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GB 5009.266-2016 English PDF (GB5009.266-2016)

GB 5009.266-2016 English PDF (GB5009.266-2016)

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GB 5009.266-2016: Analytical methods of wine and fruit wine

This method specifies the determination method of methanol in alcohol, distilled wine, prepared wine and fermented wine. This method is applicable to the determination of methanol in alcohol, distilled wine, prepared wine and fermented wine.
GB 5009.266-2016
GB
NATIONAL STANDARD OF
THE PEOPLE REPUBLIC OF CHINA
National Food Safety Standard ?€?
Determination of methanol in food stuffs
ISSUED ON. DECEMBER 23, 2016
IMPLEMENTED ON. JUNE 23, 2017
Issued by. National Health and Family Planning Commission of the
People 's Republic of China;
State Administration of Food and Drug Administration.
3. No action is required - Full-copy of this standard will be automatically & immediately delivered to your EMAIL address in 0~60 minutes.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Principle... 4
3 Reagents and materials ... 4
4 Instruments and equipment ... 5
5 Analysis steps ... 5
6 Expression of analysis results ... 6
7 Precision... 7
8 Other ... 7
Annex A Methanol and internal standard tert-amyl alcohol standard gas
chromatogram ... 8
National Food Safety Standard ?€?
Determination of methanol in food stuffs
1 Scope
This method specifies the determination method of methanol in alcohol,
distilled wine, prepared wine and fermented wine.
This method is applicable to the determination of methanol in alcohol, distilled wine, prepared wine and fermented wine.
2 Principle
The distillation removes fermented wine and non-volatile substances in its prepared wine. Add into internal standard (alcohol, distilled wine as well as its prepared wine can be directly added into the internal standard). Separate through gas chromatography. Use hydrogen flame ionization detector to
detect. Determine its nature according to retention time. Quantify it according to the external standard method.
3 Reagents and materials
Unless otherwise stated, the reagents used in this method are of analytical grade and water is grade-two water specified in GB/T 6682.
3.1 Reagent
Ethanol (C2H6O). chromatographic pure
3.2 Preparation of reagent
Ethanol solution (40%, volume fraction). weigh 40 mL of ethanol; use water to set volume to 100 mL; mix evenly.
3.3 Standard sample
3.3.1 Methanol (CH4O, CAS number. 67-56-1). purity ???99%; or standard
substances that are certified by the State and are awarded to the standard substance certificate.
3.3.2 Tert-amyl alcohol (C5H12O, CAS number. 75-85-4). purity ???99%.
The reference conditions for instrument are listed as follows.
a) chromatographic column. polyethylene glycol quartz capillary column; column length is 60 m; inner diameter is 0.25 mm; film thickness is 0.25 ??m; or equivalent column;
b) chromatographic column temperature. initial temperature is 40??C;
maintain for 1 min; rise to 130??C at 4.0??C /min, to 200??C at 20??C/min
then maintain for 5 min;
c) detector temperature. 250??C;
d) inlet temperature. 250??C;
e) carrier gas flow. 1.0 mL/min;
f) injection volume. 1.0 ??L;
g) split ratio. 20.1.
5.3 Standard curve making
Respectively pipet 10 mL of methanol series of standard working solutions into 5 test tubes. Then add 0.10 mL of tert-amyl alcohol standard solution. Evenly mix. Determine the methanol and internal standard tert-amyl alcohol peak areas. Take concentration of methanol series standard working
solutions as abscissa, the ratio of methanol to tert-amyl alcohol peak area as ordinate to draw a standard curve (see Figure A.1 for methanol and internal standard tert-amyl alcohol standard gas chromatogram).
5.4 Determination of sample solution
Pour the prepared sample solution into a gas chromatograph. Determine its nature according to retention time. Meanwhile, record the ratio of methanol to tert-amyl alcohol peak area. Obtain the methanol concentration in the solution for test according to the standard curve.
6 Expression of analysis results
6.1 Calculate the content of methanol in the sample according to equation (1).
where,
X - content of methanol in sample, in milligrams per liter (mg/L);

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