- Appendix A (recommended). Determination of the volume fraction of ethyl alcohol in liquid flavorings Appendix B (recommended). Determination of the mass fraction of moisture in flavorings Appendix B (recommended). Determination of the volume fraction of 1,2-propylene glycol in liquid flavorings
Interstate standard GOST 32049-2013
"Food flavorings. General technical conditions"
(put into effect by order of the Federal Agency for Technical Regulation and Metrology dated July 25, 2013 N 441-st)
Food flavourings. General specifications
Preface
The goals, basic principles and basic procedure for carrying out work on interstate standardization are established by GOST 1.0-92 "Interstate standardization system. Basic provisions" and GOST 1.2-2009 "Interstate standardization system. Interstate standards, rules and recommendations for interstate standardization. Rules for development, adoption, application, renewal and cancellation"
1 area of use
This standard applies to food flavorings (hereinafter referred to as flavoring agents) intended for the food industry.
This standard does not apply to flavorings for tobacco products.
Requirements ensuring the safety of flavors for human life and health are set out in 5.1.5 - 5.1.12, product quality requirements - 5.1.2 - 5.1.4, labeling requirements - 5.4.
This standard uses normative references to the following interstate standards:
Notes:
1 The term “natural flavoring” may be used if its flavoring portion consists exclusively of flavoring preparations and/or natural flavoring substances.
2 The term “natural flavor” in combination with the name of the food, food category or source of plant or animal origin can only be used if the flavoring preparations and/or natural flavoring substances contained in it are obtained from the named source, e.g. "natural apple flavor (Apple)", "natural fruit flavor (Fruity)", "natural mint flavor (Mint)".
3 The term “natural flavor” may be used when the flavorings and/or natural flavorings contained in it are obtained from a source that does not reflect their taste and aroma, for example, “natural flavor and fancy name.”
3.5 synthetic flavoring: Flavoring, the flavoring part of which contains synthetic flavoring substances.
3.6 flavoring substance: Chemically defined (chemically individual) substance with flavoring properties, possessing a characteristic aroma and/or taste (excluding sweet, sour and salty).
3.7 natural flavoring substance: A flavoring substance isolated using physical, enzymatic or microbiological processes from raw materials of plant, microbial or animal origin, including those processed by traditional methods of preparing food products.
Note - Traditional methods of preparation (production) of food products include: cooking, including steaming and under pressure (up to 120°C), baking, roasting, stewing, frying, including in oil (up to 240°C at atmospheric pressure), drying, evaporation, heating, cooling, freezing, soaking, maceration (soaking), infusion (brewing), percolation (extraction with straining), filtration, pressing (squeezing), mixing, emulsification, grinding (cutting, crushing, grinding , crushing), encapsulation, peeling, distillation (rectification), extraction (including solvent extraction), fermentation and microbiological processes.
3.8 synthetic flavoring substance: Flavoring substance obtained through chemical synthesis.
3.9 flavor precursor: A product, not necessarily having flavoring properties, intentionally added to food for the sole purpose of obtaining flavor by destruction or reaction with other components during food preparation.
Note - The flavoring precursor can be obtained both from food products and from products not used directly for food.
3.10 flavoring preparation: A mixture of flavoring or other substances isolated by physical, enzymatic or microbiological processes from food products or from food raw materials, including after processing by traditional methods of food preparation, and/or from products of plant, animal or microbial origin, not used directly as food, used as such or processed using traditional food preparation methods.
4 Classification
4.1 Depending on their purpose, food flavorings are divided into:
For flavorings for confectionery and bakery (bread) products;
Flavorings for soft drinks;
Flavorings for fat and oil products;
Flavorings for other food products.
4.2 Depending on the composition of the flavoring part, flavorings are divided into:
For flavorings based on flavoring substances (natural and synthetic);
Flavorings based on flavoring preparations (natural);
Mixed flavors.
4.3 Depending on the form of release, flavorings are divided into:
For liquids: in the form of solutions and emulsions (emulsion);
Dry: powdered, including encapsulated and granulated;
Pasty.
5 General technical requirements
5.1 Characteristics
5.1.1 Flavors are produced in accordance with the requirements of this standard, a regulatory document in accordance with which a flavor of a specific name is produced, in compliance with the requirements,
5.1.2 In terms of organoleptic indicators, flavorings must meet the requirements specified in Table 1.
Table 1 - Organoleptic indicators
|
Indicator name |
Characteristics of flavors |
||
|
pasty |
|||
|
Appearance |
Transparent or opaque |
Homogeneous powder, encapsulated or granular mixture |
Homogeneous mass |
|
Colorless or colored |
Painted or unpainted |
Painted or unpainted |
|
|
Characteristic of a particular flavoring product |
Characteristic of a particular flavoring product |
||
5.1.3 For a flavoring agent of a specific name, in a regulatory document, the manufacturer establishes individual requirements for this flavoring agent for the following organoleptic and physicochemical parameters:
Appearance, color and smell;
Density and refractive index (for liquid flavors, except emulsion, paste and colored);
The volume fraction of ethyl alcohol in alcohol-containing flavorings (for flavorings that, in accordance with legislative and regulatory legal acts in force in the territory of the state that has adopted the standard, belong to alcohol-containing food products);
Mass fraction of moisture (in dry and paste flavors);
Presence of metallomagnetic impurities (in dry flavors), the presence of metallomagnetic impurities in dry flavors is allowed no more than 3 (3 mg/kg);
Flash point (for liquid flavors).
5.1.4 Flavorings are identified by:
By name and purpose, by comparing the flavor indicated in the labeling with the name specified in the definition of the type of food product in, or regulations in force in the territory of the state that has adopted the standard;
By the appearance of the flavoring agent, comparison with the characteristics set out in the regulatory document, in accordance with which the flavoring agent of a specific name is manufactured;
According to organoleptic indicators, comparison with organoleptic characteristics (smell) set out in the regulatory document, in accordance with which the flavor of a specific name is produced;
5.1.5 Microbiological indicators of flavorings must comply with the requirements established by, or regulatory legal acts in force in the territory of the state that has adopted the standard.
5.1.8 The content of potentially hazardous biologically active substances in flavorings made using plant aromatic raw materials and/or extracts and essential oils should not lead to exceeding the permissible levels of potentially hazardous biologically active substances in food products using flavorings in accordance with the requirements, established, or regulatory legal acts in force in the territory of the state that has adopted the standard.
5.1.9 The use of potentially hazardous biologically active substances is not allowed: agaric acid, beta-asarone, aloin, hypericin, capsaicin, quassin, coumarin, mentofuran, methyl eugenol (4-allyl-1,2-dimethoxybenzene), pulegone, safrole (1- allyl-3,4-methylenedioxybenzene), hydrocyanic acid, thujone (alpha and beta), teucrine A, estragole (1-allyl-4-methoxybenzene), as flavoring agents in the production of flavorings and food products.
5.1.10 It is not permitted to use the tetraploid form of Calamus (Acorus calamus L, CE 13) as a source of flavorings, including flavoring substances and preparations.
5.1.11 When using medicinal plants and/or flavoring preparations from medicinal plants as natural sources, their content (in terms of dry raw materials or the biologically active substance contained in them) should not exceed the amount that has a pharmacological effect of 1 kg () food products when used as flavoring preparations (flavors).
5.2 Requirements for raw materials
5.2.1 Raw materials for the production of flavorings must meet the safety requirements established by, or regulatory legal acts in force in the territory of the state that has adopted the standard.
5.2.2 The ingredient composition of flavorings must comply with the requirements established by, or regulatory legal acts in force in the territory of the state that has adopted the standard.
5.2.3 For the production of alcohol-containing flavorings, rectified ethyl alcohol is used from food raw materials with a degree of purification not lower than the highest according to regulatory documents in force in the territory of the state that has adopted the standard.
5.3 Packaging
5.3.1 Packaging of flavors must comply with the requirements established or regulations in force in the territory of the state that has adopted the standard.
5.3.2 Liquid flavorings are packaged:
In polymer canisters with lids, made from materials whose use in contact with flavorings ensures their quality and safety;
Glass containers for food products;
Other containers made from materials whose use in contact with flavorings ensures their quality and safety.
5.3.3 When packaging liquid flavors, at least 5% of the free space of the total capacity of the container must be left in each container.
5.3.4 Dry and paste-like flavors are packaged in polymer conical jars with a clamping lid and a handle in accordance with the regulatory document in force in the territory of the state that has adopted the standard, using film liner bags in accordance with GOST 19360, made from materials whose use in contact with flavors ensures their quality and safety.
5.3.5 It is permitted to use other types of packaging that ensure the safety of dry and paste-like flavors during storage and transportation and are made from materials that meet the requirements established or regulations in force in the territory of the state that has adopted the standard.
5.3.6 Negative deviation of the net contents of the packaging unit from the nominal amount of flavoring must comply with GOST 8.579 (clause 4.2).
5.3.8 When transported by rail, polymer canisters with liquid flavors are packed in wooden boxes in accordance with GOST 13358 or lathing, when transported by air - in corrugated cardboard boxes in accordance with GOST 13516.
Note - Polymer canisters may be transported by road without packaging in transport containers.
5.3.9 When transported by rail and air, polymer cans with dry and paste flavors are packed in corrugated cardboard boxes in accordance with GOST 13516.
Note - Polymer cans can be transported by road without packaging in transport containers.
5.3.10 Glass containers with liquid flavors are packed in corrugated cardboard boxes in accordance with GOST 13516 or plank boxes in accordance with GOST 13358 using auxiliary packaging materials in accordance with the rules for transporting goods on the appropriate mode of transport.
5.3.11 The flaps of corrugated cardboard boxes are covered in the longitudinal and transverse directions with tape made of polymeric materials with an adhesive layer in accordance with GOST 20477 or other packaging materials are used to ensure the safety of the product and the integrity of the container during transportation.
5.3.12 Flavors sent to the Far North and equivalent areas are packaged in accordance with GOST 15846.
5.4 Marking
5.4.1 Labeling of flavors must comply with the requirements established and or regulatory legal acts in force in the territory of the state that has adopted the standard.
5.4.2 The marking of each packaging unit additionally includes the following data:
Lot number or mark identifying the lot;
Gross weight;
Storage conditions;
Designation of this standard;
Designation of the document in accordance with which the flavor of a specific name is manufactured;
Warning: "If accidentally swallowed, induce vomiting, gastric lavage and seek medical attention."
5.4.3 Transport marking - in accordance with GOST 14192 with the application of handling signs indicating the method of handling cargo - in accordance with the requirements established or regulatory legal acts in force in the territory of the state that has adopted the standard, and signs characterizing the type of hazard of the cargo - in accordance with GOST 19433.
6 Safety requirements and environmental protection
6.3 Liquid flavors are classified as flammable (flammable), flammable (GZh) or non-flammable liquids, dry - as flammable materials in accordance with GOST 12.1.044. The indicator of fire and explosion hazard of liquid flavorings - flash point - is given in the document in accordance with which a particular flavoring agent is manufactured.
6.4 When taking samples, conducting analyses, storing and using flavorings, comply with labor protection rules and fire safety rules adopted when working with flammable, combustible (GOST 12.1.004 and fire safety rules in force in the territory of the state that adopted the standard), harmful substances (GOST 12.1.007).
6.5 Fire extinguishing agents: sprayed water, air-mechanical foam, powders, for small fires - fire felt, powder fire extinguishers.
6.6 If the fragrance gets on the skin, it should be washed off with water, washed with soap, and if it gets into the eyes, rinse with plenty of water.
If the flavoring is accidentally ingested, induce vomiting, perform gastric lavage and seek medical attention.
6.7 When storing and transporting flavors, environmental protection is ensured by sealing the container. If it is violated and the flavoring gets into the environment, it must be collected and disposed of.
6.8 When storing, transporting, using and disposing of flavorings to prevent harm to the environment, health and human genetic fund, contamination of soil, surface and ground water is not allowed.
7 Acceptance rules
7.1 Flavorings are taken in batches.
A batch is considered a certain amount of a flavoring agent of the same name, obtained in one technological cycle, in the same packaging, produced by one manufacturer according to one regulatory document, accompanied by shipping documentation that ensures product traceability.
7.2 For quality control and acceptance of flavorings, the following test categories are established:
Acceptance and acceptance;
Periodic.
7.2.1 Acceptance tests are carried out for each batch of flavoring on the quality of packaging and labeling, organoleptic and physico-chemical indicators using random control. To do this, 10% of packaging units are randomly selected from the batch, but not less than three. If the number of packaging units is less than three, each packaging unit is subject to control.
To conduct tests, instantaneous, total, laboratory samples and samples for analysis are taken from the packaging units included in the sample in accordance with section 8.
7.2.2 The results of acceptance tests are documented in a test report in the form accepted by the manufacturer or reflected in a log.
7.2.3 If the results of acceptance tests are negative for at least one quality indicator, repeated tests are carried out for this indicator on a double sample from the same batch. The results of repeated tests apply to the entire batch.
7.2.4 If the results of repeated tests are unsatisfactory for at least one indicator, the entire batch of flavoring is rejected.
7.3 The procedure and frequency of monitoring the content of toxic elements, benzo(a)pyrene, benzo(a)anthracene, biologically active substances, as well as microbiological indicators are established by the manufacturer in the production control program.
7.5 The basis for making a decision to accept a batch of flavoring is the positive results of acceptance tests and preceding periodic tests.
8 Control methods
8.1 Monitoring the compliance of packaging and labeling of flavors with the requirements of this standard is carried out by external inspection of each packaging unit of products from a sample according to 7.2.1.
8.2 Sampling
8.2.1 To check the quality of flavorings according to organoleptic and physicochemical indicators and to determine toxic elements, instant samples are taken from product units included in the sample according to 7.2.1, from which a total and laboratory sample is formed.
For microbiological analyses, sampling is carried out in accordance with GOST 26668.
8.2.2 Snap sample collection, summary sample collection and separation of laboratory sample and sample for analysis
8.2.2.1 Instant samples must be equal in volume (mass). The sum of all instant samples by volume (mass) should be 1.5 - 2.0 times greater than the volume (mass) of the laboratory sample.
The volume (weight) of the laboratory sample and the sample for analysis of the flavoring agent is determined by the regulatory document in accordance with which the flavoring agent of a specific name is manufactured.
8.2.2.2 The number of instant samples of liquid flavor depends on the volume occupied by the flavor. One instant sample is taken along the entire height of the flavoring layer, if its volume is up to 1 inclusive, two instant samples to a depth of 1/3 and 2/3 from the top level, if the volume is more than 1, but does not exceed 10, three instant samples ( from the top, middle and bottom layers) in all cases when the volume of flavoring is more than 10.
8.2.2.3 Instant samples of liquid flavoring are taken with a sampling tube with an extended lower end with a diameter of 6 to 15 mm and a length exceeding the height of the container by several centimeters.
The upper hole of the tube is closed with a thumb or a stopper, immersed to the required depth, the tube is opened for a short time to fill, then closed again and the tube with the sample is removed.
8.2.2.4 Flash samples of the flavor paste are taken with a sampling tube that is lowered vertically to the bottom of the container, then tilted and withdrawn slowly to ensure that the entire contents of the tube are preserved.
When using a probe, it is immersed (screwed in) to the entire depth of the container along the vertical axis. Then the dipstick is removed.
8.2.2.5 Instant samples of dry flavoring are taken with a probe, immersing it to the entire depth of the container along the vertical axis.
8.2.2.6 Taking instant samples of products at the stage of delivery and acceptance to the warehouse is carried out before sealing the container.
8.2.2.7 Place all instant samples in a sample vessel, mix thoroughly and obtain a total sample.
8.2.2.8 A laboratory sample of liquid and paste flavoring is obtained after thoroughly mixing the total sample and simply reducing it to the laboratory sample volume.
8.2.2.9 A laboratory sample of dry flavoring is obtained by reducing the total sample using the quartering method.
8.2.2.10 The laboratory sample for small batches of flavorings may be a total sample, and the total volume or mass of instant samples must be no less than the volume or mass required for testing.
8.3 Labeling of laboratory samples
The isolated laboratory sample of flavoring is thoroughly mixed again, divided into two equal parts and placed in clean, dry glass containers. The vessels are tightly closed with cortical or plugs made of polymeric materials and labeled with the following indication:
Flavor names;
Manufacturer's name;
Type of carrier (solvent, filler, food raw material);
Lot numbers and masses;
Dates of manufacture;
Sampling dates and locations;
Surnames and signatures of the person who took the sample;
Designations of the document in accordance with which the flavor of a specific name is manufactured.
One laboratory sample is used for analysis, the second is sealed and stored for the shelf life established by the manufacturer in case of disagreement in assessing the quality of the flavor for re-analysis.
For a small batch of liquid flavorings, it is allowed to store a laboratory sample of the flavoring used for testing.
Laboratory samples are stored in a place protected from light at a temperature not exceeding 25°C (unless otherwise specified in the regulatory document in accordance with which the flavor of a particular name is manufactured), laboratory samples of dry flavors - at a relative humidity of no more than 75%.
8.5 Odor detection
The method consists of an organoleptic comparison of a sample for flavor analysis with a control sample of the flavor of the given name.
A sample of the flavor of a given name, the smell of which is approved by the manufacturer's tasting council, is taken as a control sample.
For the control sample, a laboratory sample with a volume (weight) of at least 250 (g) of flavoring produced under production conditions is taken. The control sample is stored in a hermetically sealed container for the shelf life established by the manufacturer.
8.5.1 Determination of liquid fragrance odor
Strips of filter paper 10 x 160 mm in accordance with GOST 12026 are simultaneously moistened (approximately 3 cm) in the control sample and the sample for analysis and their smell is compared.
A flavoring agent is considered to comply with the requirements of this standard if the odor of the “wet” strips of the test sample and the control sample is the same.
8.5.2 Odor determination of dry and paste flavorings
A sample for analysis of the flavor and a control sample weighing from 30 to 50 g is placed on a sheet of white filter paper according to GOST 12026 and their smell is assessed.
A flavoring agent is considered to comply with the requirements of this standard if the odor of the test sample and the control sample is the same.
8.6 Determination of the refractive index of liquid flavors - according to GOST 14618.10 (section 4).
8.7 Determination of the density of liquid flavors - according to GOST 14618.10 (section 2 or section 3).
8.8 Determination of the volume fraction of ethyl alcohol in liquid alcohol-containing flavorings is carried out according to the method outlined in Appendix A 8.12 Determination of metallomagnetic impurities - according to GOST 15113.2.
8.13 Determination of benzo(a)pyrene, benzo(a)anthracene and potentially hazardous biologically active substances - according to the regulatory document in force in the territory of the state that has adopted the standard.
9 Transportation and storage
9.1 Flavors are transported by all modes of transport in accordance with the cargo transportation rules in force for the relevant mode of transport.
9.2 Liquid and paste flavorings are stored in closed and darkened rooms at a temperature not exceeding 25°C, unless otherwise specified by the manufacturer.
Notes:
1 When storing liquid flavors, opalescence and precipitation are allowed if this is provided by the manufacturer.
2 When storing paste-like flavors, separation (separation of the liquid phase) is allowed if this is provided by the manufacturer.
3 Before use, flavors must be mixed until smooth.
9.3 Dry flavors are stored in dry, well-ventilated areas at a temperature not exceeding 25°C and relative humidity not exceeding 75%, unless otherwise specified by the manufacturer.
Note - When storing dry flavors, the presence of loosely packed lumps (easily crumbling) is allowed.
9.4 Transportation and storage of fragrances together with chemicals and strong-smelling products and materials is not allowed.
9.5 The shelf life of flavorings is set by the manufacturer.
10 Directions for use
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INTERSTATE COUNCIL FOR STANDARDIZATION, METROLOGY AND CERTIFICATION
(MGS)
INTERSTATE COUNCIL FOR STANDARDIZATION, METROLOGY AND CERTIFICATION
(ISC)
Preface
The goals, basic principles and basic procedure for carrying out work on interstate standardization are established by GOST 1.0-92 “Interstate standardization system. Basic provisions" and GOST 1.2-2009 "Interstate standardization system. Interstate standards, rules and recommendations for interstate standardization. Rules for development, adoption, application, updating and cancellation"
Standard information
1 DEVELOPED by the State Scientific Institution All-Russian Scientific Research Institute of Food Flavors, Acids and Dyes of the Russian Academy of Agricultural Sciences (GNU VNIIPAKK Rosselkhozakademii)
2 INTRODUCED by the Federal Agency for Technical Regulation and Metrology
3 ADOPTED by the Interstate Council for Standardization, Metrology and Certification (protocol dated March 25, 2013 No. 55-P)
4 By Order of the Federal Agency for Technical Regulation and Metrology dated July 25, 2013 No. 441-st, the interstate standard GOST 32049-2013 was put into effect as the national standard of the Russian Federation on January 1, 2014.
5 INTRODUCED FOR THE FIRST TIME
Information about changes to this standard is published in the annual information index “National Standards”, and the 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 monthly information index “National Standards”. Relevant information, notifications and texts are also posted in the public information system - on the official website of the Federal Agency for Technical Regulation and Metrology on the Internet
INTERSTATE STANDARD
FOOD FLAVORS
General technical conditions
Food flavourings.
General specifications
Date of introduction - 2014-01-01
1 area of use
This standard applies to food flavorings (hereinafter referred to as flavoring agents) intended for the food industry.
This standard does not apply to flavorings for tobacco products.
Requirements ensuring the safety of flavors for human life and health are set out in 5.1.5 - 5.1.12, product quality requirements - 5.1.2 - 5.1.4, labeling requirements - 5.4.
2 Normative references
This standard uses normative references to the following interstate standards:
Note - Polymer canisters may be transported by road without packaging in transport containers.
5.3.9 When transported by rail and air, polymer cans with dry and paste flavors are packed in corrugated cardboard boxes in accordance with GOST 13516.
Note - Polymer cans can be transported by road without packaging in transport containers.
5.3.10 Glass containers with liquid flavors are packed in corrugated cardboard boxes in accordance with GOST 13516 or plank boxes in accordance with GOST 13358 using auxiliary packaging materials in accordance with the rules for transporting goods on the appropriate mode of transport.
5.3.11 The flaps of corrugated cardboard boxes are covered in the longitudinal and transverse directions with tape made of polymeric materials with an adhesive layer in accordance with GOST 20477 or other packaging materials are used to ensure the safety of the product and the integrity of the container during transportation.
5.3.12 Flavors sent to the Far North and equivalent areas are packaged in accordance with GOST 15846.
5.4 Marking
5.4.1 Labeling of flavors must comply with the requirements established and or regulatory legal acts in force in the territory of the state that has adopted the standard.
5.4.2 The marking of each packaging unit additionally includes the following data:
Lot number or mark identifying the lot;
Gross weight;
Storage conditions;
Designation of this standard;
Designation of the document in accordance with which the flavor of a specific name is manufactured;
Warning: “If accidentally swallowed, induce vomiting, gastric lavage and seek medical attention.”
5.4.3 Transport marking - in accordance with GOST 14192 with the application of handling signs indicating the method of handling cargo - in accordance with the requirements established or regulatory legal acts in force in the territory of the state that has adopted the standard, and signs characterizing the type of hazard of the cargo - in accordance with GOST 19433.
6 Safety requirements and environmental protection
6.3 Liquid flavors are classified as flammable (flammable), flammable (GZh) or non-flammable liquids, dry - as flammable materials in accordance with GOST 12.1.044. The indicator of fire and explosion hazard of liquid flavors - flash point - is given in the document in accordance with which the flavor of a specific name is manufactured.
6.4 When taking samples, conducting analyses, storing and using flavorings, comply with labor protection rules and fire safety rules adopted when working with flammable, combustible (GOST 12.1.004 and fire safety rules in force in the territory of the state that adopted the standard), harmful substances (GOST 12.1.007).
6.5 Fire extinguishing agents: sprayed water, air-mechanical foam, powders, for small fires - fire felt, powder fire extinguishers.
6.6 If the fragrance gets on the skin, it should be washed off with water, washed with soap, and if it gets into the eyes, rinse with plenty of water.
If the flavoring is accidentally ingested, induce vomiting, perform gastric lavage and seek medical attention.
6.7 When storing and transporting flavors, environmental protection is ensured by sealing the container. If it is violated and the flavoring gets into the environment, it must be collected and disposed of.
6.8 When storing, transporting, using and disposing of flavorings to prevent harm to the environment, health and human genetic fund, contamination of soil, surface and ground water is not allowed.
7 Acceptance rules
7.1 Flavorings are taken in batches.
A batch is considered a certain amount of a flavoring agent of the same name, obtained in one technological cycle, in the same packaging, produced by one manufacturer according to one regulatory document, accompanied by shipping documentation that ensures product traceability.
7.2 For quality control and acceptance of flavorings, the following test categories are established:
Acceptance and acceptance;
Periodic.
7.2.1 Acceptance tests are carried out for each batch of flavoring on the quality of packaging and labeling, organoleptic and physico-chemical indicators using random control. To do this, 10% of packaging units are randomly selected from the batch, but not less than three. If the number of packaging units is less than three, each packaging unit is subject to control.
To conduct tests, instantaneous, total, laboratory samples and samples for analysis are taken from the packaging units included in the sample in accordance with Section 8.
7.2.2 The results of acceptance tests are documented in a test report in the form accepted by the manufacturer or reflected in a log.
7.2.3 If the results of acceptance tests are negative for at least one quality indicator, repeated tests are carried out for this indicator on a double sample from the same batch. The results of repeated tests apply to the entire batch.
7.2.4 If the results of repeated tests are unsatisfactory for at least one indicator, the entire batch of flavoring is rejected.
7.3 The procedure and frequency of monitoring the content of toxic elements, benzo(a)pyrene, benzo(a)anthracene, biologically active substances, as well as microbiological indicators are established by the manufacturer in the production control program.
7.4 The “smell” indicator of the flavoring according to 8.5 is controlled only by the manufacturer
7.5 The basis for making a decision to accept a batch of flavoring is the positive results of acceptance tests and preceding periodic tests.
8 Control methods
8.1 Control of compliance of packaging and labeling of flavors with the requirements of this standard is carried out by external inspection of each packaging unit of products from the sample according to 7.2.1.
8.2 Sampling
8.2.1 To check the quality of flavorings according to organoleptic and physicochemical indicators and to determine toxic elements, instant samples are taken from product units included in the sample according to 7.2.1, from which a total and laboratory sample is formed.
For microbiological analyses, sampling is carried out in accordance with GOST 26668.
8.2.2 Snap sample collection, summary sample collection and separation of laboratory sample and sample for analysis
8.2.2.1 Instant samples must be equal in volume (mass). The sum of all instant samples by volume (mass) should be 1.5 - 2.0 times greater than the volume (mass) of the laboratory sample.
The volume (weight) of the laboratory sample and the sample for analysis of the flavoring agent is determined by the regulatory document in accordance with which the flavoring agent of a specific name is manufactured.
8.2.2.2 The number of instant samples of liquid flavor depends on the volume occupied by the flavor. One instant sample is taken along the entire height of the flavoring layer, if its volume is up to 1 dm 3 inclusive, two instant samples are taken to a depth of 1/3 and 2/3 from the top level, if the volume is more than 1 dm 3, but does not exceed 10 dm 3 , three instant samples (from the upper, middle and lower layers) in all cases when the volume of flavoring is more than 10 dm 3.
8.2.2.3 Instant samples of liquid flavoring are taken with a sampling tube with an extended lower end with a diameter of 6 to 15 mm and a length exceeding the height of the container by several centimeters.
The upper hole of the tube is closed with a thumb or a stopper, immersed to the required depth, the tube is opened for a short time to fill, then closed again and the tube with the sample is removed.
8.2.2.4 Flash samples of the flavor paste are taken with a sampling tube that is lowered vertically to the bottom of the container, then tilted and withdrawn slowly to ensure that the entire contents of the tube are preserved.
When using a probe, it is immersed (screwed in) to the entire depth of the container along the vertical axis. Then the dipstick is removed.
8.2.2.5 Instant samples of dry flavoring are taken with a probe, immersing it to the entire depth of the container along the vertical axis.
8.2.2.6 Taking instant samples of products at the stage of delivery and acceptance to the warehouse is carried out before sealing the container.
8.2.2.7 Place all instant samples in a sample vessel, mix thoroughly and obtain a total sample.
8.2.2.8 A laboratory sample of liquid and paste flavoring is obtained after thoroughly mixing the total sample and simply reducing it to the laboratory sample volume.
8.2.2.9 A laboratory sample of dry flavoring is obtained by reducing the total sample using the quartering method.
8.2.2.10 The laboratory sample for small batches of flavorings may be a total sample, and the total volume or mass of instant samples must be no less than the volume or mass required for testing.
8.3 Labeling of laboratory samples
The isolated laboratory sample of flavoring is thoroughly mixed again, divided into two equal parts and placed in clean, dry glass containers. The vessels are tightly closed with cortical or plugs made of polymeric materials and labeled with the following indication:
Flavor names;
Manufacturer's name;
Type of carrier (solvent, filler, food raw material);
Lot numbers and masses;
Dates of manufacture;
Sampling dates and locations;
Surnames and signatures of the person who took the sample;
Designations of the document in accordance with which the flavor of a specific name is manufactured.
One laboratory sample is used for analysis, the second is sealed and stored for the shelf life established by the manufacturer in case of disagreement in assessing the quality of the flavor for re-analysis.
For a small batch of liquid flavorings, it is allowed to store a laboratory sample of the flavoring used for testing.
Laboratory samples are stored in a place protected from light at a temperature not exceeding 25 ° C (unless otherwise specified in the regulatory document in accordance with which the flavor of a particular name is manufactured), laboratory samples of dry flavors - at a relative humidity of no more than 75%.
8.4 Determination of appearance and color of flavorings
8.4.1 The appearance and color of liquid and paste flavoring is determined by viewing a sample for analysis in an amount of 30 to 50 cm 3 in a glass B-1(2)-50(100) according to GOST 25336 against the background of a sheet of white paper in transmitted or reflected light .
8.4.2 The appearance and color of the dry flavor is determined by viewing a sample for analysis weighing from 30 to 50 g, placed on a sheet of white filter paper according to GOST 12026, in diffuse daylight or under the light of LD fluorescent lamps according to GOST 6825.
8.4.3 A flavoring agent is considered to comply with the requirements of this standard if the appearance and color of the analytical sample meet the requirements of 5.1.3.
8.5 Odor detection
The method consists of an organoleptic comparison of a sample for flavor analysis with a control sample of the flavor of the given name.
A sample of the flavor of a given name, the smell of which is approved by the manufacturer's tasting council, is taken as a control sample.
For a control sample, a laboratory sample with a volume (weight) of at least 250 cm 3 (g) of flavoring produced under production conditions is taken. The control sample is stored in a hermetically sealed container for the shelf life established by the manufacturer.
8.5.1 Determination of liquid fragrance odor
Strips of filter paper 10x160 mm in accordance with GOST 12026 are simultaneously moistened (by approximately 3 cm) in the control sample and the sample for analysis and their smell is compared.
A flavoring agent is considered to comply with the requirements of this standard if the odor of the “wet” strips of the test sample and the control sample is the same.
8.5.2 Odor determination of dry and paste flavorings
A sample for analysis of the flavor and a control sample weighing from 30 to 50 g is placed on a sheet of white filter paper according to GOST 12026 and their smell is assessed.
A flavoring agent is considered to comply with the requirements of this standard if the odor of the test sample and the control sample is the same.
8.6 Determination of the refractive index of liquid flavors - according to GOST 14618.10 (section 4).
8.7 Determination of the density of liquid flavors - according to GOST 14618.10 (section 2 or section 3).
8.8 Determination of the volume fraction of ethyl alcohol in liquid alcohol-containing flavorings is carried out according to the method described in Appendix A.
8.9 Determination of the mass fraction of moisture in dry and paste flavors - according to GOST 14618.6 (section 3 or section 4) or according to the method outlined in Appendix B.
If disagreements arise, the method in accordance with GOST 14618.6 (section 3) is used as an arbitration method.
8.10 Determination of microbiological parameters of flavorings:
The number of mesophilic aerobic and facultative anaerobic microorganisms - according to GOST 10444.15;
The number of coliform bacteria (coliform bacteria) - according to GOST 31747;
Yeast and molds - according to GOST 10444.12;
Bacteria such as salmonella - according to GOST 31659;
The number of sulfite-reducing clostridia is according to GOST 29185.
8.11 Determination of the content of toxic elements:
8.13 Determination of benzo(a)pyrene, benzo(a)anthracene and potentially hazardous biologically active substances - according to the regulatory document in force in the territory of the state that has adopted the standard.
8.14 Determination of flash point - according to GOST 12.1.044.
8.15 Determination of the volume fraction of 1,2-propylene glycol in liquid flavorings - according to Appendix B.
9 Transportation and storage
9.1 Flavors are transported by all modes of transport in accordance with the cargo transportation rules in force for the relevant mode of transport.
9.2 Liquid and paste flavorings are stored in closed and darkened rooms at a temperature not exceeding 25 ° C, unless otherwise specified by the manufacturer.
Notes:
1 When storing liquid flavors, opalescence and precipitation are allowed if this is provided by the manufacturer.
2 When storing paste-like flavors, separation (separation of the liquid phase) is allowed if this is provided by the manufacturer.
3 Before use, flavors must be mixed until smooth.
9.3 Dry flavors are stored in dry, well-ventilated areas at a temperature not exceeding 25 ° C and a relative humidity of not more than 75%, unless otherwise specified by the manufacturer.
Note - When storing dry flavors, the presence of loosely packed lumps (easily crumbling) is allowed.
9.4 Transportation and storage of fragrances together with chemicals and strong-smelling products and materials is not allowed.
9.5 The shelf life of flavorings is set by the manufacturer.
10 Directions for use
The scope of application and maximum dosages of flavorings must comply with the requirements established or regulatory legal acts in force in the territory of the state that has adopted the standard and are established by the manufacturer.
Determination of the volume fraction of ethyl alcohol in liquid flavorings
This chromatographic method is designed to determine the volume fraction of ethyl alcohol in liquid flavorings, using a packed column and a flame ionization detector.
The measurement range for the volume fraction of ethyl alcohol is from 1.0% to 85.0% inclusive.
A.1 Essence of the method
The method is based on the chromatographic separation of flavor components and ethyl alcohol on a polyaromatic macroporous sorbent using a “cold” sample injection (at a temperature below the boiling point of the analyte) and subsequent detection of ethyl alcohol with a flame ionization detector.
A.2 Safety requirements
A.2.1 When working on a gas chromatograph, it is necessary to comply with labor protection requirements and safety rules in accordance with the operating instructions for the device.
A.2.2 When performing the analysis, 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.
A.2.3 The room in which measurements are carried out must be equipped with general supply and exhaust ventilation in accordance with GOST 12.4.021.
A.2.4 Electrical safety when working with electrical installations - according to GOST 12.2.007.0 and according to GOST 12.1.019.
A.2.5 Organization of occupational safety training for workers - in accordance with GOST 12.0.004.
A.2.6 The laboratory premises must comply with fire safety requirements in accordance with GOST 12.1.004 GOST 12.4.009.
A.3 Measuring instruments, auxiliary equipment, glassware, reagents and materials
Gas chromatograph, equipped with a flame ionization detector with a nonane sensitivity of at least 1·10 - 11 g/cm 3
A computer or integrator that has software for a basic set of chromatography automation operations.
Volumetric flasks with a ground stopper with a capacity of 100 cm 3 of the 1st accuracy class according to GOST 1770.
Pipettes with one mark with a capacity of 25, 50 cm 3 of the 1st accuracy class according to GOST 29169.
Packed chromatographic column made of stainless steel, 1 m long and with an internal diameter of 3 mm, filled with a polyaromatic macroporous sorbent - a copolymer of styrene (60%) and divinylbenzene (40%) (Polysorb 1), with a particle size from 0.25 to 0.50 mm . It is permissible to use a longer column and increase the temperature of the column thermostat, provided that the analysis time is increased. The use of other sorbents is not allowed.
Technical hydrogen grade A - according to GOST 3022. The use of a hydrogen generator is permitted.
Rectified ethyl alcohol according to the regulatory document in force in the territory of the state that has adopted the standard.
A.4 Preparation for measurements
A.4.1 Measurement conditions
When preparing for measurement and during measurement, the following conditions must be observed:
ambient air temperature…………………………………. from 20 °C to 25 °C;
atmospheric pressure……………… from 95.0 to 106.7 kPa (from 720 to 800 mm Hg);
relative humidity ……………………………………. from 40% to 90%;
mains voltage …………………………………………………… ;
frequency of current in the electrical network…………………………………………… from 49 to 51 Hz.
A.4.2 Preparation of the chromatographic column
The chromatographic column is washed successively with water, ethyl alcohol, acetone, dried in a stream of air and filled with sorbent.
The filled column is placed in the chromatograph thermostat, connected to the evaporator without connecting to the detector, then the column is purged with a carrier gas (nitrogen) at a speed of 40 cm 3 /min in temperature programming mode: increasing the temperature to 170 °C at a speed of 4 °C/ min to 6 °C/min, then at a temperature of 170 °C for 0.5 to 1.0 hours. The prepared column is connected to the detector and the stability of the zero line is checked at the operating temperature of the column thermostat according to A.7.
A.4.3 Preparation of measuring equipment
The chromatograph is prepared for operation in accordance with its operating instructions.
The device is calibrated using calibration solutions in accordance with A.5.2.
A.4.4 Preparation of calibration solutions
As calibration solutions, solutions of ethyl alcohol in distilled water with volume fractions (vol. %) close to the specified measurement range are used.
Before preparing solutions, determine the content of the main substance in the ethyl alcohol used according to GOST 3639. To calibrate the device, prepare at least seven calibration solutions.
Into each of seven volumetric flasks with a ground stopper with a capacity of 100 cm 3 add 10 cm 3 of distilled water and the required amount of ethyl alcohol in accordance with Table A.1. The contents of the flasks are mixed and the volumes of solutions are adjusted to the mark with distilled water (calibration solutions No. 1 - 7).
Calibration solutions are stored at temperatures from 0 °C to 10 °C in sealed containers for 6 months.
Table A.1 - Composition of calibration solutions
Volume fraction of ethyl alcohol Q g, %, in calibration solutions is determined by density after holding the solutions for 2 to 3 hours with a pycnometer according to GOST 3639 (section 3), followed by converting the density values of the aqueous-alcohol solution to the alcohol content in percent (by volume).
A.5 Taking measurements
A.5.1 Measurements are performed under the following operating parameters of the chromatograph:
column thermostat temperature ………………………………… 80 C;
evaporator (injector) temperature ……………………………. from 45 °C to 55 °C;
temperature of the transition chamber……………………………. 80 C;
flow rate of carrier gas (nitrogen) …………………………… from 30 to 40 cm 3 /min;
hydrogen flow rate…………………………………………. 30 cm 3 /min;
air flow speed ……………………………………………………… 300 cm 3 /min;
sample volume for analysis …………………………………………... 0.2 mm 3.
After analysis of 20 - 30 samples, the temperature of the evaporator, column thermostat and transition chamber is increased to 150 ° C and maintained for 30 to 40 minutes to clean the chromatographic system from high-boiling compounds.
A.5.2 Establishment of calibration characteristic
To determine the calibration coefficient, it is necessary to chromatograph at least four calibration solutions with an ethyl alcohol content corresponding to the entire measurement range. Each calibration mixture is analyzed at least three times.
The dependence of the volume fraction of ethyl alcohol in the analyzed sample on the peak area is expressed by the equation
where is the arithmetic mean value of the three areas of chromatographic peaks obtained during the analysis j th calibration solution;
A j 1 , A j 2 , A j 3 - areas of chromatographic peaks of three analyzes j
Q j- volume fraction of ethyl alcohol in j-th calibration solution, % (vol.).
Calculate the average value using the formula
Where n- number of calibration solutions.
The calibration procedure is carried out periodically, at least once a week, when installing the method on a chromatograph, or after repairing the chromatograph.
A.5.3 Sample analysis
After establishing the operating parameters, turning on the analysis automation system to record chromatograms and process the obtained data, and a stable zero line on the working scale of the detector, analysis begins.
To determine the volume fraction of ethyl alcohol in the analyzed flavoring sample, use a laboratory sample according to 8.2.
3 samples are injected into the evaporator (injector) with a microsyringe of 0.2 mm and chromatographic analysis is performed under conditions A.5.1. A peak is recorded in the retention time region corresponding to ethyl alcohol. The analysis is repeated at least twice.
When calibrating and analyzing, it is imperative to use the same microsyringe.
A.6 Processing of results
A.6.1 The results are processed using the software of the personal computer or integrator included with the chromatograph in accordance with their operating instructions.
A.6.2 Volume fraction of ethyl alcohol in the analyzed flavor sample X, % (vol.), calculated by the formula
Where X- volume fraction of ethyl alcohol in flavoring, % (vol.);
δ - relative error in determining the volume fraction of ethyl alcohol, % (vol.).
The arithmetic mean of two parallel determinations is taken as the final result of the determinations. X avg, %, rounded to the first 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= 0.95%, does not exceed repeatability limit r = 10,00 %.
The absolute value of the difference between the results of two determinations obtained under reproducibility conditions at P= 0.95%, does not exceed the reproducibility limit R = 15,00 %.
The relative error limits of the method for determining the volume fraction of ethyl alcohol are ±15.0% at P = 0,95 %.
A.7 Monitoring the stability of the chromatograph zero line
Monitoring is carried out continuously during the analysis of flavors. The positive drift of the zero line, defined as the greatest shift of the zero line signal within 20 minutes from the start of the analysis, should not exceed 20% of the peak height corresponding to a volume fraction of ethyl alcohol of 1% (calibration solution No. 1). If the specified value is exceeded or side peaks appear, it is necessary to raise the temperature of the column, evaporator and transition chamber to 150 °C and maintain it for 30 to 40 minutes to accelerate the elution of high-boiling components of the analyzed mixtures.
Determination of the mass fraction of moisture in flavorings
This method is intended to measure the moisture mass fraction of flavorings dissolved in liquids that do not react with Fischer's reagent.
The method provides measurements in the range of mass fraction of moisture from 0.8% to 50% inclusive.
B.1 Essence of the method
The method is based on the interaction of iodine with sulfur oxide (IV) and water in a medium of methanol and pyridine during the titration of the analyzed sample with a Fischer reagent. The equivalence point is determined electrometrically by the appearance of a current between two electrodes with the appearance of free iodine in the solution.
B.2 Safety requirements
B.2.1 When working on an automatic titrimetric analyzer for electrometric titration of moisture according to the K. Fischer method, it is necessary to comply with labor protection requirements and safety rules in accordance with the operating instructions for the device.
B.2.2 When performing analysis, 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.
B.2.3 The room in which measurements are carried out must be equipped with general supply and exhaust ventilation in accordance with GOST 12.4.021.
B.2.4 Electrical safety when working with electrical installations - in accordance with GOST 12.2.007.0 and regulatory documents in force in the territory of the state that has adopted the standard.
B.2.5 Organization of occupational safety training for workers - in accordance with GOST 12.0.004.
B.2.6 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.
B.2.8 All operations with Fischer reagent should be carried out in a fume hood.
B.3 Measuring instruments, auxiliary equipment, glassware, reagents and materials
Scales in accordance with regulatory documents in force in the territory of the state that has adopted the standard, with a standard deviation value (RMS) not exceeding 0.3 mg, and an error from nonlinearity not exceeding ±0.6 mg.
Automatic titrimetric analyzer for electrometric titration of moisture according to the K. Fischer method with a measurement range of the mass fraction of moisture from 0.5% to 50.0% and a standard deviation limit of the relative measurement error of ±0.4% (at 25 mg of moisture).
Conical flasks Kn-1-500-40 TS, Kn-1-500-40 THS with ground section, capacity 500 cm 3 according to GOST 25336.
Microsyringe with a capacity of 0.01 cm 3 .
Fischer reagent No. 1 (sulfur dioxide in methanol), analytical grade. according to GOST 14870.
Fischer reagent No. 2 (iodine in methanol), analytical grade. according to GOST 14870.
Methanol is a poison (methyl alcohol), x. parts according to GOST 6995.
It is allowed to use other measuring instruments, materials and reagents with metrological characteristics and quality not lower than those specified.
B.4 Preparation for measurements
B.4.1 Measurement conditions
When performing measurements in the laboratory, the following conditions must be met:
Ambient air temperature .................................................... from 10 °C to 35 °C;
Atmospheric pressure from ……………… 84.0 to 106.7 kPa (from 630 to 800 mm Hg);
Relative air humidity…………………………………….. no more than 80%;
Mains voltage……………………………………………………………….
B.4.2 Sampling - according to 8.2.
B.4.3 The automatic titrimetric analyzer is prepared in accordance with its operating instructions.
B.4.4 Preparation of working solution of Fischer reagent
In a conical flask with a capacity of 500 cm 3, 100 cm 3 of Fischer reagent No. 1 and Fischer reagent No. 2 are sequentially measured, stoppered and mixed. The resulting working solution is poured into a bottle marked “Fischer reagent,” which is connected to the pump of the titration unit of an automatic titrimetric analyzer, preventing the formation of bubbles, and incubated for 24 hours.
B.4.5 Methanol poison is poured into a bottle marked “Methanol poison”, which is connected to the pump of the titration unit of an automatic titrimetric analyzer.
Note - When connecting bottles with ready-made reagents to the pump of the titration unit of an automatic titrimetric analyzer, you should make sure that all caps fit tightly and that the float in the drain bottle moves freely in a vertical plane.
B.4.6 Raise the pump cover of the titration unit until it stops and move the holder of the reaction vessel until it stops in order to completely isolate the container.
B.4.7 Calibrate the automatic titrimetric analyzer by titrating a given volume of distilled water ( V= 0.01 cm 3) daily, before taking measurements in accordance with the operating instructions for the device. Calibration is considered completed if the coefficient of variation for three results out of ten does not exceed the norm established in the operating instructions for the device.
B.4.8 Sample preparation
In a glass with a capacity of 50 cm 3, weigh from 0.2 to 0.3 g of dry flavor or from 0.2 to 1.0 g of paste flavor, or from 0.5 to 1.0 g of liquid flavor, recording the weighing result to the third decimal sign.
B.5 Taking measurements
B.5.1 The flavor sample is introduced into the reaction vessel of an automatic titrimetric analyzer, and the operation should be performed as quickly as possible to minimize the ingress of moisture from the air.
Note - If within 60 With the analyzed sample will not be added to the reaction vessel, the device will return to conditioning mode.
B.5.2 Measurements are carried out in accordance with the operating instructions for the automatic titrimetric analyzer, recording the result to the second decimal place.
B.6 Processing results
The numerical value of the final measurement result and the value of the absolute measurement error limits are expressed in no more than two significant figures.
The arithmetic mean value is taken as the final result of the determination WITH avg, %, results of two parallel determinations, if the acceptance condition is met
Where WITH cf - arithmetic mean value of the results of two parallel determinations of the mass fraction of moisture found acceptable, %;
δ - limits of relative measurement error, %.
Repeatability limit r and reproducibility R, as well as the accuracy indicator, δ, of measurements of the mass fraction of moisture in flavors are given in Table B.1.
Determination of the volume fraction of 1,2-propylene glycol in liquid flavorings is performed by chromatographic method.
The range of measured volume fractions of 1,2-propylene glycol is from 1.0% to 92.0% inclusive.
B.1 Essence of the method
The method is based on gas chromatographic separation of flavoring components on a device with a flame ionization detector and the use of two types of chromatography: gas adsorption and gas-liquid.
B.2 Measuring instruments, auxiliary equipment, glassware, materials and reagents
Scales with a standard deviation value (RMS) not exceeding 0.3 mg, and with an error from nonlinearity not exceeding ±0.6 mg.
Stopwatch of 2nd accuracy class with a counter scale capacity of 30 min, division value of 0.20 s, error ±0.60 s.
Thermometer TL-31-A, temperature measurement limits from 0 °C to 250 °C according to GOST 28498.
Gas chromatograph, equipped with a flame ionization detector with a nonane sensitivity of at least 1·10 -11 g/cm 3 .
A computer or integrator that has software for a basic set of chromatography automation operations.
Packed chromatographic column made of stainless steel, 1 m long and with an internal diameter of 3 mm. If necessary, it is possible to use a longer column and increase the temperature of the column thermostat when increasing the analysis time.
Water jet vacuum pump according to GOST 25336.
Microsyringe with a capacity of 0.5 mm 3.
Measuring glassware according to GOST 1770.
Pipettes 2-1-5, 2-1-10, 2-1-20, 2-1-25, 4-2-1 according to GOST 29227.
Glass bottles with a capacity of 5 to 15 cm 3 with silicone rubber stoppers.
Sorbent based on hydrated microamorphous silica treated with hexamethyldisilazane (Chromaton N-AW HMDS type) and polyethylene glycol 20000 (Carbowax type) in an amount of 15%, with a particle size from 0.20 to 0.36 mm.
Rectified ethyl alcohol according to regulatory documents in force in the territory of the state that has adopted the standard.
It is allowed to use similar measuring instruments, materials and reagents with metrological characteristics and quality not lower than those specified.
B.3 Preparation for measurements
B.3.1 Measurement conditions
During preparation and measurement and during measurement, the following conditions must be observed:
Ambient air temperature…………………………………… (20 ± 2) °C;
Atmospheric pressure…………… from 95.0 to 106.7 kPa (from 720 to 800 mm Hg);
Relative humidity …………………………………. from 20% to 90%;
Mains voltage………………………………………………………………. (220 ± 20) V;
Electrical frequency ……………………………………………………… (50 ± 2) Hz.
B.3.2 Preparation of the chromatographic column
Chromatographic columns are washed successively with water, ethyl alcohol, acetone, dried in a stream of air and filled with a packing.
The filled columns are placed in the chromatograph thermostat and connected to the evaporator without connecting to the detector. The column is conditioned with a carrier gas (nitrogen) at a rate of 40 cm 3 /min in temperature programming mode at a rate of 4 °C/min to 6 °C/min to 170 °C and maintained for 0.5 to 1.0 h at this temperature.
After cooling, the output end of the columns is connected to the detector and the stability of the zero line is checked at the operating temperature of the column thermostat.
B.3.3 Preparation of measuring equipment
The chromatograph is prepared for operation in accordance with the operating instructions supplied with the device.
The device is calibrated using calibration solutions.
B.3.4 Preparation of calibration solutions
Solutions of 1,2-propylene glycol in distilled water with volume fractions (vol. %) close to the specified measurement range are used as calibration solutions.
Solutions are prepared using 1,2-propylene glycol with a volume fraction of the main substance of at least 99.0%.
Eight volumetric flasks with a ground stopper with a capacity of 50 cm 3 are poured from 20 to 30 cm 3 of distilled water, added sequentially with pipettes of 0.5; 5.0; 10.0; 20.0 cm 3 and cylinders 30; 40; 46 cm 3 1,2-propylene glycol. The contents of the flasks are mixed and the volumes of solutions are adjusted to the mark with distilled water (calibration solutions No. 1 - No. 8).
The volume fraction of 1,2-propylene glycol,%, in calibration solutions is determined by the formula
Where V rp - aliquot fraction of 1,2-propylene glycol, cm 3;
Q ref - volume fraction of the main substance in 1,2-propylene glycol, %;
50 - volume of calibration solution, cm 3.
B.4 Taking measurements
B.4.1 Measurements are performed under the following operating parameters of the chromatograph for gas adsorption chromatography:
Column thermostat temperature…………………………….… 170 °C;
Evaporator (injector) temperature ………………………...... (170 ± 5) °C;
Temperature of the transition chamber…………………………….…. 170 °C;
Nitrogen carrier gas consumption……………………………………… from 30 to 40 cm 3 /min;
Hydrogen consumption …………………………………………………… 30 cm 3 /min;
Air consumption…………………………………………………….. 300 cm 3 /min;
Sample volume ……………………………………………………….. from 0.1 to 0.5 mm 3 ;
for gas-liquid chromatography:
Column thermostat temperature………………………………. 150 °C;
Evaporator (injector) temperature ………………………….. (200 ± 5) °C;
Temperature of the transition chamber……………………………..… 150 °C;
Nitrogen carrier gas consumption……………………………..….. from 30 to 40 cm 3 /min;
Hydrogen consumption……………………………………..……… 30 cm 3 /min;
Air flow…………………………………………….…… 300 cm 3 /min;
Sample volume……………………………………………………….. from 0.1 to 0.5 mm 3.
B.4.2 Establishment of calibration characteristic
The calibration of the flame ionization detector of the chromatograph is performed using the absolute calibration method.
To determine the calibration coefficient, it is necessary to chromatograph at least four calibration solutions containing 1,2-propylene glycol corresponding to the working measurement range.
Using a microsyringe with a capacity of 1.0 mm 3 , washed 8 to 10 times with the analyzed calibration solution of 1,2-propylene glycol, 0.1 to 0.5 mm 3 samples are taken and introduced into the chromatograph evaporator.
Each calibration mixture is analyzed at least three times.
The dependence of the volume fraction of 1,2-propylene glycol on the peak area is expressed by the equation
Where A j 1 , A j 2 , A j 3 - areas of chromatographic peaks of three parallel measurements j th calibration solution, units. accounts;
Q j- volume fraction of 1,2-propylene glycol j th sample, %.
The average value of the calibration coefficient is calculated using the formula
Where n- number of calibration solutions.
The calibration procedure is carried out when the method is installed on a chromatograph, after repair of the chromatograph, after a negative control result.
Periodic monitoring of calibration coefficients is carried out in accordance with B.5.4.
The calibration characteristic is checked at one of the points in the range of measured concentrations daily in accordance with B.6.5.
B.4.3 Gas chromatographic analysis of a flavor sample
When calibrating and analyzing, it is imperative to use the same syringe. After establishing the operating parameters, turning on the analysis automation system for recording chromatograms and processing the obtained data, and a stable zero line on the working scale of the detector, analysis begins.
To determine the volume fraction of 1,2-propylene glycol in the analyzed sample, three times from 0.1 to 0.5 mm 3 of the analyzed food flavoring are introduced into the chromatograph evaporator with a microsyringe, using a chromatographic column that ensures optimal separation of 1,2-propylene glycol from other components of the flavoring. Based on the obtained chromatograms of the analyzed sample, the peak areas are measured and the average peak area of 1,2-propylene glycol is calculated.
B.5 Processing of results
B.5.1 The results are processed using the software of the personal computer or integrator included with the chromatograph in accordance with their operating instructions.
B.5.2 Volume fraction of 1,2-propylene glycol in the analyzed flavor sample X, %, calculated by the formula
Where X- volume fraction of 1,2-propylene glycol in flavoring,%;
δ is the relative error in measuring the volume fraction of 1,2-propylene glycol, %.
B.5.4 Relative error δ of measuring the volume fraction of 1,2-propylene glycol in flavorings with a confidence level P= 0.95 is for flavors with a volume fraction of 1,2-propylene glycol:
From 1% to 15% inclusive.................................................... ................................... ±15%;
From 15% to 92% inclusive.................................... ...................................±8%.
B.6 Monitoring the accuracy of measurement results
When monitoring measurement accuracy using this method, perform the following operations:
B.6.1 Monitoring the stability of the chromatograph zero line
Monitoring is carried out continuously during the analysis of food flavorings. The positive drift of the zero line, defined as the greatest shift of the zero line signal within 20 minutes from the start of the analysis, should not exceed 20% of the peak height corresponding to the volume fraction of 1,2-propylene glycol 1% (calibration solution No. 1). If the specified value is exceeded or side peaks appear, it is necessary to raise the temperature of the column, evaporator and transition chamber to 200 °C and maintain it for 30 to 40 minutes to accelerate the elution of high-boiling components of the analyzed mixtures.
B.6.2 Monitoring the convergence of chromatograph output signals
The controlled parameter is the relative range of the chromatograph output signals. Control is carried out during calibration and during periodic monitoring of calibration coefficients. The control result is considered positive when the condition is met
Where A max - maximum chromatographic peak area, units. accounts;
A min - minimum chromatographic peak area, units. accounts;
Arithmetic mean value of peak areas obtained from parallel injections of samples, units. accounts;
M- relative range of the chromatograph output signal, %.
Values M depending on the value of the volume fraction of 1,2-propylene glycol are given in Table B.1
Table B.1
In percentages
B.6.3 Monitoring the correctness of the construction of the calibration characteristic
The controlled parameter is the range of calibration coefficients relative to the average value.
The calibration quality is considered satisfactory if the condition is met
Where K max - maximum value of the calibration coefficient of 1,2-propylene glycol in the range of analyzed volume fractions, %/unit. accounts;
K min - minimum value of the calibration coefficient of 1,2-propylene glycol in the range of analyzed volume fractions, %/unit. accounts;
Average value of the calibration coefficient of 1,2-propylene glycol, %/unit. accounts;
B- range of the calibration coefficient, %.
Values B depending on the value of the volume fraction of 1,2-propylene glycol are given in Table B.1.
Control is carried out each time when constructing a calibration dependence. If condition (B.9) is not met, then the device is re-calibrated.
B.6.4 Monitoring the stability of the calibration characteristic
Monitoring is carried out at least once a quarter, as well as when changing a column, washing the detector, etc. The monitoring frequency can be increased at higher intensity of operation of the device. Control is carried out using freshly prepared calibration solutions according to B.3.4. Three solutions are used at the beginning, middle and end of the working measurement range. Samples are introduced into the chromatograph using a microsyringe.
The control results are considered positive when the condition is met
Where K- previously set value of the calibration coefficient;
The average value of the calibration coefficient, calculated according to formula (B.5);
L- standard for periodic monitoring of the stability of the calibration characteristic, %.
Values L depending on the value of the volume fraction of 1,2-propylene glycol are given in Table B.1.
B.6.5 Daily monitoring of the stability of the calibration characteristic
Control is carried out daily at the beginning of the working day using a calibration solution close in value to the determined proportion of 1,2-propylene glycol. The sample is introduced into the chromatograph using a microsyringe.
The control results are considered positive when the condition is met
Where Qi- volume fraction of 1,2-propylene glycol in i-th sample, %;
A i- area of the chromatographic peak of 1,2-propylene glycol in the sample, units. accounts;
N- standard for daily monitoring of the stability of the calibration characteristic, %.
Values N depending on the volume fraction of 1,2-propylene glycol are given in Table B.1.
If the control results are negative, it is necessary to calibrate the device in accordance with B.4.2.
B.7 Safety requirements
B.7.1 When working on a gas chromatograph, it is necessary to comply with labor protection requirements and safety rules in accordance with the operating instructions for the device.
B.7.2 The room in which the measurement is carried out must be equipped with general supply and exhaust ventilation.
Bibliography
TR CU 021/2011 “On food safety”
Technical Regulations of the Customs Union TR CU 029/2012 “Safety requirements for food additives, flavorings and technological aids”
Technical Regulations of the Customs Union TR CU 005/2011 “On Packaging Safety”
Technical Regulations of the Customs Union TR CU 022/2011 “Food products regarding their labeling”
Key words: aroma food mash, classification, safety and quality indicators, technical requirements, control methods
INTERSTATE COUNCIL FOR STANDARDIZATION. METROLOGY AND CERTIFICATION
INTERSTATE COUNCIL FOR STANDARDIZATION. METROLOGY AND CERTIFICATION
INTERSTATE
STANDARD
FOOD FLAVORS
General technical conditions
Official publication
Staydarinform
Preface
The goals, basic principles and basic procedure for carrying out work on interstate standardization are established by GOST 1.0-92 “Interstate standardization system. Basic provisions" and GOST 1.2-2009 "Interstate standardization system. Interstate standards. rules and recommendations for interstate standardization. Rules for development, adoption, application, updating and cancellation"
Standard information
1 DEVELOPED by the State Scientific Institution All-Russian Scientific Research Institute of Food Flavors, Acids and Dyes of the Russian Academy of Agricultural Sciences (GNU VNIIPAKK Rosselkhozakademii)
2 INTRODUCED by the Federal Agency for Technical Regulation and Metrology
3 ADOPTED by the Interstate Council for Standardization, Metrology and Certification (protocol dated March 25, 2013 No. 55-P)
4 By Order of the Federal Agency for Technical Regulation and Metrology dated July 25, 2013 No. 441-st, the interstate standard GOST 32049-2013 was put into effect as a national standard of the Russian Federation on January 1, 2014.
5 INTRODUCED FOR THE FIRST TIME
Information about changes to this standard is published in the annual information index “National Standards”. and the text of changes and amendments is 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 monthly information index “National Standards”. Relevant information, notifications and texts are also posted in the public information system - on the official website of the Federal Agency for Technical Regulation and Metrology on the Internet
€> Standardinform. 2014
In the Russian Federation, this standard cannot be reproduced in whole or in part. replicated and distributed as an official publication without permission from the Federal Agency for Technical Regulation and Metrology
INTERSTATE STANDARD
FOOD FLAVORS
General technical conditions
Food flavourings.
General specifications
Date of introduction -2014-01-01
1 area of use
This standard applies to food flavorings (hereinafter referred to as flavoring agents) intended for the food industry.
This standard does not apply to flavorings for tobacco products.
The requirements to ensure the safety of flavors for human life and health are set out in 5.1.5-5.1.12. product quality requirements - 5.1.2-5.1.4. labeling requirements - 5.4.
2 Normative references
This standard uses normative references to the following interstate standards:
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 12.0.004-90 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 12.1.019-79 System of occupational safety standards. Electrical safety. General requirements and nomenclature of types of protection
GOST 12.1.044-89 (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 12.4.021-75 System of occupational safety standards. Ventilation systems. General requirements
GOST 12.4.103-83 System of occupational safety standards. Special protective clothing, personal protective equipment for legs and arms. Classification
GOST 1770-74 (ISO 1042-83. ISO 4788-80) Laboratory glassware. Cylinders. beakers, flasks, test tubes. General technical conditions
Official publication
GOST 2603-79 Reagents. Acetone. Technical specifications GOST 3022-80 Technical hydrogen. Specifications
GOST 3630-79 Water-alcohol solutions. Methods for determining the concentration of ethyl alcohol GOST 6709-72 Distilled water. Technical specifications GOST 6825-91 Tubular fluorescent lamps for general lighting GOST 6995-77 Reagents. Methanol is a poison. Technical specifications GOST 9293-74 (ISO 2435-73) Nitrogen, gaseous and liquid. Technical specifications GOST 10146-74 Filter fabrics made of glass twisted filament threads. Specifications
GOST 10444.12-88 Food products. Method for determination of yeast and mold fungi GOST 10444.15-94 Food products. Methods for determining the number of mesophilic aerobic and facultative anaerobic microorganisms
GOST 12026-76 Laboratory filter paper. Technical specifications GOST 13358-84 Wooden boxes for canned food. Specifications
GOST 13516-86 Corrugated cardboard boxes for canned food, preserves and food liquids. Specifications
GOST 14192-96 Marking of cargo
GOST 14618.6-78 Essential oils, fragrant substances and intermediate products of their synthesis. Water determination methods
GOST 14618.10-78 Essential oils, fragrant substances and intermediate products of their synthesis. Methods for determining density and refractive index
GOST 14870-77 Chemical products. Water determination methods
GOST 15113.2-77 Food concentrates. Methods for determining impurities and pest infestation of grain stocks
GOST 15846-2002 Products sent to the Far North and equivalent areas. Packaging, labeling, transportation and storage
GOST 17433-80 Industrial cleanliness. Compressed air. Pollution classes GOST 19360-74 Film liner bags. General technical conditions GOST 19433-88 Dangerous goods. Classification and marking GOST 20477-86 Polyethylene tape with a sticky layer. Technical specifications GOST 25336-82 Laboratory glassware and equipment. Types, main parameters and sizes
GOST 26668-85 Food and flavoring products. Sampling methods for microbiological analyzes
GOST 26927-86 Raw materials and food products. Method for determination of 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 28498-90 Liquid glass thermometers. General technical requirements. Test methods
GOST 29169-91 Laboratory glassware. Pipettes with one mark GOST 29185-91 Food products. Methods for identifying and quantifying sulfite-auditing clostridia
GOST 29227-91 (ISO 835-1-81) Laboratory glassware. Graduated pipettes. Part 1. General requirements
GOST 29229-91 (ISO 835-3-81) Laboratory glassware. Graduated pipettes. Part 3. Graduated pipettes with a waiting time of 15 s
GOST 30178-96 Raw materials and food products. Atomic absorption method for determining toxic elements
GOST 31747-2012 Food products. Methods for identifying and determining the number of coliform bacteria (coliform bacteria)
GOST 31659-2012 Food products. Method for identifying bacteria of the genus Salmonella GOST 31266-2004 Raw materials and food products. Atomic absorption method for determination of arsenic
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 Agent for Technical Regulation and Metrology on the Internet or using the annual information index “National Standards”, which was published as of January 1 of the current year, and according to the releases of the monthly information index “National Standards” for the current year. If the reference standard is replaced (changed), then when using this standard you should be guided by the replacing (changed) standard. If the reference standard is canceled without replacement, then the provision in which a reference is made to it is applied in the part that does not affect this scope.
3 Terms and definitions
8 of this standard the following terms with corresponding definitions are used:
3.1 food flavoring: A product not directly consumed by humans as food, containing a flavoring substance or a flavoring preparation, or a thermal technological flavoring agent, or a smoke flavoring agent, or flavoring precursors, or a mixture thereof (flavoring part), intended to impart flavor and/or flavor to food products flavor (excluding sweet, sour and salty), with or without the addition of other food ingredients.
3.2 smoke flavoring: A mixture of substances isolated from smokes used in traditional smoking by fractionation and purification of smoke condensates.
3.3 thermal technological flavoring: A mixture of substances obtained as a result of heating at a temperature not exceeding 180 * C and a heating duration of no more than 15 minutes of food and/or non-food ingredients, one of which must be an amino compound, and the other a reducing sugar.
Notes:
1 When producing a thermal technological flavor at temperatures below 160 'C, the heating duration doubles for every 10 *C decrease in temperature.
2 The process time should not exceed 12 hours.
3 The pH value during the process should not exceed 8.0 pH units.
3.4 natural flavoring: Flavoring, the flavoring part of which contains only flavoring preparations and/or natural flavoring substances.
Notes:
1 The term “natural flavoring” may be used if its flavoring portion consists exclusively of flavoring preparations and/or natural flavoring substances.
2 The term “natural flavor” in combination with the name of the food product, food category or plant or animal source may only be used in the following cases. if the aromatics and/or natural flavoring substances included in the couso are obtained from a named source, for example, “natural apple flavor (Apple)”, “natural fruit flavor (Fruity)”, “natural mint flavor (Mint)”.
3 The term “natural flavor” may be used if the flavorings and/or natural flavorings contained in it are obtained from a source that does not reflect their taste and aroma, for example, “natural flavor and fancy name.”
3.5 synthetic flavoring: A flavoring agent, the flavoring part of which contains synthetic flavoring substances.
3.6 flavoring substance: Chemically defined (chemically individual) substance with flavoring properties, possessing a characteristic aroma and/or taste (except for sweet, sour and salty).
3.7 natural flavoring substance: A flavoring substance isolated using physical, enzymatic or microbiological processes from raw materials of plant, microbial or animal origin, including those processed by traditional methods of preparing food products.
Note - Traditional methods of preparation (production) of food products include: cooking, including steaming and under pressure (up to 120 * C). baking, roasting, stewing, frying, including in oil (up to 240 * C at atmospheric pressure), drying, evaporation, heating, cooling, freezing. soaking, maceration (soaking), infusion (brewing), percolation (extraction with straining), filtration, pressing (squeezing), mixing, emulsification, grinding (cutting, crushing, grinding, pounding), encapsulation (encapsulation). peeling (peeling), distillation (rectification), extraction (including solvent extraction), fermentation and microbiological processes.
3b synthetic flavoring substance: a flavoring substance obtained by chemical synthesis.
3.9 flavoring precursor: A product that does not necessarily have flavoring properties. intentionally added to food products for the sole purpose of obtaining flavor and aroma by destruction or reaction with other components during the cooking process.
Note - The flavoring precursor can be obtained both from food products and from products not used directly for food.
3.10 flavoring preparation: A mixture of flavoring or other substances isolated by physical, enzymatic or microbiological processes from food products or from food raw materials, including after processing by traditional methods of preparing food products, and/or from products of plant, animal or microbial origin, not used directly as food, used as such or processed using traditional food preparation methods.
4 Classification
4.1 Depending on their purpose, food flavorings are divided into:
For flavorings for confectionery and bakery products:
Flavorings for soft drinks;
Flavorings for fat and oil products:
Flavorings for other food products.
4.2 Depending on the composition of the flavoring part, flavorings are divided into:
For flavorings based on flavoring substances (natural and synthetic);
Flavorings based on flavoring preparations (natural);
Flavors based on flavor precursors:
Thermal technological flavors:
Smoke flavors;
Mixed flavors.
4.3 Depending on the form of release, flavorings are divided into:
For liquids: in the form of solutions and emulsions (emulsion);
Dry: powdered, including encapsulated and granulated;
Pasty.
5 General technical requirements
5.1 Characteristics
5.1.1 Flavors are produced in accordance with the requirements of this standard, a regulatory document in accordance with which a flavor of a specific name is produced, in compliance with the requirements. or regulatory legal acts in force in the territory of the state that has adopted the standard.
5.1.2 In terms of organoleptic indicators, flavorings must meet the requirements specified in Table 1.
Table 1 - Organoleptic indicators
End of table 1
5.1.3 For a flavoring agent of a specific name in a regulatory document, the manufacturer establishes* individual requirements for this flavoring agent for the following organoleptic and physicochemical parameters:
Appearance. color and halls;
Density and refractive index (for liquid flavors, except emulsion, paste and colored);
Volume fraction of ethyl alcohol in alcohol-containing flavorings (for flavorings that, in accordance with legislative and regulatory legal acts in force in the territory of the state that has adopted the standard, belong to alcohol-containing food products);
Mass fraction of moisture (in dry and paste flavors);
Presence of metallomagnetic impurities (in dry flavors), the presence of metallomagnetic impurities in dry flavors is allowed no more than 3 million" 1 (3 mg/kg);
Flash point (for liquid flavors).
5.1.4 Flavorings are identified by:
By name and purpose, by comparing the flavor indicated on the label with the name. specified in the definition of the type of food product in . or regulatory legal acts in force in the territory of the state that has adopted the standard;
By the appearance of the flavor, comparison with the characteristics set out in the regulatory document. in accordance with which a flavor of a specific name is produced;
According to organoleptic indicators, comparison with organoleptic characteristics (smell) set out in the regulatory document, in accordance with which the flavor of a specific name is produced:
5.1.5 Microbiological indicators of flavorings must meet the requirements established (1). or regulatory legal acts in force on the territory of the state. adopted the standard.
5.1.8 The content of potentially hazardous biologically active substances in flavorings made using plant aromatic raw materials and/or extracts and essential oils should not lead to exceeding the permissible levels of potentially hazardous biologically active substances in food products using flavorings in accordance with the requirements, installed (2) or regulatory legal acts in force in the territory of the state that has adopted the standard.
5.1.9 The use of potentially hazardous biologically active substances is not allowed: agaric acid, beta-asarone. aloina. hypericin. capsaicin. kvassina coumarin. menthofuran. methyl eugenol (4-allyl-1,2-dimethoxybeneol), lulegone, safrole (1-allyl-3.4-methylenedioxybeneol). hydrocyanic acid, thujone (alpha and beta), teucrine A. tarragon (1-allyl-4-methoxybenzene). as flavoring agents in the production of flavorings and food products.
5.1.10 It is not permitted to use the tetraploid form of Calamus (Acorus calamus L.. CE 13) (2) as a source of flavorings, including flavoring substances and preparations.
5.1.11 When using medicinal plants and/or flavoring preparations from medicinal plants as natural sources, their content (in terms of dry raw materials or the biologically active substance contained in them) should not exceed the amount that has a pharmacological effect of 1 kg (dm 3) food products when used as flavoring preparations (flavors) (2].
5.2 Requirements for raw materials
5.2.1 Raw materials for the production of flavorings must meet the safety requirements established by (1]. or regulatory legal acts in force in the territory of the state that has adopted the standard.
5.2.2 The ingredient composition of flavorings must comply with the requirements established by (1) or regulations in force in the territory of the state that has adopted the standard.
5.2.3 For the production of alcohol-containing flavorings, rectified ethyl alcohol is used from food raw materials with a degree of purification not lower than the highest according to regulatory documents in force in the territory of the state that has adopted the standard.
5.3 Packaging
5.3.1 Packaging of flavors must comply with the requirements established or regulations in force in the territory of the state that has adopted the standard.
5.3.2 Liquid flavorings are packaged:
In polymer canisters with lids, made from materials whose use in contact with flavorings ensures their quality and safety:
Glass containers for food products;
Other containers made from materials whose use in contact with flavorings ensures their quality and safety.
5.3.3 When packaging liquid flavors, at least 5% of the free space of the total capacity of the container must be left in each container.
5.3.4 Dry and paste-like flavors are packaged in polymer conical jars with a clamping lid and handle in accordance with the regulatory document in force in the territory of the state that has adopted the standard, using film liner bags in accordance with GOST 19360, made of materials whose use in contact with flavors ensures their quality and safety.
5.3.5 It is permitted to use other types of packaging that ensure the safety of dry and paste-like flavors during storage and transportation and are made from materials that meet the requirements established or regulations in force in the territory of the state that has adopted the standard.
5.3.6 Negative deviation of the net contents of the packaging unit from the nominal amount of flavoring must comply with GOST 8.579 (clause 4.2).
5.3.7 A batch of packaged flavors in packages must meet the requirements of GOST 8.579 (clauses 5.1.5.7).
5.3.8 When transported by rail, polymer canisters with liquid flavors are packed in wooden boxes in accordance with GOST 13358 or lathing, when transported by air - in corrugated cardboard boxes in accordance with GOST 13516.
Note - Polymer canisters may be transported by road without packaging in transport containers.
5.3.9 When transported by rail and air, polymer cans with dry and paste flavors are packed in corrugated cardboard boxes in accordance with GOST 13516.
Note - Polymer cans can be transported by road without packaging in transport containers.
5.3.10 Glass containers with liquid flavors are packed in corrugated cardboard boxes in accordance with GOST 13516 or plank boxes in accordance with GOST 13358 using auxiliary packaging materials in accordance with the rules for transporting goods on the appropriate mode of transport.
5.3.11 The flaps of corrugated cardboard boxes are covered in the longitudinal and transverse directions with tape made of polymeric materials with an adhesive layer in accordance with GOST 20477 or other packaging materials are used to ensure the safety of the product and the integrity of the container during transportation.
5.3.12 Flavors sent to the Far North and similar areas. Packed in accordance with GOST 15846.
5.4 Marking
5.4.1 Labeling of flavors must comply with the requirements established and or regulatory legal acts in force in the territory of the state that has adopted the standard.
5.4.2 The marking of each packaging unit additionally includes the following data:
Lot number or mark identifying the lot:
Gross weight;
Storage conditions:
Designation of this standard;
Designation of the document in accordance with which the flavor of a specific name is manufactured;
Warning: “If accidentally swallowed, induce vomiting, gastric lavage and seek medical attention.”
5.4.3 Transport marking - in accordance with GOST 14192 with the application of handling signs indicating the method of handling cargo - in accordance with the requirements established or regulatory legal acts in force in the territory of the state that has adopted the standard. and signs characterizing the type of danger of the cargo - according to GOST 19433.
6 Safety requirements and environmental protection
6.1 In accordance with GOST 12.1.007, in terms of the degree of impact on the body, flavorings and their components belong to the third (moderately hazardous substances) and fourth (low-hazardous substances) hazard classes.
The maximum permissible concentration in the air of the working area of the main (by weight) components of fragrances - solvents - is given in the document in accordance with which the fragrance of a specific name is manufactured.
6.2 Air monitoring of the working area is carried out according to methods approved in the prescribed manner, with a frequency determined by the requirements of GOST 12.1.005.
6.3 Liquid flavors are classified as flammable (flammable). flammable (GZh) or non-flammable liquids, dry - to flammable materials in accordance with GOST 12.1.044. The indicator of the fire-explosive hazard of liquid flavorings - the flash point - is given in the document in accordance with which the flavoring agent of a specific name is manufactured.
6.4 When taking samples, conducting analyses, storing and using flavorings, comply with labor protection rules and fire safety rules adopted when working with flammable materials. flammable (GOST 12.1.004 and fire safety rules in force in the territory of the state that has adopted the standard), harmful substances (GOST 12.1.007).
6.5 Fire extinguishing agents: sprayed water, air-mechanical foam, powders, for small fires - fire felt, powder fire extinguishers.
6.6 If the fragrance gets on the skin, it should be washed off with water, washed with soap, and if it gets into the eyes, rinse with plenty of water.
If the flavoring is accidentally ingested, induce vomiting, perform gastric lavage and seek medical attention.
6.7 When storing and transporting flavors, environmental protection is ensured by sealing the container. If it is violated and the flavoring gets into the environment, it must be collected and disposed of.
6.8 When storing, transporting, using and disposing of flavorings to prevent harm to the environment, health and human genetic fund, contamination of soil, surface and ground water is not allowed.
7 Acceptance rules
7.1 Flavorings are taken in batches.
A batch is considered a certain amount of a flavoring agent of the same name, obtained in one technological cycle, in the same packaging, produced by one manufacturer according to one regulatory document, accompanied by shipping documentation that ensures product traceability.
7.2 For quality control and acceptance of flavorings, the following test categories are established:
Acceptance documents:
Periodic.
7.2.1 Acceptance tests are carried out for each batch of flavoring on the quality of packaging and labeling, organoleptic and physico-chemical indicators using random control. To do this, 10% of packaging units are randomly selected from the batch, but not less than three. If the number of packaging units is less than three, each packaging unit is subject to control.
To conduct tests, instantaneous, total, laboratory samples and samples for analysis are taken from the packaging units included in the sample in accordance with Section 8.
7.2.2 The results of acceptance tests are documented in a test report in the form accepted by the manufacturer or reflected in a log.
7.2.3 If the results of acceptance tests are negative for at least one quality indicator, repeated tests are carried out for this indicator on a double sample from the same batch. The results of repeated tests apply to the entire batch.
7.2.4 If the results of repeated tests are unsatisfactory for at least one indicator, the entire batch of flavoring is rejected.
7.3 Procedure and frequency of monitoring the content of toxic elements. benzo(a)pyrene, bene(a)anthracene, biologically active substances, as well as microbiological indicators are established by the manufacturer in the production control program.
7.4 The “smell” indicator of the flavoring according to 8.5 is controlled only by the manufacturer
7.5 The basis for making a decision to accept a batch of flavoring is the positive results of acceptance tests and preceding periodic tests.
8 Control methods
8.1 Control of compliance of packaging and labeling of flavors with the requirements of this standard is carried out by external inspection of each packaging unit of products from the sample according to 7.2.1.
8.2 Sampling
8.2.1 To check the quality of flavors according to organoleptic and physico-chemical indicators and to determine toxic elements from product units included in the sample according to 7.2.1. Instant samples are taken, from which a total and laboratory sample is formed.
For microbiological analyses, sampling is carried out in accordance with GOST 26668.
8.2.2 Snap sample collection, summary sample collection and separation of laboratory sample and sample for analysis
8.2.2.1 Instant samples must be equal in volume (mass). The sum of all instant samples by volume (mass) should be 1.5-2.0 times greater than the volume (mass) of the laboratory sample.
The volume (weight) of the laboratory sample and the sample for analysis of the flavoring agent is determined by the regulatory document in accordance with which the flavoring agent of a specific name is manufactured.
8.2.2.2 The number of instant samples of liquid flavor depends on the volume occupied by the flavor. One instant sample is taken along the entire height of the flavoring layer, if its volume is up to 1 dm 3 inclusive, two instant samples are taken to a depth of 1/3 and 2/3 from the top level, if the volume is more than 1 dm 3, but does not exceed 10 dm 3 , three instant samples (from the upper, middle and lower layers) in all cases when the volume of flavoring is more than 10 dm 3.
8.2.2.3 Instant samples of liquid flavoring are taken with a sampling tube with an extended lower end with a diameter of 6 to 15 mm and a length exceeding the height of the container by several centimeters. 8
The upper hole of the tube is closed with a thumb or a stopper, immersed to the required depth, the tube is opened for a short time to fill, then closed again and the tube with the sample is removed.
8.2.2.4 Flash samples of the flavor paste are taken with a sampling tube, which is lowered vertically to the bottom of the container, then tilted and withdrawn slowly to ensure that the entire contents of the tube are preserved.
When using a probe, it is immersed (screwed in) to the entire depth of the container along the vertical axis. Then the dipstick is removed.
8.2.2.5 Instant samples of dry flavoring are taken with a probe, immersing it to the entire depth of the container along the vertical axis.
8.2.2.6 Taking instant samples of products at the stage of delivery and acceptance to the warehouse is carried out before sealing the container.
8.2.2.7 Place all instant samples in a sample vessel, mix thoroughly and obtain a total sample.
8.2.2.8 A laboratory sample of liquid and paste flavoring is obtained after thoroughly mixing the total sample and simply reducing it to the laboratory sample volume.
8.2.2.9 A laboratory sample of dry flavoring is obtained by reducing the total sample using the quartering method.
8.2.2.10 The laboratory sample for small batches of flavorings may be a total sample, and the total volume or mass of instant samples must be no less than the volume or mass required for testing.
8.3 Labeling of laboratory samples
The isolated laboratory sample of flavoring is thoroughly mixed again, divided into two equal parts and placed in clean, dry glass containers. The vessels are tightly closed with cortical or plugs made of polymeric materials and labeled with the following indication:
Flavor names;
Manufacturer's names:
Type of carrier (solvent, filler, food raw material);
Lot numbers and masses:
Dates of manufacture;
Sampling dates and locations:
Surnames and signatures of the person who took the sample;
Designations of the document in accordance with which the flavor of a specific name is manufactured.
One laboratory sample is used for analysis, the second is sealed and stored for the shelf life established by the manufacturer in case of disagreement in assessing the quality of the flavor for re-analysis.
For a small batch of liquid flavorings, it is allowed to store a laboratory sample of the flavoring used for testing.
Laboratory samples are stored in a place protected from light at a temperature not exceeding 25 * C (unless otherwise specified in the regulatory document in accordance with which the flavor of a particular name is manufactured), laboratory samples of dry flavors - at a relative humidity of no more than 75%.
8.4 Determination of appearance and color of flavorings
8.4.1 The appearance and color of liquid and paste flavoring is determined by viewing a sample for analysis in an amount of 30 to 50 cm3 in a glass B-1(2)-50(100) according to GOST 25336 against the background of a sheet of white paper in transmitted or reflected light .
8.4.2 The appearance and color of the dry flavor is determined by viewing a sample for analysis weighing from 30 to 50 g placed on a sheet of white filter paper in accordance with GOST 12026 in diffuse daylight or in the light of LD fluorescent lamps in accordance with GOST 6825.
8.4.3 A flavoring agent is considered to comply with the requirements of this standard if the appearance and color of the analytical sample meet the requirements of 5.1.3.
8.5 Odor detection
The method consists of an organoleptic comparison of a sample for flavor analysis with a control sample of the flavor of the given name.
A sample of the flavor of a given name, the smell of which is approved by the manufacturer's tasting council, is taken as a control sample.
For a control sample, a laboratory sample with a volume (weight) of at least 250 cm 3 (g) of flavoring produced under production conditions is taken. The control sample is stored in a hermetically sealed container for the shelf life established by the manufacturer.
8.5.1 Determination of liquid fragrance odor
Strips of filter paper 10 * 160 mm in accordance with GOST 12026 are simultaneously moistened (by approximately 3 cm) in the control sample and the sample for analysis and their smell is compared.
A flavoring agent is considered to comply with the requirements of this standard if the odor of the wet strips of the test sample and the control sample is the same.
8.5.2 Odor determination of dry and paste flavorings
A sample for analysis of the flavor and a control sample weighing from 30 to 50 g is placed on a sheet of white filter paper according to GOST 12026 and their smell is assessed.
A flavoring agent is considered to comply with the requirements of this standard if the odor of the test sample and the control sample is the same.
8.6 Determination of the refractive index of liquid flavors - according to GOST 14618.10 (section 4).
8.7 Determination of the density of liquid flavors - according to GOST 14618.10 (section 2 or section 3).
8.8 Determination of the volume fraction of ethyl alcohol in liquid alcohol-containing flavorings is carried out according to the method described in Appendix A.
8.9 Determination of the mass fraction of moisture in dry food paste flavorings - according to GOST 14618.6 (section 3 or section 4) or according to the method described in Appendix B.
If disagreements arise in the quality of the arbitration method, the method according to GOST 14618.6 (section 3) is used.
8.10 Determination of microbiological parameters of flavorings:
The number of mesophilic aerobic and facultative anaerobic microorganisms - according to GOST 10444.15:
The number of coliform bacteria (copiform bacteria) - according to GOST 31747;
Yeast and molds - according to GOST 10444.12:
Bacteria such as salmonella - according to GOST 31659;
The number of sulfite-producing clostridia is according to GOST 29185.
8.11 Determination of the content of toxic elements:
Arsenic - according to GOST 26930. GOST 31266;
Lead - according to GOST 26932. GOST 30178:
Cadmium - according to GOST 26933. GOST 30178:
Mercury - according to GOST 26927 and according to the regulatory document in force in the territory of the state that has adopted the standard.
8.12 Determination of metallomagnetic impurities - according to GOST 15113.2.
8.13 Definition of bene(a)pirek. benz(a)anthracene and potentially hazardous biologically active substances - according to a regulatory document in force in the territory of the state that has adopted the standard.
8.14 Determination of flash point - according to GOST 12.1.044.
8.15 Determination of the volume fraction of 1.2*propylene glycol in liquid flavorings - according to Appendix B.
9 Transportation and storage
9.1 Flavors are transported by all modes of transport in accordance with the cargo transportation rules in force for the relevant mode of transport.
9.2 Liquid and paste flavorings are stored in closed and darkened rooms at a temperature not exceeding 25 °C. unless otherwise specified by the manufacturer.
Notes:
1 When storing liquid flavors, opalescence and precipitation are allowed if this is provided by the manufacturer.
2 When storing paste-like flavors, separation (separation of the liquid phase) is allowed if this is provided by the manufacturer.
3 Before use, flavors must be mixed until smooth.
9.3 Dry flavors are stored in dry, well-ventilated areas at a temperature not exceeding 25 ° C and a relative humidity of not more than 75%. unless otherwise specified by the manufacturer.
Note - When storing dry flavors, the presence of loosely packed lumps (easily crumbling) is allowed.
9.4 Transportation and storage of fragrances together with chemicals and strong-smelling products and materials is not allowed.
9.5 The shelf life of flavorings is set by the manufacturer.
10 Directions for use
The scope of application and maximum dosages of flavorings must comply with the requirements. established or regulatory legal acts in force on the territory of the state. which has adopted the standard, and are installed by the manufacturer.
This chromatographic method is designed to determine the volume fraction of ethyl carbon dioxide in liquid flavorings using a packed column and a flame ionization detector.
The measurement range for the volume fraction of ethyl alcohol is from 1.0% to 85.0% inclusive.
A.1 Essence of the method
The method is based on the chromatographic separation of flavor components and ethyl alcohol on a polyaromatic macroporous sorbent using a “cold” sample injection (at a temperature below the boiling point of the analyzed substance) and subsequent detection of ethyl alcohol with a flame ionization detector.
A.2 Safety requirements
A.2.1 When working on a gas chromatograph, it is necessary to comply with labor protection requirements and safety rules in accordance with the operating instructions for the device.
A.2.2 When performing the analysis, 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.
A.2.3 The room in which measurements are carried out must be equipped with general supply and exhaust ventilation in accordance with GOST 12.4.021.
A.2.4 Electrical hazard when working with electrical installations - according to GOST 12.2.007.0 and GOST 12.1.019. A.
2.5 Organization of occupational safety training for workers - in accordance with GOST 12.0.004.
A.2.6 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.
A.Z Measuring instruments, auxiliary equipment, glassware, reagents and materials
Gas chromatograph, equipped with a flame ionization detector with a nonane sensitivity of at least 1-10-11 g/cm 1 .
Stopwatch of 2nd accuracy class with a counter capacity of 30 min. division price 0.20 s, error ± 0.60 s.
Volumetric flasks with a ground stopper with a capacity of 100 cm 3 of the 1st accuracy class according to GOST 1770.
Pipettes 2-1-5. 2-1-10. 2-1-20. 2-1-25 according to GOST 29227.
Pipes with one mark with a capacity of 25.50 cm 3 of the 1st accuracy class according to GOST 29169.
Pipette 4-2-1 according to GOST 29229.
Packed chromatographic column made of stainless steel, 1 m long and with an internal diameter of 3 mm. filled with polysorb with an ethical macroporous sorbent - a copolymer of styrene (60%) and divinyl benzene (40%) (Polysorb 1). with particle size from 0.25 to 0.50 mm. It is permissible to use a longer column and increase the temperature of the column thermostat, provided that the analysis time is increased. The use of other sorbents is not allowed.
Carrier gas - nitrogen o. parts according to GOST 9293:
Technical hydrogen grade A - in accordance with GOST 3022. The use of a hydrogen generator is allowed.
Compressed air in accordance with GOST 17433. It is allowed to use any type of air compressor that provides the necessary pressure and air purity in accordance with the operating instructions for the gas chromatograph.
Ethyl spirit, rectified according to the regulatory document in force in the territory of the state that has adopted the standard.
Acetone according to GOST 2603.
It is allowed to use similar measuring instruments, materials and reagents with metrological characteristics and quality not lower than those specified.
A.4 Preparation for measurements
A.4.1 Measurement conditions
When preparing for measurement and during measurement, the following conditions must be observed:
Ambient air temperature................................................................... ...........................................from 20 *С to 25 * WITH;
Atmosphere pressure................................................ ...............from 95.0 to 106.7 kPa (from 720 to 600 mm Hg);
A.4.2 Preparation of the chromatographic column
relative humidity............................................... ...........................................from 40% up to 90%:
mains voltage................................................................... ........................................................ ....................220* ^8:
frequency of current in the electrical network......................................................... ........................................................ ..............from 49 to 51 Hz.
The chromatographic column is washed successively with water, ethyl alcohol, acetone, dried in a stream of air and filled with sorbent.
The filled column is placed in the chromatograph thermostat, connected to the evaporator without connecting to the detector, then the column is purged with gaseom-nosigepvm (nitrogen) at a speed of 40 cm 5 /min in temperature programming mode: increasing the temperature to 170 * C at a speed of 4 * C / min to 6 'C/min. then at a temperature of 170 * C for 0.5 to 1.0 hours. The prepared column is connected to the detector and the stability of the zero line is checked at the operating temperature of the column thermostat according to A.7.
A.4.3 Preparation of measuring equipment
The chromatograph is prepared for operation in accordance with its operating instructions.
The device is calibrated using calibration solutions in accordance with A.5.2.
A.4.4 Preparation of calibration solutions
Solutions of ethyl alcohol in distilled water with volume fractions (vol. %) are used as calibration solutions. close to the specified measurement range.
Before preparing solutions, the content of the main substance in the ethyl alcohol used is determined according to GOST 3639. To calibrate the device, at least seven calibration solutions are prepared.
Into each of seven volumetric flasks with a ground stopper with a capacity of 100 cm 3 add 10 cm 3 of distilled water and the required amount of ethyl alcohol in accordance with Table A.1. The contents of the flasks are mixed and the volumes of solutions are adjusted to the mark with distilled water (calibration solutions No. 1-7).
Calibration solutions are stored at temperatures from 0°C to 10°C in sealed containers for six months.
Table A.1 - Composition of calibration solutions
|
Number of calibration mixture |
Volume of a typical alcohol in a graded solution, cm 3 |
Volume fraction of ethyl alcohol Q fp. %. in calibration solutions is determined by density after holding the solutions for 2 to 3 hours with a pycnometer according to GOST 3639 (section 3), followed by converting the density values of the aqueous-alcohol solution to the alcohol content in percent (by volume).
A.5 Taking measurements
A.5.1 Measurements are performed under the following operating parameters of the chromatograph:
Column thermostat temperature................................................... ....................................80 *C:
evaporator (injector) temperature............................................................ ......................„.........from 45 *C to 55 *C;
temperature of the transition chamber................................................... ....................................80 *C:
carrier gas (nitrogen) flow rate.................................................... ....................................from 30 to 40 cm 3 /min;
hydrogen flow rate................................................... ........................................................ .30 cm 3 /min:
air flow speed................................................................... ........................................................ ....300 cm e/min;
sample volume for analysis............................................................. ........................................................ .0.2 mm 3 .
After the analysis of 20-30 samples, the temperature of the evaporator, column thermostat and transition chamber is increased to 150 * C and maintained for 30 to 40 minutes to clean the chromatographic system from boiling compounds.
A.5.2 Establishment of calibration characteristic
The flame ionization detector of the chromatograph is calibrated using the absolute calibration method.
To determine the calibration coefficient, it is necessary to chromatograph at least four calibration solutions with an ethyl alcohol content corresponding to the entire measurement range. Each calibration mixture is analyzed at least once.
The dependence of the volume fraction of ethyl alcohol in the analyzed sample on the peak area is expressed by the equation
where Q is the volume fraction of ethyl alcohol in the analyzed sample. % (about.);
A is the area of the chromatographic face. units accounts;
K - calibration coefficient. % (dinner. accounts.
t Ar*A, g *A,b A<--3
where A f is the arithmetic mean value of the three areas of chromatographic peaks obtained from the analysis of the calibration solution;
Areas of chromatographic peaks of three analyzes of the calibration solution, units. accounts;
Qy is the volume fraction of ethyl alcohol in the calibration solution. % (about.).
Calculate the average value of K using the formula
The calibration procedure is carried out periodically, at least once a week, when installing the method on a chromatograph, or after repairing the chromatograph.
A.5.3 Sample analysis
After establishing the operating parameters, turning on the analysis automation system to record chromatograms and process the obtained data, and a stable zero line on the working scale of the detector, analysis begins.
To determine the volume fraction of ethyl alcohol in the analyzed flavoring sample, use a laboratory sample according to 8.2.
3 samples are injected into the evaporator (injector) with a microsyringe of 0.2 mm and chromatographic analysis is performed under conditions A.5.1. A peak is recorded in the retention time region corresponding to ethyl alcohol. The analysis is repeated at least twice.
When calibrating and analyzing, it is imperative to use the same microsyringe.
A.6 Processing of results
A.6.1 The results are processed using the software of the personal computer or integrator included with the chromatograph in accordance with their operating instructions.
A.6.2 The volume fraction of ethyl alcohol in the analyzed flavoring sample X, % (vol.), is calculated using the formula
X = K A, (A. 5)
where K is the arithmetic mean value of the ethyl alcohol calibration coefficient. % (dinner. accounts;
A is the peak area of ethyl alcohol, units. accounts.
A.6.3 The result of determining the volume fraction of ethyl alcohol. % (vol.) in flavoring is presented as
XYU.016X. (A.6)
where X is the volume fraction of ethyl alcohol in the flavoring agent. % (about.);
5 - relative error in determining the volume fraction of ethyl alcohol. % (about.).
The final result of the determinations is taken as the arithmetic mean value of two parallel determinations X (p, %, rounded to the first 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 = 0.95%. does not exceed the repeatability limit r = 10.00%.
The absolute value of the difference between the results of two determinations, obtained under 8 reproducibility conditions at P = 0.95%. does not exceed the reproducibility limit R = 15.00%.
The relative error limits of the method for determining the volume fraction of ethyl alcohol are ±15.0% at P ® 0.95%.
A.7 Monitoring the stability of the chromatograph zero line
Control is carried out continuously during the analysis of flavors. The positive drift of the zero line, defined as the largest shift of the zero line signal within 20 minutes from the start of the analysis, should not exceed 20% of the peak height corresponding to the volume fraction of ethyl alcohol 1% (N91 calibration solution). If the specified value is exceeded or side peaks appear, it is necessary to raise the temperature of the column, evaporator and transition chamber to 150 * C and maintain it for 30 to 40 minutes to accelerate the elution of high-boiling components of the analyzed mixtures.
This method is intended to measure the moisture mass fraction of flavorings dissolved in liquids that do not react with Fischer's reagent.
The method provides measurements in the range of mass fraction of moisture from 0.8% to 50% inclusive.
B.1 Essence of the method
The method is based on the interaction of iodine with sulfur oxide (IV) and water in a medium of methanol and pyridine during titration of the analyzed sample with Fischer's reagent. The equivalence point is determined electrometrically by the appearance of a current between two electrodes with the appearance of free iodine in the solution.
B.2 Safety requirements
B.2.1 When working on an automatic titration analyzer for electrometric titration of moisture according to the K. Fischer method, it is necessary to comply with labor protection requirements and safety rules in accordance with the operating instructions for the device.
B.2.2 When performing analysis, 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.
B.2.3 The room in which measurements are carried out must be equipped with general supply and exhaust ventilation in accordance with GOST 12.4.021.
B.2.4 Electrical safety when working with electrical installations - in accordance with GOST 12.2.007.0 and regulatory documents. valid in the territory of the state that has adopted the standard.
B.2.5 Organization of training for workers in pile safety - in accordance with GOST 12.0.004.
B.2.6 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.
B.2.8 All operations with Fischer reagent should be carried out in a fume hood.
B.Z Measuring instruments, auxiliary equipment, glassware, reagents and materials
Scales according to regulatory documents in force in the geo-territory of the state that has adopted the standard, with the value of the standard deviation (MSD). not exceeding 0.3 mg. and an error from nonlinearity of no more than ± 0.6 mg.
Automatic titrimetric analyzer for electrometric titration of moisture according to the K. Fischer method with a measurement range of the mass fraction of moisture from 0.5% to 50.0% and a standard deviation limit of the relative measurement error of ± 0.4% (at 25 mg of moisture).
Cylinder 1-100-1 according to GOST 1770.
Conical flasks Kn-1-500-40 TS. Kn-1-500-40 THS with ground section, capacity 500 cm 3 according to GOST 25336.
Cup SV-14/V according to GOST 25336.
Filtered paper according to GOST 12026.
Microsprays with a capacity of 0.01 cm 1.
Fischer reagent No. 1 (sulfur dioxide in methanol), analytical grade. according to GOST 14670.
Fischer reagent No. 2 (iodine in methanol), analytical grade. according to GOST 14870.
Methanol is a poison (methyl alcohol), x. parts according to GOST 6995.
Distilled water according to GOST 6709.
It is allowed to use other measuring instruments, materials and reagents with metrological characteristics and quality not lower than those specified.
B.4 Preparation for measurements
B.4.1 Measurement conditions
When performing measurements in the laboratory, the following conditions must be met:
Ambient temperature................................................................... ................................from 10 *С to 35 *С:
Atmosphere pressure................................................ ........................................................ .from 84.0 to 106.7 kPa
(from 630 to 800 mm Hg);
Relative humidity............................................... .............................without pain 80%;
Mains voltage........................................................ ........................................................ ..........220"|££в.
B.4.2 Sampling - according to 8.2.
B.4.3 The preparation of the automatic tigrimetric analyzer is carried out in accordance with the instructions for its operation.
B.4.4 Preparation of working solution of Fischer reagent
In a conical flask with a capacity of 500 cm 3, 100 cm 3 of Fischer reagent N91 and Fischer reagent No. 2 are sequentially measured. close with a stopper and stir. The resulting working solution is poured into a bottle marked “Fischer reagent,” which is connected to the pump of the titration unit of an automatic hytrimegric analyzer, avoiding the formation of bubbles, and incubated for 24 hours.
B.4.5 Me ha no-poison is poured into a bottle marked “Methanol-poison*, which is connected to the pump of the titration unit of the automatic hytrimegric analyzer.
Note - When connecting bottles with ready-made reagents to the pump of the titration unit of an automatic titrimetric analyzer, you should make sure that the caps fit tightly and the float in the drain bottle moves freely in a vertical plane.
B.4.6 Raise the pump cover of the titration unit until it stops and move the holder of the reaction vessel until it stops in order to completely isolate the container.
B.4.7 Calibrate the automatic titrimetric analyzer by titrating a given volume of distilled water (U = 0.01 cm3) daily, before taking measurements in accordance with the operating instructions for the device. Calibration is considered completed if the coefficient of variation for three results out of ten does not exceed the norm established in the operating instructions for the device.
B.4.8 Sample preparation
In a glass with a capacity of 50 cm 3, weigh from 0.2 to 0.3 g of dry flavor or from 0.2 to 1.0 g of paste flavor, or from 0.5 to 1.0 g of liquid flavor, recording the weighing result to the third decimal place.
B.5 Taking measurements
B.5.1 The flavor sample is introduced into the reaction vessel of an automatic hytrimegric analyzer, and the operation should be performed as quickly as possible to minimize the ingress of moisture from the air.
Note - If within 60 s the analyzed sample is not added to the reaction vessel, the device will return to its conditioning mode.
B.5.2 Measurements are carried out in accordance with the operating instructions for the automatic titrimetric analyzer, recording the result to the second decimal place.
B.c Processing of results
The numerical value of the final measurement result and the value of the absolute measurement error limits are expressed in no more than two significant figures.
The arithmetic mean value C avg is taken as the final result of the determination. %. results of two parallel determinations, if the acceptance condition is met
BllBllOOSr, (B.1)
where C,. C, - results of analyzes of the results of two parallel determinations of the mass fraction of moisture, performed under repeatability conditions. %;
C av - arithmetic mean value of the results of two parallel determinations of the mass fraction of moisture. performed under repeatable conditions. %; g - repeatability limit value. % given in Table B.1.
The result of the analysis is presented as:
C CD ±0.016C W , at P = 0.95, (B.2)
cav is the arithmetic mean value of the results of two parallel determinations of the mass fraction of moisture, considered acceptable. %;
6 - relative measurement error grants. %.
Repeatability limit g and reproducibility R. as well as an accuracy indicator. S. measurements of the mass fraction of moisture in flavorings are given in Table B.1.
Table B.1
Determination of the volumetric content of 1.2-proplenpicol in 8 liquid flavorings is performed by chromatographic method.
The range of measured volumetric percentages of 1.2-prolylene glycol is from 1.0% to 92.0% inclusive.
B.1 Essence of the method
The method is based on the taeochromatographic separation of flavoring components on a device with a flame ionization detector and the use of two types of chromatography: gas-adsorption and gas-liquid.
B.2 Measuring instruments, auxiliary equipment, glassware, materials and reagents
Scales with the value of the standard deviation (MSD). not exceeding 0.3 mg. and with an error from nonlinearity of no more than 10.6 mg.
Stopwatch of 2nd accuracy class with a counter scale capacity of 30 min. at a division price of 0.20 s. error 10.60 s.
Thermometer TL-31-A. temperature measurement limits from 0 *C to 250 *C according to GOST 2649S.
Gaeoa chromatograph. equipped with a flame ionization detector with a nonane sensitivity of at least 1-10’’ 1 g/cm 3 .
A computer or integrator that has software for a basic set of chromatography automation operations.
Packed chromatographic column made of stainless steel. 1 m long and 3 mm internal diameter. If necessary, it is possible to use a longer column and increase the temperature of the column thermostat when increasing the analysis time.
Water jet vacuum pump according to GOST 25336.
Microsyringe with a capacity of 0.5 mm 3.
Measuring glassware according to GOST 1770.
Pipettes 2-1-5.2-1-10. 2-1-20. 2-1-25.4-2-1 according to GOST 29227.
Glass bottles with a capacity of 5 to 15 cm 3 with silicone rubber stoppers.
Fiberglass according to GOST 10146.
Gaseous aeog of special purity according to GOST 9293.
Technical hydrogen grade A according to GOST 3022. The use of a hydrogen generator is allowed.
Compressed air in accordance with GOST 17433. It is allowed to use compressors of any type that provide the necessary pressure and air purity.
Distilled water according to GOST 6709.
Polyaromatic macroporous sorbent - copolymer of styrene (60%) and divicyl bvnzole (40%) (Poly-sorb 1). with particle size from 0.25 to 0.50 mm. The use of other sorbents is not allowed.
Sorbent based on hydrated microamorphous silica treated with hydroxymethyldisilaane (N-AW HMDS Chromate type) and polyethylene picol 20000 (Carbowax type) in an amount of 15%. with particle sizes from 0.20 to 0.36 mm.
Rectified ethyl alcohol according to regulatory documents in force in the territory of the state that has adopted the standard.
It is allowed to use similar measuring instruments, materials and reagents with metrological characteristics and quality not lower than those specified.
B.3 Preparation for measurements
B.3.1 Measurement conditions
During preparation and measurement and during measurement, the following conditions must be observed:
Ambient temperature................................................................... ...............................(20 ± 2) 'C:
Atmosphere pressure................................................ ........................................................ .from 95.0 to 106.7 kPa
(from 720 to 800 mm Hg);
Relative humidity............................................... ...................................from 20% to 90%;
Mains voltage................................................................... ...........................................(220 ± 20) B;
Mains frequency................................................................... ........................................................ .....(50±2)Hz.
B.3.2 Preparation of the chromatographic column
Chromatographic columns are washed successively with water, ethyl alcohol, acetone, dried in a stream of air and filled with a packing.
The filled columns are placed in the chromatograph thermostat and connected to the evaporator without connecting to the detector. The column is conditioned with gas-nosigvpem (nitrogen) at a speed of 40 cm 3 /min in program mode.
temperature control at a rate of 4 *C/min to 6 "C/min to 170 *C and maintained for 0.5 to 1.0 hours at this temperature.
After cooling, the output ends of the columns are connected to the detector and the stability of the culm line is checked at the operating temperature of the column thermostat.
B.3.3 Preparation of measuring equipment
The chromatograph is prepared for operation in accordance with the operating instructions supplied with the device.
The device is calibrated using calibration solutions.
B.3.4 Preparation of calibration solutions
Solutions of 1.2-l-propene glycol in distilled water with volume fractions (vol. %) close to the specified measurement range are used as calibration solutions.
Solutions are prepared using 1,2-propylene glycol with a volume fraction of the main substance of at least 99.0%.
Eight volumetric flasks with a ground stopper with a capacity of 50 cm 3 are poured from 20 to 30 cm 3 of distilled water, added sequentially with pipettes of 0.5: 5.0: 10.0; 20.0 cm 3 and cylinders 30:40: 46 cm 3 1,2-pro-pipvnglycol. The contents of the flasks are mixed and the volumes of solutions are adjusted to the mark with distilled water (calibration solutions N91 - N48).
Volume fraction of 1.2-propene glycol, %. in calibration solutions is determined by the formula
where is the aliquot fraction of 1,2-prolylene glycopy. cm 3:
Q Mx is the volume fraction of the main substance in 1.2-lropipene glycol,%:
50 - volume of calibration solution, cm 3.
B.4 Taking measurements
B.4.1 Measurements are performed under the following operating parameters of the chromatograph for gas adsorption chromatography:
Column thermostat temperature.................................................... ....................................170 *C;
Evaporator (injector) temperature............................................................ ...............................(170 ± 5) *С;
Temperature of the transition chamber................................................... ...................................170 *C;
Nitrogen carrier gas consumption.................................................... .........................................from 30 to 40cm e/min;
Hydrogen consumption................................................... ........................................................ ............ZOSm^/min:
Air flow................................................ ........................................................ ...............300cm e/min:
Sample volume................................................... ........................................................ ...................from 0.1 to 0.5 mm 3:
for gas-liquid chromatography:
Column thermostat temperature.................................................... ....................................150 "C;
Evaporator (injector) temperature............................................................ ...............................(200 ± 5) *С;
Temperature of the transition chamber................................................... ...................................150 "C:
Consumption of the nitrogen carrier basin.................................................... ...........................................from 30 to 40 cm 3 /min;
Hydrogen consumption................................................... ........................................................ ..........30 cm 3 /min;
Air flow................................................ ........................................................ ...............300 cm 3 /min;
Sample volume................................................... ........................................................ ...................from 0.1 to 0.5 mm 3.
B.4.2 Establishment of calibration characteristic
The calibration of the flame ionization detector of the chromatograph is performed using the absolute calibration method.
To determine the calibration coefficient, it is necessary to chromatograph at least four identical solutions containing 1,2-propylene glycol corresponding to the working measurement range.
A microsclerium with a capacity of 1.0 mm 3, washed 8-10 times with the analyzed calibration solution of 1,2-propylene picol. 3 samples are taken from 0.1 to 0.5 mm and introduced into the chromatograph evaporator.
Each calibration mixture is analyzed at least three times.
The dependence of the volume fraction of 1.2-prolylene picol on the face area is expressed by the equation
O = KA, (B.2)
where O is the volume fraction of 1.2-lropylene glycopy in the sample. %;
K - calibration coefficient, %/unit. accounts:
A is the area of the chromatographic peak. units accounts.
The value of the calibration coefficient for each i-th calibration solution is calculated using the formula
*,4
A!\ * A)t * A)b
where A ft . Af2. A (h - areas of chromatographic peaks of three parallel measurements of the /th calibration solution. counting units:
Qf is the volume fraction of 1.2-prolylenepicol in the /th sample. %.
The average value of the calibration coefficient is calculated using the formula
I*,
where l is the number of calibration solutions.
The calibration procedure is carried out when the method is installed on a chromatograph, after repair of the chromatograph, after a negative control result.
Periodic monitoring of calibration coefficients is carried out in accordance with B.5.4.
The calibration characteristic is checked at one of the points in the range of measured concentrations daily in accordance with B.6.5.
B.4.3 Gas chromatographic analysis of a flavor sample
When calibrating and analyzing, it is imperative to use the same syringe. After establishing the operating parameters, turning on the analysis automation system for recording chromatograms and processing the obtained data, and a stable zero line on the working scale of the detector, analysis begins.
To determine the volume fraction of 1.2-prolylene picol in the analyzed sample, three times from 0.1 to 0.5 mm 3 of the analyzed food flavoring are introduced into the chromatograph evaporator with a microsyringe, using a chromatographic column that ensures optimal separation of 1.2-prolylene picol from other components of the flavoring. Based on the obtained chromatograms of the analyzed sample, the peak areas are measured and the average peak area of 1.2-prolylenepicol is calculated.
B.5 Processing of results
B.5.1 The results are processed using the software included in the chromatograph kit of a personal computer or integrator in accordance with their operating instructions.
B.5.2 Volume fraction of 1.2-lrogmpvnglykopya in the analyzed baked goods flavoring X.%. calculated by the formula
X = CD. (AT 6)
where K is the arithmetic mean value of the calibration coefficient of 1.2-propylenethicol. %/unit accounts:
A is the average peak area of 1,2-lropylene glycol from three parallel determinations of the flavor sample. bill units
B.5.3 The result of measurements of the volume fraction of 1.2-propylene glycol in the flavoring agent is presented in the form
X t0.01.sx, (B.7)
where X is the volume fraction of 1.2-propylene glycol in the flavoring agent. %;
& is the relative error in measuring the volume fraction of 1.2-propylene and cola. %.
B.5.4 The relative error & measurement of the volume fraction of 1.2-propylene glycol in flavorings with a confidence probability of P = 0.95 is for flavorings with a volume fraction of 1.2-propylene glycol:
From 1% to 15% inclusive.................................................... ...........................................± 15% :
Xie. 15% to 92% inclusive................................................. ........................................... ± 8%.
B.6 Monitoring the accuracy of measurement results
When monitoring measurement accuracy using this method, perform the following operations:
B.6.1 Monitoring the stability of the chromatograph zero line
Monitoring is carried out continuously during the analysis of food flavorings. The positive drift of the zero line, defined as the greatest shift of the zero line signal 20 days from the start of the analysis, should not exceed 20% of the height of the face corresponding to a volume fraction of 1.2-propylene glycol 1% (calibration solution N91). If the specified value is exceeded or side peaks appear, it is necessary to raise the temperature of the column, evaporator and transition chamber to 200 * C and maintain it for 30 to 40 minutes for accelerated elution of high-grade components of the analyzed mixtures.
B.6.2 Monitoring the convergence of chromatograph output signals
The controlled parameter is the relative range of the chromatograph output signals. Control is carried out during calibration and during periodic monitoring of calibration coefficients. The control result is considered positive when the condition is met
Apl, -At P100$m (V.8)
where Achya is the maximum area of the chromatographic peak, units. accounts:
Minimum chromatographic peak area. units accounts:
A is the arithmetic mean value of the peak areas obtained from parallel injections of samples, counting units:
M is the relative range of the chromatograph output signal. %.
The values of the M value depending on the value of the volume fraction of 1.2-prspylvngpicol are given in gebgmts B.1 Table B.1
In percentages
B.6.3 Monitoring the correctness of the construction of the calibration characteristic
The controlled parameter is the range of calibration coefficients relative to the average value.
The calibration quality is considered satisfactory if the condition is met
where Ksh, is the maximum value of the calibration coefficient of 1.2-propylene thicol in the 8 range of analyzed volume fractions, %/unit. accounts:
K min - minimum value of the calibration coefficient of 1.2-propene glycol in the range of analyzed volume fractions, %/unit. accounts:
K is the average value of the calibration coefficient of 1.2-prolylene glycol. %/unit accounts:
B is the range of the calibration coefficient. %.
The values of value B depending on the volume fraction of 1.2-prolylene glycol are given in Table B.1.
Control is carried out each time when constructing a calibration dependence. If condition (B.9) is not met. then the device is re-calibrated.
B.6.4 Monitoring the stability of the calibration characteristic
Monitoring is carried out at least once a quarter, as well as when changing a column, washing the detector, etc. The monitoring frequency can be increased at higher intensity of operation of the device. Control is carried out using freshly prepared calibration solutions according to B.3.4. Three solutions are used at the beginning, middle and end of the working measurement range. Samples are introduced into the chromatograph using a microsyringe.
The control results are considered positive when the condition is met
|K ~ g| 10Q4f.. (Q.10)
where K is the previously established value of the calibration coefficient;
K is the average value of the calibration coefficient, calculated according to formula (B.5):
L - standard for periodic monitoring of the stability of the calibration characteristic. %.
The values of L depending on the volume fraction of 1 ^-propylene glycol are given in Table B.1.
If the control results are negative, it is necessary to calibrate the device in accordance with B.4.2. 8.6.5 Daily monitoring of the stability of the calibration characteristic
Control is carried out daily at the beginning of the working day using a calibration solution close in value to the determined proportion of 1.2-propylene glycol. The sample is introduced into the chromatograph using a microsyringe.
The control results become positive when the condition is met
where K is the calibration coefficient established earlier, %/counting unit;
K, - calibration coefficient of the calibration controlled solution, %/unit. accounts calculated using the formula
where Q. is the volume fraction of 1.2-propipenticol in the th sample. %;
D is the area of the chromatographic peak of 1.2-propylene glycol in the sample, counting units;
(V is the standard for daily monitoring of the stability of the calibration characteristic. %.
The values of N depending on the volume fraction of 1,2-propylene glycol are given in Table B.1. If the control results are negative, it is necessary to calibrate the device in accordance with B.4.2.
B.7 Safety requirements
B.7.1 When working on a gas chromatograph, it is necessary to comply with labor protection requirements and safety rules in accordance with the operating instructions for the device.
B.7.2 The room in which the measurement is carried out must be equipped with general supply and exhaust ventilation.
Bibliography
Technical Regulations of the Customs Union TR CU 021/2011 “On the safety of food products”
Technical Regulations of the Customs Union TR CU 029/2012 “Safety requirements for food additives, flavorings and technological aids”
Technical Regulations of the Customs Union TR CU 005/2011 “On Packaging Safety”
Technical Regulations of the Customs Union TR CU 022/2011 “Food products regarding their labeling”
UDC: 663.05:006.354 MKS 67.220.20 N91
Key words: food flavorings, classification, safety and quality indicators, technical requirements, control methods
Editor N.E. Nikulina Technical editor A.I. Belov Proofreader I. A. Belova Computer layout AS. Shapovalova
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FOOD FLAVORS
General technical conditions
Moscow
IPC Standards Publishing House
2004
Preface
The tasks, basic principles and rules for carrying out work on state standardization in the Russian Federation are established by GOST R 1.0-92 “State standardization system of the Russian Federation. Basic provisions" and GOST R 1.2-92 "State standardization system of the Russian Federation. The procedure for developing state standards"
Standard information
1 DEVELOPED by the State Institution All-Russian Scientific Research Institute of Food Flavors, Acids and Dyes (GU VNIIPAKK) of the Russian Academy of Agricultural Sciences
2 INTRODUCED by the Technical Committee for Standardization TC 154 “Food acids, aromatic essences and flavorings, synthetic food colorings”
3 APPROVED AND ENTERED INTO EFFECT by Resolution of the State Standard of Russia dated December 29, 2003 No. 407-st
4 INTRODUCED FOR THE FIRST TIME
Information about changes to this standard is published in the “National Standards” index, and the text of these changes- in the information signs “National Standards”. In case of revision or cancellation of this standard, the relevant information will be published in the information index “National Standards”
GOST R 52177-2003
NATIONAL STANDARD OF THE RUSSIAN FEDERATION
Date of introduction - 2005-01-01
1 area of use
This standard applies to food flavorings intended for the food industry.
Codes of OKP products covered by the standard are given in the Appendix.
This standard does not apply to flavorings for tobacco products.
The documentation in accordance with which a flavor of a specific name is produced must contain requirements not lower than those established by this standard.
Requirements ensuring the safety of food flavorings are set out in - and , requirements for product quality - , labeling requirements - .
(Changed edition, Amendment No. 1).
2 Normative references
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 12.1.004-91 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 12.1.044-89 (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 1770-74 Laboratory glassware. Cylinders, beakers, flasks, test tubes. General technical conditions
GOST 3022-80 Technical hydrogen. Specifications
GOST 3639-79 Water-alcohol solutions. Methods for determining the concentration of ethyl alcohol
GOST 6709-72 Distilled water. Specifications
GOST 6825-91 (IEC 81-84) Tubular fluorescent lamps for general lighting
GOST 6995-77 Methanol is a poison. Specifications
GOST 7328-2001 Weights. General technical conditions
GOST 9293-74 (ISO 2435-73) Nitrogen, gaseous and liquid. Specifications
GOST 10146-74 Filter fabrics made of glass twisted filament threads. Specifications
GOST 10444.12-88 Food products. Method for determining yeast and mold fungi
GOST 10444.15-94 Food products. Methods for determining the number of mesophilic aerobic and facultative anaerobic microorganisms
GOST 12026-76 Laboratory filter paper. Specifications
GOST 13358-84 Wooden boxes for canned food. Specifications
GOST 13516-86 Corrugated cardboard boxes for canned food, preserves and food liquids. Specifications
GOST 14192-96 Marking of cargo
GOST 14618.6-78 Essential oils, fragrant substances and intermediate products of their synthesis. Water determination methods
GOST 14618.10-78 Essential oils, fragrant substances and intermediate products of their synthesis. Methods for determining density and refractive index
GOST 14870-77 Chemical products. Water determination methods
GOST 15113.2-77 Food concentrates. Methods for determining impurities and pest infestation of grain stocks
GOST 15846-2002 Products sent to the Far North and equivalent areas. Packaging, labeling, transportation and storage
GOST 17433-80 Industrial cleanliness. Compressed air. Pollution classes
GOST 19360-74 Film liner bags. General technical conditions
GOST 19433-88 Dangerous goods. Classification and labeling
GOST 20477-86 Polyethylene tape with a sticky layer. Specifications
GOST 25336-82 Laboratory glassware and equipment. Types, main parameters and sizes
GOST 26668-85 Food and flavoring products. Sampling methods for microbiological analyzes
GOST 26927-86 Raw materials and food products. Mercury determination method
GOST 26930-86 Raw materials and food products. Arsenic determination method
GOST 26932-86 Raw materials and food products. Lead determination methods
GOST 26933-86 Raw materials and food products. Methods for determining cadmium
GOST 28498-90 Liquid glass thermometers. General technical requirements. Test methods
GOST 29185-91 Food products. Methods for identifying and determining sulfite-reducing clostridia
GOST 29227-91 (ISO 835-1-81) Laboratory glassware. Graduated pipettes. Part 1. General requirements
GOST 30178-96 Raw materials and food products. Atomic adsorption method for determining toxic elements
GOST R 8.563-96 State system for ensuring the uniformity of measurements. Measurement techniques
GOST R 50779.10-2000 (ISO 3534-1-93) Statistical methods. Probability and basic statistics. Terms and Definitions
GOST R 51474-99 Packaging. Markings indicating how the goods are handled
GOST R 51650-2000 Food products. Methods for determining the mass fraction of benzo(a)pyrene
GOST R 51652-2000 Rectified ethyl alcohol from food raw materials. Specifications
GOST R 51760-2001 Polymer consumer containers. General technical specifications OK 005-93 All-Russian Product Classifier
GOST R 51766-2001 Raw materials and food products. Atomic absorption method for determination of arsenic
GOST R 52464-2005 Flavoring and food flavoring additives. Terms and Definitions
GOST R 8.563-2009 State system for ensuring the uniformity of measurements. Techniques (methods) for performing measurements
GOST R 52814-2007 (ISO 6579:2002) Food products. Method for detecting bacteria of the genus Salmonella
GOST R 52816-2007 Food products. Method for identifying and determining the number of coliform bacteria (coliform bacteria)
(Changed edition, Amendment No. 1, 2).
Note - When using this standard, it is advisable to check the validity of reference standards and classifiers using the “National Standards” index compiled as of January 1 of the current year, and according to the corresponding information indexes published in the current year. If the reference document is replaced (changed), then when using this standard you should be guided by the replaced (changed) standard. If the reference document is canceled without replacement, then the provision in which a reference to it is given applies to the part that does not affect this reference.
3 Terms and definitions
This standard uses the following terms according to GOST R 52464.
(New edition, Amendment No. 1).
4 Classification
4.1 Depending on their purpose, food flavorings (hereinafter referred to as flavorings) are divided into:
For confectionery and bakery (bread) products;
For soft drinks;
For margarine products;
For other food products.
4.3 Depending on the form of release, flavorings are divided into:
Liquid: in the form of solutions and emulsions (emulsion);
Dry: powdered and granular;
Pasty.
5 General technical requirements
5.1 Characteristics
5.1.1 Flavors must be produced in accordance with the requirements of this standard, the document in accordance with which the flavor of a specific name is produced, and the technological documentation for the flavor of a specific name, approved in the prescribed manner, in compliance with sanitary standards and rules.
5.1.2 Liquid flavors in appearance are colorless or colored, transparent or opaque liquids.
5.1.4 Paste-like flavorings in appearance are a homogeneous mass, colored or uncolored.
5.1.5 Characteristics of appearance and color are established in the document in accordance with which the flavor of a specific name is manufactured.
5.1.6 The smell must be characteristic of the flavor of a particular name.
5.1.7 The density and refractive index of the liquid flavor must comply with the standards established in the document in accordance with which the flavor of a particular name is manufactured.
Note - For flavors with dyes, emulsion and paste flavors, the refractive index is not determined.
5.1.8 The volume fraction of ethyl alcohol in liquid alcohol-containing flavors must comply with the standards established in the document in accordance with which the flavor of a particular name is manufactured.
Note - The volume fraction of ethyl alcohol is a mandatory indicator for flavors with a volume fraction of ethyl alcohol of more than 1.5%.
5.1.8 (New edition, Amendment No. 1, 2).
5.1.9 The mass fraction of moisture in dry and paste flavors must comply with the standards established in the document in accordance with which the flavor of a particular name is manufactured.
___________
* Until the introduction of the corresponding regulatory legal acts of the Russian Federation - regulatory documents of the Federal executive authorities.
___________
* Until the introduction of the relevant regulatory legal acts of the Russian Federation - regulatory documents of federal executive authorities.
5.1.10 –5.1.13
5.1.14 (Deleted, Amendment No. 1).
5.2 Requirements for raw materials
5.2.1 Raw materials in terms of safety indicators must comply with the standards established by regulatory legal acts of the Russian Federation*.
___________
*Prior to the introduction of the relevant regulatory legal acts of the Russian Federation - regulatory documents of federal executive authorities and.
5.2.2 The ingredient composition of flavorings, including its flavoring and aromatic part, is in accordance with the requirements established by regulatory legal acts of the Russian Federation*.
__________
*Prior to the introduction of the relevant regulatory legal acts of the Russian Federation - regulatory documents of federal executive authorities.
5.2.1, 5.2.2 (New edition, Amendment No. 1).
5.2.2.1 Ethyl alcohol, water, 1,2-propylene glycol, triacetin, vegetable oils and other raw materials, food products and substances, the use of which ensures the quality and safety of flavorings, are used as solvents.
5.2.2.2 Carbohydrates and their processed products, gums, salt, spices and other raw materials, food products and substances, the use of which ensures the quality and safety of flavors, are used as carriers (fillers) for dry flavors.
5.2.2.1, 5.2.2.2 (Changed edition, Amendment No. 1).
5.2.3 For the production of alcohol-containing flavorings, rectified ethyl alcohol from food raw materials with a degree of purification not lower than the highest according to GOST R 51652 must be used.
5.3 Packaging
5.3.1 Liquid flavorings are packaged:
In polyethylene canisters with lids that meet the requirements of GOST R 51760, including imported ones, made from materials whose use in contact with flavorings ensures their quality and safety;
In glass containers for food products;
In other containers made from materials whose use in contact with flavorings ensures their quality and safety.
(Changed edition, Amendment No. 1).
5.3.2 When packaging liquid flavors, at least 5% of the free space of the total capacity of the container must be left in each container.
5.3.3 Dry and paste-like flavors are packaged in polyethylene conical jars with a clamping lid and handle that meet the requirements of GOST R 51760, using film liner bags in accordance with GOST 19360, made from materials whose use in contact with flavors ensures their quality and safety.
5.3.4 It is permitted to use other types of packaging that ensure the safety of dry and paste-like flavors during storage and transportation, and made from materials whose use in contact with flavors ensures their quality and safety.
5.3.3, 5.3.4 (Changed edition, Amendment No. 1).
5.3.5 Negative deviation of the net contents of the packaging unit from the nominal amount of flavor must comply with GOST 8.579.
5.3.6 A batch of packaged flavors in packages must meet the requirements of GOST 8.579.
5.3.7 When transported by rail, polyethylene canisters with liquid flavors are packed in wooden boxes in accordance with GOST 13358 or lathing, when transported by air - in corrugated cardboard boxes in accordance with GOST 13516.
Note - Polyethylene canisters can be transported by road without packaging in transport containers.
5.3.8 When transported by rail and air, polyethylene cans with dry and paste flavors are packed in corrugated cardboard boxes in accordance with GOST 13516.
Note - Polyethylene cans may be transported by road without packaging in transport containers.
5.3.9 Glass containers with liquid flavors are packed in corrugated cardboard boxes in accordance with GOST 13516 or plank boxes in accordance with GOST 13358 using auxiliary packaging materials in accordance with the rules for transporting goods on the appropriate mode of transport.
5.3.10 The flaps of corrugated cardboard boxes are covered in the longitudinal and transverse directions with polyethylene tape with an adhesive layer in accordance with GOST 20477 or other packaging materials are used to ensure the safety of the product and the integrity of the container during transportation.
5.3.11 Flavors sent to the Far North and equivalent areas are packaged in accordance with GOST 15846.
5.4 Marking
5.4.1 Each packaging unit is marked or affixed a label containing the following data:
Name and location (address) of the manufacturer, name of the country;
Manufacturer's trademark (if available);
Full name of the flavor;
Batch number;
Net weight;
Date of manufacture;
Storage period and conditions;
Designation of the document in accordance with which the flavor of a specific name is produced;
Warning: “For industrial use only. If accidentally swallowed, induce vomiting, rinse the stomach and seek medical attention."
Gross weight
(Changed edition, Amendment No. 1, 2).
5.4.2 Transport marking - in accordance with GOST 14192 with the application of handling marks in accordance with GOST R 51474 and signs characterizing the type of hazard of the cargo in accordance with GOST 19433, specified in the document, in accordance with which a flavor of a specific name is produced.
5.4.2 (Introduced additionally, Amendment No. 1).
6 Safety requirements and environmental protection
6.1 In accordance with GOST 12.1.007, based on the degree of impact on the body, flavorings and their components are classified into the third (moderately hazardous substances) and fourth (low-hazardous substances) hazard classes.
The maximum permissible concentration in the air of the working area of the main (by weight) components of flavoring agents - solvents - is given in the document, in accordance with which the flavoring agent of a specific name is manufactured.
The size of the sanitary protection zone when organizing the production of flavors is agreed upon with the authorized body.
6.2 Air monitoring of the working area is carried out according to methods approved in the prescribed manner, with a frequency determined by the requirements of GOST 12.1.005 and agreed with the authorized body in the prescribed manner.
6.3 Liquid flavors are classified as flammable (flammable), flammable (GZh) or non-flammable liquids, dry - as flammable materials in accordance with GOST 12.1.044. The indicator of fire and explosion hazard of liquid flavorings - flash point - is given in the document in accordance with which a particular flavoring agent is manufactured.
6.4 When taking samples, conducting analyses, storing and using flavorings, comply with labor protection rules and fire safety rules adopted when working with flammable, combustible (GOST 12.1.004), harmful substances (GOST 12.1.007).
6.5 Fire extinguishing agents: sprayed water, air-mechanical foam, powders, for small fires - fire felt, powder fire extinguishers.
6.6 If the fragrance gets on the skin, it should be washed off with water, washed with soap, and if it gets into the eyes, rinse with plenty of water.
If the flavoring is accidentally ingested, induce vomiting, perform gastric lavage and seek medical attention.
6.7 When storing and transporting flavors, environmental protection is ensured by sealing the container. If it is violated and the flavoring gets into the environment, it must be collected and disposed of.
6.8 When storing, transporting, using and disposing of flavorings to prevent harm to the natural environment, human health and genetic fund, do not pollute the soil, surface and ground waters.
6.9, 6.10 (Excluded, Amendment No. 1).
7 Acceptance rules
7.1 Flavorings are taken in batches. A batch is considered to be any number of flavors of the same name, manufactured within a certain time interval, according to the same technological documentation, identically packaged, intended for simultaneous delivery and acceptance and issued with one certificate of quality and safety indicating:
Certificate number and date of issue;
Names and location (address) of the manufacturer, name of the country;
Full name of the flavor;
Lot numbers;
Dates of manufacture;
Net lot weights;
Number of units of transport packaging;
Test results data;
Storage period and conditions;
Type of solvent or dry carrier (filler);
Purpose of flavoring;
7.2 For quality control and acceptance of flavorings, the following test categories are established:
Acceptance;
7.4 The results of acceptance tests are documented in a test report in the form accepted by the manufacturer, or reflected in a journal.
7.5 If the results of acceptance tests are negative for at least one quality indicator for this indicator, repeat tests are carried out on a double sample from the same batch. The results of repeated tests are applied to the entire batch.
7.6 If the results of repeated tests are unsatisfactory for at least one indicator, the entire batch of flavoring is rejected.
7.7 Procedure and frequency of monitoring the content of toxic elements, benzo(a)pyrene. Biologically active substances, as well as microbiological indicators, are established by the manufacturer in the production control program.
(Changed edition, Amendment No. 1).
7.8 The “smell” indicator of the flavoring agent is controlled only by the manufacturer.
(Changed edition, Amendment No. 1).
7.9 The basis for making a decision to accept a batch of flavoring is the positive results of acceptance tests and preceding periodic tests carried out within the established time frame.
8 Control methods
8.1 Control of compliance of packaging and labeling of flavors with the requirements of this standard is carried out by external inspection of each packaging unit of products from a sample according to.
8.2 To check the quality of flavorings according to organoleptic, physico-chemical and safety indicators, instant samples are taken from the product units included in the sample, from which total and laboratory samples are formed.
For microbiological analyses, sampling is carried out in accordance with GOST 26668.
8.3 Snapshot sampling, total sample collection, and separation of laboratory and analytical samples
8.3.1 Instant samples must be equal in volume (mass). The sum of all instant samples by volume (mass) should be 1.5-2.0 times greater than the volume (mass) of the laboratory sample.
The volume (weight) of the laboratory sample and the sample for analysis of the flavoring agent is determined by the document in accordance with which the flavoring agent of a specific name is manufactured.
8.3.2 The number of instant samples of liquid flavor depends on the volume occupied by the flavor. One instant sample is taken along the entire height of the flavoring layer, if its volume is up to 1 dm 3 inclusive, two instant samples are taken to a depth of 1/3 and 2/3 from the top level, if the volume is more than 1 dm 3, but does not exceed 10 dm 3 , three instant samples (from the upper, middle and lower layers) in all cases when the volume of flavoring is more than 10 dm 3.
8.3.3 Instant samples of liquid flavoring are taken with a sampling tube with an extended lower end, with a diameter of 6 to 15 mm, and a length exceeding the height of the container by several centimeters.
The upper hole of the tube is closed with a thumb or a stopper, immersed to the required depth, the tube is opened for a short time to fill, then closed again and the tube with the sample is removed.
8.3.4 Flash samples of the flavor paste are taken with a sampling tube that is lowered vertically to the bottom of the container, then tilted and withdrawn slowly to ensure that the entire contents of the tube are preserved.
When using a probe, it is immersed (screwed in) to the entire depth of the container along the vertical axis. Then the dipstick is removed.
8.3.5 Instant samples of dry flavoring are taken with a probe, immersing it to the entire depth of the container along the vertical axis.
8.3.6 Sampling of instant samples of products at the stage of delivery - acceptance to the warehouse is carried out before sealing the container.
8.3.7 All instant samples are placed in a sample vessel, mixed thoroughly and a total sample is obtained.
8.3.8 Isolation of laboratory sample
8.3.8.1 A laboratory sample of liquid and paste flavoring is obtained after thoroughly mixing the total sample and simply reducing it to the laboratory sample volume.
8.3.8.2 A laboratory sample of dry flavoring is obtained by reducing the total sample using the quartering method.
8.3.8.3 The laboratory sample for small volume batches of flavorings may be a total sample, and the total volume or mass of the instant samples must be no less than the volume or mass required for testing.
8.4 Labeling of laboratory samples
The isolated laboratory sample of flavoring is thoroughly mixed again, divided into two equal parts and placed in clean, dry glass containers. The vessels are tightly closed with cork or polyethylene stoppers and labeled with the following indication:
Flavor names;
Manufacturer's name;
Type of solvent (carrier);
Lot numbers and masses;
Dates of manufacture;
Sampling dates and locations;
Surnames and signatures of the person who took the sample;
Designations of the document in accordance with which the flavor of a specific name is produced.
One part of the laboratory sample is used for testing, the second is sealed and stored for a specified storage period in case of disagreement in assessing the quality of the flavor for re-analysis.
For a small batch of liquid flavorings, it is allowed to store a laboratory sample of the flavoring used for testing.
Laboratory samples are stored in a place protected from light at a temperature not exceeding 25 ° C (unless otherwise specified in the document in accordance with which the flavor of a particular name is produced), laboratory samples of dry flavors - at a relative humidity of no more than 75%.
8.5 Determination of appearance and color of flavorings
8.5.1 The appearance and color of liquid and paste flavoring is determined by viewing a sample for analysis in an amount of 30 to 50 cm 3 in a glass B-1(2)-50(100) according to GOST 25336 against the background of a sheet of white paper in transmitted or reflected light .
8.5.2 The appearance and color of the dry flavor is determined by viewing a sample for analysis weighing from 30 to 50 g, placed on a sheet of white filter paper according to GOST 12026, in diffuse daylight or under the light of LD fluorescent lamps according to GOST 6825.
8.5.3 A flavoring agent is considered to comply with the requirements of this standard if the appearance and color of the sample for analysis comply with the requirements of the document in accordance with which the flavoring agent of a particular type is manufactured.
8.6 Odor detection
The method consists of an organoleptic comparison of a sample for flavor analysis with a control sample (standard) of the flavor of a given name.
A sample of the flavor of a given name, the smell of which is approved by the manufacturer's tasting council, is taken as a control sample (standard).
For a control sample, a laboratory sample with a volume (weight) of at least 250 cm 3 (g) of flavoring produced under production conditions is taken. The control sample is stored in a hermetically sealed container for the shelf life established in the document in accordance with which the flavor of a particular name is manufactured.
8.6.1 Determination of liquid fragrance odor
Strips of filter paper 10´ 160 mm according to GOST 12026 are simultaneously moistened (approximately 3 cm) in the control sample and the sample for analysis and their smell is compared.
A flavoring agent is considered to comply with the requirements of this standard if the odor of the “wet” strips of the test sample and the control sample is the same.
8.6.2 Odor determination of dry and paste flavorings
A sample for analysis of the flavoring agent and a control sample weighing from 30 to 50 g is placed on a sheet of white filter paper according to GOST 12026 and their odor is assessed.
A flavoring agent is considered to comply with the requirements of this standard if the odor of the test sample and the control sample is the same.
8.7 Determination of the refractive index of liquid flavors - according to GOST 14618.10 (section 4).
8.8 Determination of the density of liquid flavors - according to GOST 14618.10 (section 2 or section 3).
8.9 Determination of the volume fraction of ethyl alcohol in liquid alcohol-containing flavorings is carried out according to the method (Appendix).
Note - The method is not arbitration.
8.10 (Deleted, Amendment No. 2).
8.11 Determination of the mass fraction of moisture in dry and paste flavors - according to GOST 14618.6 or according to the method (Appendix).
8.12 Determination of microbiological parameters of flavorings:
The number of mesophilic aerobic and facultative anaerobic microorganisms - according to GOST 10444.15;
The number of bacteria of the E. coli group - according to GOST R 52816;
Yeast and molds - according to GOST 10444.12;
Bacteria such as salmonella - according to GOST R 52814;
The number of sulfite-reducing clostridia is according to GOST 29185.
(Changed edition, Amendment No. 2).
8.13 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 and.
(Changed edition, Amendment No. 1).
8.14 Determination of metallomagnetic impurities - according to GOST 15113.2.
8.15 Determination of benzo(a)pyrene - according to GOST R 51650.
8.16 Determination of the flash point of liquid flavors - according to GOST 12.1.044 (subsection 4.4).
8.17 (Deleted, Amendment No. 1)..
9 Transportation and storage
9.1 Flavors are transported by all modes of transport in accordance with the cargo transportation rules in force for the relevant mode of transport.
9.2 Liquid flavors are stored in closed and darkened rooms at a temperature not exceeding 25 ° C, unless otherwise stated in the document in accordance with which the flavor of a specific name is manufactured.
Note - When storing liquid flavors, opalescence and precipitation are allowed if this is provided for in the document in accordance with which the flavor of a particular name is manufactured.
9.3 Dry flavors are stored in dry, well-ventilated areas at a temperature not exceeding 25 ° C and a relative humidity of not more than 75%, unless otherwise specified in the document in accordance with which the flavor of a specific name is produced.
Note - When storing dry flavors, loosely packed lumps (easily crumbling) are allowed.
9.4 Transportation and storage of fragrances together with chemicals and strong-smelling products and materials is not allowed.
9.5 The shelf life of flavors is established in the document in accordance with which the flavor of a specific name is manufactured.
10 Directions for use
The scope of use of flavorings and their maximum dosages in food products is established by the manufacturer in accordance with the requirements established by 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.
(New edition, Amendment No. 1).
Appendix A
(required)
Product codes according to OK 005
|
OKP code |
Name of product |
|
91 4560 |
Flavorings for food products |
|
91 4561 |
For margarine products |
|
91 4562 |
For various food industry products |
|
91 5430 |
Food flavorings |
|
91 5431 |
For confectionery and bakery products |
|
91 5432 |
For soft drinks |
|
91 5434 |
For other food products |
Determination of the volume fraction of ethyl alcohol in liquid food flavorings
Determination of the volume fraction of ethyl alcohol in liquid food flavorings (hereinafter referred to as flavorings) is performed by the chromatographic method on an instrument with a flame ionization detector. The range of measured volume fractions of ethyl alcohol is from 1.0% to 85.0% inclusive.
B.1 Essence of the method
The method is based on the use of a variant of gas adsorption chromatography in combination with “cold” introduction of the sample for analysis and the special properties of the Polysorb-1 sorbent in relation to ethyl alcohol. “Cold input” (introducing a sample for analysis at a temperature below the boiling point of the analyzed substance) allows you to completely separate ethyl alcohol from low-boiling and high-boiling flavor components.
B.2 Equipment, measuring instruments, auxiliary equipment, materials and reagents
The following laboratory equipment is used for testing:
Gas chromatograph equipped with a flame ionization detector with a nonane sensitivity of at least 1 × 10 -11 g/cm 3 ;
A computer or integrator that has software for a basic set of chromatography automation operations;
Laboratory scales with limits of permissible absolute error of single weighing ±0.0015 g;
Set of weights (10 g - 500 g) F 1 according to GOST 7328;
Stopwatch of 2nd accuracy class with a counter scale capacity of 30 min, division value of 0.20 s, error ± 0.60 s;
Thermometer TL-31-A, measurement range from 0 °C to 250 °C according to GOST 28498;
Microsyringe with a capacity of 0.5 mm 3 from Agilent Technologies (catalog no. 5183-4580 from 2000/2001) or similar;
Measuring glassware according to GOST 1770;
Pipettes 2-1-5, 2-1.10, 2-1-20, 2-1-25, 4-2-1 according to GOST 29227;
Packed chromatographic column made of stainless steel, 1 m long and with an internal diameter of 3 mm. If necessary, it is possible to use a longer column and increase the temperature of the column thermostat when increasing the analysis time;
Water jet vacuum pump according to GOST 25336;
Glass bottles with a capacity of 5 to 15 cm 3 with silicone rubber stoppers;
Fiberglass according to GOST 10146;
Gaseous nitrogen of special purity according to GOST 9293;
Technical hydrogen grade A according to GOST 3022. The use of a hydrogen generator is allowed;
Compressed air according to GOST 17433. It is allowed to use compressors of any type that provide the necessary pressure and air purity;
Distilled water according to GOST 6709;
- “Polysorb-1”, fraction 0.25 - 0.50 mm;
Rectified ethyl alcohol according to GOST R 51652.
It is allowed to use other measuring instruments, materials and reagents with metrological characteristics and quality not lower than those specified, except for the Polysorb-1 sorbent.
(Changed edition, Amendment No. 2).
B.3 Preparation for measurements
B.3.1 Measurement conditions
When preparing for measurement and during measurement, observe the following conditions:
|
Ambient air temperature.........................…………………... |
(20 ± 2) °С |
|
Atmosphere pressure...............................…………………………... |
from 95.0 to 106.7 kPa |
|
(from 720 to 800 mmHg) |
|
|
Relative humidity......................…………………… |
from 20% to 90% |
|
Mains voltage................................................................................. |
(220 ± 20) V |
|
Frequency of current in the electrical network................................……………………….. |
(50 ± 2) Hz |
B.3.2 Preparation of the chromatographic column
The chromatographic column is washed successively with water, ethyl alcohol, acetone, dried in a stream of air and filled with a packing.
The filled column is placed in the chromatograph thermostat and connected to the evaporator without connecting to the detector. The column is conditioned with a carrier gas (nitrogen) at a rate of 40 cm 3 /min in temperature programming mode at a rate of 4 °C/min to 6 °C/min to 170 °C and another 0.5 to 1.0 h at this temperature. After cooling, the output end of the column is connected to the detector and the stability of the zero line is checked at the operating temperature of the column thermostat.
B.3.3 Preparation of measuring equipment
The chromatograph is prepared for operation in accordance with the operating instructions supplied with the device.
The device is calibrated using calibration solutions.
B.3.4 Preparation of calibration solutions
Solutions of ethyl alcohol in distilled water with concentrations close to the specified measurement range are used as calibration solutions.
Before preparing solutions, the content of the main substance in the ethyl alcohol used is determined according to GOST 3639.
In seven volumetric flasks with a ground stopper with a capacity of 100 cm 3, pour from 20 to 30 cm 3 of distilled water, add sequentially with pipettes of 1.0; 5.0; 10.0; 15.0; 25.0 cm 3 and cylinders 50.0; 85.0 cm 3 ethyl alcohol. The contents of the flasks are mixed and the volumes of solutions are adjusted to the mark with distilled water (calibration solutions No. 1 - 7).
The volume fraction of ethyl alcohol Q g% in calibration solutions is determined by the density determined after keeping the solutions for 2 to 3 hours with a pycnometer according to GOST 3639 (section 3) with subsequent conversion of the density of the aqueous-alcohol solution to the alcohol content in percent (by volume ).
(Changed edition, Amendment No. 1).
B.4 Taking measurements
B.4.1 Measurements are performed under the following operating parameters of the chromatograph:
|
Column thermostat temperature...................................……………………….. |
80 °C |
|
Evaporator (injector) temperature................................……………………… |
(50 ± 5) °С |
|
Temperature of the transition chamber...................................………………………... |
80 °C |
|
Nitrogen carrier gas consumption............................................................................... |
from 30 to 40 cm 3 /min |
|
Hydrogen consumption......................................................................................... ... |
30 cm 3 /min |
|
Air flow.....................................…………………………… …….. |
300 cm 3 /min |
|
Sample volume for analysis.................................................................... |
0.2 mm 3 |
After analyzing 20 - 30 samples for analysis, increase the temperature of the evaporator, column thermostat and transition chamber to 150 ° C and maintain it for 30 to 40 minutes to clean the chromatographic system from high-boiling compounds.
Checking the calibration characteristic at one of the points in the range of measured concentrations is carried out daily in accordance with.
B.4.3 Gas chromatographic analysis of a laboratory sample of flavoring
After establishing the operating parameters, turning on the analysis automation system to record chromatograms and process the obtained data, and a stable zero line on the working scale of the detector, analysis begins.
To determine the volume fraction of ethyl alcohol of the flavor being studied, two 0.2 mm 3 doses taken from a laboratory sample of the flavor are injected into the chromatograph evaporator using a microsyringe.
The same syringe is used for calibration and analysis.
B.5 Processing results
B.5.1 The results are processed using the software of the personal computer or integrator included with the chromatograph in accordance with their operating instructions.
B.5.2 Volume fraction of ethyl alcohol in a laboratory sample of flavoring X, %, is calculated using the formula:
Where X- volume fraction of ethyl alcohol in the flavoring agent;
d - relative error in determining the volume fraction of ethyl alcohol, %.
B.5.4 Permissible relative error 5 in determining the volume fraction of ethyl alcohol in flavorings with a confidence level P = 0.95 is ±15%.
B.6 Monitoring the accuracy of measurement results
When monitoring measurement accuracy using this method, perform the following operations:
B.6.1 Monitoring the stability of the chromatograph zero line
Monitoring is carried out continuously during the analysis of flavors. The positive drift of the zero line, defined as the greatest shift of the zero line signal within 20 minutes from the start of the analysis, should not exceed 20% of the peak height corresponding to a volume fraction of ethyl alcohol of 1% (calibration solution No. 1). If the specified value is exceeded or side peaks appear, the temperature of the column, evaporator and transition chamber is raised to 150 °C and maintained for 30 to 40 minutes to accelerate the elution of high-boiling components of the analyzed mixtures.
B.6.2 Monitoring the convergence of chromatograph output signals
The controlled parameter is the relative range of the chromatograph output signals. Control is carried out during calibration and during periodic monitoring of calibration coefficients.
The control result is considered positive when the condition is met
|
|
Where A m Oh - maximum chromatographic peak area, units. accounts;
A min - minimum chromatographic peak area, units. accounts;
- arithmetic mean value of peak areas obtained from parallel injections of samples for analysis, units. accounts.
B.6.3 Monitoring the correctness of the construction of the calibration characteristic
The controlled parameter is the range of calibration coefficients relative to the average value. The calibration quality is considered satisfactory if the condition is met
Where K max- maximum value of the calibration coefficient of ethyl alcohol in the range of concentrations under study, % / unit. accounts;
Kmin- minimum value of the calibration coefficient of ethyl alcohol in the range of concentrations under study, % / unit. accounts;
TO- arithmetic mean value of the calibration coefficient of ethyl alcohol, % / unit. accounts.
Control is carried out each time when constructing a calibration dependence. If condition () is not met, then the device is re-calibrated.
If the control results are negative, the device is calibrated in accordance with.
B.7 Safety requirements
B.7.1 When working on a gas chromatograph, it is necessary to comply with labor protection requirements and safety rules in accordance with the operating instructions for the device.
B.7.2 The room in which the measurement is made must be equipped with general supply and exhaust ventilation.
Appendix B (Deleted, Amendment No. 2)
Determination of the mass fraction of moisture in food flavorings
This method is intended to measure the mass fraction of moisture in food flavorings (hereinafter referred to as flavoring agents) dissolved in liquids that do not react with the Fischer reagent.
D.1 Ranges and standards of measurement error
The technique ensures that measurements are performed within the range and with the limits of permissible absolute error given in Table D.1.
Table D.1
In percentages
D.2 Measuring instruments, auxiliary equipment, reagents and materials
D.2.1 Laboratory scales of special (I) accuracy class, verification scale (e) 0.5 mg, maximum weighing limit 200 g, operating error limit ± 3.0 e according to GOST 24104.
D.2.2 Titrimetric laboratory analyzer model AF8 from Orion Research, Inc with a measurement range of the mass fraction of moisture from 0.5% to 50.0% and a standard deviation limit of the relative measurement error of ± 0.4% (at 25 mg of moisture), consisting of:
Electronic unit,
Titration block,
Bottles for reagents, capacity 1 dm 3.
D.2.3 Measuring cylinder with a capacity of 100 cm 3 versions 1, 1 accuracy class according to GOST 1770.
D.2.4 Conical flask with a capacity of 500 cm 3 with a ground section, type Kn-1-500-40 TS; Kn-1-500-40 THS according to G.2.8; the quality is not worse than the above.
D.3 Measurement method
The measurement method is based on volumetric analysis, based on the interaction of iodine and sulfur dioxide in a methanol solution in the presence of water. Due to the reversibility of the reaction, pyridine is used to complete it.
The titrimetric laboratory analyzer model AF8 from Orion Research, Inc is designed for measuring the mass fraction of moisture and is a device with a fully automated process of measurement and processing of results.
D.4 Safety requirements
When performing measurements, it is necessary to comply with the requirements set out in the documentation for the titrimetric laboratory analyzer model AF8 from Orion Research, Inc.
D.5 Measurement conditions
When performing measurements in the laboratory, the following conditions are observed:
|
Ambient air temperature......... |
from 10 °C to 35 °C |
|
Atmosphere pressure..............................………… |
from 84.0 to 106.7 kPa |
|
(from 630 to 800 mmHg) |
|
|
Relative humidity.....................…... |
no more than 80% |
|
Mains voltage...................................…………… |
|
|
The room where work with the Fischer reagent is carried out is provided with supply and exhaust ventilation |
|
|
All operations with Fischer reagent are carried out in a fume hood |
|
D.6 Sampling
Selection of spot samples of flavoring agents is carried out in accordance with the requirements of the document in accordance with which the flavoring agent of a specific name is manufactured.
D.7 Preparation for measurements
D.7.1 The laboratory titrimetric analyzer model AF8 from Orion Research, Inc is prepared for measurements in accordance with its operating instructions.
D.7.2 Preparation of Fischer reagent
D.7.2.1 In a fume hood, 100 cm 3 of Fischer reagent No. 1 is poured into a measuring cylinder, then 100 cm 3 of Fischer reagent No. 2 is poured into another measuring cylinder and sequentially poured into a conical flask with a capacity of 500 cm 3.
D.7.2.2 The resulting mixture is poured into a bottle marked “Fischer reagent”, which is connected to the pump of the titration unit (peristaltic pump).
D.7.3 Methanol poison is poured into a bottle marked “Methanol poison”, which is also connected to the pump of the titration unit.
Note - When connecting bottles with ready-made reagents to the titration unit pump, make sure that all caps fit tightly and that the float in the drain bottle moves freely in a vertical plane.
D.7.4 Raise the pump cover of the titration unit until it stops and move the holder of the reaction vessel until it stops in order to completely isolate the container.
D.7.5 Preparation of laboratory sample for measurements
D.7.5.1 Weigh a sample for analysis of a bulk dry laboratory sample of flavoring weighing from 0.2 to 0.3 g on filter paper or a sample for analysis of a liquid laboratory sample weighing from 0.5 to 1.0 g in a glass bottle.
D.7.5.2 Add the sample for analysis into the reaction vessel, and this operation should be performed as quickly as possible to minimize the ingress of moisture from the air.
Note - If the test sample is not added to the reaction vessel within 60 s, the titrator will return to conditioning mode.
D.8 Taking measurements
D.8.1 Calibration of the titrimetric laboratory analyzer model AF8 from Orion Research, Inc is carried out in accordance with the operating instructions for the device.
D.8.2 Checking the correct calibration of the titrimetric laboratory analyzer model AF8 from Orion Research, Inc. carried out by titrating a given volume of distilled water (V = 10 µl) daily before taking measurements. Calibration is considered completed if the coefficient of variation for three results out of ten does not exceed the norm established in the operating instructions for the device. If the coefficient of variation for three titrations out of ten exceeds the specified norm, then the next sample should be added for calibration.
D.8.3 Measurements are carried out in accordance with the operating instructions for the titrimetric laboratory analyzer model AF8 from Orion Research, Inc. Three measurements are taken.
D.9 Registration of results
The result of the determination is taken as the arithmetic mean of three measurements, the discrepancy between which (convergence) should not exceed 0.5%.
The result of the analysis is presented as X,%.
The measurement results are recorded in the work log in accordance with the “Instructions for Technical Control”.
D.10 Monitoring the accuracy of measurement results
The accuracy of measurement results is monitored by online control of convergence.
Operational control of convergence is carried out upon receipt of each result. Convergence control is carried out by comparing the discrepancy between the measurement results (X 1, X 2 and X 3) with the permissible discrepancy, which should not exceed 0.5%.
If the permissible discrepancies are exceeded, the measurements are repeated using another sample for analysis. If the specified standard is exceeded again, the reasons are found out and eliminated, and if necessary, a new calibration is carried out.
Bibliography
SanPiN 2.3.2.1293-03 Hygienic requirements for the use of food additives (with additions and changes)
SanPiN 2.3.2.1078-2001 Hygienic requirements for the safety and nutritional value of food products
PPB-01-93 Fire safety rules in the Russian Federation
MU 5178-90 Guidelines for the determination of mercury in food products
(New edition, Amendment No. 1, 2).
Keywords: food flavorings, classification, safety and quality indicators, technical requirements, control methods
(Changed edition, Amendment No. 1).
Interstate standard GOST 32049-2013
"FOOD FLAVORS. GENERAL TECHNICAL CONDITIONS"
(put into effect by order of the Federal Agency for Technical Regulation and Metrology dated July 25, 2013 N 441-st)
Food flavourings. General specifications
Preface
The goals, basic principles and basic procedure for carrying out work on interstate standardization are established by GOST 1.0-92 "Interstate standardization system. Basic provisions" and GOST 1.2-2009 "Interstate standardization system. Interstate standards, rules and recommendations for interstate standardization. Rules for development, adoption, application, renewal and cancellation"
1 area of use
This standard applies to food flavorings (hereinafter referred to as flavoring agents) intended for the food industry.
This standard does not apply to flavorings for tobacco products.
Requirements ensuring the safety of flavors for human life and health are set out in 5.1.5 - 5.1.12, product quality requirements - 5.1.2 - 5.1.4, labeling requirements - 5.4.
2 Normative references
This standard uses normative references to the following interstate standards:
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 12.0.004-90 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 12.1.019-79 System of occupational safety standards. Electrical safety. General requirements and nomenclature of types of protection
GOST 12.1.044-89 (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 12.4.021-75 System of occupational safety standards. Ventilation systems. General requirements
GOST 12.4.103-83 System of occupational safety standards. Special protective clothing, personal protective equipment for legs and arms. Classification
GOST 1770-74 (ISO 1042-83, ISO 4788-80) Laboratory glassware. Cylinders, beakers, flasks, test tubes. General technical conditions
GOST 2603-79 Reagents. Acetone. Specifications
GOST 3022-80 Technical hydrogen. Specifications
GOST 3639-79 Water-alcohol solutions. Methods for determining the concentration of ethyl alcohol
GOST 6709-72 Distilled water. Specifications
GOST 6825-91 Tubular fluorescent lamps for general lighting
GOST 6995-77 Reagents. Methanol is a poison. Specifications
GOST 9293-74 (ISO 2435-73) Nitrogen, gaseous and liquid. Specifications
GOST 10146-74 Filter fabrics made of glass twisted filament threads. Specifications
GOST 10444.12-88 Food products. Method for determining yeast and mold fungi
GOST 10444.15-94 Food products. Methods for determining the number of mesophilic aerobic and facultative anaerobic microorganisms
GOST 12026-76 Laboratory filter paper. Specifications
GOST 13358-84 Wooden boxes for canned food. Specifications
GOST 13516-86 Corrugated cardboard boxes for canned food, preserves and food liquids. Specifications
GOST 14192-96 Marking of cargo
GOST 14618.6-78 Essential oils, fragrant substances and intermediate products of their synthesis. Water determination methods
GOST 14618.10-78 Essential oils, fragrant substances and intermediate products of their synthesis. Methods for determining density and refractive index
GOST 14870-77 Chemical products. Water determination methods
GOST 15113.2-77 Food concentrates. Methods for determining impurities and pest infestation of grain stocks
GOST 15846-2002 Products sent to the Far North and equivalent areas. Packaging, labeling, transportation and storage
GOST 17433-80 Industrial cleanliness. Compressed air. Pollution classes
GOST 19360-74 Film liner bags. General technical conditions
GOST 19433-88 Dangerous goods. Classification and labeling
GOST 20477-86 Polyethylene tape with a sticky layer. Specifications
GOST 25336-82 Laboratory glassware and equipment. Types, main parameters and sizes
GOST 26668-85 Food and flavoring products. Sampling methods for microbiological analyzes
GOST 26927-86 Raw materials and food products. Mercury determination method
GOST 26930-86 Raw materials and food products. Arsenic determination method
GOST 26932-86 Raw materials and food products. Lead determination methods
GOST 26933-86 Raw materials and food products. Methods for determining cadmium
GOST 28498-90 Liquid glass thermometers. General technical requirements. Test methods
GOST 29169-91 Laboratory glassware. Single mark pipettes
GOST 29185-91 Food products. Methods for identifying and quantifying sulfite-reducing clostridia
GOST 29227-91 (ISO 835-1-81) Laboratory glassware. Graduated pipettes. Part 1. General requirements
GOST 29229-91 (ISO 835-3-81) Laboratory glassware. Graduated pipettes. Part 3. Graduated pipettes with a waiting time of 15 s
GOST 30178-96 Raw materials and food products. Atomic absorption method for determining toxic elements
GOST 31747-2012 Food products. Methods for identifying and determining the number of coliform bacteria (coliform bacteria)
GOST 31659-2012 Food products. Method for detecting bacteria of the genus Salmonella
GOST 31266-2004 Raw materials and food products. Atomic absorption method for determination of arsenic
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 using the annual information index "National Standards", which was published as of January 1 of the current year, and according to the releases of the monthly information index "National Standards" for the current year. If the reference standard is replaced (changed), then when using this standard you should be guided by the replacing (changed) standard. If the reference standard is canceled without replacement, then the provision in which a reference is made to it is applied in the part that does not affect this reference.
3 Terms and definitions
The following terms with corresponding definitions are used in this standard:
3.1 food flavoring: A product not directly consumed by humans as food, containing a flavoring substance or a flavoring preparation, or a thermal technological flavoring agent, or a smoke flavoring agent, or flavoring precursors, or a mixture thereof (flavoring part), intended to impart flavor and/or flavor to food products flavor (excluding sweet, sour and salty), with or without the addition of other food ingredients.
3.2 smoke flavoring: A mixture of substances isolated from smokes used in traditional smoking by fractionation and purification of smoke condensates.
3.3 thermal technological flavoring: A mixture of substances obtained as a result of heating at a temperature not exceeding 180°C and a heating duration of no more than 15 minutes of food and/or non-food ingredients, one of which must be an amino compound, and the other a reducing sugar.
Notes:
1 When producing a thermal technological flavor at temperatures below 180°C, the heating duration doubles for every 10°C decrease in temperature.
2 The process time should not exceed 12 hours.
3 The pH value during the process should not exceed 8.0 units. pH.
3.4 natural flavoring: Flavoring, the flavoring part of which contains only flavoring preparations and/or natural flavoring substances.
Notes:
1 The term “natural flavoring” may be used if its flavoring portion consists exclusively of flavoring preparations and/or natural flavoring substances.
2 The term “natural flavor” in combination with the name of the food, food category or source of plant or animal origin can only be used if the flavoring preparations and/or natural flavoring substances contained in it are obtained from the named source, e.g. "natural apple flavor (Apple)", "natural fruit flavor (Fruity)", "natural mint flavor (Mint)".
3 The term “natural flavor” may be used when the flavorings and/or natural flavorings contained in it are obtained from a source that does not reflect their taste and aroma, for example, “natural flavor and fancy name.”
3.5 synthetic flavoring: A flavoring agent, the flavoring part of which contains synthetic flavoring substances.
3.6 flavoring substance: Chemically defined (chemically individual) substance with flavoring properties, possessing a characteristic aroma and/or taste (except for sweet, sour and salty).
3.7 natural flavoring substance: A flavoring substance isolated using physical, enzymatic or microbiological processes from raw materials of plant, microbial or animal origin, including those processed by traditional methods of preparing food products.
Note - Traditional methods of preparation (production) of food products include: cooking, including steaming and under pressure (up to 120°C), baking, roasting, stewing, frying, including in oil (up to 240°C at atmospheric pressure), drying, evaporation, heating, cooling, freezing, soaking, maceration (soaking), infusion (brewing), percolation (extraction with straining), filtration, pressing (squeezing), mixing, emulsification, grinding (cutting, crushing, grinding , crushing), encapsulation, peeling, distillation (rectification), extraction (including solvent extraction), fermentation and microbiological processes.
3.8 synthetic flavoring substance: A flavoring substance obtained by chemical synthesis.
3.9 flavoring precursor: A product, not necessarily having flavoring properties, intentionally added to food products for the sole purpose of obtaining flavor by destruction or reaction with other components during food preparation.
Note - The flavoring precursor can be obtained both from food products and from products not used directly for food.
3.10 flavoring preparation: A mixture of flavoring or other substances isolated by physical, enzymatic or microbiological processes from food products or from food raw materials, including after processing by traditional methods of preparing food products, and/or from products of plant, animal or microbial origin, not used directly as food, consumed as such or processed using traditional food preparation methods.
4 Classification
4.1 Depending on their purpose, food flavorings are divided into:
For flavorings for confectionery and bakery (bread) products;
Flavorings for soft drinks;
Flavorings for fat and oil products;
Flavorings for other food products.
4.2 Depending on the composition of the flavoring part, flavorings are divided into:
For flavorings based on flavoring substances (natural and synthetic);
Flavorings based on flavoring preparations (natural);
Flavorings based on flavoring precursors;
Thermal technological flavors;
Smoke flavors;
Mixed flavors.
4.3 Depending on the form of release, flavorings are divided into:
For liquids: in the form of solutions and emulsions (emulsion);
Dry: powdered, including encapsulated and granulated;
Pasty.
5 General technical requirements
5.1 Characteristics
5.1.1 Flavors are produced in accordance with the requirements of this standard, a regulatory document in accordance with which a flavor of a specific name is produced, in compliance with the requirements, or regulations in force in the territory of the state that has adopted the standard.
5.1.2 In terms of organoleptic indicators, flavorings must meet the requirements specified in Table 1.
Table 1 - Organoleptic indicators
5.1.3 For a flavoring agent of a specific name, in a regulatory document, the manufacturer establishes individual requirements for this flavoring agent for the following organoleptic and physicochemical parameters:
Appearance, color and smell;
Density and refractive index (for liquid flavors, except emulsion, paste and colored);
The volume fraction of ethyl alcohol in alcohol-containing flavorings (for flavorings that, in accordance with legislative and regulatory legal acts in force in the territory of the state that has adopted the standard, belong to alcohol-containing food products);
Mass fraction of moisture (in dry and paste flavors);
Presence of metallomagnetic impurities (in dry flavors), the presence of metallomagnetic impurities in dry flavors is allowed no more than 3 million -1 (3 mg/kg);
Flash point (for liquid flavors).
5.1.4 Flavorings are identified by:
By name and purpose, by comparing the flavor indicated in the labeling with the name specified in the definition of the type of food product in, or regulations in force in the territory of the state that has adopted the standard;
By the appearance of the flavoring agent, comparison with the characteristics set out in the regulatory document, in accordance with which the flavoring agent of a specific name is manufactured;
According to organoleptic indicators, comparison with organoleptic characteristics (smell) set out in the regulatory document, in accordance with which the flavor of a specific name is produced;
5.1.5 Microbiological indicators of flavorings must comply with the requirements established by, or regulatory legal acts in force in the territory of the state that has adopted the standard.
5.1.8 The content of potentially hazardous biologically active substances in flavorings made using plant aromatic raw materials and/or extracts and essential oils should not lead to exceeding the permissible levels of potentially hazardous biologically active substances in food products using flavorings in accordance with the requirements, established, or regulatory legal acts in force in the territory of the state that has adopted the standard.
5.1.9 The use of potentially hazardous biologically active substances is not allowed: agaric acid, beta-asarone, aloin, hypericin, capsaicin, quassin, coumarin, mentofuran, methyl eugenol (4-allyl-1,2-dimethoxybenzene), pulegone, safrole (1- allyl-3,4-methylenedioxybenzene), hydrocyanic acid, thujone (alpha and beta), teucrine A, estragole (1-allyl-4-methoxybenzene), as flavoring agents in the production of flavorings and food products.
5.1.10 It is not permitted to use the tetraploid form of Calamus (Acorus calamus L, CE 13) as a source of flavorings, including flavoring substances and preparations.
5.1.11 When using medicinal plants and/or flavoring preparations from medicinal plants as natural sources, their content (in terms of dry raw materials or the biologically active substance contained in them) should not exceed the amount that has a pharmacological effect of 1 kg (dm 3) food products when used as flavoring preparations (flavors).
5.2 Requirements for raw materials
5.2.1 Raw materials for the production of flavorings must meet the safety requirements established by, or regulatory legal acts in force in the territory of the state that has adopted the standard.
5.2.2 The ingredient composition of flavorings must comply with the requirements established by, or regulatory legal acts in force in the territory of the state that has adopted the standard.
5.2.3 For the production of alcohol-containing flavorings, rectified ethyl alcohol is used from food raw materials with a degree of purification not lower than the highest according to regulatory documents in force in the territory of the state that has adopted the standard.
5.3 Packaging
5.3.1 Packaging of flavors must comply with the requirements established or regulations in force in the territory of the state that has adopted the standard.
5.3.2 Liquid flavorings are packaged:
In polymer canisters with lids, made from materials whose use in contact with flavorings ensures their quality and safety;
Glass containers for food products;
Other containers made from materials whose use in contact with flavorings ensures their quality and safety.
5.3.3 When packaging liquid flavors, at least 5% of the free space of the total capacity of the container must be left in each container.
5.3.4 Dry and paste-like flavors are packaged in polymer conical jars with a clamping lid and handle in accordance with the regulatory document in force in the territory of the state that has adopted the standard, using film liner bags in accordance with GOST 19360, made of materials whose use in contact with flavors ensures their quality and safety.
5.3.5 It is permitted to use other types of packaging that ensure the safety of dry and paste-like flavors during storage and transportation and are made from materials that meet the requirements established or regulations in force in the territory of the state that has adopted the standard.
5.3.6 Negative deviation of the net contents of the packaging unit from the nominal amount of flavoring must comply with GOST 8.579 (clause 4.2).
5.3.7 A batch of packaged flavors in packages must meet the requirements of GOST 8.579 (clauses 5.1, 5.7).
5.3.8 When transported by rail, polymer canisters with liquid flavors are packed in wooden boxes in accordance with GOST 13358 or lathing, when transported by air - in corrugated cardboard boxes in accordance with GOST 13516.
Note - Polymer canisters may be transported by road without packaging in transport containers.
5.3.9 When transported by rail and air, polymer cans with dry and paste flavors are packed in corrugated cardboard boxes in accordance with GOST 13516.
Note - Polymer cans can be transported by road without packaging in transport containers.
5.3.10 Glass containers with liquid flavors are packed in corrugated cardboard boxes in accordance with GOST 13516 or plank boxes in accordance with GOST 13358 using auxiliary packaging materials in accordance with the rules for transporting goods on the appropriate mode of transport.
5.3.11 The flaps of corrugated cardboard boxes are covered in the longitudinal and transverse directions with tape made of polymeric materials with an adhesive layer in accordance with GOST 20477 or other packaging materials are used to ensure the safety of the product and the integrity of the container during transportation.
5.3.12 Flavors sent to the Far North and equivalent areas are packaged in accordance with GOST 15846.
5.4 Marking
5.4.1 Labeling of flavors must comply with the requirements established and or regulatory legal acts in force in the territory of the state that has adopted the standard.
5.4.2 The marking of each packaging unit additionally includes the following data:
Lot number or mark identifying the lot;
Gross weight;
Storage conditions;
Designation of this standard;
Designation of the document in accordance with which the flavor of a specific name is manufactured;
Warning: "If accidentally swallowed, induce vomiting, gastric lavage and seek medical attention."
5.4.3 Transport marking - in accordance with GOST 14192 with the application of handling signs indicating the method of handling cargo - in accordance with the requirements established or regulatory legal acts in force in the territory of the state that has adopted the standard, and signs characterizing the type of hazard of the cargo - in accordance with GOST 19433.
6 Safety requirements and environmental protection
6.1 In accordance with GOST 12.1.007, in terms of the degree of impact on the body, flavorings and their components belong to the third (moderately hazardous substances) and fourth (low-hazardous substances) hazard classes.
The maximum permissible concentration in the air of the working area of the main (by weight) components of flavoring solvents is given in the document in accordance with which the flavoring agent of a particular name is manufactured.
6.2 Air monitoring of the working area is carried out according to methods approved in the established order, with a frequency determined by the requirements of GOST 12.1.005.
6.3 Liquid flavors are classified as flammable (flammable), flammable (GZh) or non-flammable liquids, dry - as flammable materials in accordance with GOST 12.1.044. The indicator of fire and explosion hazard of liquid flavorings - flash point - is given in the document in accordance with which a particular flavoring agent is manufactured.
6.4 When taking samples, conducting analyses, storing and using flavorings, comply with labor protection rules and fire safety rules adopted when working with flammable, combustible (GOST 12.1.004 and fire safety rules in force in the territory of the state that adopted the standard), harmful substances (GOST 12.1.007).
6.5 Fire extinguishing agents: sprayed water, air-mechanical foam, powders, for small fires - fire felt, powder fire extinguishers.
6.6 If the fragrance gets on the skin, it should be washed off with water, washed with soap, and if it gets into the eyes, rinse with plenty of water.
If the flavoring is accidentally ingested, induce vomiting, perform gastric lavage and seek medical attention.
6.7 When storing and transporting flavors, environmental protection is ensured by sealing the container. If it is violated and the flavoring gets into the environment, it must be collected and disposed of.
6.8 When storing, transporting, using and disposing of flavorings to prevent harm to the environment, health and human genetic fund, contamination of soil, surface and ground water is not allowed.
7 Acceptance rules
7.1 Flavorings are taken in batches.
A batch is considered a certain amount of a flavoring agent of the same name, obtained in one technological cycle, in the same packaging, produced by one manufacturer according to one regulatory document, accompanied by shipping documentation that ensures product traceability.
7.2 For quality control and acceptance of flavorings, the following test categories are established:
Acceptance and acceptance;
Periodic.
7.2.1 Acceptance tests are carried out for each batch of flavoring on the quality of packaging and labeling, organoleptic and physico-chemical indicators using random control. To do this, 10% of packaging units are randomly selected from the batch, but not less than three. If the number of packaging units is less than three, each packaging unit is subject to control.
To conduct tests, instantaneous, total, laboratory samples and samples for analysis are taken from the packaging units included in the sample in accordance with Section 8.
7.2.2 The results of acceptance tests are documented in a test report in the form accepted by the manufacturer or reflected in a log.
7.2.3 If the results of acceptance tests are negative for at least one quality indicator, repeated tests are carried out for this indicator on a double sample from the same batch. The results of repeated tests apply to the entire batch.
7.2.4 If the results of repeated tests are unsatisfactory for at least one indicator, the entire batch of flavoring is rejected.
7.3 The procedure and frequency of monitoring the content of toxic elements, benzo(a)pyrene, benzo(a)anthracene, biologically active substances, as well as microbiological indicators are established by the manufacturer in the production control program.
7.4 The “smell” indicator of the flavoring according to 8.5 is controlled only by the manufacturer
7.5 The basis for making a decision to accept a batch of flavoring is the positive results of acceptance tests and preceding periodic tests.
8 Control methods
8.1 Control of compliance of packaging and labeling of flavors with the requirements of this standard is carried out by external inspection of each packaging unit of products from the sample according to 7.2.1.
8.2 Sampling
8.2.1 To check the quality of flavorings according to organoleptic and physicochemical indicators and to determine toxic elements, instant samples are taken from product units included in the sample according to 7.2.1, from which a total and laboratory sample is formed.
For microbiological analyses, sampling is carried out in accordance with GOST 26668.
8.2.2 Snap sample collection, summary sample collection and separation of laboratory sample and sample for analysis
8.2.2.1 Instant samples must be equal in volume (mass). The sum of all instant samples by volume (mass) should be 1.5 - 2.0 times greater than the volume (mass) of the laboratory sample.
The volume (weight) of the laboratory sample and the sample for analysis of the flavoring agent is determined by the regulatory document in accordance with which the flavoring agent of a specific name is manufactured.
8.2.2.2 The number of instant samples of liquid flavor depends on the volume occupied by the flavor. One instant sample is taken along the entire height of the flavoring layer, if its volume is up to 1 dm 3 inclusive, two instant samples are taken to a depth of 1/3 and 2/3 from the top level, if the volume is more than 1 dm 3, but does not exceed 10 dm 3 , three instant samples (from the upper, middle and lower layers) in all cases when the volume of flavoring is more than 10 dm 3.
8.2.2.3 Instant samples of liquid flavoring are taken with a sampling tube with an extended lower end with a diameter of 6 to 15 mm and a length exceeding the height of the container by several centimeters.
The upper hole of the tube is closed with a thumb or a stopper, immersed to the required depth, the tube is opened for a short time to fill, then closed again and the tube with the sample is removed.
8.2.2.4 Flash samples of the flavor paste are taken with a sampling tube that is lowered vertically to the bottom of the container, then tilted and withdrawn slowly to ensure that the entire contents of the tube are preserved.
When using a probe, it is immersed (screwed in) to the entire depth of the container along the vertical axis. Then the dipstick is removed.
8.2.2.5 Instant samples of dry flavoring are taken with a probe, immersing it to the entire depth of the container along the vertical axis.
8.2.2.6 Taking instant samples of products at the stage of delivery and acceptance to the warehouse is carried out before sealing the container.
8.2.2.7 Place all instant samples in a sample vessel, mix thoroughly and obtain a total sample.
8.2.2.8 A laboratory sample of liquid and paste flavoring is obtained after thoroughly mixing the total sample and simply reducing it to the laboratory sample volume.
8.2.2.9 A laboratory sample of dry flavoring is obtained by reducing the total sample using the quartering method.
8.2.2.10 The laboratory sample for small batches of flavorings may be a total sample, and the total volume or mass of instant samples must be no less than the volume or mass required for testing.
8.3 Labeling of laboratory samples
The isolated laboratory sample of flavoring is thoroughly mixed again, divided into two equal parts and placed in clean, dry glass containers. The vessels are tightly closed with cortical or plugs made of polymeric materials and labeled with the following indication:
Flavor names;
Manufacturer's name;
Type of carrier (solvent, filler, food raw material);
Lot numbers and masses;
Dates of manufacture;
Sampling dates and locations;
Surnames and signatures of the person who took the sample;
Designations of the document in accordance with which the flavor of a specific name is manufactured.
One laboratory sample is used for analysis, the second is sealed and stored for the shelf life established by the manufacturer in case of disagreement in assessing the quality of the flavor for re-analysis.
For a small batch of liquid flavorings, it is allowed to store a laboratory sample of the flavoring used for testing.
Laboratory samples are stored in a place protected from light at a temperature not exceeding 25°C (unless otherwise specified in the regulatory document in accordance with which the flavor of a particular name is manufactured), laboratory samples of dry flavors - at a relative humidity of no more than 75%.
8.4 Determination of appearance and color of flavorings
8.4.1 The appearance and color of liquid and paste flavoring is determined by viewing a sample for analysis in an amount of 30 to 50 cm 3 in a glass B-1(2)-50(100) according to GOST 25336 against the background of a sheet of white paper in transmitted or reflected light .
8.4.2 The appearance and color of the dry flavor is determined by viewing a sample for analysis weighing from 30 to 50 g, placed on a sheet of white filter paper according to GOST 12026, in diffuse daylight or under the light of LD fluorescent lamps according to GOST 6825.
8.4.3 A flavoring agent is considered to comply with the requirements of this standard if the appearance and color of the analytical sample meet the requirements of 5.1.3.
8.5 Odor detection
The method consists of an organoleptic comparison of a sample for flavor analysis with a control sample of the flavor of the given name.
A sample of the flavor of a given name, the smell of which is approved by the manufacturer's tasting council, is taken as a control sample.
For a control sample, a laboratory sample with a volume (weight) of at least 250 cm 3 (g) of flavoring produced under production conditions is taken. The control sample is stored in a hermetically sealed container for the shelf life established by the manufacturer.
8.5.1 Determination of liquid fragrance odor
Strips of filter paper 10 x 160 mm in accordance with GOST 12026 are simultaneously moistened (approximately 3 cm) in the control sample and the sample for analysis and their smell is compared.
A flavoring agent is considered to comply with the requirements of this standard if the odor of the “wet” strips of the test sample and the control sample is the same.
8.5.2 Odor determination of dry and paste flavorings
A sample for analysis of the flavor and a control sample weighing from 30 to 50 g is placed on a sheet of white filter paper according to GOST 12026 and their smell is assessed.
A flavoring agent is considered to comply with the requirements of this standard if the odor of the test sample and the control sample is the same.
8.6 Determination of the refractive index of liquid flavors - according to GOST 14618.10 (section 4).
8.7 Determination of the density of liquid flavors - according to GOST 14618.10 (section 2 or section 3).
8.8 Determination of the volume fraction of ethyl alcohol in liquid alcohol-containing flavorings is carried out according to the method described in Appendix A.
8.9 Determination of the mass fraction of moisture in dry and paste flavors - according to GOST 14618.6 (section 3 or section 4) or according to the method outlined in Appendix B.
If disagreements arise, the method in accordance with GOST 14618.6 (section 3) is used as an arbitration method.
8.10 Determination of microbiological parameters of flavorings:
The number of mesophilic aerobic and facultative anaerobic microorganisms - according to GOST 10444.15;
The number of coliform bacteria (coliform bacteria) - according to GOST 31747;
Yeast and molds - according to GOST 10444.12;
Bacteria such as salmonella - according to GOST 31659;
The number of sulfite-reducing clostridia is according to GOST 29185.
8.11 Determination of the content of toxic elements:
Arsenic - according to GOST 26930, GOST 31266;
Lead - according to GOST 26932, GOST 30178;
Cadmium - according to GOST 26933, GOST 30178;
Mercury - according to GOST 26927 and according to the regulatory document in force in the territory of the state that has adopted the standard.
8.12 Determination of metallomagnetic impurities - according to GOST 15113.2.
8.13 Determination of benzo(a)pyrene, benzo(a)anthracene and potentially hazardous biologically active substances - according to the regulatory document in force in the territory of the state that has adopted the standard.
8.14 Determination of flash point - according to GOST 12.1.044.
8.15 Determination of the volume fraction of 1,2-propylene glycol in liquid flavorings - according to Appendix B.
9 Transportation and storage
9.1 Flavors are transported by all modes of transport in accordance with the cargo transportation rules in force for the relevant mode of transport.
9.2 Liquid and paste flavorings are stored in closed and darkened rooms at a temperature not exceeding 25°C, unless otherwise specified by the manufacturer.
Notes:
1 When storing liquid flavors, opalescence and precipitation are allowed if this is provided by the manufacturer.
2 When storing paste-like flavors, separation (separation of the liquid phase) is allowed if this is provided by the manufacturer.
3 Before use, flavors must be mixed until smooth.
9.3 Dry flavors are stored in dry, well-ventilated areas at a temperature not exceeding 25°C and relative humidity not exceeding 75%, unless otherwise specified by the manufacturer.
Note - When storing dry flavors, the presence of loosely packed lumps (easily crumbling) is allowed.
9.4 Transportation and storage of fragrances together with chemicals and strong-smelling products and materials is not allowed.
9.5 The shelf life of flavorings is set by the manufacturer.
10 Directions for use
The scope of application and maximum dosages of flavorings must comply with the requirements established or regulatory legal acts in force in the territory of the state that has adopted the standard and are established by the manufacturer.
