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GB 12488-2008: Food additive -- Sodium cyclamate
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PDF similar to GB 12488-2008
Basic data | Standard ID | GB 12488-2008 (GB12488-2008) | | Description (Translated English) | Food additive -- Sodium cyclamate | | Sector / Industry | National Standard | | Classification of Chinese Standard | X42 | | Classification of International Standard | 67.220.20 | | Word Count Estimation | 10,158 | | Date of Issue | 2008-06-25 | | Date of Implementation | 2009-01-01 | | Older Standard (superseded by this standard) | GB 12488-1995 | | Quoted Standard | GB/T 601-2002; GB/T 602-2002; GB/T 603-2002; GB/T 5009.76-2003; GB/T 6678-2003; GB/T 6682-2008; GB/T 9724-2007 | | Adopted Standard | CODEX JECFA-2004, NEQ | | Regulation (derived from) | Announcement of Newly Approved National Standards No. 12 of 2008 (No. 125 overall) | | 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 Chinese standard specifies the food additive sodium cyclamate requirements, test methods, inspection rules and signs, packaging, transportation, storage and so on. This standard applies to cyclohexylamine as raw material, chlorosulfonic acid or amino acid synthesis cyclohexyl sulfamic acid and sodium hydroxide role in the system of sodium cyclamate. The product is used as a food sweetener. | GB 12488-2008: Food additive -- Sodium cyclamate---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.
Food additive.Sodium cyclamate
ICS 67.220.20
X42
National Standards of People's Republic of China
Replacing GB 12488-1995
Food Additives
Cyclohexylamino sodium (sodium cyclamate)
Posted 2008-06-25
2009-01-01 implementation
Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
Standardization Administration of China released
Foreword
Chapters 6 and 9.1 of this standard are mandatory, the rest are recommended.
63rd (2004) This standard is consistent with the Codex Alimentarius Commission (CODEX) "cyclamic sodium" (in English) -JECFA
The degree of non-equivalent.
This standard replaces GB 12488-1995 "Food Additives cyclamic sodium (sodium cyclamate)."
The main changes compared to the Standard and GB 12488-1995 are as follows.
--- Crystalline product relative molecular mass is amended as 237.25 from the 237.24 (1995 edition Chapter 1, Chapter 3 of this edition).
--- Addition of the amino acid project and absorbance (270nm) project indicators and test methods (see Chapter 6, 7.14 and 7.15).
--- Cyclohexylamino ≥98.0% sodium by the index revised to 98.0% 101.0%; Heating loss indicators. A type made ≤1.0%
Revised to ≤0.5%; B type by the ≤15.5% revised to 16.5%; the index sulfate ≤0.05% to 0.10% (1995
4.2 Chapter Excerpts Version 6).
--- Test Method cyclohexylamino sodium content of benzene with 1-naphthol in place of crystal violet indicator Indicator (1995 version 5.2,
Excerpts of 7.4).
--- Test Method for loss on drying was revised (1995 version 5.3, this version 7.5).
Standard Test Method for Sampling amount --- sulfate content of from 1g to 10g (1995 edition 5.5, this version 7.7).
Test Method --- heavy metal content, with the thioacetamide reagent instead of hydrogen sulphide saturated aqueous solution (1995 version 5.7, this version 7.9).
Test Method --- transparency, increased from 2.50g sample to 10g (1995 edition 5.8, this version 7.10).
--- Product warranty from two years to three years to modify the (1995 version 7.5, this version 9.4).
The standard proposed by China Petroleum and Chemical Industry Association.
This standard by the National Standardization Technical Committee branch of organic chemistry (SAC/TC63/SC2) and the National Food Additives Standardization
Committee (SAC/TC11) centralized.
This standard was drafted. Fangda additives (Yangquan) Co., Ltd.
Participated in the drafting of this standard. Jintian Enterprises (Nanjing) Co., Ltd.
The main drafters of this standard. Wenhui Ping, Huang Xiaoguang, Wang Wenping.
This standard was first released in August 1995.
Food Additives
Cyclohexylamino sodium (sodium cyclamate)
1 Scope
This standard specifies the food additive cyclohexylamino sodium (sodium cyclamate) requirements, test methods, inspection rules and signs, packaging, transportation
Transport, storage and so on.
This standard applies to cyclohexylamine as the raw material, chlorine acid or amino acid synthesis cyclamic acid and sodium hydroxide role in the system after
Cyclohexylamino obtained sodium (sodium cyclamate). The product as food sweeteners.
2 Normative references
The following documents contain provisions which, through reference in this standard and become the standard terms. For dated references, subsequent
Amendments (not including errata content) or revisions do not apply to this standard, however, encourage the parties to the agreement are based on research
Whether the latest versions of these documents. For undated reference documents, the latest versions apply to this standard.
Preparation of GB/T 601-2002 Chemical Reagent standard titration solution
GB/T 602-2002 Chemical Reagent preparation impurity standard solution measurement (ISO 6353-1. 1982, NEQ)
GB/T 603-2002 Chemical Reagent Test Methods Preparations with (ISO 6353-1. 1982, NEQ)
Determination of GB/T 5009.76-2003 arsenic in food additives
GB/T 6678-2003 General Principles for Sampling Chemical Products
GB/T 6682-2008 standard water analysis laboratories and test methods (ISO 3696. 1987, MOD)
GB/T 9724-2007 Chemical Reagent pH value measurement General (ISO 6353-1. 1982, NEQ)
3 formula, relative molecular mass and structural formula
Molecular formula. C6H12NNaO3S · like H2O (crystalline products like = 2, dry goods like = 0)
Structural formula
NHSO3 Na
Molecular Weight. 237.25 crystalline product,
Dry goods 201.22 (according to 2007 international relative atomic mass)
4 Classification and designation
Food additives Sodium cyclohexylamino divided into A and B-type (having two crystal water), are known cyclohexylamino Sodium Type A
Sodium and cyclohexylamino B type.
5 Traits
A type is a white crystalline powder, needle-like crystals; B-type white needle, flaky crystal; odorless, has a sweet taste.
6 Requirements
Food Additives cyclohexylamino sodium shall comply with the technical requirements in Table 1 below.
Table 1 Technical Requirements
project
index
A B
Cyclohexylamino sodium (dry basis), /% ≥ 98.0 ~ 101.0
Loss on drying, /% ≤ 0.5 16.5
pH value (100g/L aqueous solution) 5.5-7.5
Sulfate (SO4 dollars), /% ≤ 0.10
Arsenic (As), /% ≤ 0.0001
Heavy metals (Pb), /% ≤ 0.001
Transparency (expressed as transmittance 100g/L solution) /% ≥ 95
Cyclohexylamine, /% ≤ 0.0025
Dicyclohexylamine passing the test
Sulfamic acid, /% ≤ 0.15
Absorbance (100g/L solution) ≤ 0.10
7 Test methods
7.1 Warning
Some test procedures prescribed test method can lead to dangerous situations, the operator shall take the appropriate safety and health practices.
7.2 General Provisions
Unless otherwise indicated in the analysis using only recognized as analytical reagents and GB/T 6682-2008 the provisions of tertiary water.
Used in the analysis standard titration solution, impurity standard solution, preparations and products, did not indicate when the other requirements, according to GB/T 601-
2002, GB/T 602-2002, regulations preparation GB/T 603-2002 in.
7.3 Identification Test
7.3.1 Reagents
7.3.1.1 ether;
7.3.1.2 nitric acid;
7.3.1.3 silver nitrate solution. 17g/L;
7.3.1.4 sodium nitrite solution. 100g/L;
7.3.1.5 hydrochloric acid solution. 3 → 10;
7.3.1.6 nitric acid solution. 3 → 50;
7.3.1.7 barium chloride solution. 50g/L;
7.3.1.8 sodium hydroxide solution. 50g/L.
7.3.2 Analysis of step
7.3.2.1 take platinum wire dipped little of this product, a colorless combustion flame, the flame that was yellow.
3g laboratory samples 7.3.2.2 Weigh, to the nearest 0.1g, was dissolved in 20mL water, remove 1mL, silver nitrate solution was added 2mL, 30s
After generating cyclohexylamino white precipitate of silver nitrate.
7.3.2.3 Weigh 0.3g laboratory samples, accurate to 0.1g, dissolved in 20mL water, hydrochloric acid and sodium nitrite solution 5mL solution
Solution 3mL, heated on a water bath for about 15min, removed after cooling, extracted with ether 20mL shaken (aqueous layer after extraction test done 7.3.2.4),
The ether layer was placed in an evaporating dish, evaporated on a water bath to remove the ether, add water 1mL, plus 0.5mL nitric acid on a water bath heated 20min
After the sand bath evaporated to dryness without charring. After cooling water was added 3mL residue was dissolved in a nitric acid solution and a sodium hydroxide solution adjusted to pH
4.5 to 7.0, was added silver nitrate 1mL, a white precipitate. Nitric acid was added, a white precipitate was dissolved.
7.3.2.4 7.3.2.3 draw water layer was extracted, the barium chloride solution was added 1mL, a white precipitate formed.
7.4 Determination cyclohexylamino sodium content
7.4.1 Method summary
After drying the sample in glacial acetic acid as the solvent, 1-naphthol in the presence of benzene indicator solution, titration with perchloric acid standard solution titration, according to consumption
The volume of perchloric acid standard titration solution content was calculated cyclohexylamino sodium.
7.4.2 Reagents
7.4.2.1 glacial acetic acid;
7.4.2.2 perchloric acid standard titration solution. Ba (HClO4) = 0.1mol/L;
7.4.2.3 1- naphthol benzene indicator solution. 2g/L. 1-naphthol benzene weighed 0.2g, dissolved in glacial acetic acid, diluted to 100mL with glacial acetic acid.
7.4.3 Analysis of step
7.4.3.1 7.5.2 says learn 0.3g sample after drying, accurate to 0.0002g, ice acetic acid 30mL, heated to dissolve, cooled
To room temperature, 1-naphthol benzene indicator solution (5-6) drops of perchloric acid titration standard solution titration solution from yellow to green as the end point.
7.4.3.2 measured at the same time, according to the same procedure and the determination of the sample without using the same amount of reagent blank test solution.
7.4.4 Calculation Results
Cyclohexylamino sodium (dry basis) content of the mass fraction of 1% to the value expressed by the formula (1).
1 =
(Vp Vp 1- 2) Ba M
100 (1)
Where.
Vp 1 --- sample consumption of perchloric acid titration standard solution (7.4.2.2) the value of the volume, in milliliters (mL);
Vp 2 --- blank titration consumption of perchloric acid standard solution (7.4.2.2) the value of the volume, in milliliters (mL);
Ba --- perchloric acid standard titration solution concentration accurate value of units of moles per liter (mol/L);
Numerical molar mass of the M --- cyclohexylamino sulfonate, units of grams per mole (g/mol) (M = 201.22).
Calculation result to two decimal places.
Take two parallel determination results of the arithmetic average of the measurement results, the results of two parallel determination of the absolute difference is not more than 0.3%.
7.5 Determination of loss on drying
7.5.1 Method summary
Excretion was measured at a certain temperature in the sample can be volatile substance.
7.5.2 Analysis of step
Weigh about 10g laboratory samples, accurate to 0.0001g, placed in advance (105 ± 2) ℃ dried to constant mass weighing bottle,
Paved 5mm or less layers. 2h ~ 4h dried in oven temperature (105 ± 2) ℃ and placed on the dryer to cool 30min weighing, straight
To constant weight.
7.5.3 Calculation Results
Loss on drying mass fraction of 2% to the value expressed by the formula (2).
(2)
Where.
Take two parallel determination results of the arithmetic average of the measurement results, the results of two parallel determination of the absolute difference is not more than 0.05%.
Conducted in accordance with GB/T 9724-2007 of. Measured, weighed 10.0g laboratory samples, accurate to 0.01g, plus non-dioxide
Mixed with water to 100mL of carbon uniformly measured.
7.7 Determination of sulphate content
7.7.1 Reagents
7.7.1.1 hydrochloric acid solution. 3 → 10;
7.7.1.2 barium chloride solution. 250g/L;
7.7.1.3 sulphate (SO4) standard solution. 0.1mg/mL.
7.7.2 Analysis of step
Weigh 10.0g laboratory samples, accurate to 0.01g, dissolved in about 60mL of water, placed in 100mL flask (if necessary through
Filter), diluted with water to the mark. Pipette (5 ± 0.05) mL of the solution, placed in 50mL colorimetric tube, add 1mL hydrochloric acid solution
Solution under shaking dropping 3mL barium chloride solution, dilute with water to 50mL, shake, place 10min, the turbidity was not greater than the standard.
Take 5mL sulfate standard solution and standard samples simultaneously the same treatment.
7.8 Determination of Arsenic (A Ju) content of
Weigh about 1.0g laboratory samples, accurate to 0.01g. Limited amount of 1.00mL arsenic standard solution (arsenic 0.001mg). Other Press
GB/T second law provisions Gutzeit method performed in 5009.76-2003.
7.9 Determination of Heavy Metal Content
7.9.1 Method summary
Under weakly acidic conditions, the samples of heavy metals (Pb) with thioacetamide and generated brown-black, lead to the same treatment of (Pb)
Comparison of standard solution, to do limited testing.
7.9.2 Reagents
7.9.2.1 thioacetamide solution. Weigh thioacetamide 4g, accurate to 0.1g, dissolved in 100mL of water, placed in refrigerator.
Immediately prior to taking this solution 1.0mL added to the mixture in advance by the sodium hydroxide solution (1 + 25) 15mL, water 5mL and 20mL glycerol composition
5mL, placed on a water bath and heated for 20 seconds and cooled immediately.
7.9.2.2 carbon dioxide-free water.
7.9.2.3 ammonium acetate buffer, pH = 3.5. weigh 25.0 g of ammonium acetate, 25mL dissolved in water, add 45mL6mol/L salt
Acid, dilute hydrochloric acid or dilute ammonia to adjust pH = 3.5, dilute with water to 100mL.
7.9.2.4 Lead (Pb) standard solution. 1μg/mL. This solution was prepared just before use.
7.9.3 Analysis of step
Weigh 10.0g laboratory samples, accurate to 0.01g, was dissolved in about 60mL carbon dioxide-free water, placed in 100mL flask,
Diluted with carbon dioxide-free water to the mark, shake, is the sample solution. Draw the sample solution 12mL, 25mL stoppered placed colorimetric tube,
A tube is. Draw 10mL 2mL lead standard solution and the sample solution was placed in 25mL colorimetric tube with a stopper, shake, is the B tube (superscript
quasi). Absorb carbon dioxide-free water and 10mL sample solution 2mL set 25mL colorimetric tube with a stopper, shake, is the C tube (blank). in
A, B, C the tube, each 2mL was added ammonium acetate buffer solution, shake, respectively, an ammonium solution was added dropwise 1.2mL acetyl thio, rapid mixing.
With respect to the tube C, B show a light brown pipe. 2min, the color should not be deeper than the pipe A B tube.
Determination of 7.10 Transparency
Weigh the sample 10g (accurate to 0.01g), dissolved in about 60mL of water, and then placed in 100mL volumetric flask, dilute to the mark,
Shake well. Using a spectrophotometer at 1cm absorption cell transmittance measured at 420nm wavelength. With light transmittance of 100% water.
Determination of 7.11 cyclohexylamine Content
7.11.1 Reagent
7.11.1.1 alkaline disodium edetate solution. Weigh 10g of disodium edetate and sodium hydroxide 3.4g, dissolved in water, and
Diluted with water to 100mL.
7.11.1.2 methyl orange acid solution. Weigh 0.2g of methyl orange and acid 3.5g, add water 100mL, placed on a water bath heated to dissolve,
Standing more than 24h, filtered before use.
7.11.1.3 mixture of chloroform and n-butanol. 20 + 1.
7.11.1.4 a mixture of methanol and sulfuric acid. 50 + 1.
7.11.1.5 cyclohexylamine standard solution. Each ml 0.0025mg cyclohexylamine. Weigh cyclohexylamine 0.1g, accurate to 0.0002g, placed
100mL volumetric flask, add water, 50mL, hydrochloric acid 0.5mL, dissolved diluted with water to the mark. The exact amount taken 5.0mL, another set
A 100mL volumetric flask, dilute to the mark, shake. This precise amount of dilution 5.0mL, placed in 100mL flask with water
Dilute to the mark.
7.11.2 analysis step
Weigh 10g laboratory samples, accurate to 0.1g, dissolved in about 60mL of water, placed in 100mL volumetric flask, dilute to the mark with water
Degree, shake. Imbibe this solution with the standard solution of cyclohexylamine 10mL, 60mL two were placed in a separatory funnel, were added successively
The alkaline solution of ethylenediaminetetraacetic acid disodium salt 3.0mL, 15.OmL mixture of chloroform and n-butanol, shaking 2min, rested, get three
Chloride layer, the chloroform extract of the occupation 10.OmL, 60mL placed in a separatory funnel and the other two, each of the boric acid solution was added methyl orange
2.0mL, shake for 2min, rested, take the chloroform layers, each adding anhydrous sodium sulfate 1g, shaking, standing, amount of chloroform solution
5.0mL, placed in colorimetric tubes, each a mixture of sulfuric acid and methanol was added 0.5mL, shake. The sample solution can not be significantly deeper than the standard color.
7.12 dicyclohexylamine test
7.12.1 Reagent
7.12.1.1 chloroform. washed three times, each time water is 1/3 of chloroform, the chloroform layer was separated for measurement;
7.12.1.2 sodium hydroxide solution. 40g/L;
7.12.1.3 Reagent A. bromophenol blue Weigh 75mg, 60mL water, add sodium bicarbonate solution (8.4g/L) 10mL, with stirring.
Hydrochloric acid solution (1 + 55) adjusting the pH to 4.0, dilute with water to 100mL, shake, stored in a cool dark place, use within 48h;
7.12.1.4 Reagent B. (1 → 12) 20mL, glacial acetic acid 16.6mL in 100mL flask, diluted with water amount of hydrochloric acid solution to the mark
Degree, shake.
7.12.2 Instruments
7.12.2.1 Spectrophotometer. with 5cm absorption cell;
7.12.2.2 separating funnel. 250mL.
7.12.3 analysis step
Weigh 10.0g laboratory samples, accurate to 0.01g, in 250mL separating funnel, add water, 100mL dissolve, another measure
100mL water reagent blank to another separating funnel. Each 10mL was added sodium hydroxide solution, and then were washed with 10mL,
5mL and 5mL chloroform extracts were combined chloroform extracts in the other two separating funnel, add water each 100mL, reagents
B3.0mL, reagent A1.0mL, shaking 3min, dark for 30min, after standing layer separated chloroform layer is 25mL colorimetric tube
, Add chloroform to 25mL. At 410nm wavelength, with 5cm absorption cell, chloroform zero, determine the reagent blank and sample solution
Absorbance of liquid, the absorbance difference is not greater than 0.20 is qualified.
Determination of amino acid content of 7.13
7.13.1 Reagent
7.13.1.1 TLC plates. silica gel 60 TLC plate (English name SilicaGel60, silica aperture 60A0), size 20 ×
20cm, coating thickness of about 0.25mm. Growth can be cut width 12cm × 5cm, or the use of appropriate size.
7.13.1.2 eluent. volume ratio (water. ammonia. ethyl acetate. n-propanol) = mixture of 10.10.20.70.
7.13.1.3 amino acid standard solution. each 1mL containing 0.15mg amino acid. Weigh 15mg amino acid, dissolved in water and transferred to
100mL volumetric flask, dilute to the mark.
7.13.1.4 sodium hypochlorite solution. 1 + 20
7.13.1.5 potassium iodide - starch solution. Weigh 0.75g of potassium iodide, dissolved with 100mL of water, heated to boiling, stirring, adding starch solution
Solution (14.3g/L) 35mL, boiled for 2min, cooled use.
7.13.2 Instruments
7.13.2.1 micro injector (flat). 10μL;
7.13.2.2 expansion slot;
7.13.2.3 spray bottle.
7.13.3 analysis step
Weigh 10g laboratory samples, accurate to 0.01g, was dissolved in 60mL water, and then placed in 100mL flask, diluted with water to
Mark and shake. In the bottom of the TLC plate 1cm impose a pencil line. With micro sample taken 2μL above solution, point TLC plate
Videos Online. The TLC plate placed in vertical expansion slot, covered, developing solution is not more than drawing a line, when the liquid expands to expand the top TLC plate,
Immediately removed. Placed in an oven at about 105 ℃ drying 5min, taken out of the hot plate spraying sodium hypochlorite solution, placed in the air circulation in the
Dechlorination, TLC plate to drop below the point of sample KI - When the starch solution was slightly pale blue far too long to avoid dechlorination, then
TLC plate full spray potassium iodide - starch solution, amino acid spots will appear within 5min observe the color should not be dark spots
Standard.
Standard with micro-injector Imbibe 2μL amino acid standard solution, and treated in the same sample at the same time.
Determination of 7.14 absorbance values
7.14.1 Instruments
7.14.1.1 ultraviolet-visible spectrophotometer;
7.14.1.2 1cm quartz cuvette.
7.14.2 analysis step
Weigh 10g laboratory samples, accurate to 0.01g, dissolved in about 60mL of water, placed in 100mL volumetric flask, dilute to the mark with water
Degree, shake. UV-visible spectrophotometer, cuvette, the absorbance was measured at 270nm wavelength in 1cm quartz. With water
Absorbance value of zero.
8 Inspection Rules
8.1 Inspection classification
Inspection is divided into the factory inspection and type testing.
8.1.1 factory inspection
Table 1 cyclohexylamino sodium content, drying loss mass fraction, pH, sulfate mass fraction, transparent
Degree, the mass fraction of cyclohexylamine, dicyclohexylamine mass fraction and mass fraction of amino acid factory inspection items should be tested batches.
8.1.2 Type inspection
Type test items in Table 1. All items. Under normal circumstances, every six months, at least once type test. The following situation
When one of the conditions, type of inspection should be carried out.
a) update key production process;
b) The main raw material change;
c) Discontinued resumed production;
d) factory inspection results are quite different and the last type inspection;
Provisions e) contract.
8.2 Batch
In each product or batch of feed is mixed by repeatedly feeding the product batch.
8.3 Sampling
Each batch of product sampling units according to the provisions of GB/T 6678-2003 determination of each batch of the total sample volume of not less than 200g. The harvest will
Samples rapid mixing, and dividing packed in two vials (bags), paste the label bottles (bags), the stated manufacturer name, product name, batch number, Regulation
Grid sampling date and sampling name. Bottle (bag) to send inspection department, the other bottles (bags) sealed as retention samples stored for future reference.
8.4 Quality Certificate
By the manufacturer's quality inspection department inspection in accordance with this standard, the manufacturer shall ensure that products are manufactured in line with the requirements of this standard, each batch produced
Shall be accompanied by a certificate of quality products, which includes. the production plant name, product name, standard number, batch number, production date.
8.5 retest
If there is an indicator of the test results do not meet the requirements of this standard should be re-packaging unit from twice the amount of sampling re-examination. complex
Even if only a detection result indicator does not meet the requirements of this standard, the entire batch of products to be ineligible.
9 signs, packaging, transportation and storage
9.1 mark
Food Additives cyclohexylamino sodium overpack shall be marked with the product name, manufacturer's name and address, license number and logo, Wei
Health license number, net weight, standard code, batch number, manufacturing date and shelf life, and marked "food additives."
9.2 Packaging
Within the food additive sodium cyclohexylamino plastic food packaging is in line with the use of sealed, packed in cardboard boxes, drum or polypropylene
Ene bags, sealed prison. Packaging unit 1kg, 20kg and 25kg, or according to user requirement.
9.3 Transportation and storage
Food Additives cyclohexylamino sodium should be stored in a dry place to prevent moisture. This product can not be toxic, hazardous substances mix, mixed operation.
9.4 Shelf Life
In line with the standard packaging, transport and storage conditions, from the date of production, food additives cyclohexylamino sodium shelf life
3 years. Than shelf-life re-inspection, testing results meet the requirements of this standard when the product can still be used.
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