GB/T 5009.101-2003 Determination of antimony in polyester resins and their molded products for food containers and packaging materials
Some standard content:
KCS.67.040
National Standard of the People's Republic of China
R/T5009.101—2003
Replaces G3/3120—1596
Determination of antimony in polyester resins and their molded products for food containers and packaging materials
Promulgated on 2003-06-11
Ministry of Health of the People's Republic of China
National Standardization Administration
Implementation on 2004-01-01
GR/T 5009.101—2003
This standard replaces B/T15121—1906 "Determination method for antimony in polyester resins and their molded products for food containers and packaging materials". Compared with GB/T13120-a9G, the main changes of this standard are as follows: The Chinese name of the standard has been modified + the Chinese name of the standard has been changed to Determination of the endurance of resins and their molded products for food containers and packaging materials.
The structure of the original standard has been modified in accordance with GB/T200014-2301 standard Part 4: Chemical analysis methods.
This standard is proposed and funded by the Ministry of Health of the People's Republic of China. The responsible person for this standard is Shanghai Municipal Food and Drug Administration, Shanghai Municipal Food and Drug Administration, Shanghai Municipal Food and Drug Administration, Shanghai Municipal Food and Drug Administration.
The main drafters of the first method of this standard are Wang Shi, Jiu Wen, Li Min, Lao Bao. The main drafters of the second method of this standard are Shen Wen, Fang Ya, Zhang Cuihua. The original standard was first published in 1991, revised for the second time in 1996, and the second revision of this standard is 1.
GB/5009.FO12003
Determination of trace amounts of thermoplastic thermoplastic resins and their molded products for food containers and packaging materials This standard specifies the determination method of trace amounts of thermoplastic thermoplastic resins and their finished products - atomic absorption spectrophotometry and opal spectrophotometry.
This standard is applicable to the determination of trace amounts of thermoplastic thermoplastic resins and their products: it can also be used for the determination of trace amounts of thermoplastic thermoplastic resins and their products in porcelain tableware and containers. The detection limit of the second phase spectrophotometry in this standard is .g/. The second phase is the atomic absorption spectrophotometry. Principle: The raw material is a mixed salt carrier, which is complexed with trivalent alkali and dibasic dibasic acid (APDC) by chemical reduction, extracted with 4-methylcyclopentyl alcohol (methyl isobutyl ketone MTDK), and then the 3-hydroxy-1-nitropropene is determined by atomic absorption spectrophotometer. 3.14 Acetic acid: 4mE acetic acid is weighed, and water is added. Sample to 100ml, 3.26mol/L hydrochloric acid, 50IL salt, add 100ml of water. 3.31Ug/. Stirring liquid: weigh 10% potassium hydroxide, add water to 100ml (prepared before use) 3.45k/E. pyrrolidine. APD magnetically take 0.5gAP1X and put it in a 25DmL cone bottle, add 10K)ml of water and vibrate for 1min, drain and set aside (prepared before use). 3.5-2
3.6 Preparation of the cup: weigh 0.250Dg of bromine powder (50.99), return to 25tl. of sulfuric acid, slowly distill to dissolve it, and quantitatively transfer it to a 5C0mL container containing about 100ml of water, and dilute to the scale with water. Each liter of this stock solution is equivalent to 0.5tmg, 3.7 standard intermediate pool, take 1.0mL of storage tank, add 100.0mL of this instrument, each liter of this intermediate solution is equivalent to 3.9 standard use liquid: take 10.0mL of intermediate solution, add water and grind it to 100.0L, select the speed and use 0.5g of liquid per mL. 4 instrument
4.1 source and receive spectrophotometer.
4.2 Stone plate original leveler,
5 Analysis steps
5.1 Sample treatment
5.1.1 Tree (material pellets) www.bzxz.net
Weigh 4.00 (accurate 0.01g) of pure wood in a 250 ℃ flask, add 90mL of acetic acid (3.1> floor good decomposition: hot reflux on water for 2h, immediately filter with fast building paper, and wash with a small plate 7 (3.1) to make a filter volume of 100ml.
5.1.2 Molded products
According to the type and surface area, add 2ml of acetic acid (3.1) at a ratio of 1ctm to 60% by volume and 30% by volume. Filter the mixture as a test piece. 3
CB/T5009.101-2003
5.2 Standard curve construction
Take the standard solution of 0.1, 2.0, 3.0, 4.0, 2.0, 1.5, 1, 0, 1, 5, 2.0, 2.5 mL, which is equivalent to 1.0, 1.5, 1, 0, 1, 5, 2.0, 2.5 mL. First add 20 ml of acetic acid (3.1) to 125 ml of a dilution tube. Make up the volume to 5 ml with acetic acid (3.1). Add 2 mL potassium iodide solution, 3 mL saline (3.2), mix and collect for 2 min, add 10 mL AP[KC solution, mix and collect 1 mL MTRK, add 1 mL AP[KC solution, add ... 4Dl:
Turn end/nm
Milliman/grasp
Table 2 Working conditions of right-hand furnace (for reference)
Measurement formula
Peak time
Holding time/
Integral time "5
4 Flow blue uL/uim
Take 51 as sample solution 5cm bone 125m filter funnel, take another 50mL acetic acid (3.1) as The reagent is empty, and the following can be operated according to 5.2. 2n. The potassium storage is added separately. 5.4 The result is calculated by formula (1): Wherein: X-the potassium content in the technical pool or the national flow is in micrograms per year or liter/nL) 4 The measured amount in the reservoir is in micrograms (8) - the measured amount in the reagent solution, in micrograms (ug) V-the new amount taken The unit is drop-liter (mI).
The absolute difference between the results of two independent determinations obtained under quantitative conditions shall not exceed 29% of the arithmetic mean. The second method is the pore green spectrophotometry method.
7 Principle
The pentavalent ion can react with the trivalent methane dye pore green (ucii core) to form a colored Complex number: It can be extracted by acetaldehyde in a certain H medium. Of course, only with pentavalent potassium can it form a complex with the green dye: Therefore, it is necessary to first reduce the antimony ions in the system to trivalent antimony, and then oxidize them to pentavalent antimony ions to achieve the purpose of complex extraction determination: 9 Test
8.1 Anhydrous sodium hyaluronate: analytical grade.
8.2 Technical definition of ester, analytical grade,
GB/T 5009.101—2003
83 Oxidizing agent: 128% chloride (2H2O), heat with 15 mL hot acid to decompose, add water to 100 mL.-
8.4 Nitrite: 20% sodium nitrate (Na2O3).0% water and dilute to 100L8.5 Base aqueous solution (1+1)
8.6 Dilute salt solution: 5% acid, add water, weigh and decompose to 1 volume, BB citric acid: 20g C1, Na2O3). Add water to 100mL8.9 Dilute sulfuric acid: 1 part acid in 5 parts water8.10 Acid: analytical grade.
2.17 Format: Collect 0.2500 ml of concentrated sulfur in a small baking cup, heat it to make it dissolve, transfer quantitatively to 500 ml. Put it into a volumetric bottle, and mark it with water. The concentration of this stock solution is 0.5 mg/mL8.2. Take 2 drops slowly and adjust the concentration to 1/10. 9 Instruments
Spectrophotometer.
10 Analysis steps
10.1 Sample preparation
Continue with 5.1.
t0.2 Standard curve preparation
Standard solution (8, 10, 9.1.0.3.0, 5, 0,7,1.0mL (equivalent to F0,1.0,3.0,5,0.7,3,10.) volume in advance 4L request, 4L salt age (8.6) 12roL filter test bucket, add chemical nitrate. Zinc (8.3) 2 full. Diffuse until effective, add 1% sodium citrate (10%) and blow with a rubber bulb to drive out the oxide gas in the funnel, then add 25ml of urine aqueous solution (8.5), shake thoroughly and place on the filter until there is no gas backflow, add 10% sodium citrate (8%) into the funnel, shake thoroughly, place and separate, discard the organic phase, pass through a small funnel with a little anhydrous sodium androphosphate in advance, collect the dehydrated organic phase in a small test tube, use the zero tube as a blank: use a 1cm pathlength colorimetric blood, measure at 622m as the embedding length, and make the concentration-gradient acquisition standard. TO.3 sample measurement
Take 5.1 in the Xiangjingfan 0TL material steam just to rub (8.10) 2 business in the water Ten (0.5m>, use 4L hydrochloric acid 8.5? oz. to wash the contents until there is 1L of water in the washing bottle. Then add 3L of water in batches, combine the washing solutions into the separatory funnel, add 2 drops of oxidizing agent (5.3), and then place it in the chamber for 5 hours. The following can be done according to 19.2*, add 1m. to the acid solution (8.4).\. At the same time, use 50m4% 2% 2-acid as the reagent: 10.4 The calculation of the concentration is calculated according to formula (2):
In the play:
The effective content in the concentrated solution is in micrograms per unit (mA) The effective content in the collected sample solution is in micrograms (); A-the amount of reagent extracted is in micrograms (AR) V-the volume of the sample soluble in water, in units of liters (ml.) 2)
GB/T 5009.101—2003
The difference between the results of two independent tests under complex conditions shall not exceed 20% of the arithmetic mean.
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