SN/T 1504.2-2005 Plastic raw materials for food containers and packaging Part 2: Determination of phenolic antioxidants and erucic acid amide lubricants in linear low-density polyethylene Liquid chromatography SN/T1504.2-2005 standard download decompression password: www.bzxz.net

People's Republic of China Entry-Exit Inspection and Quarantine Industry Standard SN/T 1504.2—2005
Part 2:
Plastic raw materials for food containers and packaging
Determination of phenolic antioxidants and erucanideslip additives in linear low-density polvethylene-Liquid chromatography
Published on 2005-02-17
People's Republic of China
General Administration of Quality Supervision, Inspection and Quarantine
Implementation on 2005-07-01
SN/T1504 Plastic raw materials for food containers and packaging are divided into five parts: SN/T 1504.2—2005 Part 1: Determination of phenolic antioxidants and amine lubricants in polyolefin homopolymers by liquid chromatography; Part 2: Determination of phenolic antioxidants and amine lubricants in linear low-density polyethylene by liquid chromatography; Part 3: Determination of phenyl ether (BIIT) in the hydroxyl groups of ethylene polymers and EVA copolymers by gas chromatography; Part 1: Determination of phenolic antioxidants in high-density polyethylene by liquid chromatography; Part 5: Determination of the content of impurity elements in olefins by X-ray carbon spectrometry. This part is the second part of SN/T 1504. This part is modified to adopt the content of ASTM D58-5-1996, and the title is changed to "Determination of phenolic antioxidants and erucic acid amide lubricants in linear low density polyethylene of plastic raw materials for food containers and packaging by liquid chromatography". Appendix A of this part is an informative appendix. This part is proposed and imported by the National Certification and Accreditation Administration of China. This part is organized by the People's Republic of China Exit and Entry Inspection Bureau. The main organizers are: Liu Shaocong, Liu Jun, Zhang Lai, Lu Gang, Ma Xia. This part is an exit and entry inspection and quarantine industry standard issued for the first time. 1 Scope Plastic raw materials for food containers and packaging Part 2: Determination of phenolic antioxidants and erucic acid amide lubricants in linear low density polyethylene by liquid chromatography SN/T 1504. 2—2005
This part of SN/T1504 specifies the method for determining the content of phenolic antioxidants and amine lubricants in linear low-density polyethylene for food containers and packaging for import and export
This part is applicable to the separation and determination of phenolic antioxidants and amine lubricants in linear low-density polyethylene for food containers and packaging. 2 Method Summary
Grind the linear low-density polyethylene (LLDPE) sample to a short diameter of 20 mm, and then extract it with isobutyl alcohol or isobutyl alcohol. Benzene extract liquid chromatograph internal standard
Note: For low-density LLIDFE (density less than 0.925>, it is recommended to use tinuvin P as the extractant; for high-density LIIDPE containing Irganox 11), it is recommended to use isobutylene oxide as the extractant: 3 Reagents and solutions
3.1 Inuvin-: 2 (2\-hydroxy-5'-amino) isobutylene oxide. 3.2 Isopropyl alcohol: Liquid chromatography grade, spectral grade or chromatographic grade reagents 3.3 Isopropyl alcohol: Liquid chromatography grade, spectral grade or chromatographic grade reagents, 3.4 Internal standard solution: Add Tinuvin P internal standard to isopropyl alcohol (or isopropyl alcohol) to prepare a solution with a mass concentration of 51.8 Ig/L.
3.5 Water: Degas by passing high-purity nitrogen gas or vacuum filtration. 3.6 Ethyl acetate: Liquid chromatography grade, spectral grade or chromatographic grade reagents. 4.1 Liquid chromatography: equipped with external detector, heating system and gradient elution device, equipped with 10μL sample injection valve. 4.2 Wiley mill: equipped with 20-day sieve and water cooling system to prevent thermal decomposition of anti-xenon reagent. 4.3 Flow extraction device: composed of cooling tube (20/40 centrifugal mill 1i), 125rL flat-bottom flask (with 22/40 glass mill 1i) and heating plate with magnetic stirring. For sample extraction device, see circle A, 1.4.4 Filter device: Polytetraoxyethylene filter, used for non-aqueous solvents (pore size 0.22 mm), equipped with 5mlL syringe. 4.5 Analytical scale: accurate to -C.0001g. 5 Liquid chromatography conditions
Chromatography: Reverse phase Cl, 5p, 150: ×4.6n5.1
5.2 Detector: UV detector wavelength set at 200, absorbance range set to 0.1A. 5.3 Gradient elution program:
a) Initial mobile phase: Acetonitrile water (5950) SN/T 1504. 2-2005
Final mobile phase condition: Ico ※ acetonitrile,
c) Gradient length: 11 min; Gradient line: White line flow distance: 1.0 rrl/rin. Maintain 100% acetonitrile for 8 min. =19.1min Adjust mobile phase acetonitrile: water = 59:50, flow rate 1.5mL/min, d)
Maintain for 51min:
e) At 25 min, throttle the flow rate to 1.0 mL/min, 5.4 Column temperature 60℃.
5.5 Sample volume, 10 1.
6 Analysis steps
6.1 Sample preparation
6. 1. 1 Grind the sample to a particle size of 2 mesh using Wilcy mill (see 4.2). Note: When grinding 7g~8g sample, the grinding time should be shortened as much as possible to avoid thermal separation of additives in the polymer. 6.1.2 Weigh 5 ± 9.01 ml of sample into a 125 tmJ flat-bottom flask, insert a stirring rod, transfer 50.0 tmT.TP internal standard solution (see 3.4), stir with a flow device and boil for 90 min. Note: For low-precipitation LLDFE, it is recommended to use isobutyl alcohol as the extractant, and for high-precipitation LLIDPE (containing Irax), it is recommended to use isobutyl alcohol as the extractant. 6.1.3 Remove the flat-bottom flask from the heating plate 1 (still connected to the flow condenser), and cool the solution to room temperature. 6.1.4 Directly transfer 9 mL of the extract from the cooled bottle to a volumetric flask of 10 mL. 6.1.5 Add 1 mL of propylamine (without internal standard) to 9 mL of the extract and cover thoroughly. 6.1.6 Place the filter disk on a 5 μl syringe with a 1/2-tip, gently inject 1 mL of the extract solution into the syringe, gently pressurize with the piston, and filter the extract into a small sample bottle. For the final preparation of the sample extraction, refer to Figure A.2.6.2 Calibration of internal standard 6.2.1 Accurately weigh 50 μg of the test component and place it in a 125 mL flat-bottom flask. Add 51.8 mg of Tinuvin-P and 5 mL of 10 mL of warm isopropanol or isopropanol to dissolve it. Transfer it to a 1:1 volumetric flask and dilute it to the mark with isopropanol or isopropanol and shake thoroughly.
2 Under the HPLC conditions described in Chapter 5, adjust the response value of the HPLC detector to a constant value by introducing 10I of sample. 6.2.3 According to the chromatographic front area, calculate the relative response factor using formula (1): Ri-SXA
Wherein:
R——relative average factor;
concentration of the component to be measured, in milligrams per (mg/I)A.get the area of ​​the component to be measured;
concentration of the internal standard in milligrams per (m)
peak area of ​​the internal standard.
6.2.4 Repeat the test three times to get the average response factor. Note: If Tinirein-P may be the component to be measured in the test column, Tinasi--P cannot be used as an internal standard. 6.3 Determination 6.3.1 Ensure that the conditions of the liquid chromatograph are as described in Chapter 5 of this Part. 6.3.2 Set up a liquid chromatograph system with sample solution. The chromatogram is shown in Figure A.3. 7 Calculation of results The content of the analyte is expressed as mass fraction and is calculated using formula (2): 2 Where: 8 Precision X = 4XR.XXY Mass fraction of the analyte, in milligrams per gram (mg/l): Peak area of ​​the analyte in the sample:
Response factor;
Concentration of internal standard, in milligrams per liter (mg/l): Volume of internal standard solution added, in milliliters (mL); Sample mass,Unit is gram (g);
peak area of ​​flash standard substance.
$N/T 1504. 2—2005
Seven test spaces were used to test four pairs of materials according to the method specified in this section. The content levels and precisions of phenolic antioxidants and hydroxyl acyl lubricants are shown in Table 1.
Test precision of additive components in linear low-density polyethylene Table 1
Isonox-29
Isonox_29
Irganoxlolo
Irganoxlolc
Irganxl078
Irganox1075
Krucanide
Erucanide
Standard value
. aThe average value of standard pseudo blue in the laboratory. bThe product value of standard deviation between laboratories.
c Repeatability within the test rate -2.8sr
(Repetition rate between tests is -2.S.SR
Average
Unit is grams per kilogram
SN/T 1504. 2—2005
Appendix A
(Informative Appendix)
Experimental device and chromatogram
24/40 ground mouth
—12GL burning sticking
Magnetic small stirring sample
Heating pole/magnetic stirring
Figure A. Sample extraction device
一5 m., syringe
Extractant
一Let the combustor
4 irL was sampled and bottle
Final preparation of sample extract
Chromatogram of six added components
$N/T 1504. 2—2005
SN/T 1504. 2-2005
Chinese People's Republic of China Border Inspection and Quarantine
Industry Standardswww.bzxz.net
Plastic materials for food containers and packaging Part 2: Determination of phenolic antioxidants and erucic acid amide lubricants in linear low-density polyethylene Liquid chromatography SN/T 1504, 2—2005
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