GB 5009.225-2016 English PDF

Delivery: 3 seconds. Download true-PDF + Invoice.
Get Quotation: Click GB 5009.225-2016 (Self-service in 1-minute)
Historical versions (Master-website): GB 5009.225-2016
Preview True-PDF (Reload/Scroll-down if blank)

GB 5009.225-2016: National Food Safety Standard -- Determination of ethanol concentration
GB 5009.225-2016
Method for analysis of hygienic standard of distilled wines and mixed wines
National Standards of People's Republic of China
National Food Safety Standard
Determination of the concentration of ethanol in wine
Issued on. 2016-08-31
2017-03-01 implementation
People's Republic of China
National Health and Family Planning Commission released
Foreword
This standard replaces GB/T 5009.48-2003 "distilled liquor and wine analysis method of preparation hygiene standards", GB/T 394.2-2008 "wine
Proficient with analysis method ", GB/T 4928-2008" beer analysis method ", GB/T 15038-2006" wine, wine party general analysis
Method ", GB/T 10345-2007" Liquor analysis method ", GB/T 13662-2008" wine ", GB/T 11856-2008" brandy "
GB/T 11857-2008 "whiskey", GB/T 11858-2008 "vodka (Vodka)" a total of nine national standards related to alcohol content
test methods.
This standard compared with GB/T 5009.48-2003, main changes are as follows.
--- Standard name was changed to "national food safety standards for determining the concentration of ethanol in wine";
--- Modify the scope of the standard;
--- Increasing the density bottle method, gas chromatography and digital density meter method.
National Food Safety Standard
Determination of the concentration of ethanol in wine
1 Scope
This standard specifies the method for determination of alcohol, distilled spirits, and the preparation of fermented wine alcohol content.
This standard applies to alcohol, distilled spirits, wine fermented and determination of alcohol formulation. Wherein. the first method is suitable for distillation density bottle method
Wine, wine fermented and formulated the second law alcohol count method is suitable for the alcohol and distilled spirits, and the preparation of fermented wine (except beers), the third gas chromatography method
Spectroscopy applied to wine, wine and beer, a fourth method of digital density meter method is suitable for beer, brandy, whiskey and vodka.
The first method density bottle method
Principle 2
To distillation to remove non-volatile substances in the sample, with density bottle method to measure the density of the sample at 20 ℃ (aqueous ethanol), check the appendix
A, obtained at 20 ℃, the volume fraction of ethanol content, namely alcohol.
3 instruments and equipment
3.1 Analysis of balance. a sense of the amount of 0.0001g.
3.2 all-glass distillation. 500mL.
3.3 constant temperature water bath. Temperature accuracy ± 0.1 ℃.
3.4 a thermometer density bottles. 25mL or 50mL.
Step 4 Analysis
4.1 Sample Preparation
4.1.1 distilled spirits, wine fermented and formulated sample preparation (not including beer and sparkling wine)
With a clean, dry 100mL volumetric flask, accurately it weighed sample (liquid temperature of 20 deg.] C) in 100mL 500mL distillation flask, with
50mL water rinse three times a volumetric flask, 500mL lotion into the distillation flask, add a few zeolite (or glass beads), serpentine condenser connected to
Samples are taken for the receiver (external ice bath) with original volumetric flask, open cooling water (cooling water temperature should be less than 15 ℃), slowly heated distillation, collecting distillate
A liquid. When approaching the mark, remove the flask, stoppered, for 30min at 20 ℃ water bath, supplemented with water to volume, mix and set aside.
4.1.2 Sample Preparation beer and sparkling wine
4.1.2.1 Samples removing carbon dioxide
To ensure a representative sample, no loss or less loss of alcohol under the premise, with shaking, stirring or ultrasound, etc. to remove the wine samples
Carbon dioxide gas. There are two ways to remove carbon dioxide sample.
a) The first method. the wine thermostat to 15 ℃ ~ 20 ℃ about 300mL sample is poured into 1000mL Erlenmeyer flask, add rubber stopper, in a thermostat
Indoors, gently shake, Kayseri deflated (began to "pop" sound), the cover plug. Repeatedly, until gas evolution ceased. Single layer
The quick-drying paper (funnel above the surface of the cover glass) and filtered.
b) The second method. using ultrasonic or magnetic stirring method degassing the wine thermostat to 15 ℃ ~ 20 ℃ about 300mL sample moved with exhaust
Stoppered bottle and placed in an ultrasonic tank (or stirrer), ultrasound (or stirred) a certain time, with a single layer of filter paper over Sugan
Filter (upper surface of the cover glass funnel).
NOTE. To determine the results were similar to the first method by comparison to alcohol to determine if ultrasound (or stirring) time and temperature.
After the removal of carbon dioxide samples, collected in a stoppered Erlenmeyer flask, the temperature was maintained at 15 ℃ ~ 20 ℃, sealed, confined within 2h
use.
4.1.2.2 Samples distillation
With 4.1.1.
4.2 Determination of the sample solution
4.2.1 Wash and dried density bottles with thermometer and the side escutcheon weighing. Repeat the drying and weighing until a constant weight (m).
4.2.2 Remove the stopper with a thermometer, cooling to 15 ℃ boiled water column is full of constant weight density bottle cork plug with thermometer
(Bottle not have bubbles), immediately immersed in a constant temperature bath 20.0 ℃ ± 0.1 ℃, the temperature of the contents to be up to 20 deg.] C and kept constant 20min
After quickly with filter paper to absorb the liquid overflow pipe side, so that the liquid surface and the side of the side tube and Tube flush immediately cover the side of the hole cover, remove the density bottle with
Dry filter paper outer wall of the bottle of liquid water, and immediately weighed (m1).
The water poured out, first with ethanol, and then rinsed with ether density bottles, dry (or drying in an oven), using a sample of distillate repeatedly washed tight
Bottle of 3 to 5 times, and then filled. 4.2.2 Operation according weighed (m2).
5 expression analysis
Sample density (ρ2020) 20 ℃ according to formula (1) to calculate the air buoyancy correction value (A) according to equation (2).
ρ2020 = ρ0 ×
m2-m A
m1-m A
(1)
A = ρu ×
m1-m
997.0
(2)
Where.
ρ2020 --- density of the sample at 20 ℃, in units of grams per liter (g/L);
When distilled water density ρ0 --- 20 ℃ (998.20g/L);
Quality, unit m2 --- 20 ℃ when the density of the sample bottles and grams (g);
Mass m --- density bottles in grams (g);
A --- air buoyancy correction;
m1 --- 20 ℃ when the mass density of the bottle with water, in grams (g);
ρu --- dry air at 20 ℃, when the density 1013.25hPa (≈1.2g/L);
997.0 --- the difference between distilled water at 20 ℃ and dry air density values in grams per liter (g/L).
Ρ2020 according to the density of the sample, check Appendix A, to obtain alcohol by volume fraction "% vol" representation.
The arithmetic mean of two under the same condition of independent determination results indicated that the results of reservations to one decimal place.
6 precision
Two independent determination results of the absolute difference between beer samples under the repeatability condition must not exceed 0.1% vol; other sample weight
Two independent determination results under the absolute difference between refolding conditions must not exceed 0.5% vol.
The second method alcohol meter method
Principle 7
To distillation to remove non-volatile substances in the sample, as measured by alcohol alcohol volume fraction of indication, in accordance with Appendix B for temperature correction, seeking
The volume fraction of ethanol content was at 20 ℃, is alcohol.
8 instruments and equipment
8.1 Alcohol meter precision. Indexing is 0.1% vol.
8.2 all-glass distillation. 500mL, 1000mL.
9 analysis step
9.1 Sample Preparation
9.1.1 distilled spirits
With 4.1.1.
9.1.2 Alcohol
With a clean, dry flask of 100mL, 100mL sample is accurately weighed, set aside.
9.1.3 fermented wine (not including beer) and mixed wines
With a clean, dry 200mL volumetric flask, accurately weighed 200mL (specific sample volume requirements should decrease alcohol meter) sample (liquid
Temperature 20 ℃) or in 1000mL 500mL distillation flask, the following actions with 4.1.1.
9.2 Determination of the sample solution
9.2.1 Alcohol and distilled spirits
The sample solution (9.1.1) or alcohol (9.1.2) into a clean, dry 100mL graduated cylinder and allowed to stand for several minutes, until the bubbles disappear wine,
Into a clean, dry alcohol meter, then gently press, should not touch the cylinder wall, while inserting a thermometer, a balance of about 5min, the level of observation,
Reads the meniscus cut indication of the scale, and record the temperature.
9.2.2 fermented wine (not including beer) and mixed wines
The sample solution (9.1.3) into a clean, dry 200mL measuring cylinder and allowed to stand for a few minutes, until the wine bubble disappears, into a clean, wipe
Dry alcohol meter, then gently press, should not touch the cylinder wall, while inserting a thermometer, a balance of about 5min, the level of observation, reading and meniscus
Scale indication tangent at the same time record temperature.
10 analysis results presentation
According to the measured alcohol meter indication and temperature, check Appendix B, converted to alcohol at 20 ℃ sample volume fraction "% vol" representation.
The arithmetic mean of two under the same condition of independent determination results indicated that the results of reservations to one decimal place.
11 Precision
Two independent determination results under the absolute difference in repeatability condition must not exceed 0.5% vol.
The third method gas chromatography
Principle 12
When the sample into the gas chromatograph column, due to the different gas-solid adsorption coefficient, leaving ethanol and other components can be divided
From using a flame ionization detector to detect and control standards, based on retention time qualitative and quantitative use of an internal standard.
13 Reagents and materials
Unless otherwise indicated, the methods used were of analytical grade reagents and water as a water GB/T 6682 regulations.
13.1 Standards
13.1.1 ethanol (C2H6O). purity ≥99.0%.
13.1.2 butanol [CH3 (CH2) 3OH]. purity ≥99.0%.
13.1.3 4-methyl-2-pentanol (C6H14O). purity ≥99.0%.
13.2 Standard Solution
Ethanol series of standard working solution. take five 100mL flask were sucked 2.00mL, 3.00mL, 4.00mL, 5.00mL, 7.00mL
Ethanol with water to volume, and mix the solution for the standard curve.
14 instruments and equipment
14.1 Gas chromatograph. with hydrogen flame ionization detector (FID).
14.2 GC column. stationary phase Chromosorb103,177μm (80 mesh) ~ 250μm (60 mesh) (2m × 2mm or 3m ×
Other columns 3mm) or with an equivalent effect analysis.
15 analysis steps
15.1 Sample Preparation
15.1.1 Beer
Beer samples taken 10.0mL removing carbon dioxide (4.1.2.1) in 10mL volumetric flask, 0.50mL internal standard was added n-butanol,
Mix well.
15.1.2 Wine
Take wine distillate (4.1.1) and accurately diluted 4-fold (or appropriate dilution according to alcohol), and then draw a diluted sample 10.0mL
Goods in 10mL flask, add 0.20mL internal standard 4-methyl-2-pentanol, and mix.
15.2 Instrument Reference conditions
15.2.1 Column temperature.200 ℃.
15.2.2 gasification chamber and detector temperature. 240 ℃.
15.2.3 carrier gas (high purity nitrogen) flow rate. 40mL/min.
15.2.4 hydrogen flow rate. 40mL/min.
15.2.5 Air flow. 500mL/min.
15.2.6 Injection volume. 1.0μL.
Note. according to the different instruments, through experiments to select the best chromatographic conditions to make ethanol and the internal standard component get completely separated.
15.3 standard curve
Pipette different concentrations of ethanol series of standard working solution (13.2) each 10.0mL in five 10mL volumetric flask, were added
0.50mL butanol (beer analysis) or 0.20mL4- methyl-2-ol (wine analysis) and mix. 15.2 according to the chromatographic conditions,
Ethanol concentration as abscissa, a ratio of ethanol and the internal standard peak area (or peak height ratio) as the ordinate, drawing working curve.
Note. The use of ethanol standard solution should be formulated with the use of day, do at least twice each concentration, averaging plotted or calculated.
15.4 Determination of the sample solution
15.2 instrument in accordance with the reference conditions, the sample solution is injected into the gas chromatograph, the ratio of the sample to obtain ethanol and the internal standard peak area,
Ethanol concentration of the test solution is calculated from the standard curve.
16 analysis results presentation
Ethanol content of the sample according to equation (3) Calculated.
X = C × f (3)
Where.
X --- sample content of ethanol, volume fraction (% vol) representation;
Liquid content of ethanol in C --- sample measurement, volume fraction (% vol) representation;
f --- test solution dilution.
The arithmetic mean of two under the same condition of independent determination results indicated that the results of reservations to one decimal place.
17 Precision
Two independent determination results of the absolute difference between beer samples under the repeatability condition must not exceed 0.1% vol; other sample weight
Two independent determination results under the absolute difference between refolding conditions must not exceed 0.5% vol.
The fourth method of digital density meter method
Principle 18
The sample was poured into the U-shaped tube through at 20 ℃ compared with two standard density determined as frequency, calculate the sample in
20 ℃, the volume fraction of ethanol content, namely alcohol.
19 instruments and equipment
19.1 digital density meter.
19.2 constant temperature water bath. temperature control accuracy of ± 0.02 ℃.
19.3 syringe. 10mL.
20 analysis steps
20.1 Sample Preparation
20.1.1 brandy, whiskey and vodka sample preparation
With 4.1.1.
20.1.2 Beer Sample Preparation
With 4.1.2.
20.2 Instrument Calibration (calibration can be carried out according to the respective manufacturer's instructions)
In (20.00 ± 0.02) ℃ observe and record the U-shaped tube (clean, dry) "T" value in the air. Syringe with the upper end of the U-shaped tube
Even at the mouth of pla...