GB 5009.229-2016 (GB5009.229-2016) & related versions
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National Food Safety Standard -- Determination of Acid Value in Foods
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GB 5009.229-2016
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GB 5009.229-2016
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GB 5009.229-2016: PDF in English
GB 5009.229-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard -
Determination of Acid Value in Foods
ISSUED ON. AUGUST 31, 2016
IMPLEMENTED ON. MARCH 1, 2017
Issued by. National Health and Family Planning Commission of the
People’s Republic of China
Table of Contents
Foreword ... 4
1 Application Scope ... 5
Method I - The Cold Solvent Indicator Titration Method ... 5
2 Principle ... 5
3 Reagents and Materials ... 6
4 Apparatus ... 7
5 Analytical Procedures ... 7
6 Expression of Analytical Results ... 9
7 Precision ... 10
Method II - The Cold Solvent Automatic Potentiometric Titration Method ... 10
8 Principle ... 10
9 Reagents and Materials ... 10
10 Apparatus ... 10
11 Analytical Procedures ... 11
12 Expression of Analytical Results ... 14
13 Precision ... 14
Method III - The Hot Ethanol Indicator Titration Method ... 14
14 Principle ... 14
15 Reagents and Materials ... 14
16 Apparatus ... 14
17 Analytical Procedures ... 14
18 Expression of Analytical Results ... 15
19 Precision ... 15
Annex A Impurity Removal and Dehydration of Specimens of Fat-oil ... 16
Annex B Treatment of Specimens of Solid Fat-oil ... 18
Annex C Treatment of Specimens of Emulsifying Fat-oil ... 19
Annex D Crushing of Samples ... 20
Annex E Criteria for the End Point of Titration of the Automatic Potentiometric
Titration Method ... 21
Foreword
This Standard replaces. 4.1 of GB/T 5009.37-2003, Method for Analysis of Hygienic
Standard of Edible Oils; 14.3 of GB/T 5009.44-2003, Method for Analysis of Hygienic
Standard of Meat and Meat Products; 4.1, 4.2 and 4.3 of GB/T 5009.56-2003, Method
for Analysis of Hygienic Standard of Pastry; 4.1 of GB/T 5009.77-2003, Method for
Analysis of Hygienic Standard of Edible Hydrogenated Oil; GB/T 15689-2008, Oilseeds
- Determination of Acidity of Oils; GB/T 14489.3-1993, Method for Determination of
Free Fatty Acids Content of Oils in Oilseeds; and GB/T 5530-2005, Animal and
Vegetable Fats and Oils - Determination of Acid Value and Acidity.
Compared with 4.1 of GB/T 5009.37-2003, the main changes of this Standard are as
follows.
-- the standard name is modified into “National Food Safety Standard -
Determination of Acid Value in Foods”;
-- the application scope of the standard is modified;
-- the phenolphthalein indicator titration method is modified as Method I, i.e. the cold
solvent indicator titration method;
-- the cold solvent automatic potentiometric titration method is added as Method II;
-- the hot ethanol indicator titration method is added as Method III;
-- the specification for the preparation of test specimens of food samples is added;
-- the requirements for the weight of specimens are added;
-- the requirements for precision are modified.
National Food Safety Standard -
Determination of Acid Value in Foods
1 Application Scope
This Standard specifies the three methods for the determination of acid value in all
kinds of foods - the cold solvent indicator titration method (Method I), the cold solvent
automatic potentiometric titration method (Method II), and the hot ethanol indicator
titration method (Method III).
Method I applies to the samples of edible fat-oil which can be completely dissolved by
a cold solvent into a clarified solution at normal temperature; the application scope
covers 7 categories -- including edible vegetable oil (except chilli oil), edible animal oil,
edible hydrogenated oil, shortening, margarine, non-dairy cream and vegetable
oilseeds.
Method II applies to the samples of edible fat-oil and the samples of fat-oil extracted
from oil-containing foods, which can be completely dissolved by a cold solvent into a
clarified solution at normal temperature; the application scope covers 19 categories --
including edible vegetable oil (including chilli oil), edible animal oil, edible
hydrogenated oil, shortening, margarine, non-dairy cream, oilseeds, fried food, puffed
food, roasted foods, nut food, pastry, bread, biscuit, fried instant noodle, sauce of nuts
and seeds, animal dried aquatic products, preserved meat products and edible-oil-
added chilli sauce.
Method III applies to the samples of edible fat-oil which cannot be dissolved by a cold
solvent into a clarified solution at normal temperature; the application scope covers 6
categories -- including edible vegetable oil, edible animal oil, edible hydrogenated oil,
shortening, margarine and non-dairy cream.
Method I - The Cold Solvent Indicator Titration Method
2 Principle
Use an organic solvent to dissolve the samples of fat-oil into the sample solution; use
potassium hydroxide or sodium hydroxide standard titration solution to neutralize and
titrate the free fatty acid; decide the end point of titration based on the colour change
of the indicator; finally, calculate the acid value of the specimen of fat-oil based on the
volume of standard titration solution consumed at the end point of titration.
3 Reagents and Materials
Unless specified otherwise, all reagents used in this Standard are analytically pure; all
water is grade-3 water specified in GB/T 6682.
3.1 Reagents
3.1.1 Isopropanol (C3H8O).
3.1.2 Diethyl ether (C4H10O).
3.1.3 Methyl tertiary butyl ether (C5H12O).
3.1.4 95% ethyl alcohol (C2H6O).
3.1.5 Phenolphthalein (C20H14O4), indicator, CAS. 77-09-8.
3.1.6 Thymol phenolphthalein (C28H30O4), indicator, CAS. 125-20-2.
3.1.7 Alkali blue 6B (C37H31N3O4), indicator, CAS. 1324-80-7.
3.1.8 Anhydrous sodium sulphate (Na2SO4), which is fully dried at 105°C ~ 110°C
and then loaded in a closed container for cooling and storage.
3.1.9 Anhydrous diethyl ether (C4H10O).
3.1.10 Petroleum ether, of a boiling range 30°C ~ 60°C.
3.2 Reagent preparation
3.2.1 Potassium hydroxide or sodium hydroxide standard titration aqueous solution,
of a concentration 0.1 mol/l or 0.5 mol/l, may be prepared and calibrated as specified
in GB/T 601, or may be the commercial reagent available in the market.
3.2.2 Diethyl ether-isopropanol mixed liquid. diethyl ether + isopropanol = 1 + 1,
which is prepared immediately before use by fully mixing 500 ml of diethyl ether and
500 ml of isopropanol.
3.2.3 Phenolphthalein indicator. weigh 1 g of phenolphthalein; add 100 ml of 95%
ethyl alcohol and stir to dissolve completely.
3.2.4 Thymol phenolphthalein indicator. weigh 2 g of thymol phenolphthalein; add
100 ml of 95% ethyl alcohol and stir to dissolve completely.
3.2.5 Alkali blue 6B indicator. weigh 2 g of alkali blue 6B; add 100 ml of 95% ethyl
alcohol and stir to dissolve completely.
4 Apparatus
4.1 10-ml micro burettes. of minimum scale value 0.05 ml.
4.2 Balance. of sensitivity 0.001 g.
4.3 Thermostat water bath.
4.4 Thermostat drying box.
4.5 Centrifuge. of the highest rotational speed not lower than 8 000 r/min.
4.6 Rotary evaporator.
4.7 Soxhlet fat extraction unit.
4.8 Oilseeds pulverizer and grinder.
5 Analytical Procedures
5.1 Specimens’ preparation
5.1.1 Preparation of specimens of edible fat-oil
If the samples of edible fat-oil are in the liquid state and are clarified liquid, then they
may be sampled directly after dully mixed up; otherwise, they shall be treated by
impurity removal and dehydration. If the samples of edible fat-oil are in the solid state,
then they shall be prepared as specified in Annex B. If the samples are edible fat-oil
processed by emulsification, then they are prepared as specified in Annex C.
5.1.2 Preparation of specimens of oilseeds
Firstly, use a pulverizer or grinder to crush oilseeds into uniform fine particles. the
oilseeds of high brittleness (such as soybean, sunflower seed, cottonseed, rapeseed
and so on) shall be crushed to particles of grain diameter 0.8 mm ~ 3 mm or even finer;
while the oilseeds of low brittleness (such as copra, palm kernel and so on) s...
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| Standard ID | GB 5009.229-2016 (GB5009.229-2016) | | Description (Translated English) | National Food Safety Standard -- Determination of Acid Value in Foods | | Sector / Industry | National Standard | | Classification of Chinese Standard | X09 | | Word Count Estimation | 15,121 | | Date of Issue | 2016-08-31 | | Date of Implementation | 2017-03-01 | | Older Standard (superseded by this standard) | GB/T 5530-2005; GB/T 5009.77-2003; GB/T 5009.56-2003; GB/T 5009.44-2003; GB/T 5009.37-2003; GB/T 15689-2008; GB/T 14489.3-1993 | | Regulation (derived from) | Announcement of the State Administration of Public Health and Family Planning 2016 No.11 |
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