GOST food additives specifications. Specifications and guests as control over the use of food additives

FEDERAL AGENCY
FOR TECHNICAL REGULATION AND METROLOGY

Foreword

The goals and principles of standardization in the Russian Federation are established by the Federal Law of December 27, 2002 No. 184-FZ "On Technical Regulation", and the rules for the application of national standards of the Russian Federation - GOST R 1.0-2004 "Standardization in the Russian Federation. Basic Provisions»

Information about changes to present standard published in annually published informational index "National standards", a text changes and amendments - per month published information signs "National standards". AT case revision (substitutions) or cancellation present standard corresponding notification will published in monthly published informational index "National standards". Relevant information, notification and texts are placed also in informational system general use - on the official website Federal agencies on technical regulation and metrology in networks Internet

GOST R 52823-2007

NATIONAL STANDARD OF THE RUSSIAN FEDERATION

Introduction date - 2009-01-01

1 area of ​​use

This standard applies to the E339 sodium phosphate food additive, which is 1-substituted (i), 2-substituted (ii) and 3-substituted (iii) sodium salts of orthophosphoric acid (hereinafter referred to as food sodium monophosphates) and intended for use in the food industry .

Requirements to ensure the safety of food sodium monophosphates are set out in 4.1.5, quality requirements - in 4.1.3, 4.1.4, labeling requirements - in 4.4.

2 Normative references

This standard uses normative references to the following standards:

GOST R ISO 2859-1-2007 Statistical methods. Procedures for selective control on an alternative basis. Part 1: Sampling plans for successive lots based on acceptable quality levels

GOST R 51652-2000 Rectified ethyl alcohol from food raw materials. Specifications

GOST R 51766-2001 Food raw materials and products. Atomic absorption method for the determination of arsenic

GOST R 52824-2007 Food additives. Sodium and potassium triphosphates E451. Specifications

GOST 8.579-2002 State system for ensuring the uniformity of measurements. Requirements for the quantity of packaged goods in packages of any kind during their production, packaging, sale and import

GOST 12.1.005-88 System of labor safety standards. General sanitary and hygienic requirements for the air of the working area

GOST 12.1.007-76 Occupational safety standards system. Harmful substances. Classification and general safety requirements

GOST 61-75 Reagents. Acetic acid. Specifications

GOST 3118-77 Reagents. Hydrochloric acid. Specifications

GOST 3760-79 Reagents. Ammonia water. Specifications

GOST 3765-78 Reagents. Ammonium molybdate. Specifications

GOST 4198-75 Reagents. Potassium phosphate monosubstituted. Specifications

GOST 4201-79 Reagents. Sodium carbonate acid. Specifications

GOST 4204-77 Reagents. Sulfuric acid. Specifications

GOST 4233-77 Reagents. Sodium chloride. Specifications

GOST 4328-77 Reagents. sodium hydroxide. Specifications

GOST 4461-77 Reagents. Nitric acid. Specifications

GOST 4517-87 Reagents. Methods for the preparation of auxiliary reagents and solutions used in the analysis

GOST 4919.1-77 Reagents and highly pure substances. Methods for preparing indicator solutions

GOST 5100-85 Technical soda ash. Specifications

GOST 5789-78 Reagents. Toluene. Specifications

GOST 6016-77 Reagents. Isobutyl alcohol. Specifications

GOST 6259-75 Reagents. Glycerol. Specifications

GOST 6709-72 Distilled water. Specifications

GOST 6825-91 (IEC 81-84) Fluorescent tubular lamps for general lighting

GOST 8515-75 Diammonium phosphate. Specifications

GOST 9147-80 Laboratory porcelain glassware and equipment. Specifications

GOST 10354-82 Polyethylene film. Specifications

GOST 10485-75 Reagents. Methods for determining the content of arsenic impurities

GOST 10678-76 Orthophosphoric thermal acid. Specifications

GOST 11078-78 Purified caustic soda. Specifications

GOST 14192-96 Marking of goods

GOST 14919-83 Household electric stoves, electric stoves and ovens. General specifications

GOST 14961-91 Linen and linen threads with chemical fibers. Specifications

GOST 15846-2002 Products shipped to the Far North and equivalent areas. Packaging, marking, transportation and storage

GOST 17308-88 Twines. Specifications

GOST 18389-73 Wire from platinum and its alloys. Specifications

GOST 19360-74 Film liners. General specifications

GOST 24104-2001 Laboratory balance. General technical requirements

GOST 25336-82 Laboratory glassware and equipment. Types, basic parameters and dimensions

GOST 25794.1-83 Reagents. Methods for preparing titrated solutions for acid-base titration

GOST 26930-86 Food raw materials and products. Arsenic determination method

GOST 26932-86 Food raw materials and products. Lead determination method

GOST 27752-88 Electronic-mechanical quartz desktop, wall and alarm clocks. General specifications

GOST 28498-90 Liquid glass thermometers. General technical requirements. Test Methods

GOST 29169-91 (ISO 648-77) Laboratory glassware. Pipettes with one mark

GOST 29227-91 (ISO 835-1-81) Laboratory glassware. Pipettes graduated. Part 1. General requirements

GOST 29251-91 (ISO 385-1-84) Laboratory glassware. Burettes. Part 1. General requirements

GOST 30090-93 Bags and bag fabrics. General specifications

Note - When using this standard, it is advisable to check the validity of reference standards in the public information system - on the official website of the Federal Agency for Technical Regulation and Metrology on the Internet or according to the annually published information index "National Standards", which was published as of January 1 of the current year , and according to the corresponding monthly published information signs published in the current year. If the reference standard is replaced (modified), then when using this standard, you should be guided by the replacing (modified) standard. If the referenced standard is canceled without replacement, the provision in which the reference to it is given applies to the extent that this reference is not affected.

3 Classification

Food sodium monophosphates (E339) are divided into sodium orthophosphates:

E339(i), 1-substituted sodium orthophosphate;

E339(ii), 2-substituted sodium orthophosphate;

E339(iii), 3-substituted sodium orthophosphate.

Designations, names, chemical names, formulas and molecular weights of food sodium monophosphates are given in table 1.

Table 1 - Designations, names, chemical names, formulas and molecular weights of food sodium monophosphates

4 General technical requirements

4.1 Characteristics

4.1.1 Food sodium monophosphates are produced in accordance with the requirements of this standard, according to technological regulations or instructions approved in the prescribed manner.

4.1.2 Edible sodium monophosphates are hygroscopic or slightly hygroscopic, highly soluble in water and insoluble in ethanol.

4.1.3 In terms of organoleptic indicators, food sodium monophosphates must comply with the requirements specified in Table 2.

Table 2 - Organoleptic indicators

4.1.4 In terms of physicochemical parameters, food sodium monophosphates must comply with the requirements specified in Table 3.

Table 3 - Physical and chemical parameters

4.1.5 In terms of safety indicators, food sodium monophosphates must meet the requirements specified in table 4.

Table 4 - Safety indicators

4.2 Requirements for raw materials

4.2.1 For the production of food sodium monophosphates, the following raw materials are used:

Orthophosphoric acid grade A according to GOST 10678;

Caustic soda brand A according to GOST 11078;

Sodium carbonate according to GOST 83;

Sodium carbonate acid according to GOST 4201;

Soda ash brand B according to GOST 5100.

4.2.2 Raw materials must ensure the quality and safety of dietary sodium monophosphates.

4.3 Packaging

4.3.1 Food monophosphates of sodium are packed in paper three-layer bags of the PM brand according to GOST 2226 or in bag-liners according to GOST 19360 from food grade H polyethylene unstabilized film, at least 0.08 mm thick according to GOST 10354, placed in grocery bags according to GOST 30090 or in paper open three-layer bags of the NM brand according to GOST 2226.

4.3.2 Polyethylene bags-liners, after filling them, are welded or tied with twine from bast fibers according to GOST 17308 or double-strand polished twine according to the document in accordance with which it is made.

4.3.3 The top seams of fabric and paper bags must be machine-sewn with linen thread according to GOST 14961.

4.3.4 It is allowed to use other types of containers and packaging materials made from materials whose use in contact with food sodium monophosphates ensures their quality and safety.

4.3.5 The net weight of the packaging unit must be no more than 25 kg.

4.3.6 The negative deviation of the net weight from the nominal weight of each packaging unit must comply with the requirements of GOST 8.579 (Table A.2).

4.3.7 Food sodium monophosphates shipped to the regions of the Far North and equivalent areas are packaged in accordance with GOST 15846.

4.4 Marking

4.4.1 Each packaging unit with edible sodium monophosphates is marked in any way that ensures its clear identification, indicating:

Name of food additive and its index * ;

Mass fraction of the main substance;

Name and location (legal address) of the manufacturer;

Trademark of the manufacturer (if any);

Net weights;

Gross weights;

Batch numbers;

Manufacturing dates;

Terms and conditions of storage according to 8.3 and 8.2;

Symbols of this standard.

* Index according to the European Codification System for Food Additives.

4.4.2 The transport marking must comply with the requirements of GOST 14192 with the application of handling marks "Keep away from moisture" and "Do not take with hooks."

5 Safety requirements

5.1 Food sodium monophosphates are non-toxic, fire- and explosion-proof.

5.2 According to the degree of impact on the human body, food sodium phosphates in accordance with GOST 12.1.007 belong to the third hazard class.

5.3 Work with food sodium monophosphates must be carried out in special clothing, using personal protective equipment, while observing the rules of personal hygiene.

5.4 Production facilities in which work is carried out with food sodium monophosphates must be equipped with supply and exhaust ventilation.

5.5 Air control of the working area is carried out by the manufacturer in accordance with GOST 12.1.005.

6 Acceptance rules

6.1 Dietary sodium monophosphates are taken in batches.

A batch is considered to be the amount of food sodium monophosphates obtained in one technological cycle, one date of manufacture, in the same package, simultaneously presented for testing and acceptance, issued with one document certifying their quality and safety.

6.2 A document certifying the quality and safety of food sodium monophosphates must contain the following information:

Mass fraction of the main substance;

Name and location (legal address) of the manufacturer;

Batch number;

date of manufacture;

Net weight;

Shelf life;

Organoleptic and physico-chemical quality indicators according to this standard and actual;

The indicators that ensure safety, according to this standard and the actual ones, determined in accordance with 6.9;

6.3 To check the compliance of food sodium monophosphates with the requirements of this standard, acceptance tests are carried out for the quality of packaging, correct labeling, net weight, organoleptic and physico-chemical indicators and periodic tests for indicators that ensure safety.

6.4 When conducting acceptance tests, a single-stage sampling plan is used with normal control and a special control level S-4 with an acceptable quality level AQL equal to 6.5, according to GOST R ISO 2859-1.

The sampling of packaging units is carried out by random selection in accordance with table 5.

Table 5

6.5 The quality control of packaging and the correctness of labeling is carried out by an external inspection of all packaging units in the sample.

6.6 The control of the net weight of food sodium monophosphates in each packaging unit included in the sample is carried out by the difference between the gross mass and the mass of the packaging unit, freed from the contents. The limit of permissible negative deviations from the nominal net weight of edible sodium monophosphates in each packaging unit - according to 4.3.3.

6.7 Acceptance of a batch of food sodium monophosphates by net weight, quality of packaging and correct labeling of packaging units

6.7.1 The batch is accepted if the number of packaging units in the sample that do not meet the requirements for packaging quality and correct labeling, net weight of edible sodium monophosphates is less than or equal to the acceptance number (see Table 5).

6.7.2 If the number of packaging units in the sample that do not meet the requirements for packaging quality and correct labeling, net weight of edible sodium monophosphates is greater than or equal to the rejection number (see Table 5), control is carried out on a double sample size from the same lot. The lot is accepted if the conditions of 6.7.1 are met.

A batch is rejected if the number of packaging units in a double sample size that do not meet the requirements for packaging quality and correct labeling and net weight of edible sodium monophosphates is greater than or equal to the rejection number.

6.8 Acceptance of a batch of food sodium monophosphates according to organoleptic and physico-chemical parameters

6.8.1 To control the organoleptic and physico-chemical parameters of the product, from each packaging unit included in the sample in accordance with the requirements of Table 5, instantaneous sampling is carried out and a total sample is compiled according to 7.1.

6.8.2 If unsatisfactory results are obtained in terms of organoleptic and physico-chemical indicators for at least one of the indicators, repeated tests are carried out for this indicator on a double sample size from the same batch. The retest results are final and apply to the entire batch.

Upon repeated receipt of unsatisfactory test results, the batch is rejected.

6.8.3 The organoleptic and physico-chemical parameters of food sodium monophosphates in damaged packaging are checked separately. The test results apply only to edible monosodium phosphates in this package.

6.9 The procedure and frequency of control of indicators that ensure safety (content of fluorides, arsenic and lead) are established by the manufacturer in the production control program.

7 Control methods

7.1 Sampling

7.1.1 To compile a total sample of dietary sodium monophosphates, instantaneous samples are taken from different places of each packaging unit taken according to 6.4. The mass of the instant sample should not exceed 100 g.

The mass of the instant sample and the number of instant samples from each packaging unit included in the sample must be the same.

Instant samples are taken using samplers or metal tubes made of a material that does not react with food sodium monophosphates, immersing the sampler in food sodium monophosphates at least 3/4 of the depth.

Instant samples are placed in a dry, clean glass or polyethylene container and mixed thoroughly.

The mass of the total sample must be at least 500 g.

7.1.2 To reduce the total sample to 500 g, use the quartering method. To do this, the total sample is poured onto a clean table and leveled with a thin layer in the form of a square. Then it is poured with wooden planks with beveled ribs from two opposite sides to the middle so that a roller is formed. The total sample from the ends of the roller is also poured into the middle of the table, again it is leveled with a layer of 1.0 to 1.5 cm in the form of a square and the bar is divided diagonally into four triangles. Two opposite parts of the sample are discarded, and the remaining two are connected, mixed and again divided into four triangles. The operation is repeated until the mass of the total sample reaches 500 g.

7.1.3 The prepared bulk sample is divided into two parts and each part is placed in a clean, dry, tightly closed glass or polyethylene container.

The container with the first part of the sample is used for testing.

The container with the second part of the sample is sealed, sealed and left for re-testing in case of disagreement in assessing the quality of food sodium monophosphates. This part of the total sample is kept until the end of the storage period.

7.1.4 Sample containers are labeled with the following information:

The name of the food additive and its index;

Mass fraction of the main substance;

Name and location of the manufacturer;

Batch number;

Lot net weight;

The number of packaging units in the lot;

date of manufacture;

date of sampling;

Surnames of the persons who carried out the selection of this sample;

Designation of this standard.

7.2 Determination of organoleptic characteristics

The method is based on the organoleptic determination of the appearance, color and smell of dietary sodium monophosphates.

7.2.1 Measuring instruments, materials, reagents

Laboratory scales according to GOST 24104 with the limits of the permissible absolute error of a single weighing ± 0.1 g.

Glass stick.

The paper is white.

Cup SV-34/12 according to GOST 25336.

7.2.2 Sampling - according to 7.1.

7.2.3 Test conditions

The room for testing should be provided with supply and exhaust ventilation. All tests should be carried out in a fume hood.

7.2.4 Testing

7.2.4.1 The appearance and color of food sodium monophosphates is determined by viewing a sample weighing 50 g, placed on a sheet of white paper or on a glass plate, in diffused daylight or lighting with fluorescent lamps of the LD type according to GOST 6825. The illumination of the desktop surface should be at least 500 lux.

7.2.4.2 To determine the odor, prepare a solution with a mass fraction of 2%. To do this, dissolve a sample weighing 2 g in 98 cm 3 of distilled water in a glass with a capacity of 250 cm 3. A clean, odorless glass is filled with 100 cm 3 of the prepared solution. The glass is closed with a lid and incubated for 1 hour at an air temperature of (20 ± 5) °C.

The smell is determined organoleptically at the level of the edge of the cup immediately after opening the lid.

7.3 Sodium ion test

The method is based on the qualitative determination of sodium ions by the formation of a yellow precipitate with a solution of uranyl acetate zinc or by coloring a colorless flame yellow.

7.3.1 Measuring instruments, materials, reagents

Electric stove according to GOST 14919.

Glass V (N) -1-250 TC (TLC) according to GOST 25336.

Cylinder 1(3)-100 according to GOST 1770.

Glass stick.

Platinum wire according to GOST 18389.

Zinc uranyl acetate, h.

Distilled water according to GOST 6709.

7.3.2 Sampling - according to 7.1.

7.3.3 Test conditions - according to 7.2.3.

7.3.4 Preparing for the test

7.3.4.1 Preparation of a solution of acetic acid in a ratio (1:5)

A solution of acetic acid in a ratio (1:5) is prepared by diluting acetic acid by volume with a mass fraction of 99.5% (one part) with distilled water (five parts).

7.3.4.2 Preparation of zinc uranyl acetate solution, 5% by mass

A portion of zinc uranyl acetate weighing 2.5 g is dissolved by heating in 42.5 cm 3 of distilled water and 5 cm 3 of dilute acetic acid according to 7.3.4.1.

7.3.4.3 Preparation of a hydrochloric acid solution in a ratio (1:5)

A solution of hydrochloric acid in a ratio (1:5) is prepared by diluting hydrochloric acid by volume with a mass fraction of at least 35% (one part) with distilled water (five parts).

7.3.5 Conducting a test

Method 1. A portion of a sample weighing from 1.0 to 1.5 g is dissolved in 100 cm 3 of distilled water. To 5 cm 3 of the solution add with a pipette 1 to 2 cm 3 of dilute acetic acid according to 7.3.4.1, filter if necessary, then add 1 cm 3 of the zinc uranyl acetate solution with a pipette. The formation of a yellow crystalline precipitate confirms the presence of sodium ions in the solution.

Method 2. Crystals of food monophosphates of sodium, moistened with dilute hydrochloric acid according to 7.3.4.3, when introduced on a platinum wire into a colorless flame, should color the flame yellow. The yellow coloration of a colorless flame confirms the presence of sodium ions.

7.4 Phosphate ion tests

The methods are based on the qualitative determination of phosphate ions.

7.4.1 Phosphate ion test (H 2 PO 4 -)

7.4.1.1 Measuring instruments, materials, reagents

Laboratory scales in accordance with GOST 24104 with the limits of the permissible absolute error of a single weighing ± 0.01 g.

Pipettes 2-2-1-5(10) according to GOST 29227.

Glass V (N) -1-250 TC (TLC) according to GOST 25336.

Test tubes P2-21-70 according to GOST 25336.

Cylinder 1(3)-100 according to GOST 1770.

Distilled water according to GOST 6709.

Silver nitrate according to GOST 1277, part

7.4.1.2 Sampling - according to 7.1.

7.4.1.3 Test conditions - according to 7.2.3.

7.4.1.4 Test preparation

A solution of nitric acid with a mass fraction of 10%, a density of 1.055 g / cm 3 is prepared according to GOST 4517.

A solution of silver nitrate with a mass fraction of 4.2% is prepared by dissolving 4.2 g of silver nitrate in 95.8 cm 3 of distilled water, acidified with five drops of nitric acid; stored in a dark glass container.

7.4.1.5 Conducting the test

A sample weighing from 1.0 to 1.5 g is dissolved in 100 cm 3 of distilled water. To 5 cm 3 of the solution, add 1 cm 3 of a solution of silver nitrate with a pipette. From 1.6 to 2.0 cm 3 of dilute nitric acid according to 7.4.1.4 is added to the resulting yellow precipitate until it is completely dissolved, which indicates the presence of H 2 PO 4 - - ions.

7.4.2 Phosphate ion (PO) test

The method is based on the qualitative determination of phosphate ions by the formation of a bright light yellow precipitate with a solution of ammonium molybdate.

7.4.2.1 Measuring instruments, materials, reagents

Laboratory scales in accordance with GOST 24104 with the limits of the permissible absolute error of a single weighing ± 0.01 g.

Electric stove according to GOST 14919.

Pipettes 2-2-1-5(10) according to GOST 29227.

Glass V(N)-1-250 TC (TLC) according to GOST 25336.

Test tubes P2-21-70 according to GOST 25336.

Cylinder 1(3)-100 according to GOST 1770.

Glass stick.

Molybdic acid, h.

Hydrochloric acid according to GOST 3118, part

Distilled water according to GOST 6709.

Nitric acid according to GOST 4461, part

Ammonia water according to GOST 3760, h.

7.4.2.2 Sampling - according to 7.1.

7.4.2.3 Test conditions - according to 7.2.3.

7.4.2.4 Test preparation

A portion of finely powdered molybdic acid (85%) weighing 6.5 g, weighed to the second decimal place, is dissolved in a mixture of 14 cm 3 of distilled water and 14.5 cm 3 of an ammonia solution with a mass fraction of 10%, prepared according to GOST 4517. Solution cooled to room temperature and slowly added with stirring to a mixture of 40 cm 3 distilled water and 32 cm 3 nitric acid. The solution is stored in a dark place. If a precipitate forms during storage, only the solution above the precipitate is used for analysis.

7.4.2.5 Testing

A sample weighing from 1.0 to 1.5 g is dissolved in 100 cm 3 of distilled water. From 1 to 2 cm 3 of concentrated nitric acid, 5 cm 3 of ammonium molybdate are added with a pipette to 5 cm 3 of the solution and heated. The formation of a precipitate of bright light yellow “canary” color confirms the presence of PO 4 3- ions in the solution.

7.4.3 Phosphate ion test (HPO 4 2- , PO 4 3-)

The method is based on the qualitative determination of phosphate ions by the formation of a yellow precipitate with a solution of silver nitrate.

7.4.3.1 Measuring instruments, materials, reagents

Laboratory scales in accordance with GOST 24104 with the limits of the permissible absolute error of a single weighing ± 0.01 g.

Pipettes 2-2-1-5(10) according to GOST 29227.

Test tubes P2-21-70 according to GOST 25336.

Cylinder 1(3)-100 according to GOST 1770.

Acetic acid according to GOST 61, part

Distilled water according to GOST 6709.

Silver nitrate according to GOST 1277, part

7.4.3.2 Sampling - according to 7.1.

7.4.3.3 Test conditions - according to 7.2.3.

7.4.3.4 Test preparation

Preparation of a solution of silver nitrate - according to 7.4.1.4.

A solution of acetic acid in the ratio (1:16) is prepared by diluting acetic acid by volume with a mass fraction of 99.5% (one part) with distilled water (16 parts).

7.4.3.5 Conducting the test

A sample weighing from 1.0 to 1.5 g is dissolved in 100 cm 3 of distilled water. Then 5 cm 3 of the resulting solution is acidified with a solution of dilute acetic acid according to 7.4.4.4 and 1 cm 3 of a solution of silver nitrate is added with a pipette. The formation of a yellow precipitate indicates the presence of HPO 4 2-, PO 4 3- -ions.

7.5 Test for free phosphoric acid and its dibasic sodium salt

The method is based on determining the presence of free phosphoric acid and its disubstituted sodium salt by titration in the presence of methyl orange indicator.

7.5.1 Measuring instruments, accessories and reagents

Laboratory scales in accordance with GOST 24104 with the limits of the permissible absolute error of a single weighing ± 0.01 g.

Cylinder 1(3)-100 according to GOST 1770.

Glass V(N)-1-100 TC(TLC) according to GOST 25336.

Distilled water according to GOST 6709.

7.5.2 Sampling - according to 7.1.

7.5.3 Test conditions - according to 7.2.3.

7.5.4 Preparing for the test

7.5.4.1 with (NaOH) = 1 mol / dm 3 is prepared according to GOST 25794.1.

7.5.4.2 A solution of molar concentration with (H 2 SO 4) = 1 mol / dm 3 is prepared according to GOST 25794.1.

7.5.4.3 An aqueous solution of methyl orange with a mass fraction of 0.1% is prepared according to GOST 4919.1.

7.5.5 Conducting a test

A sample weighing from 1.5 to 2.0 g is placed in a glass with a capacity of 100 cm 3, dissolved in 40 cm 3 of distilled water and titrated with a solution of sodium hydroxide (not more than 0.3 cm 3) or, respectively, with a solution of sulfuric acid (not more than 0 .3 cm 3). The change in the color of the solution from red to orange or, respectively, from yellow to orange in the presence of methyl orange indicates that the food additive E339(i) passes the test for the presence of free phosphoric acid and its disubstituted sodium salt.

7.6 Determination of the mass fraction of the main substance

The method is based on potentiometric titration of food sodium monophosphate solutions in the pH range from 4.4 to 9.2.

7.6.1 Measuring instruments, auxiliary devices and reagents

pH meter with glass electrode measuring range from 1 to 14 units. pH, absolute permissible measurement error ± 0.05 units. pH.

The stirrer is magnetic.

Glass V(N)-1-100(150.250) TC(TXC) according to GOST 25336.

Burette 1-2-50-0.1 according to GOST 29251.

Distilled water according to GOST 6709.

Rectified ethyl alcohol according to GOST R 51652.

Sodium hydroxide according to GOST 4328, part

Hydrochloric acid according to GOST 3118, part

Sodium phosphate one-substituted 2-water according to GOST 245, h.

Sodium chloride according to GOST 4233, part

Thymolphthalein (indicator).

Methyl orange (indicator).

Phenolphthalein (indicator).

7.6.2 Sampling - according to 7.1.

7.6.3 Test conditions - according to 7.2.3.

7.6.4 Determination of the mass fraction of the main substance of food sodium monophosphate E339(i)

7.6.4.1 Preparation for testing

A solution of molar concentration with (NaOH) = 1 mol / dm 3 is prepared according to GOST 25794.1.

An alcohol solution with a mass fraction of thymolphthalein of 0.1% is prepared according to GOST 4919.1.

7.6.4.2 Conducting the test

A sample weighing 4 g with a record of the weighing result up to the third decimal place is placed in a beaker with a capacity of 150 cm 3, dissolved in 50 cm 3 of distilled water and titrated from a burette while stirring the solution with a magnetic stirrer with a solution of sodium hydroxide to pH 9.2. pH measurement is carried out at a temperature of (20.0 ± 0.5) °C on a pH meter in accordance with the instructions for the device.

It is allowed to carry out the determination with the indication of the equivalent point for thymolphthalein.

7.6.4.3 Handling results

The mass fraction of the main substance of food sodium monophosphate E339 (i), X 1,%, is calculated by the formula

(1)

where V- volume c (NaOH) = 1 mol / dm 3 solution used for titration of the sample to pH 9.2, cm 3;

M with(NaOH) \u003d 1 mol / dm 3 solution, g;

M(NaH 2 PO 4) = 0.1200 g, M(NaH 2 PO 4? H 2 O) \u003d 0.1380 g, M(NaH 2 PO 4? 2H 2 O) \u003d 0.1560 g;

m- weight of sample sample, g.

The final result is rounded to the first decimal place.

r R

Reproducibility limit R R

The limits of the absolute error of the method of measuring food sodium monophosphate E339 (i) ± 0.3% at R = 95 %.

7.6.5 Determination of the mass fraction of the main substance of food sodium monophosphate E339 (ii)

7.6.5.1 Preparation for testing

Molar concentration solution with(HCl) \u003d 0.5 mol / dm 3 are prepared according to GOST 25794.1.

An aqueous solution with a mass fraction of methyl orange of 0.1% is prepared according to GOST 4919.1.

7.6.5.2 Conducting the test

A sample weighing 1.5 g with a record of the weighing result up to the third decimal place is placed in a beaker with a capacity of 250 cm 3, dissolved in 100 cm 3 of distilled water and titrated from a burette while stirring the solution with a magnetic stirrer with a solution of hydrochloric acid to pH 4.4. pH measurement is carried out at a temperature of (20.0 ± 0.5) °C with a pH meter in accordance with the instructions for the device.

It is allowed to carry out the determination with indication of the equivalent point on methyl orange using a reference solution containing 2 g of dihydrate monosubstituted sodium phosphate and 2-3 drops of a solution of methyl orange in 100 cm 3 of distilled water.

7.6.5.3 Handling results

Mass fraction of the main substance of food sodium monophosphate E339 (ii) X 2 , %, calculated by the formula

(2)

where V- volume c (HCl) = 0.5 mol / dm 3 solution used for titration of the sample to pH 4.4, cm 3;

M- mass of food sodium monophosphate, corresponding to 1 cm 3 with(HCl) \u003d 0.5 mol / dm 3 solution, g; M(Na 2 HPO 4) = 0.0710 g, M(Na 2 HPO 4? H 2 O) \u003d 0.0890 g, M(Na 2 HPO 4? 7H 2 O) \u003d 0.1340 g, M(Na 2 HPO 4? 12H 2 O) \u003d 0.1791 g;

100 - coefficient of conversion to percent;

m- weight of sample sample, g.

Calculations are carried out with the result recorded to the second decimal place.

The final result is rounded to the first decimal place.

The test result is taken as the arithmetic mean of two parallel determinations.

Limit of repeatability (convergence) r is the absolute value of the difference between the results of two measurements obtained under repeatability conditions at R= 95%, should not exceed 0.2%.

Reproducibility limit R is the absolute value of the difference between the results of two measurements obtained under reproducibility conditions at R= 95%, should not exceed 0.4%.

The limits of the absolute error of the measurement method of the main substance of food sodium monophosphate E339 (ii) ± 0.3% at R = 95 %.

7.6.6 Determination of the mass fraction of the main substance of food sodium monophosphate E339(iii)

7.6.6.1 Test preparation

A solution of molar concentration with (NaOH) = 0.5 mol / dm 3 is prepared according to GOST 25794.1.

A solution of molar concentration with (HCl) = 0.5 mol / dm 3 is prepared according to GOST 25794.1.

An aqueous solution with a mass fraction of methyl orange 0.1% is prepared according to GOST 4919.1.

An alcohol solution with a mass fraction of phenolphthalein of 0.1% is prepared according to GOST 4919.1.

7.6.6.2 Conducting the test

A sample weighing 2 g with a record of the weighing result to the third decimal place is placed in a beaker with a capacity of 100 cm 3, dissolved in 50 cm 3 of distilled water and titrated while stirring the solution with a magnetic stirrer, first with a solution of hydrochloric acid to pH 4.4, and then with a solution sodium hydroxide to pH 9.2. pH measurement is carried out at a temperature of (20.0 ± 0.5) °C with a pH meter in accordance with the instructions for the device.

The double volume of sodium hydroxide solution used for titration to pH 9.2 is compared with the volume of hydrochloric acid solution used for titration to pH 4.4. From the smaller of these volumes, the content of sodium monophosphate is calculated.

It is allowed to carry out the determination with indication of the first equivalent point for methyl orange, the second - for phenolphthalein. In this case, before titration with respect to phenolphthalein, 4 g of sodium chloride is added to the analyzed solution.

7.6.6.3 Handling results

Mass fraction of the main substance of food sodium monophosphate E339 (iii) X 3 , %, calculated by the formula

(3)

(4)

where V- volume with(HCl) \u003d 0.5 mol / dm 3 solution used for titration of the sample to pH 4.4;

M- the mass of food sodium monophosphate corresponding to 1 cm 3 of a solution of hydrochloric acid or sodium hydroxide with a concentration of exactly 0.5 mol / dm 3, g; M(Na 3 PO 4) = 0.040985 g, M(Na 3 PO 4? 0.5H 2 O) \u003d 0.04324 g, M(Na 3 PO 4? H 2 O) \u003d 0.4549 g, M(Na 3 PO 4? 12H 2 O) \u003d 0.09503 g;

2V 1 - double volume exactly with(NaOH) \u003d 0.5 mol / dm 3 solution used for titration of the sample to pH 9.2, cm 3;

100 - coefficient of conversion to percent;

m- weight of sample sample, g.

If the volume of hydrochloric acid solution used for titration is more than twice the volume of sodium hydroxide solution, then the analyzed food sodium monophosphate contains free alkali.

The test result is taken as the arithmetic mean of two parallel determinations.

Limit of repeatability (convergence) r is the absolute value of the difference between the results of two measurements obtained under repeatability conditions at R= 95%, should not exceed 0.6%.

Reproducibility limit R is the absolute value of the difference between the results of two measurements obtained under reproducibility conditions at R= 95%, should not exceed 0.8%.

The limits of the absolute error of the measurement method of the main substance of food sodium monophosphate E339 (iii) ± 0.6% at R = 95 %.

7.7 Determination of the mass fraction of total phosphorus pentoxide

The method for determining the mass fraction of total phosphorus pentoxide is carried out in order to identify food monophosphates of sodium E339 (i), E339 (ii) and E339 (iii).

7.7.1 Extraction-photometric method

The method is based on the extraction of dietary sodium monophosphates in the form of phosphomolybdenum ammonium with a mixture of organic solvents and subsequent photometric measurement of the optical density of solutions.

7.7.1.1 Measuring instruments and reagents

Photoelectric colorimeter with a light filter with a maximum transmission at a wavelength of (630 ± 10) nm and cuvettes with a light-absorbing layer thickness of 10 mm.

Liquid glass thermometer measuring range from 0 °С to 50 °С, division value 1 °С according to GOST 28498.

Flasks 2-50-2, 2-100-2, 2-500-2, 2-1000-2, 2-2000-2 according to GOST 1770.

Pipettes 2-2-1, 2-2-2, 2-2-5, 2-2-10, 2-2-25 according to GOST 29169.

Burette 1-1-2-25-0.1 according to GOST 29251.

Stopwatch of the 2nd class of accuracy with a counter scale capacity of 30 minutes, with a division value of 0.20 s.

Distilled water according to GOST 6709.

Ammonium molybdate according to GOST 3765, part

Ethyl alcohol according to GOST R 51652.

Tin dichloride 2-water according to the document in accordance with which it is manufactured and can be identified.

Glycerin according to GOST 6259, part

Sulfuric acid according to GOST 4204, part

Isobutyl alcohol according to GOST 6016, part

Toluene according to GOST 5789, analytical grade.

Potassium phosphate monosubstituted according to GOST 4198, analytical grade.

7.7.1.2 Sampling - according to 7.1.

7.7.1.3 Test conditions - according to 7.2.3.

7.7.1.4 Test preparation

a) Preparation of a sulfuric acid solution

Molar concentration solution with(1/2 H 2 SO 4) \u003d 0.7 mol / dm 3 is prepared as follows: to 980 cm 3 of ethanol with a mass fraction of 99.5% and a density of 0.789 g / cm 3, prepared according to GOST 4517, carefully add 20 cm 3 sulfuric acid with a density of 1.84 g / cm 3.

b) Preparation of a solution of ammonium molybdate

A weighing of 100 g of ammonium molybdate with a record of the weighing result to the fourth decimal place is dissolved in 800 cm 3 of sulfuric acid with a molar concentration of (1/2 H 2 SO 4) = 10 mol / dm 3, the volume of the solution is adjusted with distilled water to 2000 cm 3. The solution is stored in a dark glass bottle with a ground stopper and used three days after its preparation.

c) Preparation of a solution of stannous chloride

A portion of tin dichloride weighing 0.2 g with a record of the weighing result to the fourth decimal place is dissolved in a mixture of 50 cm 3 of glycerol and 50 cm 3 of ethyl alcohol. The solution is stored at room temperature and used within seven days.

d) Preparation of a standard solution of phosphate containing 0.1 mg of phosphorus pentoxide in 1 cm 3

A portion of monopotassium phosphate weighing 1.9175 g with a weighing record up to the fourth decimal place is dissolved in distilled water in a volumetric flask with a capacity of 1000 cm 3, brought to the mark with water and mixed. Pipette 10 cm 3 of the resulting solution into a volumetric flask with a capacity of 100 cm 3, bring to the mark with distilled water and mix.

e) Preparation of reference solution

20 cm 3 of distilled water are poured into a volumetric flask with a capacity of 100 cm 3, 25 cm 3 of a mixture of solvents prepared by mixing 12.5 cm 3 of isobutyl alcohol and 12.5 cm 3 of toluene, 5 cm 3 of a solution of ammonium molybdate are added and vigorously stirred for 15 with. Then, after settling and separating the layers, 5 cm 3 of the upper organic layer are pipetted into a volumetric flask with a capacity of 50 cm 3, diluted with a solution of sulfuric acid prepared according to 7.7.1.4 a), to a volume of approximately 45 cm 3 , 1 cm 3 of a solution of stannous chloride is added, Dilute to volume with sulfuric acid and mix.

f) Construction of a calibration curve

In volumetric flasks with a capacity of 100 cm 3 contribute 1.0; 2.0; 3.0; 4.0; 5.0; 6.0 cm 3 of a standard solution of monophosphate, which corresponds to 0.1; 0.2; 0.3; 0.4; 0.5; 0.6 mg of phosphorus pentoxide, diluted with water to a volume of approximately 20 cm 3 , add 25 cm 3 of a solvent mixture prepared by mixing 12.5 cm 3 of isobutyl alcohol and 12.5 cm 3 of toluene, 5 cm 3 of a solution of ammonium molybdate and immediately mix vigorously within 15 s. Then, after settling and separating the layers, aliquots of 5 cm 3 of the upper organic layer are taken with a pipette, which corresponds to 0.02; 0.04; 0.06; 0.08; 0.10; 0.12 mg of phosphorus pentoxide, in volumetric flasks with a capacity of 50 cm 3, dilute with a solution of sulfuric acid prepared according to 7.7.1.4 a), to a volume of approximately 45 cm 3, add 1 cm 3 of a solution of stannous chloride, bring the volume to the mark with sulfuric acid and mixed.

Measurement of the optical density of the prepared solutions is carried out in relation to the reference solution, prepared simultaneously under the same conditions, in cuvettes with a thickness of the light-absorbing layer of 10 mm at a wavelength of 630 nm.

Based on the averaged results of two parallel determinations, a calibration graph is built, plotting the masses of phosphorus pentoxide in milligrams along the abscissa axis, and the corresponding values ​​of optical densities along the ordinate axis.

The calibration curve is periodically (once every 10 days) refined by three main points.

7.7.1.5 Conducting the test

A weighed sample weighing from 0.04 to 0.05 g with a record of the weighing result to the fourth decimal place is dissolved in distilled water at a temperature of (20 ± 1) ° C in a volumetric flask with a capacity of 500 cm 3, brought to the mark and mixed. Pipette 10 cm 3 of the resulting solution into a volumetric flask with a capacity of 100 cm 3. Next, the preparation of the test solution is carried out according to 7.7.1.4 e).

The measurement of the optical density of the analyzed solution is carried out in cuvettes with a thickness of the light-absorbing layer of 10 mm at a wavelength of 630 nm.

The mass of food sodium monophosphate in an aliquot part in terms of phosphorus pentoxide is determined according to the calibration curve.

7.7.1.6 Handling results

Mass fraction of total phosphorus pentoxide (anhydrous form) X 4 , %, calculated by the formula

(5)

where m 1 - mass of food sodium monophosphate in terms of phosphorus pentoxide in an aliquot of the solution, found according to the calibration graph, mg;

500 - volumetric flask capacity, cm 3;

25 - volume of a mixture of solvents (isobutyl alcohol and toluene), cm 3;

100 - conversion factor of the result into percentage;

1000 is the conversion factor for the content of food sodium monophosphates in terms of phosphorus pentoxide from milligrams to grams;

10 - the volume of dissolved food sodium monophosphate taken for testing, cm 3;

5 - an aliquot of the organic layer taken for dilution according to 7.7.1.4 e);

m- weight of sample sample, g.

The final result is rounded to the second decimal place.

The test result is taken as the arithmetic mean of two parallel determinations.

Limit of repeatability (convergence) r is the absolute value of the difference between the results of two measurements obtained under repeatability conditions at R= 95%, should not exceed 0.15%.

Reproducibility limit R is the absolute value of the difference between the results of two measurements obtained under reproducibility conditions at R= 95%, should not exceed 0.30%.

The limits of the absolute error of the method for measuring the mass fraction of the total phosphorus pentoxide of food sodium monophosphates ± 0.20% at R = 95 %.

7.7.2 Potentiometric method - according to GOST R 52824.

7.7.3 Photocolorimetric method - according to GOST R 52824.

7.8 Determination of the mass fraction of water-insoluble substances

The method is based on the dissolution of dietary sodium monophosphates in water under certain conditions and the determination of the mass fraction of water-insoluble substances.

7.8.1 Measuring instruments, auxiliary equipment, reagents

Filtering crucible type TF POR 16 according to GOST 25336.

Laboratory scales according to GOST 24104 with the limits of the permissible absolute error of a single weighing ± 0.00001 g.

Measuring cylinder 1-100-1 according to GOST 1770.

Distilled water according to GOST 6709.

7.8.2 Sampling - according to 7.1.

7.8.3 Test conditions - according to 7.2.3.

7.8.4 Conducting a test

A sample weighing 10 g with a record of the weighing result up to the fourth decimal place is placed in a beaker with a capacity of 250 cm 3 and dissolved in 100 cm 3 of hot distilled water. Then the solution is filtered through a filter crucible, previously dried to constant weight (the weight between the last two weighings should not exceed 0.0002 g). The insoluble residue on the filter is washed with hot water, dried in an oven at a temperature from 100 °C to 110 °C for 2 hours, cooled in a desiccator and weighed (the difference between the results of the last two weighings should not exceed 0.0002 g).

7.8.5 Results processing

Mass fraction of substances insoluble in water X 5,%, calculated by the formula

(6)

where m 1 - weight of the filtering crucible with a precipitate of insoluble substances after drying, g;

m 2 - weight of the filtering crucible, g;

m- weight of sample, g;

Calculations are carried out with the result recorded to the third decimal place.

The final result is recorded to the second decimal place.

The test result is taken as the arithmetic mean of two parallel determinations.

Limit of repeatability (convergence) r is the absolute value of the difference between the results of two measurements obtained under repeatability conditions at R= 95%, should not exceed 0.02%.

Reproducibility limit R is the absolute value of the difference between the results of two measurements obtained under reproducibility conditions at R= 95%, should not exceed 0.04%.

The limits of the absolute measurement error of the method of mass fraction of water-insoluble substances ±0.03% at R = 95 %.

7.9 Determination of the pH of an aqueous solution

The method is based on determining the activity index of hydrogen ions in solutions of food sodium monophosphates with a mass fraction of 1% by measuring pH using a pH meter with a glass electrode.

7.9.1 Measuring instruments, auxiliary equipment and reagents

pH meter with glass electrode measuring range from 1 to 14 units. pH, with a permissible absolute measurement error of ±0.05 units. pH.

Laboratory scales in accordance with GOST 24104 with the limits of the permissible absolute error of a single weighing ± 0.01 g.

Liquid glass thermometer measuring range from 0 °C to 50 °C, division value 0.5 °C according to GOST 28498.

Glass V(N)-1-250 TC(TXC) according to GOST 25336.

Melted glass stick.

Measuring cylinder 1-100-1 according to GOST 1770.

Distilled water according to GOST 6709.

7.9.2 Sampling - according to 7.1.

7.9.3 Test conditions - according to 7.2.3.

7.9.4 Conducting a test

A sample weighing 1.0 g with a record of the weighing result to the third decimal place is placed in a beaker with a capacity of 250 cm 3 and dissolved in 100 cm 3 of hot distilled water that does not contain carbon dioxide and prepared in accordance with GOST 4517, mix thoroughly, immerse the electrodes of the pH meter in solution and measure the pH of the solution at (20.0 ± 0.5) °C.

The readings of the pH meter are determined in accordance with the instructions for the device.

7.9.5 Processing of measurement results

The measurement results are recorded to the second decimal place.

For the final result of the pH determination, the arithmetic mean of two parallel determinations, rounded to the first decimal place, is taken.

Limit of repeatability (convergence) r is the absolute value of the difference between the results of two measurements obtained under repeatability conditions at R= 95%, should not exceed 0.1 units. pH.

Reproducibility limit R is the absolute value of the difference between the results of two measurements obtained under reproducibility conditions at R= 95%, should not exceed 0.2 units. pH.

Limits of the absolute error of the pH measurement method ± 0.1 units. pH at R = 95 %.

7.10 Determination of the mass fraction of loss on drying

The method is based on the ability of food sodium monophosphates E339(i) and E339(ii), placed in an oven, to be released from volatile substances at temperatures from 40 °C to 105 °C. The mass fraction of losses is determined by the difference in the weight of the sample of food sodium monophosphate before and after drying.

7.10.1

Drying cabinet that maintains the specified mode from 20 °С to 200 °С with an error of ±2 °С.

Laboratory scales in accordance with GOST 24104 with the limits of the permissible absolute error of a single weighing ± 0.0001 g.

Desiccator 2-250 according to GOST 25336.

Clock electronic-mechanical quartz table, wall and alarm clock according to GOST 27752.

Cup CH 45/13 according to GOST 25336.

7.10.2 Sampling - according to 7.1.

7.10.3 Test conditions - according to 7.2.3.

7.10.4 Testing for E339(i)

A clean empty weighing cup is dried with a lid open at a temperature of from 100 ° C to 105 ° C in an oven to constant weight.

A weighed sample weighing from 1 to 2 g with a record of the weighing result to the third decimal place is placed open together with a lid in an oven and dried at a temperature of 60 ° C for 1 hour, then at 105 ° C for 4 hours. After that the glass is quickly closed with a lid, cooled in a desiccator to room temperature and weighed.

7.10.5 Testing for E339(ii)

A clean empty weighing cup is dried with the lid open at a temperature of 100 °C to 105 °C in an oven for 30 minutes, then cooled in a desiccator and weighed, recording the weighing result to the third decimal place. Drying to constant weight is carried out until the difference between the results of two parallel determinations does not exceed 0.001 g.

A sample weighing from 1 to 2 g is weighed in a beaker with a record of the weighing result to the third decimal place, placed open together with a lid in an oven and dried at a temperature of 40 °C for 3 hours, then at 105 °C for 5 hours After that, the cup is quickly closed with a lid, cooled in a desiccator to room temperature and weighed.

7.10.6 Results processing

7.10.6.1 Loss on drying, by mass, dietary sodium monophosphate E339(i) X 6,%, calculated by the formula

(7)

where m- mass of a dry glass with a sample sample before drying, g;

m 1 - mass of the cup with the sample after drying, g;

m 2 - weight of dry glass, g;

100 - coefficient for converting the result into a percentage.

Calculations are carried out with the result recorded to the second decimal place.

7.10.6.2 The arithmetic mean is taken as the final result of the determination X 6 , %, of two parallel determinations, if the acceptability condition is met

, (8)

where , - test results of two parallel measurements of the mass fraction of losses during drying,%;

The average value of two parallel measurements of the mass fraction of losses during drying,%;

r

± 0.01d , at R = 0,95, (9)

Repeatability limit r and reproducibility R, as well as the accuracy index d for the measurement range, in accordance with table 3, the mass fraction of losses during drying are given in table 6.

Table 6

7.11 Determination of the mass fraction of loss on ignition

The method is based on the ability of E339(iii) food sodium monophosphates placed in a muffle furnace to be freed from volatile substances at temperatures from 120 °C to 800 °C. The mass fraction of losses is determined by the difference in the weight of the sample of food sodium monophosphate before and after calcination.

7.11.1 Measuring instruments, auxiliary equipment

Muffle furnace with heating range from 50 °С to 1000 °С, ensuring maintenance of the set temperature within ±25 °С.

Drying cabinet that maintains the specified mode from 20 °С to 200 °С with an error of ±2 °С.

Liquid glass thermometer measuring range from 0 °С to 200 °С, division value 1 °С according to GOST 28498.

Laboratory scales in accordance with GOST 24104 with the limits of the permissible absolute error of a single weighing ± 0.0001 g.

Desiccator 2-250 according to GOST 25336.

Clock electronic-mechanical quartz table, wall and alarm clock according to GOST 27752.

Porcelain crucibles according to GOST 9147.

7.11.2 Sampling - according to 7.1.

7.11.3 Test conditions - according to 7.2.3.

7.11.4 Conducting a test

Dry the clean, empty weighing crucible with the lid open at 100°C to 105°C in an oven to constant weight.

A sample weighing from 1 to 2 g with a record of the weighing result up to the third decimal place is placed openly together with a lid in a muffle furnace and calcined at a temperature of 120 °C for 2 hours, then at 800 °C for 30 minutes. After that, the crucible is quickly closed with a lid, cooled in a desiccator to room temperature and weighed.

7.11.5 Results processing

7.11.5.1 Loss on ignition mass fraction of edible sodium monophosphate E339(iii) X 7,%, calculated by the formula

(10)

where t is the weight of the dry crucible with a sample weight before calcination, g;

m 1 - mass of the crucible with the sample after calcination, g;

m 2 - mass of dry crucible, g;

100 - coefficient for converting the result into a percentage.

Calculations are carried out with the result recorded to the second decimal place.

The final result is recorded to the first decimal place.

7.11.5.2 The arithmetic mean is taken as the final result of the determination X 7 , %, of two parallel determinations, if the acceptability condition is met

, (11)

where , - test results of two parallel measurements of the mass fraction of losses on ignition,%;

The average value of two parallel measurements of the mass fraction of losses during ignition,%;

r- the value of the repeatability limit given in Table 6.

The result of the analysis is presented in the form:

± 0.01d , at R = 0,95, (12)

where - the arithmetic mean of the results of two determinations, recognized as acceptable,%;

d - limits of relative measurement error, %.

Repeatability limits r and reproducibility R, as well as the accuracy index d for the measurement range, in accordance with Table 3, the mass fraction of losses on ignition are given in Table 6.

7.12 Determination of the mass fraction of fluorides

7.12.1 Sampling - according to 7.1.

7.12.2 Test conditions - according to 7.2.3.

7.12.3 Determination of the mass fraction of fluorides - according to GOST 8515 (see 3.9).

7.13 Determination of the mass fraction of arsenic

7.13.1 Sampling - according to 7.1.

7.13.2 Test conditions - according to 7.2.3.

7.13.3 Determination of the mass fraction of arsenic - according to GOST 26930, GOST R 51766 or GOST 10485.

7.14 Determination of the mass fraction of lead

7.14.1 Sampling - according to 7.1.

7.14.2 Test conditions - according to 7.2.3.

7.14.3 Determination of the mass fraction of lead - according to GOST 26932.

8 Transport and storage

8.1 Food sodium monophosphates are transported in covered vehicles by all modes of transport in accordance with the rules for the transportation of goods in force for the respective modes of transport.

8.2 Food sodium monophosphates are stored in the manufacturer's packaging in a dry, cool place in covered storage areas.

8.3 Shelf life of food sodium monophosphates - no more than two years from the date of manufacture.

9.1 Food additive E339 is used as an acidity regulator, color stabilizer, consistency stabilizer, emulsifier, complexing agent, texturizer and water-retaining agent in the production of bakery and flour confectionery products, alcoholic beverages, products of meat, fish, oil and fat, canning and dairy industries.

9.2 Food additive E339 is used in accordance with the regulatory legal acts of the Russian Federation *.

* Before the introduction of the relevant regulatory legal acts of the Russian Federation - regulatory documents of the federal executive authorities.

GOST R 55517-2013

NATIONAL STANDARD OF THE RUSSIAN FEDERATION

Food additives

FOOD ANTIOXIDANTS

Terms and Definitions

food additives. Antioxidants of foodstuffs. Terms and definitions

OKS 01.040.67
67.220.20

Introduction date 2014-04-01

Foreword

1 DEVELOPED by the State Scientific Institution All-Russian Research Institute of Food Flavors, Acids and Dyes of the Russian Academy of Agricultural Sciences (GNU VNIIPAKK Russian Agricultural Academy)

2 INTRODUCED by the Technical Committee for Standardization TC 154 "Food Additives and Flavorings"

3 APPROVED AND PUT INTO EFFECT by Order of the Federal Agency for Technical Regulation and Metrology dated August 28, 2013 N 580-st

4 This standard takes into account the terminology of the Uniform Standard for Food Additives of the Codex Alimentarius Commission CODEX STAN 192-1995 * "General standard for foods additives" in terms of specifications for food additives - antioxidants of the Joint FAO/WHO Joint Expert Committee on Food Additives "Unified Code of Specifications for Food Additives" Combined compendium of food additive specificacion JECFA Volume 4"
________________
* Access to international and foreign documents mentioned hereinafter in the text can be obtained by clicking on the link to the site http://shop.cntd.ru. - Database manufacturer's note.

5 INTRODUCED FOR THE FIRST TIME

6 REVISION. December 2018


The rules for the application of this standard are set out in article 26 of the Federal Law of June 29, 2015 N 162-FZ "On standardization in the Russian Federation". Information about changes to this standard is published in the annual (as of January 1 of the current year) information index "National Standards", and the official text of changes and amendments - in the monthly information index "National Standards". In case of revision (replacement) or cancellation of this standard, a corresponding notice will be published in the next issue of the monthly information index "National Standards". Relevant information, notification and texts are also posted in the public information system - on the official website of the Federal Agency for Technical Regulation and Metrology on the Internet (www.gost.ru)

Introduction

Introduction

The terms established in the standard are arranged in a systematic order, reflecting the system of concepts in the field of food antioxidants.

There is one standardized term for each concept.

The parenthesized part of a term may be omitted when the term is used in standardization documents, while the non-parenthesized part of the term forms its short form.

To preserve the integrity of the terminological system in the standard, a terminological entry from another standard operating at the same level of standardization is given, which is enclosed in thin lines.

The above definitions can be changed, if necessary, by introducing derivative features into them, revealing the meanings of the terms used in them, indicating the objects included in the scope of the concept being defined. Changes should not violate the scope and content of the concepts defined in this standard.

The standard provides foreign language equivalents of standardized terms in English.

Standardized terms are in bold type, their short forms are in light type in the alphabetical index.

1 area of ​​use

This International Standard establishes terms and definitions in the field of food antioxidants.

The terms established by this standard are recommended for use in all types of documentation and literature in the field of food antioxidants that are within the scope of standardization works and (or) use the results of these works.

2 Terms and definitions

General concept

1

Alphabetical index of terms in Russian

Alphabetical index of terms in English

Electronic text of the document
prepared by Kodeks JSC and verified against:
official publication
M.: Standartinform, 2018

The statistics of the registers of sanitary and epidemiological conclusions of the Ministry of Health of Russia shows that today the market for food additives is rapidly developing, constantly replenished with new imported and domestic additives that can change the traditional taste of well-known products. In this regard, there is a problem of legislative regulation of the use of food additives. This problem is not new. Mankind has been solving it for centuries, improving the regulatory framework. However, in our time, with the development of such sciences as biotechnology and biochemistry, it is more acute than ever.

In 2003, Russia introduced a new document regulating the use of food additives - SanPiN 2.3.2.1293-03 "Hygienic requirements for the use of food additives".

It concerns the use of additives in all branches of the food industry, including the meat industry.

With the introduction of the new document, the number of E-indices allowed for use in our country has not changed and today is slightly less than 400 (according to our estimates, about 394, after the ban on the use of E216 and E217 was introduced).

The meat industry remains quite conservative in terms of the use of food additives. Of the 394 E-indices in our industry, about a hundred are allowed for use, but this is if we talk about allowed ones. As practice shows, the number of food additives most commonly used for the production of meat products, well known to the consumer by labeling on packages, is no more than 20 E-indices.

One of the most important aspects of successful control over the use of food additives is the existence of standardized methods for determining the content of food additives in meat products. But how many such standards have been developed for the meat industry? This list is very short. Methods for the determination of nitrates, nitrites, glutamic acid, glucono-delta-lactone, total phosphorus (indirect method to control the introduction of phosphates). In the same row, one can indicate the method for determining starch (but only native) and the histological method for identifying the composition, which also allows us to detect the presence of thickeners of a polysaccharide nature, for example, carrageenans.

Today, a number of preservatives (Table 1, Appendix 1) and dyes (Table 2, Appendix 2) are allowed for use in the meat industry, for which the maximum level of their content in meat products is established, but there are no control methods. Even more acute is the question of the need to develop methods for determining the content of those additives that are prohibited, such as, for example, amaranth dye (E123).

Very often lately one has heard proposals from specialists of meat processing enterprises to include various food additives in the national state standards for meat products. However, few of them think that the work on including, for example, a dye (preservative, emulsifier) ​​should begin with the development of a national standard for the method of its determination.

The same problem (but on a larger scale due to a wider list of possible food additives) arises in the development of GOSTs of the form of general technical conditions and special technical regulations.

What are the basic principles for the use of food additives defined in the new SanPiN-2.3.2.1293-03?

1. Food additives must be present in products in an amount that is minimally necessary to achieve the required technological effect, but not more than the maximum allowable level of their content (residual content) in the finished product.

2. The use of food additives must not impair the organoleptic properties of the products and/or reduce their nutritional value.

3. It is not allowed to use food additives to hide spoilage and poor quality of raw materials or finished products.

4. For food additives that do not pose a threat to human health, but an excessive amount of which can lead to technical deterioration of raw materials, the maximum level of their introduction should be determined by the technological instructions.

The specialists of the institute were guided by these basic principles when they developed the first national standard - GOST R 52196-2003 “Cooked sausage products. Specifications".

What food additives were included in the standard as a result of their evaluation and selection for compliance with safety standards and Russian meat business traditions?

To date, the standard provides for the use of the following food additives:

1. Color fixer E250.

2. Flavor and aroma enhancer Е621.

3. Acidity regulators E325, E326, E500.

4. Antioxidants E300, E301.

5. Stabilizers, emulsifiers E450-E452.

As you can see, there are not many. Of particular note is sodium nitrite E250. Perhaps today we remain the only country in the world where sodium nitrite (a highly toxic substance) is used in its pure form (in the form of solutions) in food enterprises. However, some progress has recently been made in this area: there is an order of the Russian Ministry of Health on the preparation of amendments to SanPiN 2.3.1.1293-01, which prohibit the use of pure nitrites. In this regard, curing mixtures were included in the new GOST R 52196-01 “Cooked sausage products”, and at present (for the transitional period) our institute has developed a “Technological instruction for the use of curing mixtures and sodium nitrite”.

As for complex food additives, their use should not change the traditional taste of GOST cooked sausages, and they should contain only those “E” indices that were mentioned above (for example, color fixer E250).

In order for the requirements of GOST to be met, in order to support, and our tasks in the development of national standards, first of all, of a domestic manufacturer, the institute developed a document, TU9199-675-00419779 "Spicy mixtures for boiled sausages". The document contains 38 names of complex mixtures - flavoring and phosphate-containing. However, its inclusion in GOST R does not provide for a ban on the use of other complex additives. Specifications are intended for domestic manufacturers of ingredients, they were purchased by a number of firms.

Since the text of GOST and the text of the technological instruction provide for the use of imported additives similar in composition, quality and safety, as well as materials and raw materials similar to domestic ones, then, in accordance with the principles that are enshrined in SanPiN, their use should be based on developed in the prescribed manner technological instructions. Therefore, now the institute is developing such instructions that determine the procedure for using food additives similar in composition.

Returning to the need for the development of national standards for methods, it should be emphasized that the use of additives should not be limited in any artificial way. The sole purpose of compliance with hygienic regulations for the use of food additives should be pursued, as well as correctly conveyed information to the consumer about the composition of the product.

The EU directives, taken as a basis for the development of SanPiN 2.3.2.1293-03, contain simple and understandable principles that we should also adopt. A food additive should not be used if it misleads the consumer.

The requirements for information for consumers in the relevant GOST are spelled out quite clearly, but the content of the information cannot remain unchanged: the interests of the consumer require constant adjustments to the content. In this regard, I would like to draw attention to an example of labeling (slide) that meets the directives that the European Union is currently moving to. The label indicates not only the amount of food additives, but also the amount of meat raw materials provided for in the recipe of this product. The same directives determine how much connective and adipose tissue raw meat can contain. Under this condition, having in the arsenal of control methods, clear requirements for labeling food products, the use of food additives will not cause unreasonable suspicions among the consumer.

FEDERAL AGENCY FOR TECHNICAL REGULATION AND METROLOGY

NATIONAL

STANDARD

RUSSIAN

FEDERATION

Food additives

AZO DYES

Specifications

Official edition

Stand rtinform 2014

Foreword

1 DEVELOPED by the State Scientific Institution All-Russian Research Institute of Food Flavors, Acids and Dyes of the Russian Academy of Agricultural Sciences (GNU VNIIPAKK Russian Agricultural Academy)

2 INTRODUCED by the Technical Committee for Standardization TC 154 "Food Additives and Flavorings"

3 APPROVED AND PUT INTO EFFECT by Order of the Federal Agency for Technical Regulation and Metrology dated September 6, 2013 No. 854-st

4 8 this standard takes into account the requirements of the Uniform Standard for Food Additives of the Codex Alimentarius Commission CODEX STAN 192-1995 "General Standard for Food Additives" (paragraph 3.4) in terms of Specifications for food additives azo dyes E102. E110. E122, E124. E129. E151. E155 of the FAO/WHO Joint Expert Committee on Food Additives “Combined compendium of additive food specification JECFA. Volume 4"

5 8 INTRODUCED FOR THE FIRST TIME

The rules for the application of this standard are established in GOST R 1.0-2012 (section 8). Information about changes to this standard is published in the annual (as of January 1 of the current year) information index "National Standards", and the official text of changes and amendments - in the monthly information index "National Standards". In case of revision (replacement) or cancellation of this standard, a corresponding notice will be published in the next issue of the monthly information index "National Standards". Relevant information, notification and texts are also posted in the public information system - on the official website of the Federal Agency for Technical Regulation and Metrology on the Internet (gost.ru)

© Standartinform. 2014

This standard cannot be fully or partially reproduced, replicated and distributed as an official publication without the permission of the Federal Agency for Technical Regulation and Metrology

NATIONAL STANDARD OF THE RUSSIAN FEDERATION

Food additives AZO DYES Specifications Food additives. Azo colours. Specifications

Introduction date - 2015-01-01

1 area of ​​use

This standard applies to food additives E102. E110, E122. E124, E12S. E151. E155. which are food azo dyes (hereinafter referred to as aeo dyes) and intended for use in the food industry.

NOTE The term "aerocolorants" reflects a common feature of the food additives included in this standard, associated with the presence of an azo group (N ■ N) in their structure.

Quality requirements for aerodyes are set out in 3.1.3.3.1.4 and 3.1.5. to safety - in 3.1.6. to marking - in 3.3.

2 Normative references

8 of this standard uses normative references to the following standards:

GOST 6.579-2002 State system for ensuring the uniformity of measurements. Requirements for the quantity of packaged goods in packages of any kind during their production, packaging, sale and import

GOST 12.0.004-90 Occupational safety standards system. Organization of labor safety training. General provisions

GOST 12.1.004-91 Occupational safety standards system. Fire safety. General requirements

GOST 12.1.005-88 System of labor safety standards. General sanitary and hygienic requirements for the air of the working area

GOST 12.1.007-76 Occupational safety standards system. Harmful substances. Classification and general safety requirements

GOST 12.1.044-69 (ISO 4589-84) Occupational safety standards system. Fire and explosion hazard of substances and materials. Nomenclature of indicators and methods for their determination

GOST 12.2.007.0-75 Occupational safety standards system. Electrical products. General safety requirements

GOST 12.4.009-83 Occupational safety standards system. Fire equipment for the protection of objects. Main types. Accommodation and service

GOST 12.4.011-69 System of labor safety standards. Means of protection for workers. General requirements and classification

GOST 12.4.021-75 System of labor safety standards. Ventilation systems. General requirements

GOST 12.4.103-83 Occupational safety standards system. Special protective clothing, personal protective equipment for legs and arms. Classification

Official edition

GOST 61-75 Reagents. Acetic acid. Specifications GOST 83-79 Reagents. Sodium carbonate. Specifications GOST 450-77 Technical calcium chloride. Specifications

GOST 1770-74 (ISO 1042-83, ISO 4788-80) Measuring laboratory glassware. Cylinders, beakers, flasks, test tubes. General specifications GOST 2603-79 Reagents. Acetone. Specifications GOST 3118-77 Reagents. Hydrochloric acid. Specifications GOST 3760-79 Reagents. Ammonia water. Specifications GOST 4160-74 Reagents. Potassium bromide. Specifications GOST 4197-74 Reagents. Sodium aeotoxide. Specifications GOST 4198-75 Reagents. Potassium phosphate monosubstituted. Specifications GOST 4201-79 Sodium carbonate acid. Specifications GOST 4328-77 Reagents Sodium hydroxide. Specifications

GOST 4517-87 Reagents. Methods for the preparation of auxiliary reagents and solutions used in the analysis

GOST 4919.2-77 Reagents and highly pure substances. Methods for preparing buffer solutions

GOST 5819-78 Reagents. Aniline. Specifications GOST 6006-78 Reagents. Butanol-1. Specifications GOST 6016-77 Reagents. Isobutyl alcohol. Specifications GOST 6259-75 Reagents. Glycerol. Specifications GOST 6709-72 Distilled water. Specifications

GOST 6825-91 (IEC 81-84) Tubular fluorescent lamps for general lighting GOST 10354-82 Polyethylene film. Specifications

GOST 11773-76 Reagents. Sodium phosphate dihydrate. Specifications GOST 12026-76 Laboratory filter paper. Specifications GOST 14192-96 Cargo marking

GOST 14919-83 Household electric stoves, electric stoves and ovens. General specifications

GOST 14961-91 Linen and linen threads with chemical fibers. Specifications GOST 15846-2002 Products shipped to the Far North and equivalent areas. Packaging, marking, transportation and storage

GOST 16922-71 Organic dyes, intermediates, textile auxiliaries. Test Methods

GOST 17308-88 Twines. Specifications

GOST 18300-87 Rectified technical ethyl alcohol. Specifications GOST 19360-74 Film liners. General specifications GOST 22280-76 Reagents. Sodium citrate 5.5-aqueous. Specifications GOST 22300-76 Reagents. Esters of ethyl and butyl acetic acid. Specifications

GOST 25336-82 Laboratory glassware and equipment. Types, basic parameters and dimensions

GOST 25794.1-83 Reagents. Methods for preparing titrated solutions for acid-base titration

GOST 26927-86 Food raw materials and products. Methods for determination of mercury GOST 26930-86 Food raw materials and products. Method for determination of arsenic GOST 26932-86 Raw materials and food products. Lead determination methods GOST 26933-86 Food raw materials and products. Methods for determination of cadmium GOST 27752-88 Electronic-mechanical quartz desktop, wall and alarm clocks. General specifications

GOST 28365-88 Reagents. Paper Chromatography Method

GOST 28498-90 Liquid glass thermometers. General technical requirements. Test Methods

GOST 29169-91 Laboratory glassware. Pipettes with one mark GOST 29227-91 (ISO 835-1-81) Laboratory glassware. Pipettes graduated. Part 1. General requirements

GOST 30090-93 Bags and bag fabrics. General specifications

GOST 30178-96 Food raw materials and products. Atomic absorption method for the determination of toxic elements

GOST R 12.1.019-2009 Occupational safety standards system. Electrical safety. General requirements and nomenclature of types of protection

GOST R ISO 2859-1-2007 Statistical methods. Procedures for selective control on an alternative basis. Part 1. Sampling plans for successive batches based on an acceptable level of quality

GOST R 51766-2001 Food raw materials and products. Atomic absorption method for the determination of arsenic

GOST R 53228-2008 Scales of non-automatic action. Part 1. Metrological and technical requirements. Tests

GOST R 53361-2009 Bags made of paper and composite materials. General technical

GOST R 54463-2011 Containers made of cardboard and combined materials for food products. Specifications

Note - When using this standard, it is advisable to check the validity of reference standards in the public information system - on the official website of the Federal Agency for Technical Regulation and Metrology on the Internet or according to the annually published information index "National Standards *", which was published as of January 1 of the current year , and according to the issues of the monthly published information index "National Standards" for the current year. If an undated reference standard has been replaced, it is recommended that the current version of that standard be used, taking into account all changes made to the single version. If the reference standard to which the dated reference is given is replaced, then it is recommended to use the version of this standard with the year of approval (acceptance) indicated above. If, after the approval of this standard, a change is made to the referenced standard to which a dated reference is given, affecting the provision to which the reference is given, then this provision is recommended to be applied without taking into account this change. If the reference standard is canceled without replacement, then the provision in which the reference to it is given is recommended to be applied in the part that does not affect this reference.

3 Technical requirements

3.1 Characteristics

3.1.1 Azo dyes are produced in accordance with the requirements of this standard and used in food products in accordance with and.

3.1.2 Designations, names, chemical names, formulas and molecular weights of azo dyes are given in tables 1 and 2.

Table 1 - Designations and names of dyes

End of table 1

Table 2 - Chemical names, formulas and molecular weights of azo dyes

3.1.3 In terms of organoleptic characteristics, azo dyes must meet the requirements specified in Table 3.

Table 3 - Organoleptic characteristics of azo dyes

End of table 3

3.1.4 Spectrophotometric characteristics of aerocolors are given in Table 4.

Table 4 - Spectrophotometric characteristics of azo dyes

3.1.5 In terms of physicochemical parameters, azo dyes must comply with the requirements specified in Table 5.

Table 5 - Physical and chemical parameters of azo dyes

End of table 5

3.2 Packaging

3.2.1 The packaging of aerocolorants must comply with the requirements set out in and (2).

3.2.2 Azo dyes are packed in grocery bags made of bag fabrics in accordance with GOST 30090, paper open bags of NM and PM grades in accordance with GOST R 53361. Corrugated cardboard boxes for food products in accordance with GOST R 54463. Inside grocery bags made of bag fabrics, paper bags of NM brand . boxes made of corrugated cardboard, liners should be inserted in accordance with GOST 19360 from food-grade polyethylene unstabilized film grade H with a thickness of at least 0.08 mm in accordance with GOST 10354.

The type and size of bags, the maximum weight of the packed azo dyes are set by the manufacturer.

3.2.3 Polyethylene bags-liners after filling them are welded or tied with string from bast fibers in accordance with GOST 17308.

3.2.4 The top seams of fabric and paper bags must be machine-sewn with linen threads in accordance with GOST 14961 or other threads that ensure the mechanical strength of the seam.

3.2.5 It is allowed to use other types of packaging and packaging means that meet the requirements established. (2). and made from packaging materials that meet the requirements.

3.2.6 The negative deviation of the net weight from the nominal weight of each packaging unit must comply with the requirements of GOST 8.579 (tables A.1 and A.2).

3.2.7 Azo dyes shipped to the Far North and equivalent areas are packaged in accordance with GOST 15846.

3.3 Marking

3.3.1 It is necessary that the labeling of azo dyes meets the requirements established

3.3.2 Transport marking must comply with the requirements established in with the application of handling signs in accordance with GOST 14192.

4 Safety requirements

4.1 According to the degree of impact on the human body, in accordance with GOST 12.1.007, aerodyes are classified as moderately hazardous substances - the third hazard class.

4.2 Aero dyes are classified as combustible materials according to GOST 12.1.044.

4.3 When working with aerodyes, it is necessary to use overalls, personal protective equipment according to GOST 12.4.011 and follow the rules of personal hygiene.

4.4 When conducting analyzes, it is necessary to comply with safety requirements when working with chemical reagents in accordance with GOST 12.1.007 and GOST 12.4.103.

4.5 Organization of training of workers in labor safety - according to GOST 12.0.004.

4.6 Production premises where work is carried out with azo dyes, and premises where work is carried out with reagents, must be equipped with supply and exhaust ventilation in accordance with GOST 12.4.021.

4.7 Electrical safety when working with electrical installations - according to GOST 12.2.007.0 and GOST R 12.1.019.

4.8 The laboratory room must comply with the fire safety requirements in accordance with GOST 12.1.004 and have fire extinguishing equipment in accordance with GOST 12.4.009.

5 Acceptance rules

5.1 Azo dyes are accepted in batches.

A batch is considered to be the number of azo dyes of the same name, manufactured in one technological cycle, in the same package, received by one manufacturer in one document, accompanied by shipping documentation that ensures product traceability.

5.2 To check the compliance of azo dyes with the requirements of this standard, acceptance tests are carried out for the quality of packaging, correct labeling, net weight, organoleptic and physico-chemical indicators and periodic tests for indicators that ensure safety.

5.3 When conducting acceptance tests, a one-stage sampling plan is used with normal inspection, special inspection level S-4 and an acceptable quality level AQL. equal to 6.5. according to GOST R ISO 2859-1.

The sampling of packaging units is carried out by random selection in accordance with table 6.

Table 6

5.4 The quality control of the packaging and the correctness of the labeling is carried out by an external inspection of all packaging units included in the sample.

5.5 The net weight of azo dyes in each packaging unit included in the sample is controlled by the difference between the gross mass and the mass of the packaging unit freed from the contents. The limit of permissible negative deviations from the nominal net weight of azo dyes in each packaging unit - according to 3.2.6.

5.6 Lot acceptance of azo dyes in terms of net weight, packaging quality and correctness

packaging unit markings

5.6.1 The batch is accepted if the number of packaging units in the sample does not meet the requirements for packaging quality, correct labeling and net weight of azo dyes. less than or equal to the acceptance number (see table 6).

5.6.2 If the number of packaging units in the sample does not meet the requirements for packaging quality, correct labeling and net weight of azo dyes. greater than or equal to the rejection number (see table 6). control is carried out on twice the sample size from the same batch. The lot is accepted if the conditions of 5.6.1 are met.

A batch is rejected if the number of packaging units in twice the sample size that do not meet the requirements for packaging quality, correct labeling and net weight of azo dyes is greater than or equal to the rejection number.

5.7 Acceptance of a batch of azo dyes for organoleptic and physico-chemical

indicators

5.7.1 To control the organoleptic and physico-chemical parameters of aerodyes, from each packaging unit bursting into a sample in accordance with the requirements of Table 6, instantaneous sampling is carried out and a total sample is compiled according to 6.1.

5.7.2 If unsatisfactory results are obtained for at least one of the organoleptic or physico-chemical indicators, a second control is carried out for this indicator on a double sample size from the same batch. The retest results are final and apply to the entire batch.

If unsatisfactory results are obtained during re-inspection, the batch is rejected.

5.7.3 The organoleptic and physico-chemical characteristics of aerodyes in damaged packaging are checked separately. The control results apply only to azo dyes in this package.

5.8 The procedure and frequency of control of safety indicators (the content of arsenic, lead, mercury, cadmium) is established by the manufacturer in the production control program.

6 Control methods

6.1 Sampling

6.1.1 To compile a total sample of aerocolorants from different locations in each packaging unit. selected according to 5.3, take instant samples using a sampler (probe), immersing it at least 3/4 of the depth.

The mass of the instant sample should not exceed 10 g.

The mass of the instant sample and the number of instant samples from each packaging unit included in the sample must be the same.

6.1.2 Instant samples are placed in a dry, clean glass or plastic container and mixed thoroughly.

6.1.3 If it is necessary to reduce the total sample, the quartering method may be used. To do this, the total sample is poured onto a clean table and leveled with a thin layer in the form of a square. Then it is poured with wooden planks with beveled ribs from two opposite sides to the middle like this. to form a ridge. The total sample from the ends of the roller is also poured into the middle, again leveled in the form of a square with a layer thickness of 1 to 1.5 cm, and the bar is divided diagonally into four triangles. Two opposite parts of the sample are discarded, and the remaining two are connected. mix and again divide into four triangles. The division is repeated as many times as necessary. The duration of the quartering procedure should be kept to a minimum.

6.1.4 For batches of aerodyes of small volumes, a total sample can serve as a laboratory sample, while the total mass of instantaneous samples must be not less than the mass required for testing.

The prepared total sample is divided into two equal parts, which are placed in clean, dry, tightly closed glass or polyethylene containers.

The container with the first part of the total sample is sent to the laboratory for analysis.

The container with the second part of the sample is sealed, sealed and stored for re-control in case of disagreement in assessing the quality and safety of aerodyes.

6.1.5 Sample containers are labeled with the following information:

Full name of the azo dye and its E number;

Name and location of the manufacturer;

Batch number;

Lot net weight;

The number of packaging units in the lot;

date of manufacture;

date of sampling;

Terms and conditions of storage:

Surnames of persons. who took this sample;

Designation of this standard.

6.2 Determination of appearance and color

6.2.1 Essence of the method

The method consists in visual comparison of the color of the azo dye with the color of the control sample of the dye of the given name.

For the control sample, a dye sample of this name is taken, the indicators of which * meet the requirements of ^ B:

6.3.5 Preparing for analysis

6.3.5.1 Preparation of a buffer solution with a solution pH of 7.0 units. pH

Solution 1. A solution of disubstituted sodium phosphate with a molar concentration of (Na 2 HP0 4) - 0.2 mol / dm 3 is prepared according to GOST 4919.2.

Solution 2. A solution of potassium phosphate one-substituted molar concentration c (KH 2 RO d) - 0.2 mol / dm 3 is prepared by LOGOST 4919.2.

Buffer solution with a solution pH of 7.0 units. pH is prepared according to GOST 4919.2 in a 100 cm 3 flask by diluting 32.0 cm 3 of solution 1 and 18 cm 3 of solution 2 with distilled water to a volume of 100 cm 3 .

6.3.5.2 Preparation of azo dye solutions

In a glass with a capacity of 50 cm 3 weigh 0.25 g of the control azo dye with the result recorded to the fourth decimal place. Then add 20 cm 3 of distilled water or buffer solution no. 6.3.5.1 to the beaker. in accordance with table 4. and stir with a glass rod until completely dissolved. To intensify the dissolution, it is allowed to heat the solution in a glass in a water bath to a temperature not exceeding 90 °C. Then the solution is cooled to (20 ± 1) "C. transferred quantitatively into a volumetric flask (with a ground stopper) with a capacity of 250 cm 3, the volume of the solution in the flask is adjusted with the same solvent, the flask is closed with a stopper and thoroughly mixed (solution A).

Pipette 10 cm 3 of solution A and transfer it to a volumetric flask (with a ground stopper) with a capacity of 100 cm 3 . Bring the volume of the solution in the flask to the mark with the same solvent, close the flask with a stopper and mix thoroughly (solution B).

10 cm 3 of solution B are taken with a pipette and transferred to a volumetric flask (with a ground stopper) with a capacity of 100 cm o.e. Bring the volume of the solution in the flask to the mark with the same solvent, close the flask with a stopper and mix thoroughly (solution B).

6.3.5.3 Preparation of solutions of analyzed azo dyes is carried out according to 6.3.5.2.

6.3.6 Conducting analysis

The prepared solutions of the control azo dye (solution 8 no 6.3.5.2) and the analyzed aeo dye (solution B according to 6.3.5.3) are dosed with a pipette into the cuvettes of the spectrophotometer and the absorption spectra are recorded relative to the optical density of distilled water in the wavelength range from 350 to 700 nm in accordance with the instructions for the operation of the spectrophotometer.

The absorption spectra of the control and analyzed azo dyes should be identical, and the wavelength corresponding to the maximum absorption of the analyzed azo dye. must match the wavelength corresponding to the maximum light absorption of the control azo dye (see table 4).

6.4 Determination of the mass fraction of the main colorant of the aerocolor

6.4.1 Method essence

The method is based on determining the mass fraction of the main coloring matter of the azo dye by measuring the color intensity of its solution by the spectrophotometric method at a wavelength corresponding to the maximum light absorption of the azo dye of this name according to Table 4.

6.4.2 Measuring instruments, auxiliary equipment, reagents and materials

For analysis, you should use measuring instruments, auxiliary equipment. reagents and materials according to 6.3.2.

6.4.3 Sampling - step 1.

6.4.4 Analysis conditions

When preparing and conducting a measurement, the following conditions must be met:

Ambient air temperature ........... from 10 * C to 35 * C;

Relative Humidity .............. 40% to 95%:

Mains voltage ..................220*]" £ V:

The frequency of the current in the mains .................. from 49 to 51 Hz.

6.4.5 Preparation for analysis according to 6.3.5.

6.4.6 Conducting analysis

The cuvette of the spectrophotometer is filled with the solution of the analyzed azo dye prepared according to 6.3.5.3 and the optical density is measured at a wavelength corresponding to the maximum light absorption relative to the optical density of the solvent (see Table 4).

The optical density of the analyzed dye solution should be in the range from 0.3 to 0.7 units. about. l.

6.4.7 Processing and presentation of measurement results

Mass fraction of the main coloring matter in the analyzed aerodye X.%. calculated according to the formula

where 4 is the optical density of the solution of the analyzed azo dye according to p. 3.5.3. measured under conditions. indicated in table 4;

V is the volume of Apo6.3.5.3 solution, cm e; V- 250cm;

V, is the volume of solution B according to 6.3.5.3. cm 3; V, \u003d 100 cm 3;

V 2 - the volume of solution A. taken for the preparation of solution B according to 6.3.5.3. cm 3;

V 3 - volume of solution B according to 6.3.5.3, cm 3; \u003d 100 cm 3;

V i - the volume of solution B. taken for the preparation of the solution in no 6.3.5.3. cm 3;

V 4 - 10 cm 3;

Specific coefficient of light absorption in accordance with table 4. numerically equal to the optical density of the dye solution, with a mass fraction of the dye 1% (1 g / 100 cm 3) with an absorbing layer thickness of 1 cm% - 1 - cm - 1; d is the thickness of the absorbing layer, cm; d - 1 cm;

m - mass of the analyzed azo dye sample taken for analysis, g, no 6.3.5.3.

6.4.8 Checking the accuracy of measurement results

For the final result of the determinations, the arithmetic mean of two parallel determinations X ev, % is taken. rounded to the first decimal place if the eligibility conditions are met; the absolute value of the difference between the results of two determinations obtained under repeatability conditions at P - 95%. does not exceed the repeatability limit r - 0.60%.

The absolute value of the difference between the results of two determinations obtained under reproducibility conditions at P * 95% does not exceed the reproducibility limit R - 1.20%.

The limits of the absolute error of the method for determining the mass fraction of azo dye is ±0.6% at Р* 95%.

6.5 Determination of the mass fraction of substances insoluble in water

6.5.1 Sampling - according to 6.1.

6.5.2 The mass fraction of substances insoluble in water is determined according to GOST 16922 (see 1.1), while a sample of azo dye weighing (5.0 ± 0.5) g is taken for analysis.

6.6 Determination of the mass fraction of substances extractable with ether

6.6.1 Method essence

The method is based on the extraction of substances soluble in ether, the distillation of the ether at a temperature of (55 ± 5) ® C and the determination of the mass of the dry residue.

6.6.2 Measuring instruments, auxiliary equipment, utensils, reagents and materials Scales with a standard deviation (RMS) not exceeding 0.3 mg. and with

non-linearity error i0.6 mg.

Thermometer liquid glass with temperature measurement range from 0 ®С to 150 ®С. price division 1 * C according to GOST 28498.

Electronic-mechanical clock according to GOST 27752.

Electric stove according to GOST 14919.

Drying cabinet providing maintenance of the set temperature mode from 20 *С to 150 ®С with an error of ±2 ®С.

Desiccator 2-100 according to GOST 25336 with calcium chloride, previously calcined at a temperature of (300150) * C for 2 hours.

Soxhlet extractor, consisting of a nozzle for extracting NET-100 TS according to GOST 25336, a refrigerator ХШ-1-200-14/23ХС according to GOST 25336 and a flask K-1-50-14/23 TS according to GOST 25336 with interchangeable polished joints.

Installation for distillation of the solvent, consisting of a nozzle H1 > 19/26 * 14/23 TS lo GOST 25336, refrigerator KhPT-1-100-14/23 XC according to GOST 25336. allonge AKP-14/23-14/23 TS lo GOST 25336 and receiving flask K*1*250*29/32 TS lo GOST 25336 with interchangeable ground joints.

Cylinder 1-50*1 according to GOST 1770.

Filter paper according to GOST 12026.

Glycerin bath.

Diethyl ether. dried over sodium sulfate or calcium chloride.

Glycerin according to GOST 6259.

6.6.3 Sample selection - step 1.

6.6.4 Analysis conditions

When preparing and conducting a measurement, the following conditions must be observed:

Ambient temperature ........... from 20°C to 25*C:

Relative Humidity .............. 40% to 90%:

Voltage in the mains .............. 220 *] "* V;

The frequency of the current in the mains .................. from 49 to 51 Hz.

The room where work with reagents is carried out must be provided with supply and exhaust ventilation*.

All handling of reagents should be carried out in a fume hood.

6.6.5 Preparing for analysis

6.6.5.1 Preparing the Soxhlet Extractor

The flask for the Soxhlet extractor is dried in an oven at a temperature of (120 ± 5) * C for 2 hours, then cooled in a desiccator for 40 minutes and weighed with a record of the weighing result to the third decimal place. The drying of the flask is continued until until the difference between the results of two consecutive determinations is less than 0.001.

The filtering paper is weighed with bg of the analyzed azo dye, recording the result up to the third decimal place. Then roll up the filter paper with the air stain in the form of a cartridge and place the cartridge in the extraction nozzle.

6.6.5.2 Preparing the stripper

Assemble the installation for the distillation of the solvent, connecting the nozzle in series with a refrigerator * com. and a refrigerator with a receiving flask through the allonge.

6.6.6 Conducting analysis

Extraction nozzle with an air dye cartridge placed in it. connect with a cleat prepared according to p.6.5.1. 40 cm 3 of diethyl ether are poured into it and the extraction nozzle is connected to the refrigerator. The flask is placed in a glycerol bath heated to a temperature of (55 ± 5) * C, which ensures uniform moderate boiling of diethyl ether. The extraction is carried out for 5 hours, after which the flask is separated from the nozzle for extraction, connected to the nozzle of the installation for distillation of the solvent, and placed in a glycerol bath heated to a temperature of (55 ± 5) °C. The contents of the flask are evaporated to dryness, after which they are dried in an oven at a temperature of (100 ± 2) * C for 1 hour, then cooled in a desiccator for 40 minutes and weighed, recording the weighing result to the fourth decimal place. The drying of the flask is continued until until the difference between the results of two successive determinations is less than 0.001 g.

6.6.7 Processing and presentation of measurement results

Mass fraction of substances extractable with ether X, %. calculated according to the formula

x=M! __M L i (3)

where M, is the mass of the flask with the dry residue of substances extracted with ether, g;

M 2 is the mass of an empty flask, g.

M is the mass of the azo dye sample lo 6.6.5.1. G.

Calculations are carried out with the result recorded to the third decimal place.

6.6.6 Checking the accuracy of measurement results

For the final result of the determinations, the arithmetic mean of two parallel determinations is taken, Xp,%. rounded up to the second decimal enac. if the acceptance conditions are met: the absolute value of the difference between the results of two determinations obtained under repeatability conditions at P-95%. does not exceed the repeatability limit r = 0.020%

The absolute value of the difference between the results of two determinations obtained under conditions of reproducibility at P - 95%. does not exceed the reproducibility limit R = 0.030%.

The limits of the absolute error of the method for determining substances extractable with ether J.O.02% at P-95%.

6.7 Determination of the mass fraction of associated colorants

6.7.1 Method essence

The method is based on the separation of the main and accompanying coloring substances of azo dyes by chromatography on paper, extraction of the obtained chromatographic zones. corresponding to the main and accompanying coloring substances, and determining the optical density of extracts at wavelengths corresponding to the light absorption maxima of the main and accompanying coloring substances.

The specific coefficients of light absorption of the main and accompanying coloring substances are assumed to be equal.

6.7.2 Measuring instruments, auxiliary equipment, glassware, reagents and materials

Scales with the value of the standard deviation (RMS). not exceeding 0.3 mg. and with

non-linearity error i0.6 mg.

Liquid glass thermometer with temperature measurement range from 0 *С to 100 °С. price division 1 ® C according to GOST 28498.

Spectrophotometer with a measurement range in the wavelength range from 350 to 700 nm. permissible absolute error of the transmittance is not more than 1%.

Quartz cuvettes with an absorbing layer thickness of 1 cm.

Chromatographic chamber with cover.

Electric stove according to GOST 14919.

Bath water.

Drying cabinet that maintains the specified temperature regime from 20 *C to 100 *C with an error of ±2 *C.

Microsyringe with a capacity of 0.1 cm 3 with a division price of not more than 0.002 cm 3.

Pipettes graduated according to GOST 29227 with a capacity of 1.5.10 cm 3 of the first accuracy class.

Volumetric flasks with ground stoppers with a capacity of 50.100 cm 3 of the first accuracy class according to GOST 1770.

Cups for weighing SV-19/9 (24/10) or SN-34/12 according to GOST 25336.

Glass V(N)-1-100 TC(TXC) according to GOST 25336.

Glass stick.

Chromatographic paper with a size of at least 20 x 20 cm.

Laboratory filter paper FOB-HI according to GOST 12026.

Azo dyes in accordance with 3.1.

Distilled water according to GOST 6709.

Ammonia water in accordance with GOST 3760. h. d. a., solution of mass concentration 250 g / dm 3.

Acetone according to GOST 2603.

Acetic acid according to GOST 61. x. h. glacial, solution with a mass fraction of acetic acid 3%; prepared according to GOST 4517.

Sodium citrate 5.5-aqueous according to GOST 22280. h.

Rectified technical ethyl alcohol of the highest grade according to GOST 18300.

Butanol-1 according to GOST 6006. analytical grade.

Isobutyl alcohol according to GOST 6016.

Sodium carbonate acid according to GOST 4201. analytical grade.

Prolyl alcohol. X. h.

Ethyl acetate according to GOST 22300.

Acid sodium carbonate according to GOST 4201. analytical grade, solution of mass concentration 4.2 g/dm 3 .

It is allowed to use other measuring instruments in terms of metrological and technical characteristics and reagents in quality that are not inferior to the above and provide the necessary accuracy of determination.

6.7.3 Sampling - front.1.

6.7.4 Conditions for the analysis - lob.6.4.

6.7.5 Preparing for analysis

6.7.5.1 Preparation of eluent Preparation of eluent 1

6 cm 3 distilled water, 2 cm 3 ethyl acetate and 12 cm 3 prolyl slirt. The flask is closed with a glass stopper and mixed thoroughly.

Preparation of eluent 2

In a volumetric flask with a capacity of 50 cm 3, pipettes are added, individual for each reagent,

7 cm 3 isobutyl alcohol, 7 cm 3 ethyl alcohol and 7 cm 3 distilled water. The flask is closed with a glass stopper and mixed thoroughly.

The solution is used freshly prepared.

Preparation of eluent 3

In a volumetric flask with a capacity of 50 cm 3 make pipettes, individual for each reagent. 12 cm 3 butyl alcohol. 4 cm 3 of ethyl alcohol and 6 cm 3 of a solution of acetic acid with a mass concentration of 3 g / dm 3. The flask is closed with a glass stopper and mixed thoroughly.

The solution is used freshly prepared.

Preparation of eluent 4

In a volumetric flask with a capacity of 50 cm 3 make pipettes, individual for each reagent.

8 cm 3 prolilac slirt. 6 cm 3 ethyl acetate and 6 cm 3 distilled water. The flask is closed with a glass stopper and mixed thoroughly.

The solution is used freshly prepared.

Preparation of eluent 5

In a volumetric flask with a capacity of 50 cm 3 add pipettes, individual for each reagent, 8 cm 3 of butyl alcohol, 2 cm 3 of glacial acetic acid and 10 cm 3 of distilled water. The flask is closed with a glass stopper and mixed thoroughly.

The solution is used freshly prepared.

Preparation of eluent 6

In a volumetric flask with a capacity of 50 cm 3 make pipettes, individual for each reagent. 10 cm 3 butyl alcohol. 2.25 cm 3 of ethyl alcohol, 4.4 cm 3 of distilled water and 0.1 cm 3 of aqueous ammonia. The flask is closed with a glass stopper and mixed thoroughly.

The solution is used freshly prepared.

6.7.5.2 Extractant preparation

In a volumetric flask (with a ground stopper) with a capacity of 50 cm 3, pipettes are added, individual for each reagent, 10 cm 3 of acetone and 10 cm 3 of distilled water. The flask is closed with a glass stopper and mixed thoroughly.

The solution is used freshly prepared.

6.7.6 Preparation of azo dye solutions

In a glass with a capacity of 50 cm 3 weigh 0.5000 g of the control azo dye in accordance with table 5. Then add 20 cm 3 of distilled water and stir with a glass rod until completely dissolved. To intensify the dissolution, it is allowed to heat the solution in a beaker in a water bath to a temperature not exceeding 90 °C. Then the solution is cooled to a temperature of (20 ± 1) °C, quantitatively transferred into a volumetric flask (with a ground stopper) with a capacity of 100 cm 3, the volume of the solution in the flask is adjusted to the mark with distilled water, the flask is closed with a stopper and thoroughly mixed.

Mass fraction of the control dye in the resulting solution C, = 1%.

6.7.7 Preparation of solutions of analyzed azo dyes

In a beaker with a capacity of 50 cm 3 weigh 0.5000 g of the analyzed azo dye. Then add 20 cm 3 of distilled water and stir with a glass rod until completely dissolved. To intensify the dissolution, it is allowed to heat the solution in a beaker in a water bath to a temperature not exceeding 90 °C. Then the solution is cooled to a temperature of (20 ± 1) *C. transfer quantitatively into a volumetric flask (with a ground stopper) with a capacity of 100 cm 3, bring the volume of the solution in the flask to the mark with distilled water, close the flask with a stopper and mix thoroughly. Mass fraction of the analyzed dye in the resulting solution C l * 1%.

6.7.8 Preparation of the chromatographic chamber - according to GOST 28365.

6.7.9 Preparing the chromatography paper

Chromatographic paper is prepared according to GOST 28365 by applying to the start line in the form of strips of 0.1 cm 3 solutions of the control and analyzed azo dyes with a distance between them of at least 20 mm.

6.7.10 Conducting analysis

The analysis is carried out according to GOST 28365 using any of the eluents. prepared according to 6.7.5.1. Elution is completed when the eluent reaches 18 cm from the start line. At the end of the elution, the chromatogram is taken out with tweezers, dried in an oven at a temperature of (55 ± 5) °C for 15 min. cool and cut out the colored zones corresponding to the main coloring substance of the control azo dye and the accompanying coloring substances of the analyzed azo dye.

At the same time, uncolored zones of the chromatographic paper are cut out, equal in area to the corresponding colored zones.

The zones cut out from the chromatogram are placed in four individual beakers with a capacity of 50 cm 3 . In the first glass - the zones corresponding to the accompanying coloring substances in the analyzed aerodye (solution 1). in the second - the zone corresponding to the main coloring matter of the control dye (solution 2). in the third - unstained zones, equal in area to the zones of accompanying coloring substances of the analyzed azo dye (solution 3), in the fourth - unstained zone, equal in area to the zone of the main coloring matter of the analyzed azo dye (solution 4). Then add 5 ml of the extractant prepared according to 67.5.2 to each beaker by pipette and shake for 3 minutes. then 15 cm 3 of a solution of sodium hydrogen carbonate is added to each glass with a pipette, shaken, the obtained extracts are filtered through paper filters into quartz cuvettes.

The optical densities of the obtained filtrates are determined at a wavelength corresponding to the maximum light absorption in accordance with Table 4. Using the corresponding uncolored filtrates as reference solutions (solution 1 against solution 3 and solution 2 against solution 4).

6.7.11 Processing and presentation of measurement results

Mass fraction of accompanying coloring substances in the analyzed aerodye X 2 , %. calculated according to the formula

where C is the mass fraction of colorants in the analyzed aerodye according to 6.4. %;

A c - optical density of the associated dyes of the analyzed aero dye according to 6.7.10 (solution 1);

A a - optical density of the solution of the main coloring matter of the control azo dye according to

6.7.10 (solution 2).

Calculations are carried out with the result recorded to the second decimal place.

6.7.12 Checking the accuracy of measurement results

The final result of the determinations is taken as the arithmetic mean of two parallel determinations X 3<р, %. округленное до первого десятичного знака, если выполняются условия приемлемости: абсолютное значение разности между результатами двух определений, полученными вусловиях повторяемости при Р - 95%, не превышает предела повторяемости г - 0.02 %.

The absolute value of the difference between the results of two determinations obtained under conditions of reproducibility at P = 95%. does not exceed the reproducibility limit R - 0.03%.

The limits of the absolute error of the method for determining the mass fraction of accompanying coloring substances in the analyzed aerodye is 10.2% at P = 95%.

6.8 Determination of the mass fraction of non-sulfonated primary aromatic amines

6.8.1 Method essence

The method is based on the extraction of non-sulfonated primary aromatic amines from an alkaline solution of an aerodye with toluene, re-extraction from toluene into hydrochloric acid, subsequent diazotization with sodium nitrite, combination with 2-naphthol-6-sulfonic acid, and spectrophotometric measurement of the optical density of the obtained colored compounds.

6.8.2 Measuring instruments, auxiliary equipment, glassware, reagents and materials

Scales in accordance with GOST R 53228. providing weighing accuracy with the limits of the absolute permissible error iO, 1 g.

Scales with the value of the standard deviation (RMS). not exceeding 0.3 mg. and an error from non-linearity of ±0.6 mg.

Liquid glass thermometer with temperature measurement range from O *C to 100 *C. division price 1 * C according to GOST 28498.

Electronic-mechanical clock according to GOST 27752.

Spectrophotometer with a measurement range in the wavelength range from 350 to 700 nm. permissible absolute error of the transmittance is not more than 1%.

Quartz cuvettes with an absorbing layer thickness of 4 cm.

Electric stove according to GOST 14919.

Bath water.

Pipettes graduated according to GOST 29227 with a capacity of 0.5.1.10 cm 3 of the 1st accuracy class.

Pipettes with one mark according to GOST 29169 with a capacity of 5.10.15.20.25 cm 3 of the 1st accuracy class.

Funnel VD-1-250 XC according to GOST 25336.

Flask Kn-2-250-40 TLC according to GOST 25336.

Flask Kn-1-100-18 TLC according to GOST 25336.

Volumetric flasks with ground stoppers with a capacity of 25.100 cm 3 of the 1st accuracy class according to GOST 1770.

Glass B (H> -1 -100 TC (TXC) according to GOST 25336.

Glass stick.

Distilled water according to GOST 6709.

Hydrochloric acid according to GOST 3118. x. h.

Potassium bromide according to GOST 4160, x. h.

Sodium carbonate according to GOST 83. h.

Sodium hydroxide according to GOST 4328. analytical grade.

Sodium nitrous acid according to GOST 4197, analytical grade.

Aniline according to GOST 5819. analytical grade, boiling point from 183 * C to 185 ® C.

2-naphthol-3.6-disulfonic acid disodium salt (Schaeffer's salt), analytical grade

It is allowed to use other measuring instruments, in terms of metrological and technical characteristics and reagents in quality, that are not inferior to the above and provide the necessary accuracy of determination.

6.8.3 Sampling - according to 6.1.

6.8.4 Conditions for the analysis - according to 6.6.4.

6.8.5 Preparing for analysis

6.8.5.1 A solution of hydrochloric acid with a molar concentration of (HC!) -1 mol / dm 3 is prepared according to GOST 25794.1.

6 8.5.2 A solution of hydrochloric acid with a molar concentration with (HC!) = 3 mol / dm 3 is prepared according to GOST 25794.1 in a flask with a capacity of 1000 cm 3 by diluting 270.0 cm 3 of hydrochloric acid with a density of 1.174 g / cm 3 or 255.0 cm 3 of hydrochloric acid with a density of 1.188 g / cm 3 with distilled water up to a volume of 1000 cm 3.

The solution is stored at a temperature of (20 ± 2) *C for 1 month.

6.6.5.3 Preparation of a solution of potassium bromide with a mass fraction of 50%

Potassium bromide weighing 10 g is dissolved in 10 cm 3 of distilled water in a flask with a capacity of 100 cm 3.

The solution is used freshly prepared.

6.6.5.4 Preparation of sodium carbonate solution with molar concentration c(Na ; C0 3) = = 1 mol/dm 3

Sodium carbonate weighing 106 g is placed in a volumetric flask with a capacity of 1000 cm 3 . dissolved in 300 cm 3 of distilled water, bring the volume to the mark with distilled water and mix.

The solution is stored at a temperature of (20 ± 2) *C for 1 month.

6.6.5.5 A solution of sodium hydroxide with a molar concentration of (NaOH) = 1 mol/dm 3 is prepared according to GOST 25794.1.

The solution is stored at a temperature of (20 ± 2) *C for 1 month.

6.8.5.6 Sodium hydroxide solution of molar concentration c (NaOH) = 0.1 mol/dm 3 is prepared according to GOST 25794.1.

The solution is stored at a temperature of (20 ± 2) *C for 1 month.

6.8.5J A solution of sodium nitrite with a molar concentration of (NaN0 2) = 0.5 mol/dm 3 is prepared according to GOST 25794.1.

The solution is used freshly prepared.

6.8.5.8 Preparation of a solution of 2-naphthol-3,6-disulfonic acid disodium salt (Scheffer's salt)

The disodium salt of 2-naphthol-3,6-disulfonic acid (Scheffer's salt) weighing 15.2 g is placed in a volumetric flask with a capacity of 1000 cm 3, dissolved in 300 cm 3 of distilled water, the volume is adjusted to the mark with distilled water and mixed.

The solution is used freshly prepared.

6.8.5.9 Preparation of aniline solution

Aniline weighing 0.1000 g is placed in a volumetric flask with a capacity of 100 cm 3, 30 cm 3 of a hydrochloric acid solution prepared according to 6.8.5.2 is added. dilute to the mark with distilled water and mix thoroughly (solution A).

10 cm 3 of solution A are placed in a volumetric flask with a ground stopper with a capacity of 100 cm 3 . Bring the volume of the solution in the flask to the mark with distilled water, stopper the flask and mix thoroughly (solution 5). 1 cm 3 of solution B contains 0.0001 g of aniline.

The solution is used freshly prepared.

6.8.5.10 Into a flask with a capacity of 250 cm 3 add 10 cm 3 of a solution of 2-caphthol-3.6-disulfonic acid disodium salt (Scheffer's salt) according to 6.8.5.8. add 100 ml of sodium carbonate solution according to 6.8.5.4 and mix thoroughly (solution C).

The solution is used freshly prepared.

6.8.5.11 Preparation of reference solution

In a volumetric flask with a capacity of 25 cm 3, add 10 cm 3 of hydrochloric acid solution according to p. 8.5.1. add 10 cm 3 of sodium carbonate solution according to 6.8.5.4 and 2 cm 3 of 2-naphthol-3.b-di-sulfonic acid disodium salt solution (Schaeffer's salt) no. 6.8.S.8. dilute the volume of the solution in the flask to the mark with distilled water and mix thoroughly.

6.8.6 Building a calibration curve

8 each volumetric flask with a capacity of 100 cm 3 contribute, respectively, 5.10.15.20.25 cm 3 of solution B according to 6.8.5.E. Dilute the volume in each flask to the mark with the hydrochloric acid solution of 6.8.5.1 and mix thoroughly.

From each flask, 10 cm 3 of the solution are taken and added to dry volumetric flasks with a capacity of 25 cm 3, the flasks are placed in an ice bath and cooled for 10 minutes. Then, 1 cm 3 of a solution of potassium bromide no. 6.8.5.3 and 0.05 cm 3 of a solution of sodium nitrate according to clause 8.5.7 are added to each flask, after which they are mixed. The flasks are kept in an ice bath for Yumin. Then add 11 ml of solution C according to 6.8.5.10 to each flask. Then bring the volume in each kobbe to the mark with distilled water, stopper, mix thoroughly and place in a dark place for 15 minutes. after which the optical density of the solutions is measured on a spectrophotometer at a wavelength of 510 nm against the reference solution according to 6.8.5.11.

The calibration dependence is built by plotting the content of aniline (g) in grading solutions along the abscissa axis, and the corresponding values ​​of the measured optical density along the ordinate axis.

6.8.7 Conducting analysis

8 glass with a capacity of 100 cm 3 weigh 2.0000 g of the analyzed azo dye. Then add 50 cm 3 of distilled water and stir with a glass rod until complete dissolution. To intensify dissolution, it is allowed to heat the solution in a beaker in a water bath to a temperature not exceeding 90 °C.

Then the solution is cooled to a temperature of (20 ± 1) *C. transfer quantitatively to a separating funnel using 50 cm 3 of distilled water, add 5 cm 3 of sodium hydroxide solution in 6.8.5.5.50 cm 3 of toluene and shake vigorously for (5 ± 1) minutes.

After phase separation, the upper toluene layer is transferred to a flask with a capacity of 250 cm 3 and the procedure is repeated, adding 50 cm 3 of toluene to the aqueous layer remaining in the separating funnel. The lower aqueous layer is then discarded and the resulting toluene extracts are combined in a separating funnel.

8 separating funnel with combined toluene extract, add 10 cm 3 of sodium hydroxide solution according to step 8.5.6 and shake vigorously for (5 ± 1) min. After phase separation, the lower layer is discarded. Repeat the washing procedure until a colorless bottom layer is obtained in a separating funnel.

Then add 10 ml of hydrochloric acid solution according to 6.8.5.2 to the separating funnel with the washed toluene extract and shake vigorously for (5 ± 1) min. After phase separation, the bottom layer is transferred to a 100 cm 3 volumetric flask. The procedure is repeated two more times.

after which the volume in the flask is adjusted to the mark with distilled water and mixed thoroughly (solution D).

10 cm 3 of solution E are added to a 25 cm 3 volumetric flask, the flask is placed in an ice bath and cooled for 10 minutes. Then add 1 cm 3 of potassium bromide solution according to 6.8.5.3 and 0.05 cm 3 of sodium nitrite solution according to 6.8.5 7. then mix. The flask was kept in an ice bath for Yumin. Then add 11 cm 3 of solution C forehead.8.5.10. bring the volume to the mark with distilled water, stopper, mix thoroughly and place in a dark place for 15 minutes. Measure the optical density of the solution on a spectrophotometer at a wavelength of 510 nm against reference solution no 6.8.5.11.

According to the calibration dependence, the amount of aniline is found.

6.8.8 Processing and presentation of measurement results

Mass fraction of lervic nonsulfonated aromatic amines X 3 %. calculated according to the formula

X 3 \u003d ^-100.< 5 »

where K is the amount of primary non-sulfonated aromatic amines (aniline) found from the calibration curve, g;

100 is the coefficient for converting the result into percentages: t is the mass of the aerodye sample according to 6.8.7, g.

Calculations are carried out with the result recorded to the fourth decimal place.

6.8.9 Checking the accuracy of measurement results

For the final result of the determinations, the arithmetic mean of two parallel determinations X^, %, is taken. rounded to the third decimal place if the acceptance conditions are met: the absolute value of the difference between the results of two determinations obtained under repeatability conditions at P - 95%. does not exceed the repeatability limit r - 0.0010%.

The absolute value of the difference between the results of two determinations obtained under reproducibility conditions at P - 95% does not exceed the reproducibility limit R - 0.0020%.

The limits of the absolute error of the method for determining substances extracted by ether

10.001% at P = 95%.

6.9 Determination of the mass fraction of loss on drying

6.9.1 Method essence

The method is based on the thermogravimetric determination of losses during drying of azo dyes to constant weight.

6.9.2 Measuring instruments, auxiliary equipment, glassware, reagents and materials

Scales with a standard deviation (RMS) value not exceeding 0.3 mg. and

non-linearity error 10.6 mg.

Liquid glass thermometer with a temperature measurement range from 0 * C to 200 ® C, division value 1 in C according to GOST 28498.

Electronic-mechanical clock according to GOST 27752.

Drying cabinet, providing maintenance of the specified temperature regime from 20 C to 150 ®C. error ±2 *С.

Desiccator 2-100 according to GOST 25336 with calcium chloride, pre-calcined at a temperature of (300 ± 50) ® C for 2 hours.

Cups for weighing SV-19/9 (24/10) or SN-34/12 according to GOST 25336.

Calcium chloride according to GOST 450.

It is allowed to use other measuring instruments in terms of metrological and technical characteristics and reagents in quality that are not inferior to the above and provide the necessary accuracy of determination.

6.9.3 Sampling - according to 6.1.

6.9.4 Conditions for the analysis - according to 6.3.4.

6.9.5 Conducting analysis

An open glass cup with a lid is placed in an oven heated to a temperature of 135 °C and kept for 1 hour. Then the cup is closed with a lid, placed in a desiccator, cooled to a temperature of (20 ± 2) * C and weighed.

Drying the glass with a lid is repeated under the same conditions until lor. until the difference between the results of two successive weighings is no more than 0.0001 g.

Then, 2,000 g of a sample is added to the beaker, weighed, placed open together with the lid in an oven and dried for 4 hours at a temperature of 135°C. Then the beaker with the sample is closed with a lid, placed in a desiccator, cooled to a temperature of (20 ± 2) *C and weighed.

Drying of the beaker with the sample under the same conditions is continued until then. until the difference between the results of two consecutive weighings is no more than 0.0001 g.

6.9.6 Processing and presentation of measurement results Mass fraction of losses during drying X 4 . %. calculated according to the formula

Y 4 a 10Q | (b)

where m is the mass of a dry cup, g

t, - mass of the glass with the sample before drying, n t 2 - weight of the glass with the sample after drying, g;

100 - coefficient for converting the result into a percentage.

calculations are carried out with the result recorded to the second decimal place.

The final result is recorded to the first decimal place.

6.9.7 Checking the accuracy of measurement results

The arithmetic mean X 4ce is taken as the final result of the determination. %. two parallel determinations of the mass fraction of loss on drying, obtained under repeatability conditions, if the acceptance condition is met

(X*m£ ~ Xin)100/X^ £G, (7)

where X nms is the maximum mass fraction of losses during drying;

X yin - the minimum mass fraction of losses during drying;

X 4ut - the average value of two parallel measurements of the mass fraction of losses during drying;

r is the value of the repeatability limit. %. given in table 7.

The result of the analysis is presented in the form

X"

where X 4 is the arithmetic mean of the results of the two determinations, which were found to be acceptable. %;

5 - limits of relative measurement error. %.

The limit of repeatability r and reproducibility R, as well as the accuracy factor b for measurements of the mass fraction of losses during drying, are presented in Table 7.

Table 7

6.10 Determination of the content of toxic elements:

Arsenic - according to GOST 26930. GOST R 51766;

Lead - according to GOST 26932. GOST 30178;

Cadmium - according to GOST26933, GOST 30178;

Mercury - according to GOST 26927.

7 Transport and storage

7.1 Azo dyes are transported in covered vehicles by all modes of transport in accordance with the rules for the transportation of goods in force for the respective modes of transport.

7.2 Azo dyes are stored in the manufacturer's packaging in dry, heated warehouses on wooden racks or pallets at a temperature of (20 ± 5) * C and a relative air humidity of not more than 60%.

7.3 Transportation and storage of azo dyes together with strong oxidizing agents is not allowed. acids, alkalis, bleaching and strong-smelling chemicals.

7.4 The shelf life of azo dyes is set by the manufacturer.

Bibliography

(1) Technical regulation of the Customs Union TR CU 029/2012 "Safety requirements for food additives, flavors and technological aids"

(2) Technical regulation of the Customs Union TR TS 021/2011 "On food safety"

(3) Technical regulation of the Customs Union TR CU 005/2011 "On the safety of packaging"

(4) Technical regulation of the Customs Union TR CU 022/2011 "Food products in terms of their labeling"

UDC 663.05:006.354 OKS 67.220.20 N91 OKP24 6372

Keywords: food additive, food azo dye, quality and safety indicators, packaging, labeling, acceptance, test methods, transportation and storage

Editor A.V. Pavlov Technical editor VN Prusakova Proofreader UM. Pershina Computer imposition /O-v. Deenina

Handed over to the set 09/22/2014. Signed and stamped 10/17/2014. Format 60 to 94^£ Headset Ariap.

Uel. oven paragraph 2.79. Uch.-ed. paragraph 2.35. Circulation 73 echoes For*. 4299.

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