This standard specifies the analysis methods for various hygienic indicators of epoxy phenolic resin coatings on the inner wall of food cans. This standard is applicable to the analysis of various hygienic indicators of epoxy phenolic resin coatings on the inner wall of food cans. GB/T 5009.69-2003 Analysis methods for hygienic standards of epoxy phenolic resin coatings on the inner wall of food cans GB/T5009.69-2003 Standard download decompression password: www.bzxz.net

1CS G7. 04C
National Standard of the People's Republic of China
GB/T 5009.69—2003
HSS H/500S-1396
Method for analysis of hygienic slandard nf cpoxyphenolic coatings for inner wall of food cans Issued on August 11, 2003 Implemented on January 1, 2004 Ministry of Health of the People's Republic of China
National Standardization Administration of China
GH/1 5009.69—2003
This standard replaces GB/T 5009.69
JSS Method for analysis of hygienic standard for inner wall of food cans Compared with n/3009.6-1% S6, this standard mainly has the following features: According to (1T20001.42001 cup contraction rules part 4, chemical analysis method has been modified to the original standard structure.
This standard is proposed and regulated by the Ministry of Health of the People's Republic of China. This standard was drafted by the Food Fermentation Industry Research Institute of the Ministry of Light Industry, Shanghai Institute of Food Industry and Shanghai Municipal Health Commission.www.bzxz.net
This standard was issued in 1985 and revised for the first time. This is the second renewal. 528
1 Scope
Analysis method of hygienic standard for epoxy phenolic coating on the inner wall of food
This standard specifies the analysis method of various parameters of epoxy phenolic coating on the inner wall of food. This standard is used for the analysis of various parameters of phenolic additives in food. 2 Normative references
CB/T 5009.69—2003
The clauses in the following documents shall be the clauses of this standard through the date of the introduction of the standard. For any document with a date of introduction, all subsequent amendments (excluding those made incorrectly or taken inappropriately) shall be applicable to this standard. However, if the parties fail to reach an agreement based on this standard, the latest versions of these documents shall apply. GB48 Hygienic Standard for Film Materials Containing Auxiliary Products/5(GS: Polyethylene, containing oxadiazole, etc.) 3.1 When the same standard is issued, the packaging of the same standard shall be called a cargo group. If the number of packages is less than 0, it shall be called a cargo group. 3.2 Take the cargo group at random and conduct inspection. If the cargo is not 2 packages, two packages shall be arranged for inspection. 3.3 Take 7 photos (total 21 photos) at random on the upper, lower and lower parts of each package to be inspected. Goods: Bige certificate · Carry out soft change of miscellaneous materials, use chemical separation test and appearance inspection, keep 3 strong "pieces" in the appearance inspection sample, in order to prepare for other analysis.
4 Sensory control (including raw materials and type products) 41 Case material stock: golden white, uniform, after no immersion in simulated liquid, including normal · no white, falling off now cool, 4.2 Case root film no unique color, too different international temperature oil should comply with the provisions of GH4805
5 Test column treatment
5.1 Cut the Xu material into pieces, use fertilizer No. Apply the water-based powder to the surface of the whole body 5 times; brush the surface of the skin (especially the skin surface) back and forth 15 times, rinse with water for 1 minute, and then add water to clean it again, and then add 2ml of water per square meter according to the foaming amount.
5.2 Take 3 or 4 bottles of the same size, brush 5 times with water or soap powder, rinse with water, and then rinse with water, dry, add liquid (11-7r), cover well, add paper, and then seal it tightly, and then use a hard or glass container.
5 Wet foam parts
6.1h.95.3crn.
5.2Zn%c: m
6.32Acid 4%6.30i.
GB/T5009.69—2003
6.4N-hexane:37.2h
The above water content limit for foaming and analysis water shall not contain chlorine. Generally, add 1% free acid (1) to the water after adsorption of active iodine, and add half of it to the water for color analysis. 10 minutes of full development are ready for use. Physical and chemical test
7. 1 Free acid
. 1.1 Titration method (suitable for tree membrane)
7. 1. 1. 1 Principle
Combine iodine with phenol or triphenylmethane, and use the remaining iodine to precipitate out of the membrane. Therefore, the amount of sodium iodide that is dissolved in the membrane is calculated by the method of the above method: 7. 1, 1. 2 Test data
7. 1. 1. 2. 1 Hydrochloric acid,
7. 1. 1. 2.2
7.1,1.2.3 ethanol.
7.1.1.2.4 saturation rate.
7.1. 1.2.5 potassium hydroxide (3)1.
7.1.1.2.6 starch solution, weigh 0.5g of extrudable, carefully adjust to a constant temperature with water, then put in 10m. boiling water, to obtain
7..1.2.7 standard solution wave c172Br.) = .1 mol/1._.7.1.1.2.8 Sodium sulfide standard solution (m:S:0.) = .1mol/L7.:.1.3 Analysis step
Weigh about 1 liter of resin or epoxy resin (preferably freshly produced), steam it carefully, dissolve it in 20ml of fresh water), add 50ml of water and heat it for 5 minutes, and then add 300l--400aL of freshly steamed liquid sample in 4cm~tmin, fill it up with cold water: white precipitate, which proves that it has been heated up, and you can stop steaming, heat the liquid with water, wait for it to be fully heated, and set it aside.
Absorb 100mL of the distilled liquid in 500ml of a container, add 25ml, read the standard liquid (c, 11m/.ml. salt, place in a room temperature for 10min. into a chemical evaluation of 10℃/L), place in a dark place, add 1cm/., add 1:1ml. half-monocyanate, titrate with sodium monothiocarbate standard (U.1ml/L) until the color changes to a certain level, and the powder concentration is determined to be 1:1. The blue color is the end point. Dilute with ethanol to 500ml), then absorb the liquid for 30min (if the water level drops, use 100ml water for short test)
7. 1. 1. 2 Calculation of results
See formula 1):
X_VoXcxG.G15 sxju
The content of sodium thiosulfate in the sample is in grams per hundred. The unit is: sxju
The unit is grams per hundred. The unit is: sxju
The unit is grams per hundred. The unit is: The unit is: sxju
The unit is grams per hundred. The unit is: The unit is: sxju
The unit is grams per hundred. The unit is: The unit is: sxju
The unit is grams per hundred. The unit is: The unit is: sxju
The unit is grams per hundred. The unit is: The unit is: sxju
The unit is grams per hundred. The unit is: The unit is: sxju
The unit is grams per hundred. The unit is: sxju
The unit is: The unit is: sxju
The unit is: 5009.69—2503
The absolute difference between the results of the two independent determinations obtained under repeated conditions shall not exceed 5% of the arithmetic mean. 7.1.2 Colorimetric method (applicable to free ions in the solution): 7.1.2.1 Principle
Under the conditions of 9-10%> of the injection solution, 4-aminoantipyrine is reacted with potassium hydroxide to produce a full-color antipyrine dye. The depth of the dye is proportional to the color of the organic phase. The dye is then compared with the standard for quantitative analysis. 7.1.2.2 Reagents
7.1.2.2.1 Instantane (1-9)
1.1. 2.2.2 Standard sodium sulfoxide solution 4NS ()> = U.025 mol/L 7.1.2.2.3 Replacement of chemical solution: 2.78 g of sodium sulfoxide solution was collected and dissolved in water, and the solution was filtered by sieving. 7.1.2.2.4 7.1.2.2.5 Copper sulfoxide solution (1 cg/L)
4-Aqueous solution (%) can be stored in ice for a period of time, 7.1.2.2.6
7. 1.2. 2. 7
Aike chemical solution (acg/).
7.2.2.8 Flushing liquid (2H9.8): weigh 2nR oxidation pressure in 10m oxygen water, add 1 argon, 7. *. 2. 2. 9, 7.1.2.2.10 Drying and cleaning liquid: prepare as before. 7. 1. 2. 2. 11. 7. 1.2. 2. 1. Standard solvent: weigh 32~10ml of distilled water, add 000ml of water, and add water to the mixture until the mixture reaches the required concentration.
7.1.2.2.13 Micropipette 10 μm of the standard chain for determination, add 6 cm water, 13 ml filter shear liquid to stimulate it, then add 5 μm hydrochloric acid, plug it well, keep the standard line moving, at the same time take 1 μm. Do the blank test as above, use sodium thiosulfate standard solution (m/L) to titrate the blank and standard solution. When the liquid turns yellow, add 2 mL of the indicator liquid and the blue line disappears as the end point. Technical article (2) Calculate the content of the standard X= (V -V)X+215.GR
In the above formula:
Y——the volume of the standard titration liquid in the standard apparatus is grams per liter gW
Check the consumption of the standard titration bottle of sodium sulfoxide standard titration liquid, unit is milliliter (mL); the actual liquid content of the standard sodium sulfoxide standard titration liquid, unit is milliliters (mL); the calibration pressure is the standard volume of the standard liquid, unit is milliliters (mL): with 1.1. sodium sulfoxide N5(.)=333mn.. the mass of the standard titration liquid and the equivalent, unit is grams (M).
Based on the calculated amount of phenol, add 1/3L of the standard material to 1/3L of the standard material, dissolve it in 1000ml of water and add 1ml of pure oxygen, absorb 10.1L of the standard volume per bottle, add water until the phenol is diluted to the specified level. 7. 1.2. 3 Instruments
See spectrophotometer,
7.1.2.4, Analytical procedures
GD/T5009.69—2003
7.1.2.4.7 Preparation of standard curve
Pipette 0, 2.4.0, 8.0.12.0.16.C.22.0.33.Cml.* cup standard position (material is equivalent to 9.2.0, 4.0, 3.0.2, 11e.c.23.0.3 0.0g of this substance was divided into 253mL of 4, each into phenol water to 20ml. Each into 1ml of 4 groups of pyrrolidone (20/1) 1ml of rat chemical solution (8/1.), each adding 1:1 dose of each reagent to control the mixture, heat the stomach [min.] Add 1 nitrogen gas to obtain the probe? After standing for 5 minutes, the chloroform layer was diluted with aqueous sulfuric acid to replace the energy in a colorimetric cup, and the zero point was adjusted with a 2m colorimetric cup to zero, and the absorbance limit at 6m was drawn to draw the standard curve, 7. 1. 2. 4. 2 Determination
Take 250ml of sample solution, add 5g/1.5% sodium hydroxide (1g/1.2g) to the whole bottle until the solution is red. Then add a small amount of sodium hydroxide (1g/1.2g) to the 250ml sample solution or bottle. Pass the sodium hydroxide solution through the receiving tube and collect the solution until it reaches 2ml. Fill the receiving tube with 253L of reagent vacuum and perform the test.
Add 50ml of the above test solution to the test tube and add 100ml of the above test solution to the test tube. Then add 100ml of the above test solution to the test tube and compare it with the standard vacuum. .5 Calculation formula: (x1-xXsx2); (x2-xXsx2); (x3-xXsx2); (x4-xXsx2); (x5-xXsx2); (x6-xXsx2); (x7-xXsx2); (x8-xXsx2); (x9-xXsx2); and (x1-xXsx2); (x1-xXsx2); and (x7-xXsx2); and (x8-xXsx2); and (x9-xXsx2); and (x8-xXsx2); and (x9-xXsx2); and (x9-xXsx2); and (x9-xXsx2); and (x9-xXsx2); and (x9-xXsx2); and (x9-xXsx2); and (x9-xXsx2); and (x9-xXsx2); and (x9-xXsx2); and (x9-xXsx2); and (x9-xXsx2); and (x9-xXsx2); and (x9-xXsx2); and (x9-xXsx2); and (x9-xXsx2); and (x9-xXsx2); and (x9-xXsx2); and (x9-xXsx2); and (x9-xXsx2); and (x9-xXsx2); and (x9-xXsx2); and (x9-xXsx2); and
7.1.2.6 Precision
The absolute difference between the results of two modified tests obtained under repeated conditions shall not exceed 105 of the arithmetic half-tablet value. 7.2 Free formaldehyde
7.2.1 Principle
The whitening compound in the acid solution is a color compound, and the color is selected to be lighter than the content in the solution. The color is compared with the marked ratio. 7.2.5 Test
7.2.2.1 Comparison.
7.2.2.2 Acid (1-1):
7.2.2.3 Titanium hydroxide solution (40/1)
7.2.2.4 Sodium hydroxide solution (40/1)
7.2.2.5 Acid resistance (1-35)
7.2.2.6 Sulfuric acid (+359):
7.2.2.7 Prepare the precipitate solution (10g/L) before use. 7.2.2.8 Prepare the standard solution of mol/l (1/2I) = 0.1mol/l. 7.2.2.9 Prepare the standard solution of mol/l (0.1mol/l) GB/T5009.69—20C3
7.2.2.10 Chromotropic acid Take 0.3 chromotropic acid, add a little water, transfer to 1% 3% water in a bottle until it is dissolved, and then add 5% chromotropic acid to 10% 3% water. 7.2.2.11 Formaldehyde standard: absorb 1mmT, add 0.mL sulfur (+35) to 530mL bottle, add water to release. Filter spoon: collect 5tr:L, place in 259mL iodine plate bottle, draw 43l standard liquid (1ml/I! 15 oxidation hook powder (40%/1.). Weigh, add 3㎡l acid (1+1) [or 20L sulfur (1+35) to acidify, then put in the stomach for 10min~.15min, add 10umL water. Uniformly titrate with sodium thiosulfate (0.1 rl/1.3 mL). Add 1 M starch and continue titrating until the blue color disappears. At the same time, do a reagent blank test. The concentration of formaldehyde standard solution is according to the formula (): X=(V.-V)xex15
Wherein:
X—concentration of formaldehyde standard suspension, unit: /.); V, the volume of sodium thiosulfate standard titration solution consumed by the titration of the sample, unit: liter (m); V: the volume of sodium thiosulfate standard titration solution consumed by the sample, unit: μl = (mI), ∫ - actual content of the standard solution, expressed as volume per volume (vol/L): 1.0 ml - equivalent to 1.0 ml of the standard titration solution (1/21) - 1.0 mmol/L, expressed in grams (mR); 5. The volume of the standard solution used for the standardization is expressed in liters (vols). 7.2.2.12 Detailed description of the standard: Based on the calculated content above, reduce the standard aldehyde to 1 g aldehyde per liter. 7.2.3 Use a spectrophotometer. 7.2. 4 Analysis steps
7.2.4.1 Preparation of standard curve
Take 3.2.0.4.0.8.0.12.3.15.0.20.0.30.0ml of medium fermentation standard liquid equivalent to 3, 2.0, 4.0, 8.0.12.0, 15.0, 20.0, 3.8% fermentation, respectively, and put them into 200ml volumetric bottles, add water to each until cold, mix well, pipette 1) ... 7.2.4.2 Determination
Take 254 ml of water and mix it with the mixture. Place it in a 500L steamer and add 5 ml of aldehyde ([+35]) to the 200 or 250L volumetric plate. Insert the receiving tube under the acid liquid surface to receive the hot distillation. Collect 2 ml of the hot distillation solution: At the same time, add 25 ml of water and steam it according to the above method. Test the reagent in the vacuum chamber. The sample is not thick and can be steamed without steaming.
Take 1 ml of the above solution. Let the solution be steamed in 25% colorimetric solution. Add 1 ml of the color changing solution to the cold part until it reaches the temperature. Or select 7.2.4.1 and package it. 7.2.4.3 Calculation of results See formula 6 Where: X_(mm)×100 CB/I 5CC9.69—2003 The mass of the aldehyde in the sample solution is measured in grams per liter (μm) 25 The volume of the distilled liquid is measured in liters. The aldehyde content in the sample solution is 2 ml/em The methanol content in the distilled liquid is 7.1. The calculated results are guaranteed to be accurate. 7.2. 4.4 Precision The absolute difference between the results of two independent determinations under reproducible conditions shall not exceed 1% of the arithmetic mean. 7.3 Permanganate disinfection Follow the procedure of step 1 in CB/Tb609.6C-200% . 7.4 Residue check 7.4.1 Analytical step Take 200 ml of each pool solution and store them at 105-110℃ in an evaporator or in a water bath. After drying at 105℃, take a small amount and cool it in a flask. When the solution is 200 ml, make a reagent blank test. 7.4.2 Calculation of results See formula (): X=(m)x1cce1 000
Test the heat release of the clear solution, in grams per liter (mg/1.): The test is to use the detailed formula to evaporate the clear solution, in grams (): The amount of reagent benzene released, in grams (in grams) (the sample is in liters (L): The flow rate is the same as 1.2.5. Calculate and save one significant figure
7.2.3 The absolute value of the repeated conditions for obtaining the correct measurement results for the drug period shall not exceed 10% of the arithmetic mean, 524
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