GB/T 5009.37-2003 English PDF (GB/T5009.37-2003)

GB/T 5009.37-2003: Method for analysis of hygienic standard of edible oils
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GB/T 5009.37-2003
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 67.040
C 53
Replacing GB/T 5009.37-1996
Method for analysis of hygienic standard of edible oils
ISSUED ON. AUGUST 11, 2003
IMPLEMENTED ON. JANUARY 01, 2004
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine of the People's Republic of China;
Standardization Administration of the People's Republic of
China.
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Normative references ... 4 
3 Sensory inspection ... 4 
4 Physical and chemical inspection ... 5 
Foreword
This standard replaces GB/T 5009.37-1996 “Method for analysis of hygienic
standard of edible oils”.
As compared with GB/T 5009.37-1996, the main changes of this standard are
as follows.
- ADD the peroxide value colorimetric method as the second method;
- MODIFY the structure of the original standard in accordance with GB/T
20001.4-2001 “Rules for drafting standards - Part 4. Methods of chemical
analysis”;
- MODIFY the determination method of carbonyl.
This standard was proposed by AND shall be under the jurisdiction of the
Ministry of Health of the People's Republic of China.
This standard was responsibly drafted by Shanghai Municipal Health and
Epidemic Prevention Station, Tianjin Municipal Health and Epidemic Prevention
Station, Anhui Provincial Health and Epidemic Prevention Station, Shaanxi
Provincial Health and Epidemic Prevention Station, Liaoning Provincial Health
and Epidemic Prevention Station, Hunan Provincial Health and Epidemic
Prevention Station, the Ministry of Health Food Hygiene Supervision and
Inspection Station.
This standard was first released in 1985, first revised in 1996. This is the second
revision.
Method for analysis of hygienic standard of edible oils
1 Scope
This standard specifies the analysis method for edible vegetable oil hygiene
indicators.
This standard applies to the analysis of edible vegetable oil hygiene indicators.
The detection limit of the residual solvent in this method is 0.10 mg/kg, the
detection limit of the second method of peroxide value is 0.003 meq/kg.
2 Normative references
The provisions in following documents become the provisions of this Standard
through reference in this Standard. For the dated references, the subsequent
amendments (excluding corrections) or revisions do not apply to this Standard;
however, parties who reach an agreement based on this Standard are
encouraged to study if the latest versions of these documents are applicable.
For undated references, the latest edition of the referenced document applies.
GB/T 5009.11 Determination of total arsenic and abio-arsenic in food
GB/T 5009.22 Determination of aflatoxin B1 in foods
GB/T 5009.27 Determination of benzo(a)pyrene in foods
GB/T 5009.138 Determination of nickel in foods
3 Sensory inspection
3.1 Color
3.1.1 Instruments
Beaker. 50 mm in diameter, 100 mm in height.
3.1.2 Analytical procedures
MIX the specimen uniformly, FILTER it into the beaker, the height of oil layer
shall not be not less than 5 mm, OBSERVE it at room temperature first in natural
light, then OBSERVE it in front a white background using its reflected light, USE
X - Specimen acid value (by potassium hydroxide), in milligrams per gram
(mg/g);
V - Volume of potassium hydroxide standard titration solution consumed by
the specimen, in milliliters (mL);
c - Actual concentration of potassium hydroxide standard titration, in moles
per liter (mol/L);
m - Specimen mass, in grams (g);
56.11 - Milligrams of potassium hydroxide equivalent to 1.0 mL of potassium
hydroxide standard titration solution [c (KOH) = 1.000 mol/L].
The calculation results retain two significant figures.
4.1.5 Precision
The absolute difference between two independent determinations obtained
under repeatability conditions shall not exceed 10% of the arithmetic mean.
4.2 Peroxide value
4.2.1 Method I -- Titration method
4.2.1.1 Principle
Peroxide is produced in the oxidation of oil, peroxide reacts with the potassium
iodine to produce free iodine, which is titrated by sodium thiosulfate solution,
the content is calculated.
4.2.1.2 Reagents
4.2.1.2.1 Saturated potassium iodide solution. WEIGH 14 g of potassium iodide,
ADD 10 mL of water to dissolve it, HEAT it slightly to dissolve it if necessary,
COOL it down, PRESERVE it in a brown bottle.
4.2.1.2.2 Chloroform - glacial acetic acid mixture. MEASURE 40 mL of
chloroform, ADD 60 mL of glacial acetic acid, MIX it uniformly.
4.2.1.2.3 Sodium thiosulfate standard titration solution [c (Na2S2O3) = 0.0020
mol/L].
4.2.1.2.4 Starch indicator (10 g/L). WEIGH 0.50 g of soluble starch, ADD a small
amount of water, MAKE it into paste, POUR it into 50 mL of boiling water to mix
it uniformly, MAKE it be boiling, PREPARE it before use.
4.2.1.3 Analytical procedures
chloroform + methanol (7 + 3) mixed solvent to dilute it to the mark, MIX it
uniformly, each milliliter of this solution is equivalent to 10.0 µg of iron.
4.2.2.3 Instruments
4.2.2.3.1 Spectrophotometer.
4.2.2.3.2 10 mL glass colorimetric tube with plug.
4.2.2.4 Analytical procedures
4.2.2.4.1 Preparation of specimen solution
Precisely WEIGH about 0.01 g ~ 1.0 g of specimen (accurate to the scale
0.0001 g) into a 10 mL volumetric flask, ADD the chloroform + methanol (7 + 3)
mixed solvent to dilute it to the mark, MIX it uniformly.
Respectively and precisely ABSORB 0, 0.2, 0.5, 1.0, 2.0, 3.0, 4.0 mL
(respectively equivalent to iron concentration of 0, 2.0, 5.0, 10.0, 20.0, 30.0,
40.0 µg) of iron standard use solution (10.0 µg/mL) into dry 10 mL colorimetric
tube, USE the chloroform + methanol (7 + 3) mixed solvent to dilute it to the
mark, MIX it uniformly. ADD 1 drop (about 0.05 mL) of potassium thiocyanate
(300 g/L), MIX it uniformly. PLACE it at room temperature (10 °C ~ 35 °C) for 5
min, TRANSFER it into a 1 cm cuvette, USE the chloroform + methanol (7 + 3)
mixed solvent as reference, DETERMINE the absorbance at the wavelength
500 nm, DEDUCT the absorbance of each point by zero tube absorbance,
DRAW the standard curve or CALCULATE the linear regression equation.
4.2.2.4.2 Specimen determination
Precisely ABSORB 1.0 mL of specimen into a dry 10 mL colorimetric tube, ADD
1 drop (about 0.05 mL) of ferrous chloride (3.5 g/L) solution, USE the chloroform
+ methanol (7 + 3) mixed solvent to dilute it to the mark, MIX it uniformly.
OPERATE in accordance with 4.2.2.4.1 from “ADD 1 drop (about 0.05 mL) of
potassium thiocyanate (300 g/L)”. The specimen absorbance is deducted by
the zero tube absorbance, then it is compared with the curve or placed in the
regression equation to calculate the content.
4.2.2.5 Result calculation
The peroxide value in the specimen is calculated in accordance with the formula
(4).
anhydrous sodium sulfate, USE total glass distillation device to distill and collect
the distillate.
4.3.2.3 2,4-dinitrophenylhydrazine solution. WEIGH 50 mg of 2,4-
dinitrophenylhydrazine, DISSOLVE it into 100 mL of refined benzene.
4.3.2.4 Trichloroacetic acid solution. WEIGH 4.3 g of solid trichloroacetic acid,
ADD 100 mL of refined benzene to dissolve it.
4.3.2.5 Potassium hydroxide - ethanol solution. WEIGH 4 g of potassium
hydroxide, ADD 100 mL of refined ethanol to dissolve it, PLACE it in a cold dark
place overnight, TAKE the upper clear solution to prepare for use. If the solution
changes into yellow brown, it shall prepare it again.
4.3.3 Instruments
Spectrophotometer.
4.3.4 Analytical procedures
Precisely WEIGH about 0.025 g ~ 0.5 g of specimen, PLACE it into a 25 mL
volumetric flask, ADD benzene to dissolve the specimen and DILUTE it to the
mark. ABSORB 5.0 mL, PLACE it into a 25 mL test tube with plug, ADD 3 mL
of trichloroacetic aci...
GB/T 5009.37-2003
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 67.040
C 53
Replacing GB/T 5009.37-1996
Method for analysis of hygienic standard of edible oils
ISSUED ON. AUGUST 11, 2003
IMPLEMENTED ON. JANUARY 01, 2004
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine of the People's Republic of China;
Standardization Administration of the People's Republic of
China.
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Normative references ... 4 
3 Sensory inspection ... 4 
4 Physical and chemical inspection ... 5 
Foreword
This standard replaces GB/T 5009.37-1996 “Method for analysis of hygienic
standard of edible oils”.
As compared with GB/T 5009.37-1996, the main changes of this standard are
as follows.
- ADD the peroxide value colorimetric method as the second method;
- MODIFY the structure of the original standard in accordance with GB/T
20001.4-2001 “Rules for drafting standards - Part 4. Methods of chemical
analysis”;
- MODIFY the determination method of carbonyl.
This standard was proposed by AND shall be under the jurisdiction of the
Ministry of Health of the People's Republic of China.
This standard was responsibly drafted by Shanghai Municipal Health and
Epidemic Prevention Station, Tianjin Municipal Health and Epidemic Prevention
Station, Anhui Provincial Health and Epidemic Prevention Station, Shaanxi
Provincial Health and Epidemic Prevention Station, Liaoning Provincial Health
and Epidemic Prevention Station, Hunan Provincial Health and Epidemic
Prevention Station, the Ministry of Health Food Hygiene Supervision and
Inspection Station.
This standard was first released in 1985, first revised in 1996. This is the second
revision.
Method for analysis of hygienic standard of edible oils
1 Scope
This standard specifies the analysis method for edible vegetable oil hygiene
indicators.
This standard applies to the analysis of edible vegetable oil hygiene indicators.
The detection limit of the residual solvent in this method is 0.10 mg/kg, the
detection limit of the second method of peroxide value is 0.003 meq/kg.
2 Normative references
The provisions in following documents become the provisions of this Standard
through reference in this Standard. For the dated references, the subsequent
amendments (excluding corrections) or revisions do not apply to this Standard;
however, parties who reach an agreement based on this Standard are
encouraged to study if the latest versions of these documents are applicable.
For undated references, the latest edition of the referenced document applies.
GB/T 5009.11 Determination of total arsenic and abio-arsenic in food
GB/T 5009.22 Determination of aflatoxin B1 in foods
GB/T 5009.27 Determination of benzo(a)pyrene in foods
GB/T 5009.138 Determination of nickel in foods
3 Sensory inspection
3.1 Color
3.1.1 Instruments
Beaker. 50 mm in diameter, 100 mm in height.
3.1.2 Analytical procedures
MIX the specimen uniformly, FILTER it into the beaker, the height of oil layer
shall not be not less than 5 mm, OBSERVE it at room temperature first in natural
light, then OBSERVE it in front a white background using its reflected light, USE
X - Specimen acid value (by potassium hydroxide), in milligrams per gram
(mg/g);
V - Volume of potassium hydroxide standard titration solution consumed by
the specimen, in milliliters (mL);
c - Actual concentration of potassium hydroxide standard titration, in moles
per liter (mol/L);
m - Specimen mass, in grams (g);
56.11 - Milligrams of potassium hydroxide equivalent to 1.0 mL of potassium
hydroxide standard titration solution [c (KOH) = 1.000 mol/L].
The calculation results retain two significant figures.
4.1.5 Precision
The absolute difference between two independent determinations obtained
under repeatability conditions shall not exceed 10% of the arithmetic mean.
4.2 Peroxide value
4.2.1 Method I -- Titration method
4.2.1.1 Principle
Peroxide is produced in the oxidation of oil, peroxide reacts with the potassium
iodine to produce free iodine, which is titrated by sodium thiosulfate solution,
the content is calculated.
4.2.1.2 Reagents
4.2.1.2.1 Saturated potassium iodide solution. WEIGH 14 g of potassium iodide,
ADD 10 mL of water to dissolve it, HEAT it slightly to dissolve it if necessary,
COOL it down, PRESERVE it in a brown bottle.
4.2.1.2.2 Chloroform - glacial acetic acid mixture. MEASURE 40 mL of
chloroform, ADD 60 mL of glacial acetic acid, MIX it uniformly.
4.2.1.2.3 Sodium thiosulfate standard titration solution [c (Na2S2O3) = 0.0020
mol/L].
4.2.1.2.4 Starch indicator (10 g/L). WEIGH 0.50 g of soluble starch, ADD a small
amount of water, MAKE it into paste, POUR it into 50 mL of boiling water to mix
it uniformly, MAKE it be boiling, PREPARE it before use.
4.2.1.3 Analytical procedures
chloroform + methanol (7 + 3) mixed solvent to dilute it to the mark, MIX it
uniformly, each milliliter of this solution is equivalent to 10.0 µg of iron.
4.2.2.3 Instruments
4.2.2.3.1 Spectrophotometer.
4.2.2.3.2 10 mL glass colorimetric tube with plug.
4.2.2.4 Analytical procedures
4.2.2.4.1 Preparation of specimen solution
Precisely WEIGH about 0.01 g ~ 1.0 g of specimen (accurate to the scale
0.0001 g) into a 10 mL volumetric flask, ADD the chloroform + methanol (7 + 3)
mixed solvent to dilute it to the mark, MIX it uniformly.
Respectively and precisely ABSORB 0, 0.2, 0.5, 1.0, 2.0, 3.0, 4.0 mL
(respectively equivalent to iron concentration of 0, 2.0, 5.0, 10.0, 20.0, 30.0,
40.0 µg) of iron standard use solution (10.0 µg/mL) into dry 10 mL colorimetric
tube, USE the chloroform + methanol (7 + 3) mixed solvent to dilute it to the
mark, MIX it uniformly. ADD 1 drop (about 0.05 mL) of potassium thiocyanate
(300 g/L), MIX it uniformly. PLACE it at room temperature (10 °C ~ 35 °C) for 5
min, TRANSFER it into a 1 cm cuvette, USE the chloroform + methanol (7 + 3)
mixed solvent as reference, DETERMINE the absorbance at the wavelength
500 nm, DEDUCT the absorbance of each point by zer...