Specifications and guests as control over the use of food additives. Specifications and GOSTs as control over the use of food additives Determination of the mass fraction of the main substance

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, a new document regulating the use of food additives was put into effect in Russia - 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 food additives that can be used) 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

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 be published in monthly published informational index "National standards". Relevant information, notification and texts are placed also in informational system general use - on the official site 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 packaging, 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 bevelled 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 of distilled water and 32 cm 3 of 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 color change of the solution from red to orange or yellow to orange, respectively, in the presence of methyl orange indicates that 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 weighed sample weighing 4 g with a record of the weighing result 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 buret 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- 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 the 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- 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) = 0.7 mol / dm 3 is prepared as follows: to 980 cm 3 of ethyl alcohol 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 50 cm 3 volumetric flask, diluted with a sulfuric acid solution prepared according to 7.7.1.4 a), to a volume of approximately 45 cm 3 , 1 cm 3 of a solution of tin dichloride 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- 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 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- 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 glass 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 according to 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- 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 the 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.

Weigh a sample weighing from 1 to 2 g in a glass with recording the weighing result to the third decimal place, place it open together with the lid in an oven and dry 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) edible 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.