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ASTM D 4483 : 2020

Current

Current

The latest, up-to-date edition.

Standard Practice for Evaluating Precision for Test Method Standards in the Rubber and Carbon Black Manufacturing Industries

Available format(s)

Hardcopy , PDF

Language(s)

English

Published date

01-06-2020

1.1This practice covers guidelines for evaluating precision and serves as the governing practice for interlaboratory test programs (ITP) used to evaluate precision for test methods as used in the rubber manufacturing and the carbon black industries. This practice uses the basic one way analysis of variance calculation algorithms of Practice E691. Although bias is not evaluated in this practice, it is an essential concept in understanding precision evaluation.

1.2This practice applies to test methods that have test results expressed in terms of a quantitative continuous variable. Although exceptions may occur, it is in general limited to test methods that are fully developed and in routine use in a number of laboratories.

1.3Two precision evaluation methods are given that are described as robust statistical procedures that attempt to eliminate or substantially decrease the influence of outliers. The first is a General Precision procedure intended for all test methods in the rubber manufacturing industry, and the second is a specific variation of the general precision procedure designated as Special Precision, that applies to carbon black testing. Both of these procedures use the same uniform level experimental design and the Mandel h and k statistics to review the precision database for potential outliers. However, they use slight modifications in the procedure for rejecting incompatible data values as outliers. The Special Precision procedure is specific as to the number of replicates per database cell or material-laboratory combination.

1.4This practice is divided into the following sections:

Section

Scope

1

Referenced Documents

2

Terminology

3

Significance and Use

4

Precision Evaluation—General Precision and Special Precision

5

Steps in Organizing an Interlaboratory Test Program (ITP)

6

Overview of the General Precision Analysis Procedure

7

General Precision: Analysis Step 1

8

 Preliminary Graphical Data Review

8.1

 Calculation of Precision for Original Database

8.2

 Detection of Outliers at 5 % Significance Level Using h and k Statistics

8.3

 Generation of Revision 1 Database Using Outlier Treatment Option 1 or 2

8.4

General Precision: Analysis Step 2

9

 Calculation of Precision for Revision 1 Database

9.1

 Detection of Outliers at 2 % Significance Level Using h and k Statistics

9.1

 Generation of Revision 2 Database Using Outlier Treatment Option 1 or 2

9.1.2

General Precision: Analysis Step 3

10

 Calculation of Precision Using Revision 2 Database

10.1

Special Precision Analysis—Carbon Black Testing

11

Format for Precision Table and Clause in Test Method Standards

12

Preparation of Report for Precision Analysis

13

Definitions for Selected Terms Concerned with Precision and Testing

Annex A1

Statistical Model for Interlaboratory Testing Programs

Annex A2

Calculating the h and k Consistency Statistics for Outliers

Annex A3

Spreadsheet Calculation Formulas, Table Layout, and Calculation Sequence

Annex A4

Procedure for Calculating Replacement Values of Deleted Outliers

Annex A5

Example of General Precision Evaluation—Mooney Viscosity Testing

Annex A6

1.5Six annexes are presented; these serve as supplements to the main body of this practice. Annex A1 and Annex A2 are given mainly as background information that is important for a full understanding of precision evaluation. Annex A3 – Annex A5 contain detailed instructions and procedures needed to perform the operations as called for in various parts of the practice. The use of these annexes in this capacity avoids long sections of involved instruction in the main body of this practice. This allows for a better presentation and understanding of the central concepts involved in the evaluation of precision. Annex A6 is also important; it gives a complete example of precision evaluation that illustrates all of the procedures and options likely to be encountered in any precision evaluation, from the simple to the most complex.

1.6This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.

1.7This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Committee
D 11
DocumentType
Standard Practice
Pages
59
PublisherName
American Society for Testing and Materials
Status
Current
Supersedes

ASTM D 1646 : 2019 : REV A Standard Test Methods for Rubber—Viscosity, Stress Relaxation, and Pre-Vulcanization Characteristics (Mooney Viscometer)
ASTM D 1512 : 2015 : REV B Standard Test Methods for Carbon Black—pH Value
ASTM D 2632 : 2015 : R2019 Standard Test Method for Rubber Property—Resilience by Vertical Rebound
ASTM D 6049 : 2003 : R2017 Standard Test Method for Rubber Property—Measurement of the Viscous and Elastic Behavior of Unvulcanized Raw Rubbers and Rubber Compounds by Compression Between Parallel Plates
ASTM D 6124 : 2006 : R2017 Standard Test Method for Residual Powder on Medical Gloves
ASTM D 6284 : 2017 Standard Test Method for Rubber Property—Effect of Aqueous Solutions with Available Chlorine and Chloramine
ASTM D 572 : 2004 : R2019 Standard Test Method for Rubber—Deterioration by Heat and Oxygen
ASTM D 4578 : 2006 : R2017 Standard Test Methods for Rubber Chemicals—Determination of Percent Sulfur by Extraction
ASTM D 4934 : 2002 : R2017 Standard Test Method for Rubber Compounding Materials: 2-Benzothiazyl Sulfenamide Accelerators—Insolubles
ASTM D 6370 : 1999 : R2019 Standard Test Method for Rubber—Compositional Analysis by Thermogravimetry (TGA)
ASTM D 3314 : 2002 : R2017 Standard Test Method for Rubber—Chemical Analysis for Polystyrene Blocks In SBR (Styrene-Butadiene Rubber) and Styrene-Reinforced Latices
ASTM D 926 : 2017 Standard Test Method for Rubber Property—Plasticity and Recovery (Parallel Plate Method)
ASTM D 7121 : 2005 : R2018 Standard Test Method for Rubber Property—Resilience Using Schob Type Rebound Pendulum
ASTM D 7772 : 2015 : R2019 Standard Test Method for Carbon Black Extractables – Absorbance of Cyclohexane Extract
ASTM D 1630 : 2016 Standard Test Method for Rubber Property—Abrasion Resistance (Footwear Abrader)
ASTM D 3188 : 2006 : R2017 Standard Test Methods for Rubber—Evaluation of IIR (Isobutene-Isoprene Rubber)
ASTM D 1508 : 2012 : R2017 Standard Test Method for Carbon Black, Pelleted Fines and Attrition
ASTM D 297 : 2015 : R2019 Standard Test Methods for Rubber Products—Chemical Analysis
ASTM D 7427 : 2016 Standard Test Method for Immunological Measurement of Four Principal Allergenic Proteins (Hev b 1, 3, 5 and 6.02) in Hevea Natural Rubber and Its Products Derived from Latex
ASTM D 945 : 2016 Standard Test Methods for Rubber Properties in Compression or Shear (Mechanical Oscillograph)
ASTM F 421 : 2015 Standard Test Method for Measuring Groove and Void Depth in Passenger Car Tires
ASTM F 1806 : 2014 Standard Practice for Tire Testing Operations–Basic Concepts and Terminology for Reference Tire Use
ASTM D 1514 : 2015 Standard Test Method for Carbon Black—Sieve Residue
ASTM D 3265 : 2019 : REV B Standard Test Method for Carbon Black—Tint Strength
ASTM D 1513 : 2005 : R2017 Standard Test Method for Carbon Black, Pelleted—Pour Density
ASTM D 5051 : 2006 : R2017 Standard Test Method for Rubber Compounding Materials—Benzothiazyl Disulfide (MBTS)—Assay
ASTM D 3484 : 2006 : R2016 Standard Test Methods for Rubber—Evaluation of Oil-Extended Solution BR (Polybutadiene Rubber)
ASTM D 5774 : 1995 : R2019 Standard Test Methods for Rubber—Chemical Analysis of Extractables
ASTM D 4574 : 2006 : R2017 Standard Test Methods for Rubber Compounding Materials—Determination of Ash Content
ASTM D 5376 : 2006 : R2017 Standard Test Method for Rubber Compounding Materials—Determination of the Basic Nitrogen Content in Rubber Antioxidant: Polymerized TMQ
ASTM D 3848 : 2003 : R2018 Standard Test Methods for Rubber—Evaluation of NBR (Acrylonitrile-Butadiene Copolymers) Mixed With Carbon Black
ASTM D 750 : 2012 : R2017 Standard Practice for Rubber Deterioration Using Artificial Weathering Apparatus
ASTM D 6147 : 1997 : R2020 Standard Test Method for Vulcanized Rubber and Thermoplastic Elastomer—Determination of Force Decay (Stress Relaxation) in Compression
ASTM D 5666 : 1995 : R2019 Standard Test Method for Rubber Chemical Antidegradants—Purity of <emph type="bdit" >p</emph>-Phenylenediamine (PPD) Antidegradants by High Performance Liquid Chromatography
ASTM D 6845 : 2018 Standard Test Method for Silica, Precipitated, Hydrated—CTAB (Cetyltrimethylammonium Bromide) Surface Area
ASTM D 3568 : 2003 : R2018 Standard Test Methods for Rubber—Evaluation of EPDM (Ethylene Propylene Diene Terpolymers) Including Mixtures With Oil
ASTM D 2240 : 2015 : EDT 1 Standard Test Method for Rubber Property—Durometer Hardness
ASTM D 5964 : 2016 Standard Practice for Rubber IRM 901, IRM 902, and IRM 903 Replacement Oils for ASTM No. 1, ASTM No. 2, ASTM No. 3 Oils, and IRM 905 formerly ASTM No. 5 Oil
ASTM F 1957 : 1999 : R2017 Standard Test Method for Composite Foam Hardness-Durometer Hardness
ASTM D 1414 : 2015 Standard Test Methods for Rubber O-Rings
ASTM D 6515 : 2000 : R2016 Standard Test Method for Rubber Shaft Seals Determination of Recovery From Bending
ASTM D 2137 : 2011 : R2018 Standard Test Methods for Rubber Property—Brittleness Point of Flexible Polymers and Coated Fabrics
ASTM D 7662 : 2015 Standard Test Method for Carbon Content in Carbon Black Feedstock Oils
ASTM D 991 : 1989 : R2020 Standard Test Method for Rubber Property—Volume Resistivity Of Electrically Conductive and Antistatic Products
ASTM D 3192 : 2009 : R2019 Standard Test Methods for Carbon Black Evaluation in NR (Natural Rubber)
ASTM D 471 : 2016 : REV A Standard Test Method for Rubber Property—Effect of Liquids
ASTM D 6499 : 2018 Standard Test Method for Immunological Measurement of Antigenic Protein in Hevea Natural Rubber (HNR) and its Products
ASTM D 5044 : 2006 : R2017 Standard Test Method for Rubber Compounding Materials—Free 2-Mercaptobenzothiazole (MBT) in Benzothiazyl Disulfide (MBTS)
ASTM D 1415 : 2018 Standard Test Method for Rubber Property—International Hardness
ASTM D 5963 : 2004 : R2019 Standard Test Method for Rubber Property—Abrasion Resistance (Rotary Drum Abrader)
ASTM D 6739 : 2020 Standard Test Method for Silica—pH Value
ASTM F 623 : 2019 Standard Performance Specification for Foley Catheter
ASTM D 1917 : 2003 : R2017 Standard Test Methods for Rubber Property—Shrinkage of Raw and Compounded Hot-Polymerized Styrene-Butadiene Rubber (SBR)
ASTM D 6204 : 2019 : REV A Standard Test Method for Rubber—Measurement of Unvulcanized Rheological Properties Using Rotorless Shear Rheometers
ASTM D 6281 : 2015 Standard Test Method for Airborne Asbestos Concentration in Ambient and Indoor Atmospheres as Determined by Transmission Electron Microscopy Direct Transfer (TEM)
ASTM D 3900 : 2017 Standard Test Methods for Rubber—Determination of Ethylene Units in Ethylene-Propylene Copolymers (EPM) and in Ethylene-Propylene-Diene Terpolymers (EPDM) by Infrared Spectrometry
ASTM D 7605 : 2011 : R2016 Standard Test Method for Thermoplastic Elastomers—Measurement of Polymer Melt Rheological Properties and Congealed Dynamic Properties Using Rotorless Shear Rheometers
ASTM D 623 : 2007 : R2019 Standard Test Methods for Rubber Property—Heat Generation and Flexing Fatigue In Compression
ASTM D 3493 : 2019 : REV A Standard Test Method for Carbon Black—Oil Absorption Number of Compressed Sample (COAN)
ASTM D 1937 : 2018 Standard Test Method for Carbon Black, Pelleted—Mass Strength
ASTM D 2084 : 2019 : REV A Standard Test Method for Rubber Property—Vulcanization Using Oscillating Disk Cure Meter
ASTM D 3191 : 2010 : R2014 Standard Test Methods for Carbon Black in SBR (Styrene-Butadiene Rubber)—Recipe and Evaluation Procedures
ASTM D 1618 : 2018 Standard Test Method for Carbon Black Extractables—Transmittance of Toluene Extract
ASTM D 1619 : 2016 : REV A Standard Test Methods for Carbon Black—Sulfur Content
ASTM D 4571 : 2006 : R2017 Standard Test Methods for Rubber Compounding Materials—Determination of Volatile Material
ASTM D 7558 : 2009 : R2019 Standard Test Method for Colorimetric/Spectrophotometric Procedure to Quantify Extractable Chemical Dialkyldithiocarbamate, Thiuram, and Mercaptobenzothiazole Accelerators in Natural Rubber Latex and Nitrile Gloves
ASTM F 414 : 2015 Standard Test Method for Energy Absorbed by a Tire When Deformed by Slow-Moving Plunger
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ASTM D 6924 : 2003 : R2017 Standard Specification for Preformed Thermoplastic Vulcanizate Elastomeric Joint Seals for Bridges
ASTM D 6600 : 2000 : R2017 Standard Practice for Evaluating Test Sensitivity for Rubber Test Methods
ASTM D 4937 : 1996 : R2017 Standard Test Method for <emph type="ital">p</emph>-Phenylenediamine Antidegradants Purity by Gas Chromatography
ASTM D 378 : 2010 : R2016 Standard Test Methods for Rubber (Elastomeric) Conveyor Belting, Flat Type
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ASTM D 7679 : 2016 Standard Test Method for Sulfur Content in Carbon Black Feedstock Oils
ASTM D 6085 : 1997 : R2016 Standard Practice for Sampling in Rubber Testing—Terminology and Basic Concepts
ASTM D 412 : 2016 Standard Test Methods for Vulcanized Rubber and Thermoplastic Elastomers—Tension
ASTM D 624 : 2000 : R2020 Standard Test Method for Tear Strength of Conventional Vulcanized Rubber and Thermoplastic Elastomers
ASTM D 1417 : 2016 Standard Test Methods for Rubber Latices—Synthetic
ASTM D 5289 : 2019 : REV A Standard Test Method for Rubber Property—Vulcanization Using Rotorless Cure Meters
ASTM D 2228 : 2004 : R2019 Standard Test Method for Rubber Property—Relative Abrasion Resistance by Pico Abrader Method
ASTM D 531 : 2015 : R2019 Standard Test Method for Rubber Property—Pusey and Jones Indentation
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ASTM D 3346 : 2017 Standard Test Methods for Rubber Property—Processability of Emulsion SBR (Styrene-Butadiene Rubber) With the Mooney Viscometer (Delta Mooney)
ASTM D 6915 : 2017 : EDT 1 Standard Practice for Carbon Black—Evaluation of Standard Reference Blacks
ASTM D 5668 : 2019 Standard Test Methods for Rubber From Synthetic Sources—Volatile Matter
ASTM D 4026 : 2006 : R2017 Standard Test Method for Rubber Latex—Styrene-Butadiene Copolymer—Determination of Residual Styrene
ASTM D 4572 : 1989 : R2017 Standard Test Method for Rubber Chemicals—Wet Sieve Analysis of Sulfur
ASTM D 3958 : 2006 : R2016 Standard Test Methods for Rubber—Evaluation of BIIR and CIIR (Halogenated Isobutene—Isoprene Rubber)
ASTM D 2663 : 2014 : R2019 Standard Test Methods for Carbon Black—Dispersion in Rubber
ASTM D 6556 : 2019 : REV A Standard Test Method for Carbon Black—Total and External Surface Area by Nitrogen Adsorption
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ASTM D 4986 : 2020 Standard Test Method for Horizontal Burning Characteristics of Cellular Polymeric Materials
ASTM D 7771 : 2017 : REV A Standard Test Method for Determination of Benzo-α-Pyrene (BaP) Content in Carbon Black
ASTM D 1076 : 2015 Standard Specification for Rubber—Concentrated, Ammonia Preserved, Creamed, and Centrifuged Natural Latex
ASTM D 1278 : 1991 : REV A : R2015 Standard Test Methods for Rubber from Natural Sources—Chemical Analysis
ASTM D 1510 : 2019 : REV A Standard Test Method for Carbon Black—Iodine Adsorption Number
ASTM D 380 : 1994 : R2020 Standard Test Methods for Rubber Hose
ASTM D 395 : 2018 Standard Test Methods for Rubber Property—Compression Set
ASTM D 573 : 2004 : R2019 Standard Test Method for Rubber—Deterioration in an Air Oven
ASTM D 4569 : 2006 : R2017 Standard Test Method for Rubber Compounding Materials—Determination of Acidity in Sulfur
ASTM D 5297 : 1995 : R2019 Standard Test Methods for Rubber Chemical Accelerator—Purity by High Performance Liquid Chromatography
ASTM D 4482 : 2011 : R2017 Standard Test Method for Rubber Property—Extension Cycling Fatigue
ASTM D 3492 : 2016 Standard Specification for Rubber Contraceptives (Male Condoms)
ASTM D 3186 : 2007 : R2016 Standard Test Methods for Rubber—Evaluation of SBR (Styrene-Butadiene Rubber) Mixed With Carbon Black or Carbon Black and Oil
ASTM D 4678 : 2015 : REV A : R2019 Standard Practice for Rubber—Preparation, Testing, Acceptance, Documentation, and Use of Reference Materials
ASTM D 6047 : 2017 Standard Test Methods for Rubber, Raw—Determination of 5-Ethylidenenorbornene (ENB) or Dicyclopentadiene (DCPD) in Ethylene-Propylene-Diene (EPDM) Terpolymers
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ASTM D 751 : 2019 Standard Test Methods for Coated Fabrics
ASTM D 5099 : 2008 : R2017 Standard Test Methods for Rubber—Measurement of Processing Properties Using Capillary Rheometry
ASTM D 5712 : 2015 Standard Test Method for Analysis of Aqueous Extractable Protein in Latex, Natural Rubber, and Elastomeric Products Using the Modified Lowry Method
ASTM D 2414 : 2019 Standard Test Method for Carbon Black—Oil Absorption Number (OAN)
ASTM D 1511 : 2012 : R2017 Standard Test Method for Carbon Black—Pellet Size Distribution
ASTM D 4573 : 2003 : R2018 Standard Test Method for Rubber Chemicals—Determination of Oil Content in Oil-Treated Sulfur
ASTM D 3185 : 2006 : R2016 Standard Test Methods for Rubber—Evaluation of SBR (Styrene-Butadiene Rubber) Including Mixtures With Oil
ASTM D 3189 : 2006 : R2016 Standard Test Methods for Rubber—Evaluation of Solution BR (Polybutadiene Rubber)
ASTM D 1329 : 2016 Standard Test Method for Evaluating Rubber Property—Retraction at Lower Temperatures (TR Test)
ASTM D 1509 : 2018 Standard Test Methods for Carbon Black—Heating Loss
ASTM D 4004 : 2006 : R2017 Standard Test Methods for Rubber—Determination of Metal Content by Flame Atomic Absorption (AAS) Analysis
ASTM D 5670 : 1995 : R2019 Standard Test Method for Rubber—Determination of Residual Unsaturation in Hydrogenated Nitrile Rubber (HNBR) by Infrared Spectrophotometry
ASTM D 1229 : 2003 : R2019 Standard Test Method for Rubber Property—Compression Set at Low Temperatures
ASTM D 3616 : 1995 : R2019 Standard Test Method for Rubber—Determination of Gel, Swelling Index, and Dilute Solution Viscosity
ASTM D 3190 : 2006 : R2016 Standard Test Method for Rubber—Evaluation of Chloroprene Rubber (CR)
ASTM D 3403 : 2007 : R2016 Standard Test Methods for Rubber—Evaluation of IR (Isoprene Rubber)
ASTM D 1991 : 2015 : R2019 Standard Test Method for Rubber Chemicals—2-Mercaptobenzothiazole (MBT)—Assay
ASTM D 4936 : 2010 : R2019 Standard Test Method for Mercaptobenzothiazole Sulfenamide Assay by Reduction/Titration
ASTM D 5775 : 1995 : R2019 Standard Test Method for Rubber—Determination of Bound Styrene in Styrene Butadiene Rubber by Refractive Index
ASTM D 6746 : 2015 Standard Test Method for Determination of Green Strength and Stress Relaxation of Raw Rubber or Unvulcanized Compounds
ASTM D 4075 : 2006 : R2017 Standard Test Methods for Rubber Compounding Materials—Flame Atomic Absorption Analysis—Determination of Metals

ASTM D 6600 : 2000 : R2023 Standard Practice for Evaluating Test Sensitivity for Rubber Test Methods
ASTM E 691 : 2020 Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
ASTM E 691 : 2019 : EDT 1 Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
ASTM E 691 : 2023 Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
ASTM E 691 : 2022 Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
ASTM E 691 : 2009 Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
ASTM E 691 : 2021 Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
ASTM D 6600 : 2000 : EDT 1 Standard Practice for Evaluating Test Sensitivity for Rubber Test Methods

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