Home Pulpitis Technical conditions and guest standards as control over the use of food additives. Technical conditions and guests as control over the use of food additives Test for sodium ion

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Technical conditions and guest standards as control over the use of food additives. Technical conditions and guests as control over the use of food additives Test for sodium ion

Statistics from registers of sanitary and epidemiological conclusions of the Russian Ministry of Health indicate that today the market food additives is rapidly developing, constantly replenished with new imported and domestic additives that can change the traditional taste of long-known products. This raises a problem legislative regulation use of food additives. This problem is not new. Humanity has been solving it for centuries, improving 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 introduced in Russia - SanPiN 2.3.2.1293-03 “Hygienic requirements for the use of food additives.”

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

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

The meat industry remains fairly conservative in its use of food additives. Of the 394 E-indices in our industry, about a hundred are allowed for use, but this is only about those allowed. As practice shows, the number of food additives most often used for the production of meat products, which are quite well known to the consumer from the labeling on the packages, is no more than 20 E-indexes.

One of the most important aspects of successful control of food additives is the availability 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 for monitoring the addition of phosphates). In the same row we 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 approved for use in the meat industry, for which the maximum level of their content in meat products has been established, but there are no control methods. An even more pressing issue is the need to develop methods for determining the content of those additives that are prohibited, such as, for example, amaranth dye (E123).

Very often in Lately I hear from specialists at meat processing enterprises proposals for inclusion in national state standards various food additives for meat products. However, few of them think that 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 an even larger scale due to a wider list of food additives possible for use) arises when developing GOSTs such as 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 the minimum amount necessary to achieve the required technological effect, but not more than the maximum permissible level of their content (residual content) in the finished product.

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

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

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

These basic principles guided the institute’s specialists when they developed the first national standard - GOST R 52196-2003 “Cooked sausage products. Technical conditions".

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

Today the standard provides for the use of the following food additives:

1. Paint fixative E250.

2. Flavor and aroma enhancer E621.

3. Acidity regulators E325, E326, E500.

4. Antioxidants E300, E301.

5. Stabilizers, emulsifiers E450-E452.

As you can see, there are not many of them. It is especially worth focusing on sodium nitrite E250. Perhaps today we remain the only country in the world where sodium nitrite (a highly toxic substance) is used in pure form(in the form of solutions) at food enterprises. However, recently there has been some progress in this area: there is an order from the Russian Ministry of Health on the preparation of changes to SanPiN 2.3.1.1293-01, prohibiting the use of nitrites in their pure form. In this regard, curing mixtures were included in the new GOST R 52196-01 “Boiled sausage products”, and currently (for the transition period) our institute has developed “Technological instructions 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 fixative E250).

In order for the requirements of GOST to be met, to support our tasks in developing national standards, primarily for domestic producers, the institute developed a document, TU9199-675-00419779 “Spicy mixtures for boiled sausages”. The document contains 38 names of complex mixtures - flavored and phosphate-containing. However, its inclusion in GOST R does not provide for the introduction of a ban on the use of other complex additives. The specifications are intended for domestic producers of ingredients; they have been purchased by a number of companies.

Since the text of GOST and the text of the technological instructions 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 enshrined in SanPiN, their use should be based on those developed in the prescribed manner technological instructions. Therefore, the institute is now developing such instructions that determine the procedure for using food additives of similar composition.

Returning to the need to develop national standards for methods, it should be especially noted that the use of additives should not be limited in any way artificially. The sole purpose of complying with hygienic regulations on the use of food additives must be pursued, and information about the composition of the product must be correctly communicated to the consumer.

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 must 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 to which the European Union is currently moving. The labeling indicates not only the amount of food additives, but also the amount of raw meat 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 control methods and clear requirements for food product labeling, the use of food additives will not cause unfounded suspicion among the consumer.

FEDERAL AGENCY FOR TECHNICAL REGULATION AND METROLOGY

NATIONAL

STANDARD

RUSSIAN

FEDERATION

Food additives

AZO DYES

Specifications

Official publication

Stand Rtinform 2014

Preface

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

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

3 APPROVED AND ENTERED 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” (clause 3.4) in terms of Specifications for food additives azo dyes E102. E110. E122, E124. E129. E151. E155 of the Unified Code of Specifications for Food Additives of the Joint Expert Committee on Food Additives FAO/WHO “Combined compendium of food additive specification JECFA. Volume 4"

5 8DRIVEN FOR THE FIRST TIME

The rules for applying 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 is published in the monthly information index “National Standards”. In case of revision (replacement) or cancellation of this standard, the corresponding notice will be published in the next issue of the monthly information index “National Standards”. Relevant information, notices and texts are also posted in the information system common use- on the official website of the Federal Agency for Technical Regulation and Metrology on the Internet (gost.ru)

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

NATIONAL STANDARD OF THE RUSSIAN FEDERATION

Food additives AZO DYES Technical specifications Food additives. Azo colors. Specifications

Date of introduction - 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 azo dyes) and intended for use in the food industry.

Note - The term “aero-dyes” reflects common feature included in this standard food additives associated with the presence of an azo group (N ■ N) in their structure.

The quality requirements for aero-dyes 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 type during their production, packaging, sale and import

GOST 12.0.004-90 System of occupational safety standards. Organization of occupational safety training. General provisions

GOST 12.1.004-91 System of occupational safety standards. Fire safety. General requirements

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

GOST 12.1.007-76 System of occupational safety standards. Harmful substances. Classification and general safety requirements

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

GOST 12.2.007.0-75 System of occupational safety standards. Electrical products. General safety requirements

GOST 12.4.009-83 System of occupational safety standards. Fire fighting equipment for the protection of objects. Main types. Accommodation and service

GOST 12.4.011-69 System of occupational safety standards. Protective equipment for workers. General requirements and classification

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

GOST 12.4.103-83 System of occupational safety standards. Special protective clothing, equipment personal protection legs and arms. Classification

Official publication

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

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

GOST 4517-87 Reagents. Methods for preparing auxiliary reagents and solutions used in analysis

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

GOST 5819-78 Reagents. Aniline. Technical specifications GOST 6006-78 Reagents. Butanol-1. Technical specifications GOST 6016-77 Reagents. Isobutyl alcohol. Technical specifications GOST 6259-75 Reagents. Glycerol. Technical 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, dihydrogenated. Technical specifications GOST 12026-76 Laboratory filter paper. Technical specifications GOST 14192-96 Marking of cargo

GOST 14919-83 Household electric stoves, electric stoves and electric frying cabinets. General technical conditions

GOST 14961-91 Linen threads and linen threads with chemical fibers. Technical specifications GOST 15846-2002 Products shipped to the Far North and equivalent areas. Packaging, labeling, 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. Technical specifications GOST 19360-74 Film liner bags. General technical conditions GOST 22280-76 Reagents. Sodium citrate 5.5-water. Technical specifications GOST 22300-76 Reagents. Ethyl and butyl ethers acetic acid. Specifications

GOST 25336-82 Laboratory glassware and equipment. Types, main parameters and sizes

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

GOST 26927-86 Raw materials and food products. Methods for determining mercury GOST 26930-86 Raw materials and food products. Method for determination of arsenic GOST 26932-86 Raw materials and food products. Methods for determination of lead GOST 26933-86 Raw materials and food products. Methods for determining cadmium GOST 27752-88 Electronic-mechanical quartz table, wall and alarm clocks. General technical conditions

GOST 28365-88 Reagents. Paper chromatography method

GOST 28498-90 Liquid-liquid glass thermometer. General technical requirements. Test methods

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

GOST 30090-93 Bags and bag fabrics. General technical conditions

GOST 30178-96 Raw materials and food products. Atomic absorption method for determining toxic elements

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

GOST R ISO 2859-1-2007 Statistical methods. Alternative sampling procedures. Part 1: Post-feed sampling plans based on acceptable quality levels

GOST R 51766-2001 Raw materials and food products. Atomic absorption method for determination of arsenic

GOST R 53228-2008 Non-automatic scales. Part 1. Metrological and technical requirements. Tests

GOST R 53361-2009 Bags made of paper and combined 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 the 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 is replaced, it is recommended that the current version of that standard be used, taking into account any changes made to that version. If a reference standard to which a dated reference is given is replaced, it is recommended to use the version of that standard with the year of approval (adoption) indicated above. If, after the approval of this standard, a change is made to the referenced standard to which a dated reference is made that affects the provision referred to, it is recommended that that provision be applied without regard to that change. If the reference standard is canceled without replacement, then the provision in which a 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 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 colorants

Name ampaintya	Color index in the European Codification of Food Additives	Dye number a international system numbering of letters dobaaon (*NS)	Dye number in the international classification chemical substances(CAS No.)	Dye number in the international catalog dyes Coloui Index \|CI Nt>	Synonym for azo dye
Tartrazine (Tvptagshe)					Food Yellow 4. FO&C Yellow Ns 5
Sunet Yellow FCF					Food Yellow 3. FO&C Yellow No. 6
Aeroubin					Food Red 3. Carmoain (Car-motsine)
Ponceau 4R					Food Red 7. Cochineal Red (CocDIneal Red A)

End of table 1

Name aeohrasitslp	Index "resident of the European Codification of Food Additives"	Color Number About the International Nutrition Numbering System (INS)	Dye number in the International Classification of Chemical Substances (CAS N9)	Dye number in the international catalog Color Index dyes (Cl N9)	Synonym for the name a>o"rasitepya"
Charming Red AC (Allura Red AC)					Food Red 17. FO&C Red to 40
Brilliant Bleck BN					Food Black 1. Black BN. Black PN
Brown HT(8rown HT)					Food Brown 3. Chocolate Brown HT

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

Name of azo dye	Chemical name		Molecular weight, a e. m
Tartrazine £102 (Tartrazme)	5-Hydroxy-1-(4-sulfophenyl)-4-(4-sulfo-phenylvso)pyrazole-3-qurboxylate trisodium ethylene salt
Sunset Yellow FCF £110	2-Hydroxy-1-(4-sulfonaphthophenylazo)naphthalene-6-sulfonate divtrium salt	Ct»Ht©N2Na?OrSj
Azorubine E122 (Agogyne)	4-Hydroxy-3-(4-sulfo-1-naphthylveo>naph-tvlyn-1-sulfonvt divtrium salt
Ponceau 4 R £124 (Ponceau 4 R)	2-Hydroxy-1-(4-sulfo-1-naphthylveo>nvf-tvlin-b.v-disulfonate disodium salt	CjuH i iNjNasOtcSj
Charming red ACE129 (Allure Red AC)	2-Hydroxy-1-(2-mvtoxy-5-methyl-4-sulfo-phenylvso)naphthalene-6-sulfonvt disodium salt
Brilliant Black BN £151	4-Acetamido-5-hydroxy-6-(7-sulfo-4-(4-sulfophenylvso)-1-nvftylazo)naphthv-lin-1.7-disulfonate tetravtrium salt	SgaN i/NjNa40uS<
Brown NT E155 (Brown NT)	4.4'-(2,4-Dihydroxy-5-hydroxy-methyl-1,3-phenylene bisweo)-Di-(nvphthaline-1-sulfone) divtrium salt

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

Table 3 - Organoleptic characteristics of azo dyes

End of table 3

Name of azo dye	Indicator name
Name of azo dye	Appearance. azo dye color	Color of aqueous solution of azo dye
Aeroubin E122 (AgogyRte)	Red to maroon powder or granules
Ponceau 4R E124 (Ponceau 4R)	Red powder or granules
(Allure Red AC)	Dark red powder or granules
Black shiny PN E1S1 (Brilliant Slack 8N)	Black powder or granules	Black and blue
Brown NT E155 (Brown	Red-brown powder or granules	Brown

3.1.4 Spectrophotometric characteristics of aero dyes are given in Table 4.

Table 4 - Spectrophotometric characteristics of azo dyes

Name of azo dye	Spectrophotometric characteristics of azo dye		Solvent
Name of azo dye	We scream for a long time. corresponding to the maximum soetologist of polishing, mm	Specific coefficient of seed consumption. ^	Solvent
Tartrazine EI02			Distilled water
Sunset yellow FCFE110			Buffer solution at pH ■ 7
Azorubin E122			Distilled water
Ponceau 4R E124			Distilled aoda
Red charming AC E129			Buffer solution at pH ■ 7
Black shiny PN Е151			Distilled water
Brown NT E155			Buffer solution at pH ■ 7

3.1.5 In terms of physical and chemical indicators, azo dyes must meet the requirements specified in Table 5.

Table 5 - Physico-chemical parameters of azo dyes

Indicator name	Characteristics of the indicator
Mass fraction of the main coloring matter. %. no less than: Tartrvzin E102
Sunset yellow FCF E110
Azorubin E122
Ponceau 4R E124
Red charming AC E129
Black shiny PN E1S1
Brown HT E1S5
Substance that is insoluble in water. %. no more
Substances extractable with ether. %. no more

End of table 5

Indicator name	Characteristics of the indicator
Related coloring agents. %. no more: Tartrezine E102

Azorubin E122
Ponceau 4R E124
Red charming AC E129
Black shiny PN E151
Brown NT E155
Loss on drying at 135 ‘C. %. no more. Tartrezine E102
Sunset yellow* FCF E110
Azorubin E122
Ponceau 4R E124
Red charming AC E129
Black shiny PN E151
Brown NT E155
Non-sulfonated primary aromatic amines are not calculated as aniline. %. no more

3.2 Packaging

3.2.1 Packaging of aero-dyes must comply with the requirements established in (2).

3.2.2 Azo dyes are packaged in grocery bags made of sack fabrics in accordance with GOST 30090, open paper bags of NM and PM grades in accordance with GOST R 53361. boxes made of corrugated cardboard for food products in accordance with GOST R 54463. Inside grocery bags made of sack fabrics, paper bags of NM brand . boxes made of corrugated cardboard must be inserted into liner bags in accordance with GOST 19360 made of food-grade unstabilized polyethylene film of grade N with a thickness of at least 0.08 mm in accordance with GOST 10354.

The type and dimensions of bags, the maximum weight of packaged azo dyes are established by the manufacturer.

3.2.3 After filling, polyethylene bags-liners are welded or tied with bast fiber twine 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 others that ensure the mechanical strength of the seam.

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

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 sent 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 meet the requirements established

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

4 Safety requirements

4.1 According to the degree of impact on the human body, aero dyes, in accordance with GOST 12.1.007, 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 aerosol dyes, it is necessary to use special clothing and personal protective equipment in accordance with GOST 12.4.011 and observe the rules of personal hygiene.

4.4 When conducting analyses, 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 occupational safety training for workers - in accordance with GOST 12.0.004.

4.6 Production premises in which 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 premises must comply with 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 taken in batches.

A batch is considered to be the quantity of azo dyes of the same name, manufactured in one technological cycle, in identical packaging, received by one manufacturer under 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 on the quality of packaging, correct labeling, net weight, organoleptic and physico-chemical indicators and periodic tests on indicators that ensure safety.

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

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

Table 6

5.4 Quality control of packaging and correct labeling is carried out by external inspection of all packaging units included in the sample.

5.5 Control of the net mass of azo dyes 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 contents. The limit of permissible negative deviations from the nominal net weight of azo dyes in each packaging unit is according to 3.2.6.

5.6 Acceptance of a batch of azo dyes by net weight, packaging quality and correctness

packaging unit markings

5.6.1 A 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 a double sample size from the same batch. The batch is accepted if the conditions of 5.6.1 are met.

A batch is rejected if the number of packaging units in a double sample volume 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 based on organoleptic and physico-chemical criteria

indicators

5.7.1 To control the organoleptic and physico-chemical parameters of aero dyes, instant samples are taken from each packaging unit sampled in accordance with the requirements of Table 6 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, repeat control for this indicator is carried out on a double sample size from the same batch. The results of repeated tests are final and apply to the entire batch.

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

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

5.8 The procedure and frequency of monitoring safety indicators (arsenic, lead, mercury, cadmium content) 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 aero-dyes from different places in each packaging unit. selected according to 5.3, take instant samples using a sampler (probe), immersing it to at least 3/4 of the depth.

The mass of the instant sample should be no more than 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 polymer container and mixed thoroughly.

6.1.3 If it is necessary to reduce the total sample, the quartering method can be used. To do this, the total sample is poured onto a clean table and leveled into 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 roller. 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 divided diagonally into four triangles with a bar. Two opposite parts of the sample are discarded, and the remaining two are combined. mix and again divide into four triangles. The division is repeated the required number of times. The duration of the quartering procedure should be minimal.

6.1.4 The laboratory sample for small-volume batches of aero-dyes can be a total sample, and the total mass of instant samples must be no 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 aero-dyes.

6.1.5 Containers with samples are provided with labels that should indicate:

Full name of the azo dye and its E number;

Manufacturer's name and location;

Batch number;

Net weight of the batch;

Number of packaging units in a batch;

Date of manufacture;

Sampling date;

Storage life and conditions:

Surnames of persons. who carried out the collection of this sample;

Designation of this standard.

6.2 Determination of appearance and color

6.2.1 Essence of the method

The method consists of visually comparing the color of an azo dye with the color of a control sample of a dye of a given name.

A sample of a dye of a given name is taken as a control sample, the indicators of which meet the requirements ^B:

6.3.5 Preparation 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 monosubstituted with a molar concentration c(KH 2 PO 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 flask with a capacity of 100 cm 3 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 and record the result to the fourth decimal place. Then 20 cm 3 of distilled water or buffer solution no. 6.3.5.1 is added to the glass. in accordance with table 4. and stir with a glass rod until completely dissolved. To intensify dissolution, it is allowed to heat the solution in a glass in a water bath to a temperature of no more than 90 * C. Then the solution is cooled to (20 ± 1) "C. Transfer quantitatively to a volumetric flask (with a ground stopper) with a capacity of 250 cm 3, adjust the volume of the solution in the flask with the same solvent, close the flask with a stopper and mix thoroughly (solution A).

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

Using a pipette, 10 cm 3 of solution B is taken and transferred to a volumetric flask (with a ground stopper) with a capacity of 100 cm Oe. Adjust 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 The preparation of solutions of the 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 pipetted into spectrophotometer cuvettes and 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 operating the spectrophotometer.

The absorption spectra of the control and analyzed azo dyes must be identical, and the wavelength corresponding to the maximum absorption of the analyzed azo dye. should coincide with 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 coloring matter of the aero dye

6.4.1 Essence of the method

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

6.4.2 Measuring instruments, auxiliary equipment, reagents and materials

To carry out the analysis, measuring instruments and auxiliary equipment should be used. reagents and materials according to 6.3.2.

6.4.3 Sampling - part 1.

6.4.4 Analysis conditions

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

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

Relative air humidity......from 40% to 95%:

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

Current frequency in the electrical network.......from 49 to 51 Hz.

6.4.5 Preparation for analysis according to 6.3.5.

6.4.6 Conducting analysis

The spectrophotometer cuvette is filled with a 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 solution of the dye being analyzed should be in the range from 0.3 to 0.7 units. O. l.

6.4.7 Processing and recording of measurement results

The mass fraction of the main dye in the analyzed aerodye is X.%. calculated by the formula

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

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

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

V 2 is 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; = 100 cm 3 ;

Vi - 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 light absorption coefficient 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 is the mass of the sample of the analyzed azo dye taken for analysis, g, no 6.3.5.3.

6.4.8 Monitoring the accuracy of measurement results

The final result of the determinations is taken to be the arithmetic mean of two parallel determinations X ev, %. rounded to the first decimal place if 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 g - 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 absolute error limits of the method for determining the mass fraction of azo dye are ±0.6% at P* 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), and a sample of an 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 Essence of the method

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

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

error from nonlinearity i0.6 mg.

Liquid glass thermometer with a temperature measurement range from 0 ®C to 150 ®C. price division 1 *C according to GOST 28498.

Electronic-mechanical watches according to GOST 27752.

Electric stove according to GOST 14919.

A drying cabinet that ensures maintenance of a given temperature regime from 20 *C to 150 °C with an error of ±2 °C.

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

Soxhlet extractor, consisting of a nozzle for extraction NET-100 TS in accordance with GOST 25336, a refrigerator KhSh-1-200-14/23ХС in accordance with GOST 25336 and a flask K-1 -50-14/23 TS in accordance with GOST 25336 with interchangeable ground connections.

Installation for solvent distillation, consisting of a nozzle H1 >19/26*14/23 TS lo GOST 25336, a refrigerator KhPT-1-100-14/23 XS in accordance with 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 connections.

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 Robber selection - victory 1.

6.6.4 Analysis conditions

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

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

Relative air humidity............ from 40% to 90%:

Mains voltage.................220*]"* V;

Current frequency in the electrical network.......from 49 to 51 Hz.

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

All operations with reagents should be carried out in a fume hood.

6.6.5 Preparation for analysis

6.6.5.1 Preparation of the Soxhlet extractor

The Soxhlet extractor flask 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, recording the weighing result to the third decimal place. Drying the flask continues until then. as long as the difference between the results of two consecutive determinations is less than 0.001.

Weigh the azo dye to be analyzed on a sheet of paper, recording the result to the third decimal place. Then the filter paper with the aero dye is folded into a cartridge and the cartridge is placed in the extraction nozzle.

6.6.5.2 Preparation of the installation for solvent distillation

Assemble the installation for solvent distillation by connecting the head in series with a refrigerator. and a refrigerator with a receiving flask through an allonge.

6.6.6 Conducting analysis

A nozzle for extraction, together with a cartridge with an aero-dye placed in it. connected with a pin prepared in item 6.5.1. pour 40 cm 3 of diethyl ether into it and connect the extraction nozzle to the refrigerator. The flask is placed in a glycerin bath heated to a temperature of (55±5) *C, ensuring uniform moderate boiling of diethyl ether. The extraction is carried out for 5 hours, after which the flask is separated from the extraction nozzle, connected to the nozzle of the solvent distillation unit and placed in a glycerin bath heated to a temperature of (55 ± 5) °C. The contents of the flask are evaporated to dryness, then 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. Drying the flask continues until then. until the difference between the results of two consecutive determinations is less than 0.001 g.

6.6.7 Processing and recording of measurement results

Mass fraction of substances extracted with ether X, %. calculated by 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 - mass of an empty flask, g.

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

Calculations are carried out by recording the result to the third decimal place.

6.6.6 Monitoring the accuracy of measurement results

The arithmetic mean of two parallel determinations is taken as the final result of the determinations, %. rounded to the second 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 g = 0.020%

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 = 0.030%.

Grakits of the absolute error of the method for determining substances extracted with ether J.O.02% at P - 95%.

6.7 Determination of the mass fraction of associated coloring substances

6.7.1 Essence of the method

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

The specific light absorption coefficients 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 (MSD). not exceeding 0.3 mg. and with

error from nonlinearity i0.6 mg.

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

Spectrophotometer with a measurement range in the wavelength range from 350 to 700 nm. permissible absolute error of transmittance no more than 1%.

Quartz cuvettes with an absorbing layer thickness of 1 cm.

Chromatographic chamber with lid.

Electric stove according to GOST 14919.

Water bath.

A drying cabinet that ensures maintenance of a given 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 price division of no 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.

Weighing cups SV-19/9 (24/10) or SN-34/12 according to GOST 25336.

Glass V(N)-1-100 TS(TCS) according to GOST 25336.

Glass rod.

Chromatographic paper measuring at least 20 x 20 cm.

Laboratory filter paper FOB-HI according to GOST 12026.

Azo dye in accordance with 3.1.

Distilled water according to GOST 6709.

Aqueous ammonia according to GOST 3760. analytical grade, solution of mass concentration 250 g/dm 3.

Acetone according to GOST 2603. analytical grade.

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

Sodium citrate 5.5-water according to GOST 22280. analytical grade.

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. analytical grade.

Sodium carbonate acid according to GOST 4201. analytical grade.

Prolyl alcohol. X. h.

Ethyl acetate according to GOST 22300. analytical grade.

Sodium acid 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 - forehead.1.

6.7.4 Conditions for conducting analysis - forehead.6.4.

6.7.5 Preparation 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 alcohol. The flask is closed with a glass stopper and mixed thoroughly.

Preparation of eluent 2

Add pipettes individual for each reagent into a 50 cm3 volumetric flask.

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

Add pipettes individual for each reagent into a 50 cm3 volumetric flask. 12 cm 3 butyl alcohol. 4 cm 3 of ethyl alcohol and 6 cm 3 of acetic acid solution 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

Add pipettes individual for each reagent into a 50 cm3 volumetric flask.

8 cm 3 prolyl slurt. 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 8 cm 3 of butyl alcohol, 2 cm 3 of glacial acetic acid and 10 cm 3 of distilled water using pipettes individual for each reagent. The flask is closed with a glass stopper and mixed thoroughly.

The solution is used freshly prepared.

Preparation of eluent 6

Add pipettes individual for each reagent into a 50 cm3 volumetric flask. 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 Preparation of extractant

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

The solution is used freshly prepared.

6.7.6 Preparation of solutions of control azo dyes

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 dissolution, it is allowed to heat the solution in a glass in a water bath to a temperature of no more than 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 capped and thoroughly mixed.

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

6.7.7 Preparation of solutions of analyzed azo dyes

0.5000 g of the analyzed azo dye is weighed into a glass with a capacity of 50 cm3. Then add 20 cm 3 of distilled water and stir with a glass rod until completely dissolved. To intensify dissolution, it is allowed to heat the solution in a glass in a water bath to a temperature of no more than 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, adjust the volume of the solution in the flask to the mark with distilled water, close the flask with a stopper and mix thoroughly. The mass fraction of the analyzed dye in the resulting solution is C l * 1%.

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

6.7.9 Preparation of chromatography paper

Chromatographic paper is prepared according to GOST 28365 by applying 0.1 cm 3 solutions of control and analyzed azo dyes to the starting line in the form of strips of 0.1 cm 3 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 starting line. After elution is completed, the chromatogram is removed with tweezers and dried in an oven at a temperature of (55 ± 5) C for 15 minutes. cool and cut out the colored zones corresponding to the main dye of the control azo dye and the accompanying dyes of the analyzed azo dye.

At the same time, uncolored zones of 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 glasses with a capacity of 50 cm 3 . In the first glass - zones corresponding to the accompanying coloring substances in the analyzed aerodye (solution 1). in the second - the zone corresponding to the main dye of the control dye (solution 2). in the third - uncolored zones, equal in area to the zones of accompanying dyes of the analyzed azo dye (solution 3), in the fourth - uncolored zone, equal in area to the zone of the main dye of the analyzed azo dye (solution 4). Then add 5 cm 3 of the extractant prepared according to 67.5.2 into each glass with a pipette and shake for 3 minutes. after which 15 cm 3 of sodium hydrogen carbonate solution is added to each glass with a pipette, shaken, and the resulting extracts are filtered through paper filters into quartz cuvettes.

The optical densities of the resulting 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 versus solution 3 and solution 2 versus solution 4).

6.7.11 Processing and recording of measurement results

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

where C is the mass fraction of dyes in the analyzed aerocolorant according to 6.4. %;

A c is the optical density of the stereo-associated coloring substances of the analyzed dye according to 6.7.10 (solution 1);

A a is the optical density of the solution of the main dye of the control azo dye according to

6.7.10 (solution 2).

Calculations are carried out by recording the result to the second decimal place.

6.7.12 Monitoring 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 reproducibility conditions at P = 95%. does not exceed the reproducibility limit R - 0.03%.

The absolute error limits of the method for determining the mass fraction of associated coloring substances in the analyzed aerocolorant are 10.2% at P = 95%.

6.8 Determination of the mass fraction of unsulfurized primary aromatic amines

6.8.1 Essence of the method

The method is based on the extraction of non-sulfonated primary aromatic amines from an alkaline solution of the dye 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 resulting colored compounds.

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

Scales in accordance with GOST R 53228. ensuring weighing accuracy with an absolute permissible error of iO, 1 g.

Scales with the value of the standard deviation (MSD). not exceeding 0.3 mg. and error from nonlinearity ±0.6 mg.

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

Electronic-mechanical watches according to GOST 27752.

Spectrophotometer with a measurement range in the wavelength range from 350 to 700 nm. permissible absolute error of transmittance no more than 1%.

Quartz cuvettes with an absorbing layer thickness of 4 cm.

Electric stove according to GOST 14919.

Water bath.

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 1st accuracy class.

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

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

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

Measuring 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(TCS) according to GOST 25336.

Glass rod.

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. analytical grade.

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 acids disodium salt (Schaffer'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 conducting analysis - according to 6.6.4.

6.8.5 Preparation 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 of 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 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 a solution of sodium carbonate with a 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. dissolve 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 A solution of sodium hydroxide with a molar concentration of (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 nitrate 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 disodium salt of 2-naphthol-3,6-disulfonic acid (Schaeffer’s salt)

Disodium salt of 2-naphthol-3,6-disulfonic acid (Schaffer'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, 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 hydrochloric acid solution prepared according to 6.8.5.2 is added. bring the volume to the mark with distilled water and mix thoroughly (solution A).

10 cm 3 of solution A is placed in a volumetric flask with a ground stopper with a capacity of 100 cm 3. Bring the volume of solution in the flask to the mark with distilled water, close the flask with a stopper 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 Add 10 cm 3 of a solution of disodium salt of 2-kafthol-3.6-disulfonic acid (Schaffer’s salt) to a flask with a capacity of 250 cm 3 according to 6.8.5.8. add 100 cm 3 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

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

6.8.6 Construction of a calibration dependence

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

From each flask, 10 cm 3 of solution is 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 potassium bromide solution no. 6.8.5.3 and 0.05 cm 3 of sodium nitrous acid solution according to clause 8.5.7 are added to each flask, and then mixed. The flasks are kept in an ice bath for a period of time. Then add 11 cm 3 of solution C to each flask according to 6.8.5.10. Then bring the volume in each cup to the mark with distilled water, close with a 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 constructed by plotting the aniline content (g) in the calibration solutions along the abscissa axis, and the corresponding values of the measured optical density along the ordinate axis.

6.8.7 Conducting analysis

8 beaker 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 completely dissolved. To intensify dissolution, it is allowed to heat the solution in a glass in a water bath to a temperature of no more than 90 °C.

Then the solution is cooled to a temperature of (20 ± 1) * C. transfer quantitatively into a separating funnel using 50 cm 3 of distilled water, add 5 cm 3 of sodium hydroxide solution, 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 separatory funnel.

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

Then, 10 cm 3 of hydrochloric acid solution according to 6.8.5.2 is added to the separating funnel with the washed toluene extract and shaken vigorously for (5 ± 1) minutes. 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 D is 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 a solution of potassium bromide according to 6.8.5.3 and 0.05 cm 3 of a solution of sodium nitrous acid according to 6.8.5 7. and then mix. The flask is kept in an ice bath with Jumin. Then add 11 cm 3 of solution C forehead.8.5.10. bring the volume to the mark with distilled water, close with a stopper, mix thoroughly and place in a dark place for 15 minutes. The optical density of the solution is measured on a spectrophotometer at a wavelength of 510 nm against the reference solution no. 6.8.5.11.

The amount of aniline is determined from the calibration curve.

6.8.8 Processing and recording of measurement results

Mass fraction of lervic non-sulfonated aromatic amines X 3,%. calculated by the formula

X 3 = ^-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 aero dye sample according to 6.8.7, g.

Calculations are carried out by recording the result to the fourth decimal place.

6.8.9 Monitoring the accuracy of measurement results

The arithmetic mean of two parallel determinations X^, % is taken as the final result of the determinations. 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 g - 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%.

Absolute error limits of the method for determining substances extractable with ether

10.001% at P = 95%.

6.9 Determination of the mass fraction of losses during drying

6.9.1 Essence of the method

The method is based on 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 value (RMS) not exceeding 0.3 mg. And

error from nonlinearity 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 watches according to GOST 27752.

A drying cabinet that ensures maintenance of a given 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.

Weighing cups SV-19/9 (24/10) or SN-34/12 according to GOST 25336.

Calcium chloride according to GOST 450.

6.9.3 Sampling - according to 6.1.

6.9.4 Conditions for conducting analysis - according to 6.3.4.

6.9.5 Conducting analysis

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

Drying the cup with the lid is repeated under the same conditions until the ENT. until the difference between the results of two consecutive weighings is no more than 0.0001 g.

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

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

6.9.6 Processing and registration of measurement results Mass fraction of losses during drying X 4 . %. calculated by the formula

U 4 a 10Q | (b)

where m is the mass of the dry cup, g

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

100 is the coefficient for converting the result into percentages.

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

The final result is recorded accurate to the first decimal place.

6.9.7 Monitoring the accuracy of measurement results

The arithmetic mean value of X4ce is taken as the final result of the determination. %. two parallel determinations of the mass fraction of drying losses obtained under repeatability conditions, if the acceptance condition is met

(X*m£ ~ X in)100/X^ £G, (7)

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

Xyin is the minimum mass fraction of losses during drying;

X 4ut is 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

where X 4 is the arithmetic mean of the results of two determinations considered acceptable. %;

5 - limits of relative measurement error. %.

The repeatability limit g and reproducibility R, as well as the accuracy indicator b for measuring 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 GOST 26933, GOST 30178;

Mercury - according to GOST 26927.

7 Transportation and storage

7.1 Azo dyes are transported in covered vehicles by all types of transport in accordance with the cargo transportation rules in force for the relevant types 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 humidity of no 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 established by the manufacturer.

Bibliography

(1) Technical Regulations of the Customs Union TR CU 029/2012 “Safety requirements for food additives, flavorings and technological aids”

(2) Technical Regulations of the Customs Union TR CU 021/2011 “On the safety of food products”

(3) Technical Regulations of the Customs Union TR CU 005/2011 “On Packaging Safety”

(4) Technical regulation of the Customs Union TR CU 022/2011 “Food products regarding their labeling”

UDC 663.05:006.354 OKS 67.220.20 N91 OKP24 6372

Key words: 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 layout /O-v. Deienina

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Preface

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

Information about changes To present standard published V annually published informational index "National standards", A text changes And amendments - per month published information signs "National standards". IN case revision (replacements) or cancellations present standard appropriate notification will published V monthly published informational index "National standards". Corresponding information, notification And texts are placed Also V informational system general use - on official website Federal agencies By technical regulation And metrology V networks Internet

1 area of use. 2

3 Classification. 4

4 General technical requirements. 5

4.1 Characteristics. 5

4.2 Requirements for raw materials.. 6

4.3 Packaging. 6

4.4 Marking. 7

5 Safety requirements. 7

6 Acceptance rules. 7

7 Control methods. 9

7.1 Sampling 9

7.2 Determination of organoleptic indicators. 10

7.3 Sodium ion test. 10

7.4 Tests for phosphate ions... 11

7.5 Test for free orthophosphoric acid and its disodium salt. 13

7.6 Determination of the mass fraction of the main substance. 13

7.7 Determination of the mass fraction of total phosphorus pentoxide. 16

7.8 Determination of the mass fraction of substances insoluble in water. 19

7.9 Determination of pH of an aqueous solution. 20

7.10 Determination of the mass fraction of losses during drying. 20

7.11 Determination of the mass fraction of losses during ignition. 22

7.12 Determination of the mass fraction of fluorides. 23

7.13 Determination of the mass fraction of arsenic. 23

7.14 Determination of the mass fraction of lead. 23

8 Transportation and storage. 23

Bibliography. 24

GOST R 52823-2007

NATIONAL STANDARD OF THE RUSSIAN FEDERATION

Date of introduction - 2009-01-01

1 area of use

This standard applies to the food additive sodium phosphates E339, which are 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 ensuring 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. Alternative sampling procedures. 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 Raw materials and food products. Atomic absorption method for 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 type during their production, packaging, sale and import

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

GOST 12.1.007-76 System of occupational safety standards. 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 aqueous. Specifications

GOST 3765-78 Reagents. Ammonium molybdate acid. Specifications

GOST 4198-75 Reagents. Potassium phosphate monosubstituted. Specifications

GOST 4201-79 Reagents. Sodium carbonate is acidic. 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 preparing auxiliary reagents and solutions used in 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) Tubular fluorescent lamps for general lighting

GOST 8515-75 Diammonium phosphate. Specifications

GOST 9147-80 Porcelain laboratory utensils and equipment. Specifications

GOST 10354-82 Polyethylene film. Specifications

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

GOST 10678-76 Thermal orthophosphoric acid. Specifications

GOST 11078-78 Purified caustic soda. Specifications

GOST 14192-96 Marking of cargo

GOST 14919-83 Household electric stoves, electric stoves and electric frying cabinets. General technical conditions

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

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

GOST 17308-88 Twines. Specifications

GOST 18389-73 Wire made of platinum and its alloys. Specifications

GOST 19360-74 Film liner bags. General technical conditions

GOST 24104-2001 Laboratory scales. General technical requirements

GOST 25336-82 Laboratory glassware and equipment. Types, main parameters and sizes

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

GOST 26930-86 Raw materials and food products. Arsenic determination method

GOST 26932-86 Raw materials and food products. Lead determination method

GOST 27752-88 Electronic-mechanical quartz table, wall and alarm clocks. General technical conditions

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

GOST 29169-91 (ISO 648-77) Laboratory glassware. Single mark pipettes

GOST 29227-91 (ISO 835-1-81) Laboratory glassware. Graduated pipettes. 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 technical conditions

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

Designation and name of food grade sodium monophosphate	Chemical name		Molecular mass
E339(i) sodium orthophosphate 1-substituted	Sodium phosphate 1-substituted	NaH 2 PO 4 (anhydrous)
	Sodium phosphate 1-substituted 1-aqueous	NaH 2 PO 4 ?H 2 O (monohydrate)
	Sodium phosphate 1-substituted 2-water	NaH 2 PO 4 ? 2H 2 O (dihydrate)
E339(ii) 2-substituted sodium orthophosphate	Sodium phosphate 2-substituted	Na 2 HPO 4 (anhydrous)
	Sodium phosphate 2-substituted 2-water	Na 2 HPO 4 ? 2H 2 O (dihydrate)
	Sodium phosphate 2-substituted 7-water	Na 2 HPO 4 7H 2 O (heptahydrate)
	Sodium phosphate 2-substituted 12-water	Na 2 HPO 4 ? 12H 2 O (dodecahydrate)
E339(iii) 3-substituted sodium orthophosphate	Sodium phosphate 3-substituted	Na 3 PO 4 (anhydrous)
	Sodium phosphate 3-substituted 0.5-water	Na 3 PO 4 ? 0.5H 2 O (hemihydrate)
	Sodium phosphate 3-substituted 1-water	Na 3 PO 4 ?H 2 O (monohydrate)
	Sodium phosphate 3-substituted 12-water	Na 3 PO 4 ? 12H 2 O (dodecahydrate)

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 Food grade 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 meet the requirements specified in Table 2.

Table 2 - Organoleptic indicators

4.1.4 In terms of physical and chemical indicators, food sodium monophosphates must meet the requirements specified in Table 3.

Table 3 - Physico-chemical indicators

Indicator name	Characteristics of the indicator
Sodium ion test	Stands the test
Tests for phosphate ions:
	Stands the test


Test for free orthophosphoric acid and its 2-substituted sodium salt in E339(i)	Stands the test
Mass fraction of the main substance, %, not less than:



anhydrous, semi- and monohydrate
dodecahydrate
Mass fraction of total phosphorus pentoxide (for anhydrous form), %
	From 57.0 to 60.0 incl.
	From 48.0 to 51.0 incl.
	From 40.0 to 43.5 inclusive.
Mass fraction of water-insoluble substances, %, no more
pH of an aqueous solution with a mass fraction of sodium monophosphate 1%:
	From 4.2 to 4.6 inclusive.
	From 9.0 to 9.6 incl.
	From 11.5 to 12.5 inclusive.
Mass fraction of losses during drying, %, no more than:

anhydrous
monohydrate
dihydrate

anhydrous
dihydrate
heptahydrate
dodecahydrate
Mass fraction of losses on ignition, %

anhydrous, no more
monohydrate, no more
dodecahydrate	From 45.0 to 58.0 incl.

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

Table 4 - Indicators ensuring safety

4.2 Requirements for raw materials

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

Orthophosphoric acid grade A according to GOST 10678;

Caustic soda grade A according to GOST 11078;

Sodium carbonate according to GOST 83;

Sodium carbonate acid according to GOST 4201;

Soda ash grade B according to GOST 5100.

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

4.3 Packaging

4.3.1 Food grade sodium monophosphates are packaged in three-layer paper bags of the PM brand in accordance with GOST 2226 or in liner bags in accordance with GOST 19360 made of food-grade polyethylene unstabilized film of grade N, with a thickness of at least 0.08 mm in accordance with GOST 10354, placed in grocery bags in accordance with GOST 30090 or in open three-layer paper bags of the NM brand according to GOST 2226.

4.3.2 Polyethylene liner bags, after filling them, are welded or tied with bast fiber twine in accordance with 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 threads in accordance with GOST 14961.

4.3.4 It is permitted 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 grade sodium monophosphates sent to the Far North and equivalent areas are packaged in accordance with GOST 15846.

4.4 Marking

4.4.1 Each packaging unit containing edible sodium monophosphates shall be marked in any manner that ensures its clear identification, indicating:

Names of the food additive and its index *;

Mass fraction of the main substance;

Names and location (legal address) of the manufacturer;

Manufacturer's trademark (if available);

Net weights;

Gross weights;

Lot numbers;

Dates of manufacture;

Storage period and conditions according to 8.3 and 8.2;

Symbols of this standard.

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

4.4.2 Transport markings must comply with the requirements of GOST 14192 with the application of handling signs “Keep away from moisture” and “Do not handle with hooks”.

5 Safety requirements

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

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

5.3 Work with food-grade sodium monophosphates must be carried out in special clothing, using personal protective equipment and observing personal hygiene rules.

5.4 Production premises in which work with food sodium monophosphates is carried out 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 Food grade monosodium phosphates are taken in batches.

A batch is considered to be the amount of food sodium monophosphates produced in one technological cycle, on the same production date, in the same packaging, simultaneously presented for testing and acceptance, and documented in one document certifying their quality and safety.

6.2 The 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;

Indicators ensuring safety, according to this standard and actual, 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 on the quality of packaging, correct labeling, net weight, organoleptic and physico-chemical indicators and periodic tests on 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 at an acceptable quality level AQL equal to 6.5, according to GOST R ISO 2859-1.

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

Table 5

6.5 Quality control of packaging and correct labeling is carried out by external inspection of all packaging units included in the sample.

6.6 Control of the net mass 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 contents. The limit of permissible negative deviations from the nominal net weight of food sodium monophosphates in each packaging unit is according to 4.3.3.

6.7 Acceptance of a batch of food sodium monophosphates based on 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 food 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 food sodium monophosphates is greater than or equal to the rejection number (see Table 5), control is carried out on a double sample volume from the same batch. The batch 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 volume that do not meet the requirements for packaging quality and correct labeling and net weight of food 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 indicators

6.8.1 To control the organoleptic and physicochemical characteristics of the product, instant samples are taken from each packaging unit included in the sample in accordance with the requirements of Table 5 and a total sample is compiled according to 7.1.

6.8.2 If unsatisfactory results are obtained for organoleptic and physicochemical 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 results of repeated tests are final and apply to the entire batch.

If unsatisfactory test results are received again, the batch is rejected.

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

6.9 The procedure and frequency of monitoring indicators that ensure safety (fluoride, arsenic and lead content) 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, instant samples are taken from different places in each packaging unit selected in accordance with 6.4. The mass of the instant sample should be no more than 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 material that does not react with food-grade sodium monophosphates, immersing the sampler in food-grade sodium monophosphates to at least 3/4 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 into a thin layer in the form of a square. Then it is poured with wooden planks with beveled ribs from two opposite sides into the middle so that a roll 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 divided diagonally into four triangles with a bar. Two opposite parts of the sample are discarded, and the remaining two are combined, 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 total 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 repeated testing in case of disagreement in assessing the quality of food sodium monophosphates. This part of the total sample is stored until the end of the storage period.

7.1.4 Containers with samples are provided with labels that should indicate:

Name of the food additive and its index;

Mass fraction of the main substance;

Manufacturer's name and location;

Batch number;

Net weight of the batch;

Number of packaging units in a batch;

Date of manufacture;

Sampling date;

The names of the persons who collected this sample;

Designation of this standard.

7.2 Determination of organoleptic parameters

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

7.2.1 Measuring instruments, materials, reagents

Laboratory scales in accordance with GOST 24104 with limits of permissible absolute error of single weighing ±0.1 g.

Glass rod.

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 testing room must 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 illuminated with fluorescent lamps of the LD type according to GOST 6825. The illumination of the working table surface must be at least 500 lux.

7.2.4.2 To determine the smell, 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 kept 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 or by the coloring of a colorless flame yellow.

7.3.1 Measuring instruments, materials, reagents

Electric stove according to GOST 14919.

Glass V(N)-1-250 TS(TSH) according to GOST 25336.

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

Glass rod.

Platinum wire according to GOST 18389.

Zinc uranyl acetate, part.

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 acetic acid solution in the 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 a solution of zinc uranyl acetate with a mass fraction of 5%

A 2.5 g sample of zinc uranyl acetate 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 hydrochloric acid solution in the 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 Carrying out the test

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

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

7.4 Tests for phosphate ions

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

7.4.1 Test for phosphate ion (H 2 PO 4 -)

7.4.1.1 Measuring instruments, materials, reagents

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

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

Glass V(N)-1-250 TS(TSH) 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 Preparation for testing

A solution of nitric acid with a mass fraction of 10% and a density of 1.055 g/cm3 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 dark glass containers.

7.4.1.5 Test performance

A sample weighing from 1.0 to 1.5 g is dissolved in 100 cm 3 of distilled water. To 5 cm 3 of solution, add 1 cm 3 solution of silver nitrate with a pipette. To the resulting yellow precipitate, add from 1.6 to 2.0 cm 3 of dilute nitric acid according to 7.4.1.4 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 limits of permissible absolute error of 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 TS (TLC) according to GOST 25336.

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

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

Glass rod.

Molybdic acid, part.

Hydrochloric acid according to GOST 3118, part.

Distilled water according to GOST 6709.

Nitric acid according to GOST 4461, part.

Aqueous ammonia according to GOST 3760, part.

7.4.2.2 Sampling - according to 7.1.

7.4.2.3 Test conditions - according to 7.2.3.

7.4.2.4 Preparation for testing

A sample of finely ground 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 ammonia solution with a mass fraction of 10%, prepared according to GOST 4517. Solution cool to room temperature and slowly add, 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, then only the solution above the precipitate is used for analysis.

7.4.2.5 Test performance

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

7.4.3 Test for phosphate ions (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 limits of permissible absolute error of 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 Preparation for testing

Preparation of silver nitrate solution - according to 7.4.1.4.

A solution of acetic acid in a 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 Test performance

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 silver nitrate solution 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 orthophosphoric acid and its disodium salt

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

7.5.1 Measuring instruments, auxiliary devices and reagents

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

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

Glass V(N)-1-100 TS(TSH) 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 Carrying out the 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 (no more than 0.3 cm 3) or, respectively, a solution of sulfuric acid (no more than 0 .3 cm 3). The color transition 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 orthophosphoric 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 solutions of food-grade sodium monophosphate in the pH range from 4.4 to 9.2.

7.6.1 Measuring instruments, auxiliary devices and reagents

pH meter with glass electrode with a 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) TS(TXS) 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 monosubstituted 2-water according to GOST 245, part.

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 0.1% is prepared according to GOST 4919.1.

7.6.4.2 Test performance

A sample weighing 4 g with the weighing result recorded to the third decimal place is placed in a glass 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 indication of the equivalent point for thymolphthalein.

7.6.4.3 Processing results

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

(1)

Where V- volume of (NaOH) = 1 mol/dm 3 solution used to titrate the sample to pH 9.2, cm 3;

M With(NaOH) = 1 mol/dm 3 solution, g;

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

m- weight of the sample, g.

The final result is rounded to the first decimal place.

r R

Reproducibility limit R R

The absolute error limits 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 monosodium phosphate E339(ii)

7.6.5.1 Preparation for testing

Solution 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.

7.6.5.2 Test performance

A sample weighing 1.5 g with the weighing result recorded to the third decimal place is placed in a glass 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 determinations with indication of the equivalent point using methyl orange using a reference solution containing 2 g of monosubstituted sodium phosphate dihydrate and 2 - 3 drops of methyl orange solution in 100 cm 3 of distilled water.

7.6.5.3 Processing results

Mass fraction of the main substance of food grade monosodium phosphate E339(ii) X 2,%, calculated by the formula

(2)

Where V- volume of (HCl) = 0.5 mol/dm 3 solution used to titrate the sample to pH 4.4, cm 3;

M- mass of food grade sodium monophosphate, corresponding to 1 cm3 With(HCl) = 0.5 mol/dm 3 solution, g; M(Na 2 HPO 4) = 0.0710 g, M(Na 2 HPO 4 ? H 2 O) = 0.0890 g, M(Na 2 HPO 4 ? 7H 2 O) = 0.1340 g, M(Na 2 HPO 4 ? 12H 2 O) = 0.1791 g;

100 - conversion factor into percent;

m- weight of the sample, g.

Calculations are carried out by recording the result to the second decimal place.

The final result is rounded to the first decimal place.

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

Repeatability (convergence) limit r- 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- 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 method of measuring the main substance of food monosodium phosphate E339(ii) ±0.3% at R = 95 %.

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

7.6.6.1 Preparation for testing

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 0.1% is prepared according to GOST 4919.1.

7.6.6.2 Test performance

A sample weighing 2 g with the weighing result recorded to the third decimal place is placed in a glass 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.

Twice the 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. The content of monosodium phosphate is calculated from the smaller of these volumes.

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

7.6.6.3 Processing results

Mass fraction of the main substance of food grade monosodium phosphate E339(iii) X 3,%, calculated by the formula

(3)

(4)

Where V- volume With(HCl) = 0.5 mol/dm 3 solution, used to titrate the sample to pH 4.4;

M- the mass of food-grade 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) = 0.04324 g, M(Na 3 PO 4 ? H 2 O) = 0.4549 g, M(Na 3 PO 4 ? 12H 2 O) = 0.09503 g;

2V 1 - double volume exactly With(NaOH) = 0.5 mol/dm 3 solution, used to titrate the sample to pH 9.2, cm 3;

100 - conversion factor into percent;

m- weight of the sample, g.

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

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

Repeatability (convergence) limit r- 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- absolute value of the difference between the results of two measurements obtained under reproducibility conditions at R= 95%, should not exceed 0.8%.

The absolute error limits of the method of measuring the main substance of food monosodium phosphate 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 to identify dietary monosodium phosphates E339(i), E339(ii) and E339(iii).

7.7.1 Extraction-photometric method

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

7.7.1.1 Measuring instruments and reagents

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

Liquid glass thermometer with a measuring range from 0 °C to 50 °C, division value of 1 °C 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 accuracy class with a counter scale capacity of 30 minutes, with a division value of 0.20 seconds.

Distilled water according to GOST 6709.

Ammonium molybdate acid according to GOST 3765, part.

Ethyl alcohol according to GOST R 51652.

Tin dichloride 2-hydrate 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 Preparation for testing

a) Preparation of sulfuric acid solution

Solution molar concentration 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/cm3.

b) Preparation of ammonium molybdate solution

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

c) Preparation of a solution of stannous chloride

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

d) Preparation of a standard phosphate solution containing 0.1 mg of phosphorus pentoxide per 1 cm3

A weighed portion of monopotassium phosphate weighing 1.9175 g, with the weighing recorded to the fourth decimal place, is dissolved in distilled water in a volumetric flask with a capacity of 1000 cm 3, adjusted to the mark with water and mixed. Using a pipette, 10 cm 3 of the resulting solution is taken into a volumetric flask with a capacity of 100 cm 3, adjusted to the mark with distilled water and mixed.

e) Preparation of a reference solution

20 cm 3 of distilled water is poured into a volumetric flask with a capacity of 100 cm 3, 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 ammonium molybdate solution is added and stirred vigorously for 15 With. Then, after settling and separating the layers, pipet 5 cm 3 of the upper organic layer into a volumetric flask 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 mix.

f) Construction of a calibration graph

In volumetric flasks with a capacity of 100 cm 3 add 1.0; 2.0; 3.0; 4.0; 5.0; 6.0 cm 3 of standard monophosphate solution, 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 ammonium molybdate solution and immediately stir vigorously within 15 s. Then, after settling and separating the layers, aliquots of 5 cm 3 of the upper organic layer are selected 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 tin dichloride, adjust the volume with sulfuric acid to the mark and stir.

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

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

The calibration schedule is periodically (once every 10 days) updated at three main points.

7.7.1.5 Test performance

A sample weighing from 0.04 to 0.05 g, with the weighing result recorded 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, adjusted to the mark and mixed. Using a pipette, 10 cm 3 of the resulting solution is taken 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 d).

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

The mass of food-grade sodium monophosphate in an aliquot in terms of phosphorus pentoxide is determined using a calibration curve.

7.7.1.6 Processing results

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

(5)

Where m 1 - mass of food grade sodium monophosphate in terms of phosphorus pentoxide in an aliquot of the solution, found from the calibration curve, mg;

500 - volumetric flask capacity, cm 3;

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

100 - coefficient for converting the result into percentage;

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

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

5 - aliquot part of the organic layer, taken for dilution according to 7.7.1.4 d);

m- weight of the sample, g.

The final result is rounded to the second decimal place.

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

Repeatability (convergence) limit r- 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- absolute value of the difference between the results of two measurements obtained under reproducibility conditions at R= 95%, should not exceed 0.30%.

The absolute error limits of the method for measuring the mass fraction of 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 dissolving food sodium monophosphates in water under certain conditions and determining the mass fraction of water-insoluble substances.

7.8.1 Measuring instruments, auxiliary equipment, reagents

Filter crucible type TF POR 16 according to GOST 25336.

Laboratory scales in accordance with GOST 24104 with limits of permissible absolute error of 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 Carrying out the test

A sample weighing 10 g, with the weighing result recorded to the fourth decimal place, is placed in a glass with a capacity of 250 cm 3 and dissolved in 100 cm 3 of hot distilled water. The solution is then filtered through a filter crucible, previously dried to a 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 of 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 Processing the results

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

(6)

Where m 1 - mass of the filter crucible with a precipitate of insoluble substances after drying, g;

m 2 - mass of the filter crucible, g;

m- weight of the sample, g;

Calculations are carried out by recording the result to the third decimal place.

The final result is recorded to the second decimal place.

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

Repeatability (convergence) limit r- 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- 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 mass fraction of water-insoluble substances method are ±0.03% at R = 95 %.

7.9 Determination of pH of 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 with a measuring range from 1 to 14 units. pH, with permissible absolute measurement error ±0.05 units. pH.

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

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

Glass V(N)-1-250 TS(TXS) according to GOST 25336.

Melted glass rod.

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 Carrying out the test

A sample weighing 1.0 g with the weighing result recorded 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 pH meter electrodes in solution and measure the pH of the solution at (20.0 ± 0.5) °C.

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

7.9.5 Processing of measurement results

Measurement results are recorded to the second decimal place.

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

Repeatability (convergence) limit r- 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- 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.

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

7.10 Determination of the mass fraction of losses during drying

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

7.10.1

A drying cabinet that ensures maintenance of a given mode from 20 °C to 200 °C with an error of ±2 °C.

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

Desiccator 2-250 according to GOST 25336.

Electronic-mechanical quartz table clocks, wall clocks and alarm clocks in accordance with GOST 27752.

Cup SN 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 together with the lid open at a temperature of 100 °C to 105 °C in a drying cabinet to constant weight.

A sample weighing from 1 to 2 g, with the weighing result recorded to the third decimal place, is placed open 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 this The glass is quickly covered 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, recording the weighing result to the third decimal place, place it open with a lid in an oven and dry at 40 °C for 3 hours, then at 105 °C for 5 hours. After this, the glass is quickly closed with a lid, cooled in a desiccator to room temperature and weighed.

7.10.6 Processing the results

7.10.6.1 Mass fraction of losses during drying of edible sodium monophosphates 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 glass with the sample after drying, g;

m 2 - mass of a dry cup, g;

100 is the coefficient for converting the result into percentages.

Calculations are carried out by recording the result to the second decimal place.

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

, (8)

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

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

± 0.01d, at R = 0,95, (9)

Repeatability limit r and reproducibility R, as well as the accuracy indicator 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 losses on ignition

The method is based on the ability of food grade monosodium phosphates E339(iii), 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 mass of a sample of food-grade sodium monophosphate before and after calcination.

7.11.1 Measuring instruments, auxiliary equipment

The muffle furnace has a heating range from 50 °C to 1000 °C, ensuring maintenance of the set temperature within ±25 °C.

A drying cabinet that ensures maintenance of a given mode from 20 °C to 200 °C with an error of ±2 °C.

Liquid glass thermometer with a measuring range from 0 °C to 200 °C, division value of 1 °C according to GOST 28498.

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

Desiccator 2-250 according to GOST 25336.

Electronic-mechanical quartz table clocks, wall clocks and alarm clocks in accordance with 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 Carrying out the test

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

A sample weighing from 1 to 2 g, with the weighing result recorded to the third decimal place, is placed open 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 this, the crucible is quickly closed with a lid, cooled in a desiccator to room temperature and weighed.

7.11.5 Processing the results

7.11.5.1 Mass fraction of losses on ignition of edible sodium monophosphates E339(iii) X 7,%, calculated by the formula

(10)

Where T- mass of a dry crucible with a sample sample before calcination, g;

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

m 2 - mass of dry crucible, g;

100 is the coefficient for converting the result into percentages.

Calculations are carried out by recording the result to the second decimal place.

The final result is recorded accurate to the first decimal place.

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

, (11)

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

Average value of two parallel measurements of the mass fraction of losses on ignition, %;

r- repeatability limit value given in Table 6.

The result of the analysis is presented as:

± 0.01d, at R = 0,95, (12)

where is the arithmetic mean value of the results of two determinations considered acceptable, %;

d - limits of relative measurement error, %.

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

7.12 Determination of 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 Transportation and storage

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

8.2 Food grade sodium monophosphates are stored in the manufacturer’s packaging in a cool, dry place in covered warehouses.

8.3 The shelf life of food-grade sodium monophosphates is 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 moisture-retaining agent in the production of bakery and flour confectionery products, alcoholic beverages, products of the meat, fish, fat-and-oil, canning and dairy industries.

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

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

AZO DYES

Preface

1 area of ​​use

2 Normative references

3 Technical requirements

4 Safety requirements

5 Acceptance rules

6 Control methods

7 Transportation and storage

1 area of ​​use

2 Normative references

3 Classification

4 General technical requirements

4.1 Characteristics

4.2 Requirements for raw materials

4.3 Packaging

4.4 Marking

5 Safety requirements

6 Acceptance rules

7 Control methods

7.1 Sampling

7.2 Determination of organoleptic parameters

7.3 Sodium ion test

7.4 Tests for phosphate ions

7.5 Test for free orthophosphoric acid and its disodium salt

7.6 Determination of the mass fraction of the main substance

7.7 Determination of the mass fraction of total phosphorus pentoxide

7.8 Determination of the mass fraction of water-insoluble substances

7.9 Determination of pH of aqueous solution

7.10 Determination of the mass fraction of losses during drying

7.11 Determination of the mass fraction of losses on ignition

7.12 Determination of mass fraction of fluorides

7.13 Determination of the mass fraction of arsenic

7.14 Determination of the mass fraction of lead

8 Transportation and storage

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