BCI Battery TechnicalManual BCIS-11 Issued 3-8-2004 STANDARDIZED TESTING METHODS FOR POLYPROPYLENE RESIN INTRODUCTION Virgin and recycled polypropylene resin is used extensively in battery components including containers, covers, vents, handles, and height adaptors Physical characteristics of the resin can affect molding and finished part performance Extensive polypropylene testing standards have been established by standardizing organizations, such as ASTM (American Society for Testing Materials) and ISO (International Organization for Standardization), for use in venues throughout the world Efforts by these organizations, along with SAE (Society of Automotive Engineers), to harmonize testing methods for global automotive applications have placed the respective standards in a state of flux at this writing To address this condition, parallel and complimentary standards promulgated by standardizing organizations are referenced herein FOREWORD This document was prepared by the BCI Technical Subcommittee for Polypropylene Testing Participants have included resin suppliers, molders, and battery manufacturers TABLE OF CONTENTS 1.1 1.2 1.3 2.1 2.2 Scope Purpose: Field of Application: Product Classification: References: Applicable Documents: Reference Sources: Summary of Standard Physical and Chemical Test Methods Modifications to Standard Test Methods Revision History BCIS-11 Rev SCOPE 1.1 Purpose The purpose of this document is to provide a source of reference methods for the physical and/or chemical testing and evaluation of polypropylene resins used for all battery applications, including containers, covers, vents, and handles 1.2 Field of Application: Virgin and recycled polypropylene resin used for molding of battery components, including containers, covers, vents, handles, and height adapters Similar polypropylene testing methods produced by ASTM and ISO are identified and referenced below Test methods unique to a particular standard organization, but of potential value in evaluating polypropylene for battery applications have been included Methods particularly applicable for fire retardant polypropylene have been included for resins that may be used in marine or emergency power applications It is incumbent upon the user to determine the suitability of each test method for their specific use and to report any deviations from the reference methods cited 1.3 Product Classification: Polypropylene resin used in Flooded or VRLA battery components for SLI, marine, or stationary applications REFERENCES: The detailed test descriptions are to be found in the reference documents listed below Copies of the applicable test methods are available from the respective standards organizations cited below 2.1 Applicable Documents: The following publications form a part of this document to the extent specified herein The applicable issue of the publications will be the issue in effect on the date of publication of this document In the event of conflict between the text of this document and references cited herein, the text of this document takes precedence Nothing in this document, however, supersedes applicable laws and regulations unless a specific exemption has been obtained ASTM References D1238 Standard Test Method for Melt Flow Rates of Thermoplastics by Extrusion Plastometer D3835 Standard Test Method for Determination of Properties of Polymeric Materials by Means of a Capillary Rheometer D792 Standard Test Methods for Density and Specific Gravity (Relative Density) of Plastics by Displacement D1895 Standard Test Method for Apparent Density, Bulk Factor, and Pour Ability of Plastic Materials D955 Standard Test Method of Measuring Shrinkage from Mold Dimensions of Thermoplastics D638 Standard Test Method for Tensile Properties of Plastics D256 Standard Test Method for Determining the Izod Pendulum Impact Resistance of Plastics D6110 Standard Test Methods for Determining the Charpy Impact Resistance of Notched Specimens of Plastics BCIS-11 Rev D5420 D790 D2290 D648 D1525 D785 D1894 D4101 D3012 D570 D5630 D1603 D4218 D3418 D3763 D543 D6290 E313 D1531 D150 D3638 D2863 Standard Test Method for Impact Resistance of Flat, Rigid Plastic Specimen by Means of a Striker Impacted by a Falling Weight (Gardner Impact) Standard Test Methods for Flexural Properties of Non-Reinforced and Reinforced Plastics and Electrical Insulating Materials Standard Test Methods for Tensile, Compressive, and Flexural Creep and Creep-Rupture of Plastics Standard Test Method for Deflection Temperature of Plastics Under Flexural Load In the Edgewise Position Standard Test Method for Vicat Softening Temperature of Plastics Standard Test Method for Rockwell Hardness of Plastics and Electrical Insulating Materials Standard Test Method for Static and Kinetic Coefficients of Friction of Plastic Film and Sheeting Standard Specification for Polypropylene Injection and Extrusion Materials Standard Test Method for Thermal-Oxidative Stability of Polypropylene Using a Specimen Rotator Within an Oven Standard Test Method for Water Absorption of Plastics Standard Test Method for Ash Content in Plastics Standard Test Method for Carbon Black in Olefin Plastics Standard Test Method for Determination of Carbon Black Content in Polyethylene Compounds By the Muffle-Furnace Technique Standard Test Method for Transition Temperatures of Polymers By Differential Scanning Calorimetry Standard Test Method for High Speed Puncture Properties of Plastics Using Load and Displacement Sensors Standard Practices for Evaluating the Resistance of Plastics to Chemical Reagents Standard Test Method for Color Determination of Plastic Pellets Standard Practice for Calculating Yellowness Indices from Instrumentally Measured Color Coordinates Standard Test Methods for Relative Permittivity (Dielectric Constant) and Dissipation Factor by Fluid Displacement Procedures Standard Test Methods for AC Loss Characteristics and Permittivity (Dielectric Constant) of Solid Electrical Insulation Standard Test Method for Comparative Tracking Index of Electrical Insulating Materials Standard Test Method for Measuring the Minimum Oxygen Concentration to Support Candle-Like Combustion of Plastics (Oxygen Index) ISO References 10350-1 Plastics – Acquisition and presentation of comparable single-point data, Part 1: Molding materials 1133 Plastics-Determination of the melt mass-flow rate (MFR) and the melt volumeflow rate (MVR) of thermoplastics 11443 Plastics – Determination of the fluidity of plastics using capillary and slit-die rheometer 1183 Plastics – Methods for determining density and relative density of non-cellular plastics 60 Plastics – Determination of apparent density of material that can be poured from a specified funnel 294-4 Plastics-Injection molding of test specimens of thermoplastic materials, Part 4: Determination of molding shrinkage 527-2 Plastics-Determination of tensile properties Part 2: Test conditions for molding and extrusion plastics 180 Plastics – Determination of Izod Impact strength BCIS-11 Rev 179 178 899-1 75-2 306 2039-1 2039-2 8295 294-1 1873-2 4577 62 3451-1 6964 11357-3 6603-2 175 4599 60243-1 60112 Plastics – Determination of Charpy Impact properties, Part 1: Non-instrumented impact test Plastics – Determination of flexural properties Plastics – Determination of creep behavior, Part 1: Tensile Creep Plastics – Determination of temperature of deflection under load, Part 2: Plastics and ebonite Plastics – Thermoplastic materials – Determination of Vicat softening temperature (VST) Plastics – Determination of Hardness, Part 1: Ball Indentation Method Plastics – Determination of Hardness, Part 2: Rockwell hardness Plastic Film and Sheeting – Determination of Coefficient of Friction Plastics – Injection molding of test specimens of thermoplastic materials, Part 1: General principles and molding of multipurpose and bar test specimens Plastics – Polypropylene (PP) molding and extrusion materials, Part 2: Preparation of test specimens and determination of properties, with amendments Plastics – Polypropylene and propylene-copolymers – Determination of thermal oxidative stability in air – Oven method Plastics – Determination of water absorption Plastics – Determination of ash, Part 1: General Methods Polyolefin Pipes and Fittings – Determination of carbon black content by calcinations and pyrolysis – Test method and basic specification Plastics – Differential scanning calorimetry (DSC), Part 3: Determination of temperature and enthalpy of melting and crystallization Plastics – Determination of puncture impact behavior of rigid plastics, Part 2: Instrumented Impact Testing Plastics – Methods of test for the determination of the effects of immersion in liquid chemicals Plastics - Determination of resistance to environmental stress cracking (ESC) – Bent strip method Electrical strength of insulating materials – Test methods, Part 1: Tests at power frequencies Method for the determination of the proof and the comparative tracking indices of solid insulating materials UL Reference UL Standard 94: Standard for Tests for Flammability of Plastic Materials for Parts in Devices and Appliances SAE: J2642: Recommended Practices for Developing Specifications for Automotive Thermoplastic Materials (expected release early 2004) 2.2 REFERENCE SOURCES To obtain copies of the detailed test methods, the user should contact the referencing organizations directly at the following addresses: ASTM International, 100 Bar Harbor Drive, P.O Box C700, Conshohocken, PA 19428-2959, United States, 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail), or through the ASTM website www.astm.org ISO, 1, rue de Varembe, CH-1211 Geneva 20, Switzerland, +41 22 749 01 11 (phone), +41 22 749 09 47 (fax), or ISO website www.iso.ch IEC Central Office, 3, rue de Varembe, PO Box 131, CH-1211, Geneva, Switzerland, +41 22 919 02 11 (phone), +42 22 919 03 00 (fax) or through IEC website www.iec.ch BCIS-11 Rev SAE Automotive Headquarters, 755 W Big Beaver, Suite 1600, Troy, MI 48084, United States, Customer Service 1-877-606-7323 (U.S & Canada only), 724/776-4970 (outside U.S & Canada), 724/776-0790 (fax), or through the SAE website www.sae.org Underwriter’s Laboratory, Customer Service, 333 Pfingsten Rd., Northbrook, IL 60062-2096, 877-854-3577 (phone), 847-407-1395 (fax), customerservice.nkb@us.ul.com (email) Alternately, UL standards may be ordered directly from COMM 2000, 1414 Brook Drive, Downers Grove, IL 60515, 888-853-3503 (phone), 630-932-7312 (fax), www.comm2000.com 2.3 Definitions: The units of reporting shall be in SI units, as described in ISO 10350-1, unless an alternate is mutually agreed to between users BCIS-11 Rev SUMMARY OF STANDARD PHYSICAL AND CHEMICAL TESTING METHODS SUMMARY OF POLYPROPYLENE TEST STANDARDS Materials: Virgin, Recycled, High Heat/Fire Retardant ASTM ISO MOLDING CHARACTERISTICS Melt Flow Rate Melting Fluid Index Density Bulk Density Pellet Form Molding Shrinkage D1238 n/a D792 D1895 D1921 D955 1133 11443 1183 60 n/a 294-4 PHYSICAL PROPERTIES Tensile Yield Strength* Impact, Notched Izod @ 230C* Impact Notch Izod @ -180C* Impact, Charpy, Notched* Impact, Gardner Flexural Modulus* Flexural Creep* Deflection Temperature @ 0.45MPa* Vicat Softening Temperature* Hardness, Rockwell R* Hardness, Ball Indentation Coefficient of Friction* *Sample Prep D638 D256 D256 D6110 D5420 D790 D2290 D648 D1525 D785 n/a D1894 D4101 527 180 180 179 n/a 178 899-1 75-2 306 2039-2 2039-1 8295 294-1, 1872-2 D3012 D570 D5630 D4218,D1603 4577 62 3451-1 6964 D3418 11357-3 D3763 6603-2 D543 175, 4599 n/a n/a D6290, E313 D1531, D150 D3638 n/a D2863 n/a 60243-1 60112 n/a n/a CHEMICAL PROPERTIES Oven Oxidation Water Absorption Ash Content Carbon Black Content Melt & Crystalization Enthalpy & Temperature Ductile/Brittle Transition Temperature Chemical Resistance Metallic Impurities OTHER Color Dielectric Strength Continuous Tracking Index Burn Rating Oxygen Index n/a = not applicable Alternate BCI 4.1.2 BCI 4.1.1 UL 94 BCIS-11 Rev MODIFICATIONS OF STANDARD TESTING METHODS In addition to the standardized test methods deviations from the standard test conditions that may be unique to the battery industry are listed below 4.1 Melt Index: None 4.2 Melting Fluid Index: None 4.3 Density: None 4.4 Bulk Density: None 4.5 Pellet Form: Alternatively, the weight of a fixed number of resin pellets may be used 4.6 Molding Shrinkage: None 4.7 Tensile Yield Strength: None 4.8 Impact, Notched Izod: None 4.9 Impact, Subambient Notched Izod: None 4.10 Impact, Charpy: None 4.11 Impact, Gardner: None 4.12 Flexural Modulus: None 4.13 Flexural Creep: None 4.14 Deflection Temperature: None 4.15 Vicat Softening Temperature: None 4.16 Hardness, Rockwell R: None 4.17 Hardness, Ball Impact: None 4.18 Coefficient of Friction: None 4.19 Sample Preparation: None 4.20 Oven Oxidation: BCI 1.4.1.2 has been previously documented in this TechnicalManual It may be applied to molded parts or sections or specially molded test plaques Samples may be suspended in the oven by stationary suspension or on open racking, provided uniform temperature distribution in the oven has been demonstrated and is maintained Suspension hangers and/or racking must not accelerate the rate of sample aging 4.21 Water Absorption: None 4.22 Ash Content: With modification ASTM D5630 may be applied to the determination of carbon black in polypropylene 4.23 Carbon Black Content: ASTM D4218 is the preferred method of analysis based on simplicity, speed, and applicability With modification, D4218 is applicable to recycled materials that BCIS-11 Rev normally have a relatively high background of non-combustible inorganic matter Modification of ASTM D5630 for determination of ash content in plastics may also be used as an alternate method of analysis ASTM D1603 is a slower, more complex test method requiring the use of trichloroethylene, dry ice, and nitrogen 4.24 Melt & Crystallization Enthalpy & Temperature: ASTM methods D3417 Standard Test Method for Enthalpies of Fusion and Crystallization of Polymers by Differential Scanning Calorimetry (DSC) and D3418 Standard Test Method for Transition Temperatures of Polymers By Differential Scanning Calorimetry are currently accepted testing procedures At such time as ASTM may consolidate these individual methods into a single revised test method, the revised test method designation will become acceptable 4.25 Ductile/Brittle (Glass) Transition Temperature: None 4.26 Chemical Resistance: None 4.27 Metallic Impurities: Applicable methods are documented in this manual under 1.4.1.1, C-1, 4.28 Color: Visual standards mutually approved by supplier and customer with annual review is an acceptable alternative 4.29 Dielectric Strength: None 4.30 Continuous Tracking Index: None 4.31 Burn Rating: None 4.32 Oxygen Index: None REVISION HISTORY This is the original publication submitted for BCI Technical Committee approval Date of original publication: March 8, 2004 Editor(s): Glenn M Trischan Date of submission to BCI Technical Committee for approval: January, 2004 Editor(s): Glenn M Trischan, Johnson Controls Battery Group, Inc., P.O Box 591, Milwaukee, WI 53201, phone: 414/524-2365; fax: 414/524-2008 ... Determination of Izod Impact strength BCIS -11 Rev 179 178 899-1 75-2 306 2039-1 2039-2 8295 294-1 1873-2 4577 62 3451-1 6964 113 57-3 6603-2 175 4599 60243-1 6 0112 Plastics – Determination of Charpy... de Varembe, CH-1 211 Geneva 20, Switzerland, +41 22 749 01 11 (phone), +41 22 749 09 47 (fax), or ISO website www.iso.ch IEC Central Office, 3, rue de Varembe, PO Box 131, CH-1 211, Geneva, Switzerland,... Fluid Index Density Bulk Density Pellet Form Molding Shrinkage D1238 n/a D792 D1895 D1921 D955 113 3 114 43 118 3 60 n/a 294-4 PHYSICAL PROPERTIES Tensile Yield Strength* Impact, Notched Izod @ 230C*