Valid

GB/T 25277-2010Plastics -- Determination of phenolic antioxidants and erucamide slip additives in polypropylene homopolymer formulations -- Liquid chromatography (LC) (English PDF)

塑料 均聚聚丙烯(PP-H)中酚类抗氧剂和芥酸酰胺爽滑剂的测定 液相色谱法

Preview PDF

This is a limited preview

Buy now to download the full PDF (11 pages)

Need quotation for your management?

Get a formal quotation for GB/T 25277-2010 in 30 minutes.

Issued by

General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China

Level / Type

National · Recommended

Issue date

September 26, 2010

Implementation date

August 1, 2011

Scope

GB/T 25277-2010 is the English-translated version of 塑料 均聚聚丙烯(PP-H)中酚类抗氧剂和芥酸酰胺爽滑剂的测定 液相色谱法.

GB/T 25277-2010 — 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. alpha-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).

Found what you need?

Document preview — GB/T 25277-2010

National Standard of the People's Republic of China

ICS
83.080.20
Classification
G 31

Issued by: General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China

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

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 & 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 &

Chemical Corporation Beijing Yanshan Branch Resin Application Research

Institute.

The participating drafting organization of this standard. Beijing Institute of

Additives.

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. alpha-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 plate; COOL the solution to room temperature.

7.2.4 CONNECT the filter tray to a 5 mL glass syringe; slowly POUR out or USE

syringe to transfer appropriate amount of extract into the upper syringe;

INSERT the syringe piston; PUSH it carefully; FILTER the extract into the

sample vial (the final preparation of the sample extraction is as shown in Figure

3).

7.3 Determination of relative response factors

7.3.1 Standard solution preparation. respectively and accurately WEIGH 50 mg

± 1 mg of each additive to be determined into 125 mL flat bottom flask; ADD

51.8 mg of Tinuvin P. USE appropriate amount of isopropyl alcohol (5.13) to

dissolve it; after the dissolving is complete, COOL it to room temperature;

TRANSFER the solution into a 1000 mL volumetric flask (6.9); USE isopropanol

to dilute it to the mark; COVER the volumetric flask; SHAKE it uniformly. The

Vitamin E (5.1) must be prepared before use, OR otherwise stored in a brown

bottle to prevent photodegradation.

7.3.2 FOLLOW 7.1 to set the liquid chromatographic conditions; INJECT 10 µL

of standard solution (7.3.1) for determination.

7.3...

......

......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 11 pages — is available in the English PDF.

How to Download GB/T 25277-2010

  1. 1

    Add to cart

    Click "Download PDF" on this page and choose "Buy this standard". You can add more standards before checkout.

  2. 2

    Checkout

    Enter your email and billing details. Payment is processed securely by Stripe (cards or bank transfer). Prefer bank details? Request a quotation (min. order $300).

  3. 3

    Instant delivery (0–9 sec)

    Delivery is automatic: within seconds of payment you'll receive an email with a secure download link. The link stays valid for 72 hours.

  4. 4

    Invoice included

    A tax invoice is attached to the confirmation email. Need a custom invoice? Contact us.

Related Standards

English PDF
11 pages
Instant delivery (0–9 sec)
Invoice included
View Cart

Secure payment via Stripe

Payments accepted

VisaMastercardAmerican ExpressApple PayGoogle PayStripe

GB/T 25277-2010

$65.00