This standard specifies the analysis method of the hygienic standard of unsaturated polyester resin and its fiberglass products for food packaging. This standard is applicable to the analysis of various hygienic indicators of liquid unsaturated polyester resin made by adding styrene to polyester produced with polyols, unsaturated dicarboxylic anhydride, saturated dicarboxylic anhydride, etc. as the main raw materials, and glass fiber reinforced plastic products made of this resin. GB/T 5009.98-2003 Analysis method of hygienic standard of unsaturated polyester resin and its fiberglass products for food containers and packaging materials GB/T5009.98-2003 standard download decompression password: www.bzxz.net

ICS67.040
National Standard of the People's Republic of China
GB/T5009.98—2003
Replaces GB/T13117-1991
Method for analysis of hygienic standard ofunsaturated polyester resin and glass fibre reinforced plastics used as food containers and packaging Materials
Published on August 11, 2003Www.bzxZ.net
Ministry of Health of the People's Republic of China
Standardization Administration of the People's Republic of China
Implemented on January 1, 2004
GB/T5009.98—2003
This standard replaces GB/T13117—1991 "Analysis methods for hygienic standards of unsaturated polyester resins and their glass fiber reinforced plastic products for food containers and packaging materials".
Compared with GB/T13117—1991, the main modifications of this standard are as follows: The structure of the original standard is modified in accordance with GB/T20001.4-2001 "Standard Preparation Rules Part 4: Chemical Analysis Methods".
This standard is proposed and managed by the Ministry of Health of the People's Republic of China. This standard is drafted by Shanghai Food Hygiene Supervision and Inspection Institute, School of Public Health of Harbin Medical University, Shanghai Glass Fiber Reinforced Plastic Research Institute, and Harbin Municipal Health and Epidemic Prevention Station.
The main drafters of this standard are Zhang Cuihua, Zhu Huifen, Tang Lingguang, Hu Zhenzhe and Feng Sujie. The original standard was first issued in 1991, and this is the first revision. 696
1 Scope
Unsaturated
Polyester resins and their fiberglass products for food containers and packaging materials
Sanitary standard analysis methods
GB/T5009.98——2003
This standard specifies the analytical methods for the sanitation standards of unsaturated polyester resins and their fiberglass products for food packaging. This standard is applicable to the analysis of various sanitation indicators of liquid unsaturated polyester resins made from polyesters produced with polyols, unsaturated dicarboxylic acid anhydrides, saturated dicarboxylic acid anhydrides, etc. as the main raw materials, and styrene added to the unsaturated polyester resins, and fiberglass products made from the resins. 2 Normative references
The clauses in the following documents become the clauses of this standard through reference in this standard. For any dated referenced document, all subsequent amendments (excluding errata) or revisions are not applicable to this standard. However, parties reaching an agreement based on this standard are encouraged to study whether the latest versions of these documents can be used. For any undated referenced document, the latest version shall apply to this standard. GB/T5009.60-2003 Hygienic standard for analysis of polyethylene, polystyrene and polypropylene molded products for food packaging 3 Test specimens
3.1 Sampling method
Half of the self-made samples are used for inspection, and the other half are kept for arbitration analysis. 3.2 Sensory inspection of samples
3.2.1 Visually inspect the surface of the resin and the samples before and after immersion. 3.2.2 Visually inspect the color and transparency of the immersion liquid. 3.3 Sample processing
3.3.1 Sample preparation
3.3.1.1 Preparation of resin template (casting body) Resin samples Prepare unsaturated polyester resin samples according to production and construction technical conditions. The sample size is 0.5cmX5cm×10cm, 20 pieces per batch, indicate the batch number, sampling date and technical conditions of the plate making. 3.3.1.2 Preparation of FRP
According to the construction conditions of FRP, the FRP sample is made at the same time as the product, and the number and specifications of the sample are the same as 3.3.1.1. 3.3.2 Sample immersion conditions
Add 2mL of solution per square centimeter of contact area to the sample. 3.3.2.1 Water, 60℃, keep warm for 2h.
3.3.2.24% acetic acid, 60℃, keep warm for 2h. 3.3.2.365% ethanol, room temperature for 2h.
3.3.2.4 n-hexane, room temperature for 2h.
4 Analysis steps
4.1 Potassium permanganate consumption
After the sample is soaked in water, operate according to Chapter 4 of GB/T5009.60-2003. 4.2 Evaporation residue
After the sample is soaked in 4% acetic acid, 65% ethanol and n-hexane, operate according to Chapter 5 of GB/T5009.60-2003. 697
GB/T5009.98-2003
4.3 Heavy metals (in terms of Pb)
After the sample is soaked in 4% acetic acid, operate according to Chapter 6 of GB/T5009.60-2003. 4.4 Ethylbenzene compounds (in terms of styrene)4.4.1 Principle
Use carbon disulfide to extract ethylbenzene compounds in unsaturated polyester resin, and then determine them by gas chromatography. 4.4.2 Reagents
Carbon disulfide.
N-dodecane as internal standard.
Ethylbenzene.
4.4.2.3 Benzene.
Polyethylene glycol 6000.
6201 type chromatographic carrier, 60 mesh 80 mesh.
Nitrogen, hydrogen and air as carrier gas and combustion gas for gas chromatography. 4.4.3 Instruments
4.4.3.1 Pistol drill, for drilling unsaturated polyester resin sample and fiberglass sample into powder. 4.4.3.2 Gas chromatograph, with flame ionization detector and recorder. 4.4.3.3 Micro syringe, 1μL, 5μL. 4.4.3.4 Analytical balance, accurate to 0.1mg. 4.4.4 Sample preparation
4.4.4.1 Unsaturated polyester resin and its fiberglass sample are drilled into powder (40 mesh or more) with an electric drill. 4.4.4.2 Extraction of ethylbenzene compounds
According to the requirements of styrene monomer content, weigh 1g~2g sample (4.4.4.1) and transfer it to a 25mL volumetric flask, add carbon disulfide to exceed the sample. Shake for 15 minutes, then let it stand for 1 hour. Filter quickly with filter paper into a 25mL volumetric flask, wash with the same solvent and make up to volume, accurately add 5μL of n-dodecane and mix well for use. 4.4.5 Analysis steps
4.4.5.1 Preparation of gas chromatography standard solution Weigh appropriate amounts of ethylbenzene and styrene standards (accurate to 0.1mg) in 25mL volumetric flasks, dilute to scale with carbon disulfide. Accurately add 5μL of n-dodecane to each bottle, mix well and set aside. 4.4.5.2 Gas Chromatography Operating Conditions
Chromatographic column: stainless steel column, 2 m long, 3 mm inner diameter, filled with a support coated with 5% polyethylene glycol 6000. Column temperature: 60°C.
Vaporization chamber temperature: 150°C.
Carrier gas: nitrogen.
Flow rate: hydrogen, 20 mL/min; hydrogen, 50 mL/min; air, 800 mL/min. 4.4.5.3 Gas Chromatographic Determination
According to the sensitivity of the gas chromatograph used, inject appropriate volumes of sample solution (prepared according to 4.4.4.2) and standard solution (prepared according to 4.45.1). For the calculation of the results, the injected volumes of the sample solution and the corresponding standard solution will be the same. Operate the gas chromatograph until the component to be measured is completely eluted.
4.4.6 Expression of results
4.4.6.1 Calculation of the results of a certain ethylbenzene compound from the standard curve 4.4.6.1.1 Preparation of standard curve
Draw a standard curve of peak height ratio and each concentration (mg/mL) of the standard solution. 698
Wherein:
Standard solution peak height ratio
A—the peak height of a certain ethylbenzene compound in a standard solution; A,—the peak height of the internal standard (n-dodecane) in the standard solution. 4.4.6.1.2 Determination of percentage
Determine the corresponding ratio from the sample solution. Sample solution peak height ratio=
Wherein:
A, the peak height of a certain ethylbenzene compound in a sample solution; A, the peak height of the internal standard (n-dodecane) in a sample solution. A.
GB/T5009.98—2003
（2）
The concentration of a certain ethylbenzene compound in the sample solution can be obtained from the standard curve. Its percentage is calculated according to the sample mass using formula (3). P.
Where:
Percentage of ethylbenzene compounds, %;
mp×1000
-Concentration of ethylbenzene compounds obtained from the standard curve, in milligrams per milliliter (mg/mL); -Sample mass, in grams (g).
4,4.6.2 Calculation of the results of a certain ethylbenzene compound using a single-point standard If there is a linear relationship between the peak height and the corresponding concentration of the ethylbenzene compound, the formula (4) can be used for calculation: P
Where:
(A./A.)Xm,
(A./A,)Xmg
A,, A, Am, and P. are the same as in 4.4.6.1, - the mass of a certain ethylbenzene compound transferred into 25mL of the standard mixture (4.4.5.1), the unit is grams (g). m.
4.4.6.3 Calculation result of ethylbenzene compounds X=(XA+XB)
Wherein:
X—ethylbenzene compound (calculated as styrene) content, unit is gram per hundred gram (g/100g); Xa—ethylbenzene content, unit is gram per hundred gram (g/100g); -styrene content, unit is gram per hundred gram (g/100g). Xa
4.4.6.4 Precision
(3)
·(5)
The absolute difference between two independent determination results obtained under repeatability conditions shall not exceed the arithmetic mean: 10% for ethylbenzene and 5% for styrene.
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