GB 1886.349-2021 PDF English
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National food safety standard - Food additives - Five carbon diacetal (also known as glutaraldehyde)
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GB 1886.349-2021: National food safety standard - Food additives - Five carbon diacetal (also known as glutaraldehyde)
---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GB1886.349-2021
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard - Food Additives - Five
carbon diacetal (also known as glutaraldehyde)
ISSUED ON: SEPTEMBER 07, 2021
IMPLEMENTED ON: MARCH 07, 2022
Issued by: National Health Commission;
State Administration for Market Regulation.
Table of Contents
1 Scope ... 3
2 Chemical name, molecular formula, structural formula and relative molecular
mass ... 3
3 Technical requirements ... 3
Annex A Inspection methods ... 5
Annex B Standard reference gas chromatograms of methanol and ethanol .. 11
National Food Safety Standard - Food Additives - Five-
carbon diacetal (also known as glutaraldehyde)
1 Scope
This Standard applies to the food additive five-carbon diacetal (also known as
glutaraldehyde) obtained by that vinyl methyl ether or vinyl ethyl ether reacts
with acrolein to form 2-alkoxy-3,4-dihydropyran, which is then hydrolyzed.
2 Chemical name, molecular formula, structural
formula and relative molecular mass
2.1 Chemical name
Five-carbon diacetal (also known as glutaraldehyde)
2.2 Molecular formula
C5H8O2
2.3 Structural formula
2.4 Relative molecular mass
100.12 (according to 2018 international relative atomic mass)
3 Technical requirements
3.1 Sensory requirements
Sensory requirements shall meet the requirements of Table 1.
Annex A
Inspection methods
WARNING: Some reagents used in the inspection methods of this
Standard are toxic or corrosive. Operate in accordance with relevant
national regulations. Please be careful when using them. If it is splashed
on the skin, rinse immediately with water. In severe cases, seek medical
attention immediately. When using volatile acids, it shall be carried out in
a fume hood.
A.1 General
The reagents and water used in this Standard refer to analytically-pure reagents
and grade 3 water specified in GB/T 6682 when other requirements are not
indicated. The standard titration solution, standard solution for impurity
determination, preparations and products used in the test are prepared in
accordance with GB/T 601, GB/T 602 and GB/T 603 when other requirements
are not indicated. The solution used in the test refers to an aqueous solution
when it is not specified which solvent is used to prepare it.
A.2 Identification test
A.2.1 Solubility
Pipette about 1mL of specimen into a beaker. Add 1mLof water. Shake not less
than 30s. Observe the dissolution of the sample within 5min. The specimen
shall be easily dissolved in water.
A.2.2 Identification of the melting point of 2,4-dinitrophenylhydrazone
A.2.2.1 Method principle
Five carbon diacetal reacts with 2,4-dinitrophenylhydrazine to form 2,4-
dinitrophenylhydrazone precipitation. 2,4-dinitrophenylhydrazone has a specific
melting point.
A.2.2.2 Reagents and materials
A.2.2.2.1 2,4-dinitrophenylhydrazine solution: Take 0.8g of 2,4-
dinitrophenylhydrazine. Add 4mL of sulfuric acid. Stir until it is completely
dissolved. Continue stirring. Add 6mL of water along with the wall in drops. Add
20mL of ethanol. Mix and shake well. Filter. Take the filtrate.
A.2.2.2.2 Absolute ethanol.
The carbonyl group of glutaraldehyde can react with hydroxylamine
hydrochloride to produce glutaric oxime. Glutaraldehyde will release
hydrochloric acid while generating glutaric oxime. Triethanolamine is weakly
alkaline. It can neutralize and remove hydrochloric acid. Add excessive
triethanolamine. Use hydrochloric acid standard solution to backdrop. The
content of glutaraldehyde can be calculated by calibrating the blank
determination at the same time.
A.3.2 Reagents and materials
A.3.2.1 Triethanolamine solution: 74g/L. Dissolve 74g of triethanolamine with a
certain amount of water and transfer to a 1L volumetric flask. Use water to set
volume to the scale and mix well.
A.3.2.2 Hydroxylamine hydrochloride solution: 35g/L, pH is 3.60. Use a certain
amount of water to dissolve 35.0g of hydroxylamine hydrochloride. Transfer to
a 1L volumetric flask. Use water to set volume to the scale. Mix well. Use
triethanolamine solution to adjust pH to 3.60.
A.3.2.3 Hydrochloric acid standard titration solution: c(HCl)=0.5mol/L.
A.3.3 Instruments and equipment
A.3.3.1 Electronic balance: the resolution is 0.1g and 0.0001g.
A.3.3.2 Magnetic stirrer.
A.3.3.3 Acidity meter: the accuracy is ±0.01.
A.3.4 Determination method
Add 65.0mL of pH 3.60 hydroxylamine hydrochloride solution and 30.8mL of
triethanolamine solution into a 200mL small beaker. Put a Teflon (or equivalent
material) rotor in each small beaker. Place the small beaker on a magnetic
stirrer and stir. Accurately add a certain amount of sample (approximately
equivalent to 300mg of five carbon bisacetal). Put a lid and stir. Stir at room
temperature for at least 60min, but not more than 90min. At the same time, do
a reagent blank test without adding a specimen. After the stirring is over, use
0.5mol/L hydrochloric acid to titrate the specimen and the blank sample to pH
3.60 as the end point.
NOTE: In the process of neutralization analysis, stirring speed is a key factor. When stirring
is required, make sure that no bubbles are mixed into the solution, and the specimen and
the blank sample are always kept at the same stirring speed.
A.3.5 Result calculation
The content of five-carbon diacetal is calculated as the mass fraction w1 of
A.4.3 Instruments and equipment
A.4.3.1 Gas chromatograph with hydrogen flame ionization detector (FID).
A.4.3.2 Electronic balance: Resolution is 0.1mg.
A.4.4 GC reference conditions
A.4.4.1 Chromatographic column: Polyethylene glycol quartz capillary column;
column length is 18m, inner diameter is 0.53mm, film thickness is 1.0μm, or
equivalent column.
A.4.4.2 Chromatographic column temperature: Initial temperature is 40°C, keep
for 1min; increase to 130°C at 4.0°C /min; increase to 200°C at 20°C /min, keep
for 5min.
A.4.4.3 Detector temperature: 250°C.
A.4.4.4 Injection port temperature: 250°C.
A.4.4.5 Carrier gas flow rate: 1mL/min.
A.4.4.6 Hydrogen flow rate: 40mL/min.
A.4.4.7 Air flow rate: 400mL/min.
A.4.4.8 Injection volume: 1μL.
A.4.4.9 Split ratio: 20:1.
A.4.5 Analysis steps
A.4.5.1 Preparation of standard solution
A.4.5.1.1 Methanol standard stock solution: 5000mg/L. Accurately weigh 0.5g
of methanol standard, to the nearest of 0.0001g. Place in a 100mL volumetric
flask. Use isopropanol to set volume to the scale. Mix well. Store in a refrigerator
at 0°C ~4°C.
A.4.5.1.2 Ethanol standard stock solution: 5000mg/L. Accurately weigh 0.5g of
ethanol standard, to the nearest of 0.0001g. Place in a 100mL volumetric flask.
Use isopropanol to set volume to the scale. Mix well. Store in a refrigerator at
0°C ~4°C.
A.4.5.1.3 Mixed series standard working liquids: Pipette 0.05mL, 0.2mL, 0.4mL,
0.8mL, 1.6mL, 2mL of methanol standard stock solution and ethanol standard
stock solution respectively into six 10mL volumetric flasks. Use isopropanol to
set volume to the scale. Prepare into series standard solutions of which the
methanol and ethanol content are 25mg/L, 100mg/L, 200mg/L, 400mg/L,
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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