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GB/T 14454.13-2008 English PDF (GBT14454.13-2008)

GB/T 14454.13-2008 English PDF (GBT14454.13-2008)

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GB/T 14454.13-2008: Fragrance/Flavor substances -- Determination of carbonyl value and carbonyl compounds content
GB/T 14454.13-2008
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.100.60
Y 41
Replacing GB/T 14454.13-1993, GB/T 14454.16~14454.17-1993
Fragrance/Flavor substances - Determination of
carbonyl value and carbonyl compounds content
(ISO 1271:1983, Essential oils - Determination of carbonyl value - Free
hydroxylamine method; ISO 1279:1996, Essential oils - Determination of carbonyl
value - Potentiometric methods using hydroxylammonium chloride, MOD)
ISSUED ON: JULY 15, 2008
IMPLEMENTED ON: NOVEMBER 01, 2008
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine of the PRC;
Standardization Administration of the PRC.
Table of Contents
Foreword ... 3 
1 Scope ... 5 
2 Normative references ... 6 
3 Terms and definitions ... 6 
4 Method of cold oximation with hydroxylammonium chloride ... 6 
5 Method of hot oximation with hydroxylammonium chloride ... 9 
6 Test report ... 11 
7 Principle ... 11 
8 Reagents ... 11 
9 Apparatus ... 12 
10 Operating procedure ... 12 
11 Expression of results ... 13 
12 Test report... 14 
13 Principle ... 15 
14 Reagents ... 15 
15 Apparatus ... 15 
16 Operating procedure ... 15 
17 Expression of results ... 16 
18 Test report... 17 
Annex A (Normative) Operating procedure for determination of strongly colored
fragrance/flavor substances ... 18 
Annex B (Informative) Molecular weight and reaction time of some carbonyl
compounds ... 19 
Fragrance/Flavor substances - Determination of
carbonyl value and carbonyl compounds content
1 Scope
Method I of this Part of GB/T 14454 specifies the method for determination of
the carbonyl value of essential oils and the carbonyl compounds content in
isolated and synthetic fragrance/flavor substances using hydroxylammonium
chloride.
A cold oximation reaction with hydroxylammonium chloride of this method
applies to fragrance/flavor substances whose main constituents are easily
oximable aldehydes and ketones, with the exception of citronellal which needs
a low temperature to avoid cyclization phenomena and acetalization. A hot
oximation reaction with hydroxylammonium chloride applies to fragrance/flavor
substances whose main constituents are ketones which are in general oximable
only with difficulty.
Note 1: For the determination of essential oil containing citronellal, use free hydroxylamine
method. See Method II.
Note 2: Examples of essential oils concerned containing oximable aldehydes or ketones
are lemongrass, hesperydus and rue oils.
Note 3: Examples of essential oils concerned are vetiver, Dalmation sage and white
artemisia oils which contain methylketones oximable only with difficulty.
Method II of this Part of GB/T 14454 specifies the method for determination of
the carbonyl value of essential oils and the carbonyl compounds content in
isolated and synthetic fragrance/flavor substances using free hydroxylamine
method.
This method applies to fragrance/flavor substances which contain carbonyl
compounds (especially ketones, excluding methylketones) which are difficult to
convert to oximes by the method specified in Method I. The method is not
applicable to fragrance/flavor substances which contain substantial amounts of
esters or other alkali-sensitive constituents.
Method III of this Part of GB/T 14454 specifies the method for determination of
the carbonyl compounds content in fragrance/flavor substances using the
neutral sodium sulfite method. It is applicable to the determination of the content
of carbonyl compounds in aldehyde and certain ketone fragrance/flavor
Conversion of the carbonyl compounds to oximes by reaction with
hydroxylammonium chloride.
USE sodium hydroxide standard solution to titrate the hydrochloric acid
released by this reaction. [Translator note: “potassium hydroxide standard
solution”?]
4.2 Reagents
The reagents used are all analytically pure reagents. The water is distilled water
or water of equivalent purity. Unless otherwise specified, the preparation
method shall be carried out in accordance with GB/T 14454.14.
4.2.1 Sodium hydroxide standard solution, c(KOH)=0.5 mol/L.
4.2.2 Bromophenol blue indicator solution.
4.2.3 Hydroxylammonium chloride solution.
4.3 Apparatus
Usual laboratory equipment and, in particular, the following.
4.3.1 Beaker, of capacity 100 mL, tall form.
4.3.2 Conical flask, of capacity 250 mL.
4.3.3 pH meter.
4.3.4 Glass electrode.
4.3.5 Burette, with a capacity of 50 mL and a scale of 0.1 mL.
4.4 Operating procedure
4.4.1 Preparation of test sample
According to the requirements of GB/T 14454.1.
4.4.2 Test portion
WEIGH 1 g~1.5 g of fragrance/flavor substance in a tall-form beaker (4.3.1) or
conical flask (4.3.2), accurate to 0.0002 g.
Note: If the test sample should be larger, this will be stated in the appropriate product
standard for the fragrance/flavor substance concerned.
4.4.3 Determination
The meanings of V, c, and m are the same as formula (1).
The tolerance of the parallel test results:
1.0 for the carbonyl value; 0.5% for the carbonyl compounds content.
5 Method of hot oximation with hydroxylammonium
chloride
5.1 Principle
Conversion of the carbonyl compounds to oximes by reaction with
hydroxylammonium chloride.
USE sodium hydroxide solution to titrate the hydrochloric acid released by this
reaction. [Translator note: “potassium hydroxide standard solution”?]
5.2 Reagents
Same as 4.2.
5.3 Apparatus
Usual laboratory equipment and, in particular, the following.
5.3.1 Burette, with a capacity of 50 mL and a scale of 0.1 mL.
5.3.2 Beaker, of capacity 100 mL, tall form.
5.3.3 Saponification bottle, made of alkali-resistant glass, with frosted bottle
mouth. The capacity is 100 mL~250 mL. It is fitted with a frosted-mouth glass
air condenser with a length of at least 1 m and an inner diameter of 1 cm~1.5
cm.
5.3.4 pH meter.
5.3.5 Glass electrode.
5.3.6 Heater with magnetic stirrer.
5.4 Operating procedure
5.4.1 Preparation of test sample
According to the requirements of GB/T 14454.1.
5.4.2 Test portion
WEIGH 2 g~2.5 g of fragrance/flavor substance into the saponification bottle
(5.3.3), accurate to 0.0002 g. See the note to 4.4.2.
5.4.3 Determination
ADD 50 mL of hydroxylammonium chloride solution (4.2.3) to the test portion
(5.4.2). ADD 3 drops of bromophenol blue indicator solution (4.2.2) and mix
thoroughly. USE sodium hydroxide standard solution (4.2.1) to titrate to the
same yellow-green color as hydroxylammonium chloride solution (4.2.3).
Connect the saponification bottle to the reflux tube. PUT the saponification
bottle on the heater (5.3.6) and heat with stirring, to make the temperature
appropriate enough to maintain a constant reflux. After 10 min, cool, add 3
drops of bromophenol blue indicator solution (4.2.2); USE sodium hydroxide
standard solution (4.2.1) to titrate slowly to the same yellow-green color as
hydroxylammonium chloride solution (4.2.3). PUT the saponification bottle on
the heater. REPEAT this operation every 10 min, until the sodium hydroxide
standard solution added can ensure that the end of the titration has been
reached.
Note 1: When the color of the sample is dark, or its own color may interfere with the
judgment of the end point, the potentiometric titration method shall be used. ADD
50 mL of hydroxylammonium chloride solution (4.2.3) to the test port...
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