the deflegator (5.6).

Mix the contents of the Kjeldahl flask by gently rotating it, gently make it clear at first, avoiding any foam formation. Continue the distillation so that 150 millilitres of distillate are obtained in approximately thirty minutes.

The distillate must have a temperature below 25 ° C.

About two minutes after the end of the distillation, lower the Erlenmeyer flask so that the end of the outlet tube is not already submerged in the acidic solution, and rinse the end with a little water. Stop the heating, lift the outlet tube and rinse your inner and outer walls with some water, collecting the rinsing water in the Erlenmeyer flask.

6.5.3 Rate the distillate from the Erlenmeyer flask by the standard hydrochloric acid solution (4.7).

7. Expression of the results

7.1 Calculation mode and formula. The protein content of the sample, expressed as a percentage by mass, is equal to:

(V1 -V2) × T × 14 × 100 × 6,38	=	8.932 (V1 -V2) × T
m × 1,000		m

where:

V₁ = Volume in millilitres of the standard hydrochloric acid solution (4.7) used for determination (6.5).

V₂ = Volume in millilitres of the standard hydrochloric acid solution (4.7) used for the blank test.

T = Concentration of the standard solution of hydrochloric acid (4.7) in mol/l.

m = Mass, in gram of the test sample.

Express the protein content with accuracy of 0.1 per 100.

7.2 Reproducibility. The difference between the results of two determinations carried out in a short interval, under the same conditions and by the same analyst, should not exceed 0,5 grams of protein per 100 grams of product.

This value has a probability of not exceeding 95 per 100 of cases, if the method is performed correctly.

METHOD 3

Determining the Valuable acidity

1. Object and scope of application

The present method allows determining the appable acidity of the acidic caseins.

2. Definition

Valuable acidity of acid caseins: Volume, in millilitres of 0.1 mol/l sodium hydroxide solution, required to neutralise an aqueous extract of a gram of product.

3. Principle

Preparation and filtration of an aqueous extract of the sample at 60º C. Valuation of the filtrate by a standard solution of sodium hydroxide, in the presence of phenolphthalein as an indicator.

4. Reagents

The water used for the application of the method or the preparation of the reagents must be free of carbon dioxide (for that purpose, heating it ten minutes before use).

4.1 Sodium Hydroxide, solution at 0.1 mol/l.

4.2 Phenolphthalein used as an indicator, one gram solution in 100 millilitres of ethanol (95 per 100 in volume), neutralized in relation to an indicator.

5. Team

5.1 Analytical Balance.

5.2 Matraz Erlenmeyer, 500 millilitres, with frosted neck and stopper.

5.3 graduated pipette to 100 millilitres.

5.4 Pipette, suitable for measuring 0.5 millilitres of the indicator solution (4.2).

5.5 Matraz Erlenmeyer, 250 millilitres.

5.6 graduated test, 250 millilitres.

5.7 Bureta with 0.1 milliliter graduations.

5.8 Bath water, adjustable to a temperature of 60 ± 2º C.

5.9 Appropriate filter.

6. Procedure

6.1 For sample preparation for testing, see point 1.2 of the general provisions.

6.2 Test sample: Pesar about ten grams of the sample with precision of 10 milligrams and introduce them into the Erlenmeyer flask (5.2).

6.3 Determination: Using the 250 milliliter test (5.6), add 200 millilitres of recently ebullide and cooled water, previously heated to 60 ° C. Close the flask, mix it with agitation and place it in the bathroom. 60º C (5.8) for thirty minutes. Shake the flask every ten minutes, approximately.

Filter and allow to cool the filtrate to about 20º C. Filtering should be limpid.

Take with pipette (5.3) 100 millilitres of the cooled filter and introduce them into the flask Erlenmeyer (5.5). Add 0.5 millilitres of the phenolphthalein indicator solution (4.2) by pipette (5.4). Assess using the standard sodium hydroxide solution (4.1) until a persistent pale pink colour appears for at least thirty seconds. Note the volume used with precision of 0.01 millilitres.

7. Expression of the results

7.1 The value of the casein value is given by the formula:

		20 × V × T
	m

where

V = Volume in millilitres of the standard sodium hydroxide solution (4.1) used.

T = Concentration, in mol/l, of the standard sodium hydroxide solution (4.1).

m = Mass, in grams, of the test sample.

Express the appable acidity to two decimal places.

7.2 Reproducibility: The difference between the results of two determinations made simultaneously or with a short interval, on the same sample, under the same conditions and by the same analyst, should not exceed 0.02 millilitres of sodium hydroxide solution for a gram of product.

This value has a probability of not being exceeded 95 per 100 of the cases.

METHOD 4

Determination of ashes (P₂ OR₅ included)

1. Object and scope of application

This method allows you to determine the ashes of: Acted caseins (P₂ OR₅ included).

2. Definition

Ashes (P₂OR₅ included): Substances determined according to the method described below, expressed as a percentage by mass.

3. Principle

Incineration of a test sample at 825 ° C ± 25 ° C in the presence of magnesium acetate, intended to fix the entire phosphorus of organic origin. The residue is weighed and the mass of ash from magnesium acetate is subtracted.

4. Reagents

4.1 Tetrahydrate Magnesium Acetate

Mg (CH₃CO₂)₂, 4H₂O, 120 g/l solution

5. Team

5.1 Analytical Balance.

5.2 A graduated 5 milliliter pipette.

5.3 Silicon or platinum capsule, about 70 millimeters in diameter and 25 to 50 millimeters in depth.

5.4 Adjustable drying of 102nd C ± 1º C.

5.5 Air circulation electric heat, adjustable to 825º C ± 25º C.

5.6 Bano of boiling water.

5.7 Recently activated silica gel decker, provided with a hydrometric indicator, or an equivalent dehydrator.

6. Procedure

6.1 Preparation of the sample for testing: See point 1.2 of the general provisions.

6.2 Preparation of the capsules: Place two capsules (5.3) A and B in the electric oven (5.5), regulated at 825º C ± 25º C, for thirty minutes. Allow them to cool a little before placing them in a desiccator (5.7) until they cool to room temperature, and weigh them with a precision of 0.1 milligram.

6.3 Test sample: Pesar with precision of 0.1 milligram about three grams of sample (6.1), directly on one of the prepared capsules (A).

6.4 Determination: Introducing in capsule A, by pipette (5.2), five millilitres of the magnesium acetate solution (4.1), so that the entire test sample is wetted, and left to rest for twenty years. minutes.

In the other prepared capsule (B), enter with the pipette (5.2) 5 millilitres of the magnesium acetate solution (4.1).

Evaporate the contents of both capsules A and B into the dry water bath (5.6).

Place the two capsules on the stove (5.4), regulated at 102nd C ± 1º C, for thirty minutes.

Place the capsule A, with its contents, on a small flame, a hot plate or under an infrared lamp, until the sample is completely charred and monitoring that it does not burn.

Place the two capsules A and B in an electric oven (5.5) regulated at 825º C ± 25º C, and leave them there for at least one hour, until the carbonaceous particles of the A capsule completely disappear, allow to cool a little both capsules and place them in the desiccator (5.7) until they reach room temperature, then weighing them with a precision of 0.1 milligrams.

Repeat the heating operations for about thirty minutes in the electric, cooling and heavy oven to obtain a constant mass (with precision of one milligram), scoring the minimum mass.

7. Expression of the results

7.1 Calculation mode and formula: The ashes (P₂O₅ included) of the sample, expressed as a percentage by mass, are given by the formula:

	(m1 -m2)-(m3 -m4	× 100
	m0

where

m₀ = Mass, in grams, of the test sample.

m₁= Mass, in grams, of capsule A with its contents.

m₂ = Mass, in grams, of the empty capsule.

m₃ = Mass, in grams, of capsule B with its contents.

m₄ = Mass, in grams, of the empty capsule B.

Express the final result with precision of 0.01 per 100.

7.2 Reproducibility: the difference between the results of two determinations made simultaneously or with a short interval on the same test, under the same conditions and by the same analyst, should not exceed 0,1 grams per 100 grams of product.

This value has a probability of not being exceeded 95 per 100 of the cases.

METHOD 5

Determination of ashes (P₂OR₅ included)

1. Object and scope of application

The present method allows to determine the ash content of pure caseins.

2. Definition

Ashes (P₂OR₅ included): Substances determined according to the method described below and expressed as a percentage by mass.

3. Principle

Incineration of a test sample at 825 ° C ± 25 ° C until a constant mass is obtained. The obtained residue is weighed.

4. Team

4.1 Analytical Balance.

4.2 Silicon or platinum capsule, approximately 70 mm in diameter and 25 to 50 mm in depth.

4.3 Electrical Horno. Air circulation furnace, adjustable to 825 ° C ± 25 ° C.

4.4 Decker. With recently activated silica gel, provided with a hydrometric indicator, or any other dehydrating equivalent.

5. Procedure

5.1 Preparing the sample for testing. See point 1.2 of the "General provisions".

5.2 Capsule preparation. Place the capsule (4.2) in the electric oven (4.3), regulated at 825º C ± 25º C, for thirty minutes. Allow to cool the capsule in the desiccator (4.4) to room temperature. Weigh precisely 0.1 mg.

5.3 Test Sample. Weigh directly on the prepared capsule, with a precision of 0.1 mg, about 3 g of the sample (5.1).

5.4 Detemination. Heat the capsule, with its contents, on a small flame, a hot plate or under an infrared lamp, until the sample is completely charred and monitoring that it does not burn.

Place the capsule in an electric oven (4.3) regulated at 825º C ± 25º C and leave it there for at least one hour, until the carbonaceous particles of the capsule completely disappear. Allow the capsule to cool a little and place it in the desiccator (4.4) until it reaches the ambient temperature, then weighing it with a precision of 0.1 mg.

Repeat the heating operations for about thirty minutes in the electric, cooling and heavy furnace until a constant mass (with precision of 1 mg) is obtained.

6. Expression of the results

6.1 Method and calculation formula. The ashes (P₂O₅ included) of the sample, expressed as a percentage by mass, are given by the formula:

		m1 -m2	× 100
	m0

where

m₀ = Mass, in grams, of the test sample.

m₁ = Mass, in grams, of the capsule with its contents.

m₂ = Mass, in grams, of the empty capsule.

Express the final result with precision of 0.01 per 100.

6.2 Reproducibility. The difference between the results of two determinations made simultaneously or with a short interval on the same test, under the same conditions and by the same analyst, must not exceed 0,15 g of ashes per 100 g of product.

This value has a probability of not being exceeded 95 per 100 of the cases.

METHOD 6

Determining the pH

1. Object and scope of application

This method allows you to determine the pH of the caseinates.

2. Definition

pH of caseinates: The pH at 20 ° C of a caseinate solution, determined according to the method described below.

3. Principle

Electrometric determination of the pH of a caseinate solution by a pHmeter.

4. Reagents

Water used for the preparation of reagents or for the realization of the method (6) must be water recently distilled and protected against the absorption of carbon dioxide.

4.1 buffer solutions for Phmeter calibration. Two buffer solutions of a pH given at 20 ° C with precision of two decimal places and the range of which covers the pH of the sample; for example, a buffer solution of phthalate, of pH close to 4, and a buffer solution of borax, of pH close to 9.

5. Team

5.1 Balance, sensitivity of 0.1 g.

5.2 pHmetro. Minimum sensitivity: 0,5 pH, provided with an appropriate glass electrode and a calomel electrode or other reference electrode.

5.3 Thermometer. Precision: 0.5º C.

5.4 Matraz Erlenmeyer. 100 ml capacity, provided with a frosted glass stopper.

5.5 Glass glass of 50 ml.

5.6 Agitator.

5.7 Vaso for agitator (5.6), minimum capacity 250 ml.

6. Procedure

6.1 Preparing the sample for testing. See point 1.2 of the "general provisions".

6.2 Determination.

6.2.1 PHmeter Calibration. Set the temperature of the buffer solutions (4.1) by 20º C and regulate the pHmeter according to the manufacturer's instructions.

Remarks:

6.2.1.1 Calibration must be done by introducing the electrode for twenty minutes into the Erlenmeyer flasks at rest (6.2.2).

6.2.1.2 If the analysis of a series of samples is carried out, check the calibration of the pH at least every thirty minutes, with one or more standard buffer solutions.

6.2.2 Preparing the test solution. Enter the glass glass (5.6) 95 ml of water, add 5.0 g of the test sample (6.1) and mix by the agitator (5.5) for thirty seconds.

Let stand for twenty minutes at about 20º C, with the glass covered with a watch glass.

6.2.3 Measure of pH.

6.2.3.1 Verter about 20 ml of the solution in the glass (5.5) and immediately determine the pH of this liquid with the pHmeter (5.2), after carefully rinsing the electrodes with water.

6.2.3.2 Measure the pH.

7. Expression of the results

7.1 Reading of pH. Note the value read on the pHmeter scale corresponding to the pH of the caseinate solution, with at least two decimal places.

7.2 Repeability. The difference between the results of two determinations made simultaneously or with a short interval on the same test, under the same conditions and by the same analyst, should not exceed 0,05 units of pH.

This value has a probability of not being exceeded 95 per 100 of the cases.