concept:
1. Alcoholic beverages: Alcoholic beverages with a capacity of more than 0.5% by volume are called alcoholic beverages.
2. Liquor: Liquor is a distilled liquor made from sorghum and other grains as the main raw material, with Daqu and Xiaoqu as the saccharification starter, which is cooked, saccharified, fermented, distilled, aged and blended. It is a food for people to drink directly. Drinking in moderation will not cause harm to human health.
According to the fragrance type, the following are mainly the following five types:
1 Luzhou-flavor liquor (distilled liquor with grain-based raw material, solid-state fermentation, storage and blending, with a complex aroma of ethyl hexanoate as the main compound)
2 Qingxiang-type white spirits (distilled liquor with a complex aroma of ethyl acetate as the main raw material, which is made by saccharification, fermentation, storage and blending)
3 meters of fragrant white wine (distilled rice made from rice as a raw material, semi-solid fermentation, distillation, storage, blending, with the characteristics of small rice scent)
4 sauce-flavored liquor (distilled liquor with sorghum and wheat as raw materials, fermented, distilled, stored, blended, and characterized by sauce)
5 fragrant white wine (made from grain as the main raw material, fermented, stored, blended and brewed, distilled liquor with a strong flavor and unique flavor of sauce).
According to the production process, the following two types are used:
1 solid-state liquor (using grain as raw material, solid fermentation, storage and blending of wine cellar, solid-state liquor is rich in aroma, soft in taste, sweet and refreshing, long aftertaste)
2 liquid method white wine (grain, potato, molasses, etc. as the main raw material, the edible alcohol obtained by liquid fermentation and distillation is the wine base, and then the scented and blended white wine. The liquid method white liquor generally has no solid liquor. So good aroma and taste). Regardless of the type of liquor, regardless of the raw materials, craftsmanship, and fragrance type, and regardless of the implementation of national standards, standards or corporate standards, as long as it is a liquor, it must comply with the mandatory national standard GB2757-1981 "Standards for distilled spirits and formulated wines" Requirements.
3. The testing items of liquor are generally: alcohol, total acid, total ester, ethyl hexanoate or ethyl acetate (according to the fragrance and standard), solids, methanol, fusel oil, lead, manganese, sodium saccharin And other indicators.
The alcohol content, also known as alcohol content, is one of the important physical and chemical indicators of liquor. It refers to the number of milliliters of ethanol (alcohol) in 100 ml of white liquor at 20 ° C, that is, the percentage of volume (capacity). Usually 40° is used as the dividing line, and below 40° is called low-alcohol.
Various liquor testing and inspection basis:
- GB 10781.1—89 “Luzhou-flavor liquorâ€
- GB 10781.2 - 89 "Flavour-flavor liquor"
- GB 10781.3—89 “Milent-flavor liquorâ€
- GB 11859.1---89 "Low-flavored liquor"
- GB 11859.2—89 “Low Fragrance Liquorâ€
- GB 11859.3—89 Low-grade rice-flavor liquor
- GB/T 14867---94 "Fengxiang Liquor"
- QB 1498—92 Liquid Liquor
- GB 2757-81 "Sanitary Standards for Distilled Liquor and Blended Wine"
- GB 10344 89 "Drinking Wine Labeling Standard"
- GB 8951-88 "White Wine Factory Hygienic Specifications"
- GB 5009.48——85 “Analysis method for hygienic standard of distilled liquor and prepared wineâ€
- GB 2760---1996 "Sanitary Standards for the Use of Food Additives"
- QB/T 2305 - 97 "Special Flavor Liquor"
- GB/T 16289---1996 "Muxiang Liquor"
- QB/T 2187 - 95 "Sesame-flavor liquor"
- GB 10343——89 Edible Alcohol
- GB 10345.1—8---89 “Test Method for Liquorâ€
- GB 10346-89 "Liquor Inspection Rules"
- GB/T 349, 2 - 94 "General Test Method for Alcohol"
Method for testing some indicators of liquor:
- Sensory, alcohol, total acid, total ester, ethyl hexanoate and solids were tested according to the method specified in GB/T10345.
- Test method for n-propanol (gas chromatography)
Method summary: After the sample is vaporized, it enters the column along with the carrier gas, and the components to be measured have different partition coefficients in the gas-liquid two phases, and the difference in migration velocity is formed in the column to be separated. The separated components flow out of the column and enter the hydrogen flame ionization detector. The samples are qualitatively compared with the standard values ​​according to the peak values ​​of the peaks on the chromatogram; the peak area (or peak height) is used to quantify by internal standard method. .
Instruments and materials:
1 Gas chromatograph: equipped with a hydrogen flame ionization detector (FID).
2 Column: PEG20M cross-linked quartz capillary column, column length 25m ~ 30m, column inner diameter 0.25mm, or other columns with the same analytical effect.
3 micro syringes 10 μL.
Reagents and solutions:
1 Ethanol: Chromatographically pure (or equivalent purity). Formulated as a 60% aqueous solution of ethanol.
2 n-propanol: chromatographically pure. Used as a standard. 2% solution (formulated with 60% aqueous ethanol).
3 n-amyl acetate: chromatographically pure. Used as an internal standard. 2% solution (formulated with 60% aqueous ethanol).
Chromatographic conditions:
Carrier gas (high purity nitrogen)
Flow rate: (0.5 to 1.0) mL/min.
Split ratio: about 37:1, tail blowing about (20 ~ 30) mL / min.
Hydrogen flow rate: 33 mL/min.
Air flow rate: 400 mL/min.
Detector temperature: 220 °C.
Injector temperature: 200 ° C.
Column temperature: starting temperature 60 ° C, constant temperature 5 min, program temperature to 180 ° C at 3.5 ° C / min, continue to maintain a constant temperature of 10 min.
The chromatographic conditions of the carrier gas, hydrogen, and air flow rate vary from instrument to instrument. The best operating conditions should be selected by experiment, and the internal standard peak and other component peaks in the wine sample should be completely separated.
Determination of correction factor (f value): Pipette 1.00mL of 2% n-propanol standard solution, transfer to a 100mL volumetric flask, then add 2% n-amyl acetate internal standard solution 1.00mL, dilute to the mark with 60% ethanol solution . The concentrations of n-propanol and internal standard in the above solution were both 0.02% (V/V). After the baseline of the chromatograph is stable, inject it with a micro-injector, the amount of injection depends on the sensitivity of the instrument. The retention time of the n-propanol and the internal standard peak and its peak area (or peak height) were recorded, and the relative correction factors of n-propanol were calculated using the ratio. The relative correction factor f of n-propanol is calculated as (A1).
f=(A1/A2)×(d1/d2)........................(A1)
Where: f—the relative correction factor of n-propanol;
A1———the peak area of ​​the internal standard when the standard f value is measured;
A2—the peak area of ​​n-propanol when the standard f value is determined;
D1—the relative density of the internal standard;
D2—the relative density of n-propanol.
The results are retained to two decimal places.
Determination of the sample: Pipette 10.0mL of wine sample into a 10mL volumetric flask, add 2% internal standard solution 0.20mL, mix, and then inject under the same conditions as f value determination, determine n-propanol according to retention time The position of the peak, and the area of ​​the n-propanol and the internal standard peak (or peak height) were determined, and the ratio of the peak area (or peak height) was determined, and the ratio of n-propanol in the wine sample was calculated by the ratio. The content of n-propanol in the wine sample is calculated according to formula (A2).
X=f×(A3/A4)×0.352........................(A2)
Where: X—the content of n-propanol in the sample, g/L;
f——-relative correction factor of n-propanol;
A3—the peak area of ​​n-propanol in the wine sample;
A4—the area of ​​the peak added to the internal standard in the wine sample;
0.352———The amount of internal standard added to the wine sample, g/L.
The results are retained to two decimal places. Allowable difference of results: The difference between the two measured values ​​of the same sample shall not exceed 10% of the average value.
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