GB 5009.227-2023 PDF English
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| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivery | Name of Chinese Standard | Status |
| GB 5009.227-2023 | English | 155 |
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National food safety standard - Determination of peroxide value in foods
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| GB 5009.227-2016 | English | 75 |
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Method for analysis of hygienic standard of edible oils
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GB 5009.227-2023: National food safety standard - Determination of peroxide value in foods---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/GB5009.227-2023
GB
NATIONAL STANDARD OF THE
PEOPLE'S REPUBLIC OF CHINA
National food safety standard - Determination of peroxide
value in food
Issued on. SEPTEMBER 6, 2023
Implemented on. MARCH 6, 2024
Issued by. National Health Commission of the People's Republic of China;
State Administration for Market Regulation.
Table of Contents
Foreword... 3
1 Scope... 4
Method A - Indicator titration method... 4
2 Principle... 4
3 Reagents and materials... 4
4 Instruments and equipment... 6
5 Analysis steps... 6
6 Presentation of analysis results... 8
7 Precision... 10
Method B - Potentiometric titration... 10
8 Principle... 10
9 Reagents and materials... 10
10 Instruments and equipment... 11
11 Analysis steps... 11
12 Presentation of analysis results... 12
13 Precision... 12
Foreword
This standard replaces GB 5009.227-2016 "National food safety standard -
Determination of peroxide value in food".
Compared with GB 5009.227-2016, the main changes in this standard are as follows.
-- The scope of Method A "Indicator titration method" is modified;
-- The sample preparation for non-dairy cream and powdered oil products is added.
National food safety standard - Determination of peroxide
value in food
1 Scope
This standard specifies the method for the determination of peroxide value in food.
Method A is suitable for the determination of peroxide value in food.
Method B is suitable for the determination of peroxide value in edible animal and
vegetable oils, fats, and margarine.
Method A - Indicator titration method
2 Principle
The prepared oil and fat sample is dissolved in chloroform-glacial acetic acid solution,
the peroxide reacts with potassium iodide to generate iodine, and the precipitated iodine
is titrated with sodium thiosulfate standard titration solution. The amount of peroxide
value is expressed as the mass fraction of peroxide equivalent to iodine or the number
of millimoles of active oxygen in 1 kg of the sample.
3 Reagents and materials
Unless otherwise stated, the reagents used in this method are of analytical grade, and
the water is the third-grade water specified in GB/T 6682.
3.1 Reagents
3.1.1 Glacial acetic acid (CH3COOH).
3.1.2 Trichloromethane (CHCl3).
3.1.3 Potassium iodide (KI).
3.1.4 Petroleum ether. The boiling range is 30 ℃~60 ℃.
Confirmation of petroleum ether. Take 100 mL of petroleum ether in a rotary
evaporation bottle, and evaporate to dryness under reduced pressure by using a rotary
evaporator in a water bath not higher than 40 °C. Wash the rotary evaporation bottle
several times with 30 mL of chloroform-glacial acetic acid solution, and combine the
washing liquid into a 250 mL iodine flask. Accurately add 1.00 mL of saturated
potassium iodide solution, plug the bottle cap tightly, and shake gently for 0.5 min.
Leave it in a dark place for 3 min, add 1.0 mL of starch indicator, and mix well. If no
blue color appears, this petroleum ether can be used for the sample preparation; If a
blue color appears after adding 1.0 mL of starch indicator and mixing, the reagent needs
to be replaced.
3.1.5 Anhydrous sodium sulfate (Na2SO4).
3.1.6 Soluble starch.
3.1.7 Acetone (CH3COCH3).
3.1.8 Amylase (CAS number. 9000-92-4). The enzyme activity is ≥2000 U/g.
3.1.9 Papain (CAS number. 9001-73-4). The enzyme activity is ≥6000 U/mg.
3.1.10 Sodium thiosulfate (Na2S2O3 • 5H2O).
3.2 Reagent preparation
3.3 Preparation of standard solution
3.3.1 Sodium thiosulfate standard titration solution (0.1 mo1/L). It shall be prepared
and calibrated in accordance with the requirements of GB/T 5009.1; or a standard
titration solution with national certification and a Reference Material Certificate.
3.3.2 Sodium thiosulfate standard titration solution (0.01 mo1/L). It is prepared from
diluting 0.1 mo1/L sodium thiosulfate standard titration solution with newly boiled and
cooled water. Prepare the solution fresh just before use.
3.3.3 Sodium thiosulfate standard titration solution (0.002 mo1/L). It is prepared from
diluting 0.01 mo1/L sodium thiosulfate standard titration solution with newly boiled
and cooled water. Prepare the solution fresh just before use.
4 Instruments and equipment
4.1 Balance. The sensitivities are 0.01 g, 0.001 g, and 0.0001 g, respectively.
4.2 Electric constant-temperature drying oven.
4.3 Rotary evaporator. It is equipped with a brown rotary evaporation bottle.
4.4 Constant-temperature water bath oscillator.
4.5 High-speed refrigerated centrifuge.
4.6 Overhead stirrer.
4.7 Burette. The capacity is 10 mL, and the minimum scale is 0.05 mL.
4.8 Burette. The capacity is 25 mL or 50 mL, and the minimum scale is 0.1 mL.
5 Analysis steps
5.1 Sample preparation
Strong light shall be avoided during the sample preparation process. After preparation,
the oil and fat shall be stored in a sealed container and measured as soon as possible.
5.1.1 Animal and vegetable oils and fats
For liquid samples, shake the closed container containing the sample, mix thoroughly,
and then take a sample directly; for solid samples, select a representative sample and
place it in a closed container, mix well, and then take a sample. If necessary, place the
container containing the solid sample in a constant temperature water bath, and heat it
until the sample begins to melt; let it completely melt at this temperature, shake and
mix well, and take a sample for measurement immediately while the sample is in liquid
state.
5.1.2 Oil products
5.1.2.1 Edible hydrogenated oil, shortening, cocoa butter substitute
5.1.2.2 Margarine
Place the sample in a closed container, heat it in an electric constant-temperature drying
oven at 60 °C to 70 °C until it melts, shake and mix, continue heating until the
emulsification breaks down into layers, and filter the oil layer through the rapid
qualitative filter paper into a beaker. The filtrate in the beaker is the sample to be tested,
and the sample to be tested shall be clarified. Take a sample and measure it immediately
while the sample to be tested is in a liquid state.
5.1.2.3 Non-dairy cream
Take a representative sample in a beaker, add about 5 times the sample volume of
petroleum ether, and stir for 2 minutes by using an overhead stirrer to mix evenly. While
stirring, add anhydrous sodium sulfate of about 1.6 times the mass of the sample,
continue stirring and mixing for 5 minutes, remove the beaker, and let the solution stand
for 5 minutes to allow the petroleum ether to layer (if emulsification occurs, cover the
top of the beaker with a layer of plastic wrap, and place the beaker in a water bath of
not higher than 40 °C for 10 minutes to stratify the petroleum ether). Pour out the
supernatant, add about 2 times the sample volume of petroleum ether to the beaker, and
repeat the above stirring and standing operations; combine the petroleum ethers, filter,
and transfer the filtrate into a brown rotary evaporation bottle; in a water bath of not
higher than 40 ℃, use a rotary evaporator to evaporate the petroleum ether to dryness
under reduced pressure.
5.2 Sample determination
Sample determination shall be avoided under direct sunlight. Weigh 2 g~3 g of the
prepared sample (accurate to 0.001 g), place it in a 250 mL iodine flask, add 30 mL of
chloroform-glacial acetic acid solution, and shake the sample gently until it is
completely dissolved. Accurately add 1.00 mL of saturated potassium iodide solution,
plug the bottle cap tightly, shake gently for 0.5 min, and place in a dark place for 3 min.
Take out and add 100 mL of water, shake well and immediately use sodium thiosulfate
standard titration solution (when the estimated peroxide value is 0.15 g/100 g and below,
use 0.002 mol/L standard titration solution; when the estimated peroxide value is greater
than 0.15 g/100 g, use 0.01 mol/L standard titration solution) to titrate the precipitated
iodine. When the solution turns to light yellow, add 1 mL of starch indicator, continue
titrating, and shake vigorously until the blue color of the solution disappears, that is the
end point.
6 Presentation of analysis results
6.1 When the peroxide value is expressed as the mass fraction of peroxide equivalent
to iodine, it is calculated according to formula (1).
6.2 When the peroxide value is expressed in millimoles of active oxygen in 1 kg of the
sample, it is calculated according to formula (2).
7 Precision
The absolute difference between two independent determination results obtained under
repeatability conditions shall not exceed 10% of the arithmetic mean.
8 Principle
The prepared oil and fat sample is dissolved in isooctane-glacial acetic acid solution.
The peroxide in the sample reacts with potassium iodide to generate iodine. After the
reaction, the precipitated iodine is titrated with sodium thiosulfate standard titration
solution, and the titration end point is determined with a potentiometric titrator. The
amount of peroxide value is expressed as the mass fraction of peroxide equivalent to
iodine or the number of millimoles of active oxygen in 1 kg of the sample.
9 Reagents and materials
Unless otherwise stated, the reagents used in this method are of analytical grade,
9.1 Reagents
9.2 Reagent preparation
9.3 Preparation of standard solution
The preparation is the same as 3.3.
10 Instruments and equipment
10.1 Balance. The sensitivities are 0.01 g, 0.001 g, and 0.0001 g, respectively.
10.2 Electric constant-temperature drying oven.
10.3 Potentiometric titrator.
10.4 Magnetic stirrer.
11 Analysis steps
11.1 Sample preparation
The preparation is the same as 5.1.1 and 5.1.2.2.
11.2 Sample determination
Weigh 5 g of the prepared sample (accurate to 0.001 g) and place it into the titration
cup of the potentiometric titrator, add 50 mL of isooctane-glacial acetic acid solution,
and shake gently to completely dissolve the sample. If the solubility of the sample is
poor (such as stearin or animal fat), first add 20 mL of isooctane to the titration cup,
shake gently to dissolve the sample, then add 30 mL of glacial acetic acid, and mix well.
Accurately add 1.00 mL of saturated potassium iodide solution to the titration cup, start
the magnetic stirrer, and react at a suitable stirring speed for 60 s±1 s. Immediately add
30 mL~100 mL water to the titration cup, insert the electrode and titration head, set the
titration parameters, run the titration program, perform the titration, and observe the
titration curve and potential changes. The added amount of sodium thiosulfate standard
titration solution is generally controlled at 0.05 mL/drop~0.2 mL/drop. After reaching
the titration end point, record the volume of standard solution consumed at the titration
end point. After the titration of a sample is completed, the stirrer or stirring magnet,
titration head, and electrode need to be immersed in isooctane to clean the oils and fats
on the surface.
A blank test is performed at the same time. Carry out titration and observe the titration
curve and potential changes. The added amount of sodium thiosulfate standard titration
solution is generally controlled at 0.005 mL/drop. After reaching the titration end point,
record the volume V0 of the standard solution consumed at the titration end point. The
volume V0 of the 0.01 mo1/L sodium thiosulfate standard titration solution consumed
in the blank test shall not exceed 0.1 mL.
12 Presentation of analysis results
It is the same as Chapter 6.
13 Precision
The absolute difference between two independent determination results obtained under
repeatability conditions shall not exceed 10% of the arithmetic mean.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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