GB/T 25277-2010 English PDF (GBT25277-2010)

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GB/T 25277-2010: Plastics -- Determination of phenolic antioxidants and erucamide slip additives in polypropylene homopolymer formulations -- Liquid chromatography (LC)
GB/T 25277-2010
GB
NATIONAL STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
ICS 83.080.20
G 31
Plastics – Determination of phenolic antioxidants and
erucamide slip additives in polypropylene homopolymer
formulations – Liquid chromatography (LC)
ISSUED ON. SEPTEMBER 26, 2010
IMPLEMENTED ON. AUGUST 01, 2011
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine of the People's Republic of China;
Standardization Administration of the People's Republic of
China.
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Table of contents
Foreword ... 3 
1 Scope ... 4 
2 Normative references ... 4 
3 Method summary ... 5 
4 Precautions ... 5 
5 Reagents and materials ... 6 
6 Instruments ... 6 
7 Test procedure ... 7 
8 Calculations ... 10 
9 Precision and deviation ... 11 
10 Test report ... 11 
Appendix A (Informative) Clause number comparison between this standard
and ASTM D6042-2004 ... 12 
Appendix B (Informative) Technical differences between this standard and
ASTM D6042-2004 and their causes ... 14 
Appendix C (Informative) Precision of ASTM D6042-2004 ... 16 
Foreword
This standard modifies and adopts American Society for Testing and Materials
ASTM D6042-2004 “Standard test method for determination of phenolic
antioxidants and erucamide slip additives in polypropylene homopolymer
formulations using liquid chromatography” (English version).
This standard is redrafted in accordance with ASTM D6042-2004. In Appendix
A, it lists the detailed comparison between the clause numbers of this standard
and ASTM D6042-2004. In Appendix B, it provides the technical differences and
their causes for reference.
For ease of use, this standard is subjected to the following editorial changes.
- ADD the foreword to the national standard;
- MODIFY the “Normative references”.
Appendix A, Appendix B and Appendix C of this standard are informative.
This standard was proposed by China Petroleum and Chemical Corporation.
This standard shall be under the jurisdiction of the National Plastics
Standardization Technical Committee Petrochemical Plastic Resin Products
Branch (SAC/TC 15/SC 1).
The responsible drafting organization of this standard. China Petroleum and
Chemical Corporation Beijing Yanshan Branch Resin Application Research
Institute.
The participating drafting organization of this standard. Beijing Institute of
Additives.
The main drafters of this standard. Deng Zhengxiang, Sun Shushi, Li Jingqing,
Wang Xiaoli, Yang Chunmei, Wu Yanjin, Yang Lili, Wang Lingxiao.
Plastics – Determination of phenolic antioxidants and
erucamide slip additives in polypropylene homopolymer
formulations – Liquid chromatography (LC)
1 Scope
This standard specifies the use of liquid chromatography for the determination
of some commonly used additives in polypropylene homopolymer (PP-H).
These additives are subjected to reflux extraction by the mixed solvent of
dichloromethane/cyclohexane AND separation by liquid chromatography. The
UV absorption is measured at 200 nm AND it is quantified by internal standard
method.
This standard applies to the determination of the contents of phenolic
antioxidants and erucamide slip additives in polypropylene homopolymer
formulations. α-tocopherol or 3,4-dihydro-2,5,7,8-tetramethyl-2-(4,8,12-
trimethyl tridecyl)-2H-1-benzofuran-6-phenolic hydroxyl group (hereinafter
referred to as vitamin E), 3 (2,4-di-tert-butylphenyl) phosphite ester (hereinafter
referred to as antioxidant 168), tris-(3,5-di-tert-butyl-4-hydroxyphenyl)
isocyanurate (hereinafter referred to as antioxidant 3114), tetra-[(3,5-di-tert-
butyl-4-hydroxyphenyl) propionic acid] pentaerythrilol ester (hereinafter
referred to as antioxidant 1010), AND the (3,5-di-tert-butyl-4-hydroxyphenyl)
propionate octadecyl alcohol (hereinafter referred to as antioxidant 1076). This
standard can also be used for the detection of other antioxidants, such as
antioxidant Ultranox 626, antioxidant Ethanox 330, antioxidant Santanox R and
antioxidant BHT; however, its applicability to these antioxidants has not been
studied.
Under the best detection conditions, the detection limit of phenolic antioxidant
can reach 2 mg/kg.
Note. Other methods that can effectively extract additives from plastics include
thin film extraction method, microwave extraction method, ultrasonic extraction
method, and supercritical fluid extraction method. Other effective methods for
separating the additives include supercritical fluid chromatography (SFC) and
capillary gas chromatography (GC).
2 Normative references
The provisions in following documents become the provisions of this Standard
through reference in this Standard. For the dated references, the subsequent
amendments (excluding corrections) or revisions do not apply to this Standard;
however, parties who reach an agreement based on this Standard are
encouraged to study if the latest versions of these documents are applicable.
For undated references, the latest edition of the referenced document applies.
5 Reagents and materials
5.1 Vitamin E. Industrial reagents.
5.2 Antioxidant 168. Industrial reagents.
5.3 Antioxidants 3114. Industrial reagents.
5.4 Erucamide. Industrial reagents.
5.5 Antioxidant 1010. Industrial reagents.
5.6 Antioxidants 1076. Industrial reagents.
5.7 Tinuvin P. 2 (2'-hydroxy-5'-methylphenyl) benzotriazole, industrial reagents.
5.8 Dichloromethane. liquid chromatography grade.
5.9 Cyclohexane. liquid chromatography grade.
WARNING - Dichloromethane and cyclohexane are toxic and flammable,
so the extraction operation shall be carried out in a fume hood.
5.10 Mixed solvent of dichloromethane/cyclohexane containing internal
standard. The volume ratio of dichloromethane to cyclohexane is 75/25 AND
the concentration of internal standard Tinuvin P is 51.8 mg/L.
5.11 Water. GB/T 6682-2008, level I.
5.12 Acetonitrile. liquid chromatography grade.
5.13 Isopropanol. liquid chromatography grade.
6 Instruments
6.1 Liquid chromatograph. equipped with the UV detector of variable
wavelength OR diode array detector, column oven, and gradient elution device.
6.2 Column. C18 column, 5 μm, 150 mm × 4.6 mm.
6.3 Chromatographic workstation or integrator.
6.4 Shear grinder. with 20 mesh sieve.
6.5 Analytical balance. accurate to ± 0.0001 g.
6.6 Single line pipette. capacity 50 mL, category A in GB/T 12808-1991.
6.7 Reflux extraction device. it is composed of such devices as the condenser
(glass grinding mouth), 125 mL flat bottom flask (glass grinding mouth), the
7.2 Sample preparation
7.2.1 IMMERSE 7 g ~ 8 g of PP-H samples in liquid nitrogen; COOL it for 10
min; PLACE it into the grinding machine (6.4) to grind it to 850 μm (20 mesh) ~
425 μm (40 mesh) particles. During grinding, the grinding time is minimized to
avoid thermal degradation of the additives in the polymer.
7.2.2 Reflux extraction. WEIGH 5 g ± 0.01 g of the sample obtained from 7.2.1;
PLACE it into a 125 mL flat bottom flask; PLACE in the stirring bar; USE the
pipette (6.6) to add 50.0 mL of the mixed solvent of
dichloromethane/cyclohexane containing the internal standard (5.10); under
the stirring reflux of the reflux extraction device (6.7), MAKE it boil for 90 min.
7.2.3 REMOVE the flat bottom flask together with the condenser tube from the
heating pl...