This standard specifies the determination method of diaminotoluene in composite food packaging bags. This standard is applicable to the determination of diaminotoluene in composite food packaging bags. The detection limit of this method is 0.002mg/L. GB/T 5009.119-2003 Determination of diaminotoluene in composite food packaging bags GB/T5009.119-2003 Standard download decompression password: www.bzxz.net

H3 67.040
National Standard of the People's Republic of China
GE/T5009.f19---2003
Agency GBT14937--1994
Determination of diaminomethylbezen ofcomplex for foud packaging material2003-08-11 Issued
Ministry of Health of the People's Republic of China
China National Standardization Administration
2004-01-01Implementation
GB/T5009.119—2003
This standard replaces GH/T14937--1994 Determination of diaminomethylbezen ofcomplex for foud packaging material Method 2. Compared with GB/T14937-1954, this standard has the following main effects: the Chinese name of the standard has been revised, and the Chinese name of the standard has been changed to Determination of diaminotoluene content in composite food packaging; the original standard has been revised according to G/T21001.1-2010 Standard Part 1: Chemical analysis method.
This standard is proposed by the Ministry of the People's Republic of China and is under the jurisdiction of the Ministry of Food and Drug Administration of the People's Republic of China. The drafting units of this standard are: Ningxia Food Hygiene Supervision and Inspection Institute, Anshan Iron and Steel Health and Prevention Station, Shenyang Heping District Health and Epidemic Prevention Station, Shenyang Health Center,
Main drafters of the standard: Qiao Yongbei, Li Xueming, Wang Yiqiu, Zhang Weimin, Wu Zibiao: The original standard was first issued in 1994, and this is the first revision. 1 Scope
Current determination of diaminotoluene in food packaging
This standard stipulates the determination method of diaminotoluene in food packaging. This standard is applicable to the determination of diaminoformaldehyde in composite food packaging. The detection limit of this method is 3.002mg/..bZxz.net
2 Principle
GB/T5009.119-2003
After diaminoformaldehyde in the sample is drained with boiling water, it is cooled and then tris(2-hydroxy-1,2-dimethylformaldehyde)anhydride is added for biochemical reaction. Then the product is injected into the gas chromatograph and measured by an electron capture detector. The response value is proportional to the diazotole content within a certain concentration range, which is called qualitative and quantitative. 3 Reagents
3. T: methyl chloride.
3.2 sodium bicarbonate (purity 38):
3.3 anhydrous sulfuric acid.
3.4 ​​20x/[. Carbonic acid solution: weigh 3K sodium bicarbonate and add it to 100mT in distilled water..3.5 diaminobenzene (2.1-aminobenzene, purity 8%) standard preparation solution: accurately weigh 10mg (100.011ng) of 2.4-diaminobenzene and transfer it to a 1CC container, add dioxane to the scale, and the filtered milliliter contains 2.4 diaminobenzene*100B. Store in a container for later use.
4 4.1 Gas chromatograph: with electronic capture detector (E), 4.2 Constant temperature oven. 4.3 Concentrator (K-). 5 Analysis steps 5.1 Sampling method 10 samples should be collected for each batch. For small batches, the sampling should not be less than 10 (500mL/piece. If less than 500mL/piece, the sample holder should be added with a sample tray). One-third of the samples are for testing, one-third for re-testing, and the other third are kept for two months for arbitration analysis. The product name, batch number, and sampling date should be indicated. 5. 2 Sample preparation
5.2.1 For bags that have been packed with food: wash three times with distilled water. Calculate the amount of steamed water per 2ml./cm3. Heat seal. 5.2.2 For bags that have been packed with food: remove all food, rinse with clean water to remove dirt. Rinse with distilled water three times, calculate the amount of steamed water per 1ml./cm3. Heat seal. 5.2.3 Bag the bag after heat matching in 3.2.1 or 5.2.2, place in a constant humidity oven pre-adjusted to 10°C ±5 for 6 minutes, remove from the door and cool to room temperature. . Cut the seal and put the water into a beaker in an oven for later use. 5.3 Sample preparation
Take 5U.mL of each sample and place it in a separatory bucket. Use 10mL dichloromethane to extract twice. Extract 5mL each time, let stand for 1!mil, and then mix twice until the liquid is obtained. Pour paper under the bottom of the separatory bucket to remove the water in the benzene extract. Transfer the extract to a KD shrink tube and shrink it to about 2mL in 10mL water, or add 60L of anhydride cold, mix gently and place in a 30℃ oven with low leakage H
CB/T 5009.119—2003
Perform the derivatization inverse sequence for 30 minutes, take it out and let it cool to room temperature, then put it into a 60ml separatory funnel, add 2ml of two bottles of methane, wash the solution several times, and put it into the separatory funnel, add 5ml of 20g/L carbonic acid solution, stir gently for 2 minutes, and let it stand for 5 minutes. Transfer the chloroform layer into a 5ml colorimetric tube, add dichloromethane to make 5ml . For determination: 5.4 Standard curve drawing
5.4.12.4 Derivatization of diaminomethane: Take a certain amount of 2,4-diaminomethane standard stock solution, accurately dilute it with dichloromethane to a volume containing 0.1% of 2,4-diaminomethane, place 25.00mL of the working solution in a 60mL separatory tube, add 2C trioxygen anhydride, stir gently, and then place it at 30°C to obtain the derivatization reaction 3 0i, take out and cool to 100°C, add 10mL of 20/L sodium hydrogen ketone solution, gently stir for 2min, and let stand to separate. Pass the dimethylbenzene layer of 2,4-aminotoluene through a slurry funnel pre-loaded with about 5g of sodium hygrosulfate, collect the liquid, which is the standard working solution of 2,4-aminomethyl-dioxyacetic anhydride. The filter belt contains 2,4-dichloromethyl in 100mL. 1
5.4.2 According to the instrument Sensitivity, dilute the 2,4-dihydroformaldehyde-trichloroacetic anhydride standard working solution with dichloromethane according to different concentrations, extract 1L and put it into the gas chromatograph, connect it to the chromatographic record, and draw the standard curve of the reading height. 5.5 Determination
5.5.1 Chromatographic conditions
The color end is: fixed by 3×2m glass, 2% 0V-17, 60~80 mesh silica gel. Sample blue: 170 field fluidization temperature: 280, nitrogen gas, filter 40 positive/min,
Detector: electron capture detector,
Injection volume: 1L.
5.5.2 Determination
Absorb 1 test sample into the gas phase chromatograph and measure the peak quotient according to the colorimetric conditions in 5.5.1, and compare it with the standard curve for quantification.6 Calculation
Press or calculate:
Where:
X=XV.X100
3 The content of 2,4-diazotoluene in the sample, in milligrams per liter (mg/I).——The content of 2,4-dimethylbenzene in the standard curve, in micrograms per milliliter (ug/mL)V.—Test volume, in milliliters (mL)
V—Total volume of the sample, in milliliters
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