GB/T 19464: Evolution and historical versions
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Alkyl polyglucoside
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Alkylpolyglycosides
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Basic data | Standard ID | GB/T 19464-2014 (GB/T19464-2014) | | Description (Translated English) | Alkyl polyglucoside | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | G73 | | Classification of International Standard | 71.100.40 | | Word Count Estimation | 18,144 | | Date of Issue | 12/12/2014 | | Date of Implementation | 6/1/2015 | | Older Standard (superseded by this standard) | GB/T 19464-2004 | | Quoted Standard | GB/T 6682; GB/T 3143; GB/T 8170; GB/T 9722; GB/T 15357 | | Regulation (derived from) | National Standards Bulletin 2014 No. 30 | | Issuing agency(ies) | General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China | | Summary | This standard specifies the APG product (referred to APG) classification, technical requirements, test methods, inspection rules and signs, packaging, transportation, storage and shelf life. This standard applies to direct and exchange glycoside APG produ | GB/T 19464-2014: Alkyl polyglucoside---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Alkylpolyglycosides [Quasi-Official/Academic version - translated by Chinese Institute]
ICS 71.100.40
G73
National Standards of People's Republic of China
Replace GB/T 19464-2004
Alkyl glycoside
Released on.2014-12-22
2015-06-01 implementation
General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China
China National Standardization Administration issued
Foreword
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
This standard replaces GB/T 19464-2004 "alkyl glycoside".
The main changes of this standard compared with GB/T 19464-2004 are as follows.
--- Increased classification requirements for alkyl glycoside products (see Chapter 3);
--- Increased the technical indicators of alkyl glycosides for cosmetics, and specified the corresponding analytical methods (see 4.2);
--- Revised the sulphated ash indicator (see 4.1,.2004 edition 4.3);
--- Revised the viscosity index and the measured temperature of the C12-14 alkyl glycoside viscosity (see 4.1,.2004 edition 4.3);
--- Modified the detection method of alkyl glycoside polymerization degree and residual total fatty alcohol content (see 5.6 and 5.8,.2004 editions 5.7 and 5.9);
--- Modified the detection method of the alkyl glycoside pH value, extending the pH range of the product (see 5.4,.2004 version 5.5).
This standard was proposed by the China National Light Industry Council.
This standard is under the jurisdiction of the National Standardization Committee for Surfactants and Detergents (SAC/TC272).
This standard was drafted. Shanghai Fakai Chemical Co., Ltd., Nanjing Jinling Petrochemical Research Institute Co., Ltd., Shenzhen Changyuan Jiacaihuan
Material Co., Ltd., Infinitus (China) Co., Ltd., Zhejiang Zanyu Technology Co., Ltd., Yangzhou Chenhua Technology Group Co., Ltd., Table
Surfactant and Detergent Industry Productivity Promotion Center.
The main drafters of this standard. Feng Yu, Wang Fengshou, Zhou Yucheng, He Jianghuai, Dong Wantian, Deng Wei, Huang Yaru, Yu Zizhou, Huo Shuwen, Li Yong,
Hao Qiaolin.
The previous versions of the standards replaced by this standard are.
---GB/T 19464-2004.
Alkyl glycoside
1 Scope
This standard specifies the classification, technical requirements, test methods, inspection rules and signs, packaging, and transportation of alkyl glycoside products (referred to as APG).
Loss, storage, shelf life.
This standard is applicable to the industrial products of alkyl glycoside produced by direct method and glycosidic exchange method, and can be applied to washing, daily chemical, agricultural milk, textile, etc.
Multi-field, play the role of washing, emulsifying, penetrating, foaming and so on.
This standard does not apply to any compounded product or C16~18 based alkyl glycoside product used as emulsifier.
2 Normative references
The following documents are indispensable for the application of this document. For dated references, only dated versions apply to this article.
Pieces. For undated references, the latest edition (including all amendments) applies to this document.
GB/T 6682 Analytical laboratory water specifications and test methods
GB/T 3143 Liquid chemical product color determination method (Hazen unit - platinum-cobalt color number)
GB/T 8170 Data Rounding Rules and Representation and Determination of Limit Values
GB/T 9722 chemical reagent gas chromatography general rule
GB/T 15357 surfactant and detergent rotary viscometer for measuring the viscosity of liquid products
Cosmetics Hygiene Regulations Wei Weifa [2007] No. 1
3 Product name, classification and structural formula
Alkyl glycosides can be divided into two types according to the production process, namely direct process products and exchange process products. Direct method product means life
An alkyl glycoside prepared by the glycosidation reaction of a target high-carbon fatty alcohol and a saccharide raw material without producing a low-carbon glycoside during production.
The product does not contain a lower alkyl glycoside. The exchange method product means that a low-carbon fatty alcohol (such as butanol) reacts with a raw material of a saccharide compound to form a low-carbon sugar.
The glycoside, which is then produced, is exchanged with the target high-carbon fatty alcohol to form the target alkyl glycoside. These two steps can be followed by
It can also be carried out simultaneously, and the product contains a part of low-carbon alkyl glycosides.
The structural formula of the alkyl glycoside molecule is as follows (R is C8~18, n=1~10. In the exchange method product, R is C2 or C3 or C4, etc.
Lower alkyl glycoside; direct process products do not contain lower alkyl glycosides).
4 Technical requirements
4.1 Physical and chemical indicators of alkyl glycosides
The physicochemical indicators of alkyl glycosides should meet the requirements of Table 1.
Table 1 Index requirements for alkyl glycosides
project
Direct method product indirect method product
First-class product, second-class product, qualified product, first-class product, second-class product, qualified product
Exterior
Colorless liquid or
Paste, no different
Constant smell
Colorless or light yellow
Liquid or paste,
No abnormal smell
Colorless liquid or
Paste, no different
Constant smell
Yellow liquid or
Paste, no different
Constant smell
Color (aqueous solution of isopropanol)/Hazen ≤ 50 100 - 50 150 -
Solid content /% ≥ 50 50
pH ≥ 7.0 7.0
Sulfated ash (calculated according to solid content 50%) /% ≤ 3.0 3.0
Free total fatty alcohol /% ≤ 1.0 1.0
Lower alkyl glycoside a (calculated as solids) /% ≤ excluding 5.0 10.0 10.0
Average degree of polymerization (calculated from composition) 1.2~1.8 1.2~1.8
Viscosity/(mPa·s)
C8~10(20°C) ≥.200 100
C12~14(40°C) ≥ 1500 800
C8~14(20°C) ≥ 1000 1000
a Only applicable to products produced by the exchange process, such as the content of butyl glycosides, ethyl glycosides, propyl glycosides or a combination of several.
4.2 Alkyl Glycosides for Cosmetics
Alkyl glycosides for cosmetics should meet the requirements of the "Hygienic Specifications for Cosmetics" to ensure that the products are normal and reasonable and predictable.
Under the conditions of use, there is no safety hazard to human health.
The alkyl glycoside for cosmetics should meet the requirements of Table 2 on the basis of meeting the requirements of Table 1.
Table 2 Additional indicator requirements for alkyl glycosides for cosmetics
project
index
C8~10 alkyl glycoside C8~14 alkyl glycoside C12~14 alkyl glycoside
pH 11.5~12.5
Free total fatty alcohol /% ≤ 0.5 0.6 0.8
Total number of colonies/(CFU/g) ≤ 1000
Lead (Pb)/(mg/kg) ≤ 40
Arsenic (As)/(mg/kg) ≤ 10
Mercury (Hg)/(mg/kg) ≤ 1
5 Test methods
Unless otherwise stated, only analytically pure reagents and tertiary water specified in GB/T 6682 were used in the analysis.
5.1 Appearance, smell
Sensory measures the appearance and odor of the sample.
5.2 Color
5.2.1 Principle
The alkyl glycoside sample is formulated into a solution using a mixed solvent of isopropyl alcohol and water, and the solution is in a transparent state at a pH of 7, and
The standard platinum-cobalt color code is used for visual colorimetry, and the Hazen value of the standard platinum-cobalt color code closest to the product color is the color of the product.
5.2.2 Instruments
General laboratory equipment and the following instruments.
5.2.2.1 Spectrophotometer, wavelength range 380nm~800nm;
5.2.2.2 Nessler colorimetric tube, 50mL.
5.2.3 Reagents
5.2.3.1 40% aqueous solution of isopropanol (volume fraction), measure 40 mL of isopropanol, dilute to 100 mL with water, and shake well.
5.2.3.2 1mol/L nitric acid solution, measure 65mL of nitric acid, dilute to 1000mL with water, and mix.
5.2.4 Preparation of standard colorimetric liquid
According to the provisions of GB/T 3143, a series of platinum-cobalt standard colorimetric liquids with different Hazen values are prepared for determining the color of the sample.
5.2.5 Preparation of test solution
Weigh 30g of sample (weighed to 0.1g), add 45mL of 40% isopropanol aqueous solution (5.2.3.1) into the measuring cylinder, stir to dissolve, and prepare
Solution. Insert the pH electrode into the test solution, add 1mol/L nitric acid solution (5.2.3.2) dropwise, and adjust the pH value to 6.8~.
7.0. Take 50 mL of the test solution in a colorimetric tube, observe it vertically downward from the top of the cuvette, compare it with an equal volume of standard colorimetric solution, and test
The Hazen value of the standard colorimetric liquid closest to the color of the test is the color of the sample.
5.3 Solid content
5.3.1 Principle
After the sample was dried at 105 ° C ± 2 ° C for 4 h, the mass fraction of the residue was the solid content.
5.3.2 Instruments
General laboratory equipment and the following instruments.
5.3.2.1 Weighing bottle, φ50mm×30mm, with cover;
5.3.2.2 oven, the temperature can be controlled within the range of 105 ° C ± 2 ° C;
5.3.2.3 Glass dryer, φ240mm, with color-changing silica gel.
5.3.3 Test procedure
Weigh about 1g of the mixed test sample (weighed to 0.001g) in the constant weighing bottle (5.3.2.1), and add the paste sample first.
After the heat is dissolved, mix again, mix and sample and weigh. The weighing bottle containing the test portion is placed in an oven (5.3.2.2) at 105 ° C ± 2 ° C to dry.
4h, taken out, placed in a desiccator (5.3.2.3) for 30min, covered and weighed (weighed to 0.001g).
5.3.4 Calculation of results
The solid content is expressed in mass fraction w(S) and is calculated according to formula (1).
w(S)=
M1
M0×
100% (1)
In the formula.
M1---the mass of residual solids in grams (g);
M0---The mass of the test part in grams (g).
The arithmetic mean of the results of two parallel determinations is expressed to the nearest decimal point as the measurement result.
Precision. The absolute difference between two independent test results obtained under repeated conditions is not greater than the arithmetic mean of the two measured values.
1%, premise that it is greater than 1% and not more than 5%.
5.4 pH
5.4.1 Principle
A solution containing 20% of a sample (mass fraction) was prepared by using a mixed solution of isopropyl alcohol and water as a solvent, and the pH was measured at 25 °C.
5.4.2 Reagents and instruments
5.4.2.1 isopropanol;
5.4.2.2 pH meter, the minimum scale meets the precision requirements;
5.4.2.3 pH composite electrode, or glass electrode and calomel/potassium chloride type reference electrode;
5.4.2.4 beaker, 150mL;
5.4.2.5 volumetric flask, 100mL;
5.4.2.6 thermometer, 0 ° C ~ 100 ° C;
5.4.2.7 Thermostat.
5.4.3 Experimental steps
5.4.3.1 Test conditions
During the test, the temperature of the tested solution, standard buffer solution and washing water should be adjusted at 25 °C ± 1 °C, and according to the instrument.
Calibrate the pH meter.
5.4.3.2 Determination
First weigh 20.0g sample, accurate to 0.1g, then add 68.0g of carbon dioxide-free distilled water to dissolve, and finally add 12.0g
Isopropanol completely dissolves it. Adjust the temperature of the solution to 25 °C ± 1 °C, insert the electrode, and record after the potentiometer reading is stable for 1 min.
reading.
The same sample was measured in parallel twice and trimmed to 0.1 pH, expressed in pH units. Expressed as the arithmetic mean of the results of two parallel measurements
One point after the decimal point is the measurement result.
Precision. The absolute difference between two independent test results obtained under repeated conditions is no more than 0.1pH unit, greater than 0.1pH single
The condition of the bit is not more than 5%.
5.5 Sulfated ash
5.5.1 Principle
After the carbonized test portion, the residue was burned at 850 ° C in the presence of sulfuric acid, and the thus obtained sulfated ash was weighed.
5.5.2 Instruments
General laboratory equipment and the following instruments.
5.5.2.1 坩埚, volume of 50mL ~ 100mL porcelain enamel;
5.5.2.2 high temperature furnace, the temperature can be controlled within the range of 850 °C ± 25 °C;
5.5.2.3 Dryer with color-changing silica gel inside;
5.5.2.4 坩埚 tongs;
5.5.2.5 Temperature control electric furnace, 1kW~2kW.
5.5.3 Reagents
sulfuric acid.
5.5.4 Test procedure
5.5.4.1 Test share
Heat the crucible (5.5.2.1) in a high temperature furnace (5.5.2.2) at 850 °C ± 25 °C for 30 min, take it out, and cool it in air for 1 min~
2 min, transfer to a desiccator (5.5.2.3) for 45 min, weigh (weighed to 0.001 g), repeat the above test to constant weight. Constantly heavy
A sample of 10 g (weighed to 0.001 g) was weighed into the crucible.
5.5.4.2 Carbonization
Put the weighed test part on the temperature control electric furnace (5.5.2.5) and slowly heat it. The water in the test part gradually evaporates to form foam and adjust the electric furnace.
The temperature does not allow the foam to overflow. If the test part has more foam during the heating process, the method of fractional loading can be adopted until the test of the specified weight
All the shares are added. After a large amount of foam disappears, the temperature of the electric furnace is increased to sufficiently carbonize the test portion. There is basically no smoke in the cockroach
At the time, it was cooled, 2.0 mL of sulfuric acid (5.5.3) was added dropwise, the carbonized material was wetted, and heating was continued on the electric furnace until no white smoke appeared.
5.5.4.3 Burning
The test portion that has driven the sulfuric acid is transferred to a high temperature furnace at 850 ° C ± 25 ° C, burned for 4 h, taken out, and cooled in air for 1 min~
After 2 min, transfer to a desiccator for 45 min, weigh (weighed to 0.001 g), repeat the above operation until the difference between the two weighs is not greater than
2mg.
5.5.5 Calculation of results
The residual sulphated ash content after burning is expressed in mass fraction w(C) and is calculated according to formula (2).
w(C)=
M1
M0×
100% (2)
In the formula.
M1---the mass of the residue in the crucible, in grams (g);
M0---the mass of the test part calculated by the solid content of 50%, in grams (g).
Note. For samples with a solid content of not 50%, the mass m0 of the test part should be corrected to the value at 50% solid content, ie.
M0 = [m (weighing value) × S (%) solid content]/50%.
The arithmetic mean of the results of two parallel determinations is expressed to the nearest decimal point as the measurement result.
Precision. The absolute difference between two independent test results obtained under repeated conditions is not greater than the arithmetic mean of the two measured values.
10%, based on the fact that more than 10% of the situation does not exceed 5%.
5.6 free total fatty alcohol
Determine according to Appendix A.
5.7 lower alkyl glycoside
Determine according to Appendix B.
5.8 alkyl glycoside average degree of polymerization
Determine according to Appendix B.
5.9 viscosity
According to GB/T 15357 regulations.
5.10 total number of colonies
According to the "Hygienic Specifications for Cosmetics".
5.11 Lead
According to the "Hygienic Specifications for Cosmetics".
5.12 Arsenic
According to the "Hygienic Specifications for Cosmetics".
5.13 Mercury
According to the "Hygienic Specifications for Cosmetics".
6 Inspection rules
6.1 Inspection classification
6.1.1 Factory inspection
The factory inspection items are the appearance, odor, color, solid content, pH value, free total fatty alcohol specified in Chapter 4.
6.1.2 Type inspection
Type inspection includes all technical requirements specified in Chapter 4, and type inspection should also be carried out if.
a) Normal production should be carried out every three months;
b) Changes or abnormalities in production processes, production equipment, raw materials, catalysts, etc., and changes in production management factors (including personnel quality)
When it may affect product quality and performance;
c) when production resumes after a long-term shutdown;
d) When the factory inspection result is significantly different from the previous type inspection;
e) When the quality supervision organization or the user submits the type inspection requirements.
6.2 Group Approval and Sampling Principles
6.2.1 Alkyl glycoside products are delivered in batches and sampled, and the same type, specification, and batch number of products delivered at one time are delivered in batches.
6.2.2 The product shall be inspected by the quality inspection department of the manufacturer in accordance with the inspection methods specified in this standard, and the product quality inspection shall be issued.
The certificate can be shipped from the factory. The receiving unit shall, within one month of arrival, accept and accept the certificate, and if necessary, sample and accept according to 6.2.3.
6.2.3 Sampling
According to the batch size, determine the sample size according to Table 3, and randomly sample units are taken from the batch.
Since long carbon chain alkyl glycoside products are prone to crystal precipitation when stored in an environment below 35 ° C, they should be selected before sampling.
The sample in the sample bucket is evenly mixed and can be sampled under the premise of ensuring uniform mixing.
Table 3 Batch and sample size units are buckets
Batch 2~15 16~50 51~150 151~500 >500
Sample size 2 3 5 8 13
When sampling, use a dry clean sampling tube or other sampling vessel with a diameter of about 15 mm and insert it into the 2/3 depth of each sample bucket.
For samples, the total amount of samples should not be less than 1.0kg. The sample taken was divided into 2 parts, one for testing and one for storage.
6.3 Judgment rules and retests
The test result data should be revised according to the provisions of GB/T 8170 to the number of valid digits of the technical requirements, and then the technical requirements
The limit value specified in the determination of the inspection batch product is qualified or unqualified.
If one of the test results does not meet the standard, the sample should be resampled from the double sample and the unqualified item should be re-examined. complex
If the inspection result meets the requirements of this standard, the batch of products shall be judged as qualified; if it is still unqualified, the batch of products shall be judged as unqualified.
6.4 Arbitration
If the receiving unit finds that the product quality does not meet the requirements stipulated in this standard, it shall negotiate with the producer within one month of arrival. If due to inspection
The results are different. When the agreement cannot be obtained, both parties should sample according to 6.2.3. The total amount of sampling should not be less than 1.5kg, carefully mix the selected samples.
After that, put them into 3 clean and dry sample bottles and seal them. The product name, specification, batch number, producer name, sampling date should be indicated on the label.
Period, sampler. The parties to the settlement shall each hold one copy, and after the third is signed, the arbitration shall be used for arbitration. Samples are stored in the dark and have a shelf life of 1 month. arbitration
The test results are the final basis.
7 Marking, packaging, transportation, storage and shelf life
7.1 mark
The outer wall mark (pattern and text) of the drum should be clearly defined and marked.
a) product name, trademark, specification grade, and implementation standard number;
b) batch number, date of manufacture, shelf life (or expiration date);
c) producer name, address, zip code and contact number;
d) net content, gross weight;
e) Warning signs (waterproof, moisture-proof, careless, etc.).
7.2 Packaging
Alkyl glycosides are packaged in clean, non-corrosive, strength-stable plastic containers or metal-lined plastic containers. When the product is loaded into the container
Leave a proper amount of space and seal it well after filling to prevent water ingress. The net content of the package should be in accordance with the nominal quality.
7.3 Transportation
Sealed upward during shipment to prevent sun and rain.
7.4 Storage
The alkyl glycoside product is an aqueous solution and should be stored in a well-ventilated warehouse with an ambient temperature not lower than 0 ° C and not higher than 45 ° C to avoid rain.
And exposure.
7.5 Shelf life
Under the specified transportation and packaging and storage conditions, the product has a shelf life of not less than 12 months from the date of production. If the product is added with anti-corrosion
The agent should indicate the type and amount of preservative added.
Appendix A
(normative appendix)
Determination of free total fatty alcohol content---gas chromatography
A.1 Principle
The residual fatty alcohol component in the alkyl glycoside is separated and quantified by a combination of extraction and gas chromatography.
A.2 reagent
Unless otherwise stated, only analytically pure reagents and tertiary water specified in GB/T 6682 were used in the analysis.
A.2.1 chromatographic standards for fatty alcohols. C8OH, C10OH, C11OH, C12OH, C14OH, C16OH, C18OH, etc., all of which are chromatographically pure;
A.2.2 dichloromethane;
A.2.3 anhydrous ethanol;
A.2.4 diatomaceous earth, chemically pure, dried at 105 ° C ± 2 ° C for 2 h before use;
A.2.5 petroleum ether, boiling range 30 ° C ~ 60 ° C;
A.2.6 A petroleum ether solution containing methylene chloride. Add 7 mL of dichlorochloric acid to 100 mL of petroleum ether (A.2.5) with a boiling range of 30 ° C to 60 ° C.
Methane (A.2.2), mix;
A.2.7 carrier gas. nitrogen, purity 99.99%;
A.2.8 Auxiliary gas. hydrogen, purity 99.99%; air, supplied by cylinder or oil-free gas compressor.
A.3 Instruments
Common laboratory instruments and the following instruments.
A.3.1 Gas chromatograph, gas chromatograph with flame ionization detector and temperature programmed controller with data processing system. color
Column. packed column, stainless steel or glass tube, length 2.0m, inner diameter 2mm~4mm, carrier ChromsorbWHP, particle size is about
0.120mm~0.180mm, coated with 2% OV-101 fixative, aged for 5h~10h before use; or other separation effect is equivalent
Fill the column or capillary column.
A.3.2 Microinjector, 5μL or 10μL.
A.3.3 Volumetric flask, 5mL.
A.3.4 Pipette, 1 mL.
A.3.5 Glass chromatography column, φ18mm, column length 400mm, the right end is filled with appropriate amount of glass wool.
A.3.6 Constant temperature water bath.
A.4 Gas chromatographic conditions
The following are the suitable conditions for the packed column recommended by A.3.1. The suitable conditions for other columns are basically similar, depending on the specific
The situation is modified as appropriate.
A.4.1 carrier gas (N2) flow rate. 30mL/min;
A.4.2 hydrogen flow rate. 45mL/min;
A.4.3 Air flow rate. 450mL/min;
A.4.4 Injection port temperature. 300 ° C;
A.4.5 detector temperature. 300 ° C;
A.4.6 Column oven temperature. initial temperature 100 ° C, residence time 1 min, heating rate 5 ° C/min, final temperature 250 ° C, residence time
2min.
A.5 Relative weight correction factor determination
Accurately weigh the inner standard of n-undecyl alcohol (A.2.1) and other fatty alcohol standards (A.2.1) about 0.2g each (weighed to 0.0002g),
5 mL of dichloromethane (A.2.2) was dissolved, and an appropriate amount of the solution was taken and analyzed by injection.
The correction factor of the aliphatic alcohol with a carbon chain length of i to the internal standard n-undecyl alcohol is calculated according to formula (A.1).
Fs,i=
As×mi
Ai×ms
(A.1)
In the formula.
As---the peak area of the internal standard;
Ms---the quality of the internal standard, in grams (g);
The peak area of the Ai ---i component;
The mass of the mi---i component in grams (g).
The correction factors for other fatty alcohols for n-undecyl alcohol are the same as above.
A.6 Sample preparation and chromatographic determination
Accurately weigh the internal standard n-decyl alcohol 0.1g (weighed to 0.0002g), dissolve it with a small amount of absolute ethanol (A.2.3), transfer to 5mL capacity
In a measuring flask, rinse with absolute ethanol and dilute to the mark. This solution is an internal standard solution.
Weigh the mixed alkyl glycoside as it is, about 2g (weighed to 0.001g) in a 50mL beaker, and add 0.50mL of the internal standard solution.
And 0.50 mL of absolute ethanol. After the sample is dissolved, add 5 g of dried diatomaceous earth (A.2.4) to the beaker and stir well to make it semi-dry evenly.
The solid was placed in a gl...
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