Polymer Film Testing

Polymer Film Testing (Techniques and Analysis)
Polymer films are widely used in our every day lives. Today we will learn about the most common testing techniques used for polymer films and thin sheeting and the type of data that can be generated from those tests.
Oil, Chemicals and Agri (Caleb Brett Division)
March 2007
Industries That Commonly Use Polymer Films

Packaging
Food Non-Food
Building & Construction Trash Disposal (City and Town) Film Photography Electronics Adhesives (Tape) Medical
March 2007
Organizations for Test Standards

There are two primary standard organizations that govern the methodology of most plastics testing:
ASTM
American Society for Testing & Materials
ISO
International Organization for Standardization
March 2007
Polymer Film Testing

1. What is a film? 2. Specimen Preparation 3. Mechanical: Tensile, Puncture, Impact, Tear 4. Physical: Identification, Gage, Coefficient of Friction, Surface Energy, Density, Permeability, Blocking 5. Electrical: Dielectric Strength, DC/DF, Surface & Volume Resistivity 6. Thermal: Differential Scanning Calorimetry (DSC), Thermogravimetric Analysis (TGA), Coefficient of Thermal Expansion (CTE), Dynamic Mechanical Analysis (DMA) 7. Flammability: UL 94VTM, Oxygen Index (OI) 8. Accelerated Weathering: Xenon-arc & QUV exposure 9. Optical: Color, Gloss, Haze, Refractive Index, Yellowness Index
March 2007
What Is A Film?
A film is defined as sheeting having a thickness less than or equal to 250m (microns) which is equivalent to 0.010 (inches) which is equivalent to 10mils (thousandth of an inch) which is equivalent to 0.254mm (millimeters) If a material is greater than 250m, it is considered a sheet.
March 2007
Test Specimen Preparation
ASTM D6287 Standard Practice for Cutting Film and Sheeting Test Specimens this guide specifies techniques used for cutting narrow strips that will be used for tests like Tensile Properties of Film.
Procedure A employs the use of a Hand Rotatable Drum Cutter Procedure B employs the use of a Dual Blade Shear Cutter (used by Intertek PTL for producing Tensile specimens. This method does not address preparation of all specimens for film testing.
The objective is to produce straight, clean, parallel edges free of nicks or flaws The most important part of film testing (or any testing for that matter) is in the specimen preparation. Poorly prepared specimens will yield poor results that you do not have confidence in.
Oil, Chemicals and Agri (Caleb Brett Division) March 2007
Dual Blade Shear Cutter

Dual Blade Cutters
Support Platform
March 2007
Various Die Cutters Used For Producing Test Specimens
March 2007
Standard Laboratory Conditioning Prior To Testing

ASTM D618 Conditioning Plastics For Testing Six different procedures specified
Methods A through F Time, Temperature, Humidity, Immersion medium
Procedure A Condition 40/23/50 is common for most plastics and is the typical procedure for physical and mechanical film testing 40+ hours / 23C 2C / 50% RH 10%
March 2007
Tensile Properties of Film
Test Method: ASTM D882
Stress & Elongation

Crosshead Speed and Grip Separation are chosen based on elongation at break
Elongation less than 20% Speed = 0.5 in/min Grip Separation = 5.0 in Elongation 20% - 100% Speed = 2.0 in/min Grip Separation = 4.0 in Elongation greater than 100% Speed = 20 in/min Grip Separation = 2.0 in
Strain can be measured using crosshead displacement or extensometers
Modulus of Elasticity
Standard gage length specified is 10 inch Test speed of 1.0 in/min Stress at Yield Elongation at Yield Stress at Break Elongation at Break Modulus of Elasticity Tensile Energy to Break
Properties of Interest
March 2007
Tensile Properties
Response of a material to an axial deformation applied at a constant rate of speed.
March 2007
Tensile Properties
Tensile Strength = Force/Cross Sectional Area Tensile Strain = Change in Length/Original Length Elastic modulus = Change in Stress/Change in Strain in Elastic Region
March 2007
Tensile Properties of Film Specimen Preparation Dual Blade Shear Cutter

Dual Blade Cutters
Support Platform
March 2007
Razor Die
March 2007
Tensile Specimen In Test Grips
March 2007
Tensile Data : The Stress/Strain Curve

Yield Break
March 2007
Important Areas of the Stress/Strain Curve
Elastic and Plastic Regions Linear Elastic Region - follows Hookes law for an elastic material the stress is proportional to the strain. Plastic Region - area where permanent deformation occurs after release of load. Proportional limit Greatest Stress a material is able to sustain with out deviation from Hookes law. Elastic limit The greatest stress a material is able to withstand without permanent deformation remaining after release of load. Yield Point The first point on a stress strain curve that exhibits an increase in strain without a corresponding increase in stress.
March 2007
Flaw In Edge of Tensile Specimen
March 2007
Seal Strength
Test Method ASTM F88

Technique A: Unsupported Technique B: Supported 90 (By Hand) Technique C: Supported 180
Force required to separate a seal prepared in a test strip

Useful for monitoring package integrity Quality control and R & D Strong seals to prevent a package from being opened Sometimes the objective is to keep the force to a minimum so a package can be easily opened
March 2007
Puncture Slow Rate Penetration of Films
Test Method MIL-STD-3010B Method 2065 (formerly FTMS-101C)

1.0 inch diameter support opening 0.250 inch diameter probe end (tapered probe) Test speed = 20 in/min
Test Method ASTM F1306 (packaging materials)

1.375 inch diameter support opening 0.125 inch diameter probe end (tapered probe) Test speed = 1.0 in/min
Force At Break (Newtons or Pounds) Energy To Break (Joules or Ft-lbs/inch) Probe Penetration (Millimeters)
March 2007
Slow Rate Puncture Probes
MIL-STD-3010B Method 2065
ASTM F1306
March 2007
Base Clamp and Puncture Probe
Penetration Probe Film
Clamp Opening
March 2007
Slow Rate Puncture Graph
Layer 1 Maximum Load Layer 2 Maximum Load
March 2007
High Speed Puncture Properties of Plastic Films Using Load and Displacement Sensors
ASTM D7192
Specimen : 100 mm diameter or square (or 13mm greater than base opening diameter used) Preferred striker: 12.7mm Support diameter: 76mm Impact Velocity: 200 m/min (3.3 m/s) Other support openings and velocities can be used
March 2007
Multi Axial Impact Data Generated
Maximum load required to penetrate or break a specimen

Units: lbs or Newtons
Energy absorbed by the specimen

Units: FT-lbs or Joules
Displacement of specimen during impact

Units: inches or mm
Time of impact event

Units: milli-seconds
Load - Time (or displacement)-Energy curves
March 2007
Multiaxial Impact Tester
Weighted Crosshead
Load Cell
Electric Eye
March 2007
Multiaxial Impact Clamping Mechanism
Tup / Dart / Impact Head
Clamp
Specimen
March 2007
Typical Load-Time-Energy Curve - Ductile Material

Maximum
Load Energy @ maximum load Total Energy
Energy Curve Load Curve
March 2007
Impact Resistance of Plastic Film by the Free-Falling Dart Method

Test Method ASTM D1709
Test method A: 38 mm (1.5") diameter dart dropped from 0.66 m (26") Test method B: 51 mm (2") diameter dart dropped from 1.5 m (60")
Specimen Clamp = 125mm (5.0) diameter Property of Interest: Impact failure weight in grams force
March 2007
Close Up Of Clamping Mechanism ASTM D1709
Falling Dart
Specimen
Clamp
March 2007
March 2007
Comparison of Multiaxial Impact and Free-Falling Dart Impact Multiaxial Impact Free-Falling Dart
Test is designed so
that dart penetrates through specimen.
Bruceton Staircase
technique
Instrumented Test Data genertaed

Load Energy Displacement
Non-instrumented Data generated

Failure weight
March 2007
Tear Testing

Elmendorf Tear (ASTM D1922)
Tear propagation
Graves Tear (ASTM D1004)

Tear initiation
Trouser Tear (ASTM D1938)

Tear propagation
March 2007
Elmendorf Tear
Pendulum Tester Constant Radius Die & Specimen
March 2007
Elmendorf Tear
Specimen Types
Test Method ASTM D1922 Pendulum Impact Tester Three different specimen types
Constant Radius (preferred for plastics) Rectangular Textile Specimen
Data Generated
Tear Resistance in grams force
March 2007
Graves Tear
Grips & Specimen Die & Specimen
March 2007
Graves Tear
Test Method ASTM D1004 Tear Initiation Performed on a universal tester
1.0 grip separation 2.0 in/min test speed
One specimen type

90 degree angle to create stress concentration
Data Generated
Tear Resistance in Newtons Maximum extension in Millimeters
Not applicable for specimens that fail in a brittle manner or extend more
than four inches during test
March 2007
Trouser Tear
Test Method ASTM D1938 Tear Propagation Performed on a universal tester
2.0 grip separation 10 in/min test speed
One specimen type

Trouser specimen with two tongues
Data Generated
Tear Propagation in Newtons Maximum extension in Millimeters
Not applicable for specimens that fail in a brittle manner
March 2007
Material Identification by FTIR

A basic generic polymer identification of an unknown material can be determined by FTIR. The first logical step in identifying an unknown polymer is to generate an infrared scan of the unknown. The unknowns infrared spectral scan can then be analyzed to determine the base material of the unknown. The following cannot be determined (with confidence) by FTIR analysis: the polymer manufacturer, the specific type of nylon or polyester, whether a polyethylene is high density or low density, whether an acetal is copolymer or homopolymer, or the identification of specific additives or colorants used. Further analytical techniques are necessary for these situations.
A skilled FTIR analyst is needed to examine the computer selected spectral matches to ensure that sample identifications are both accurate and complete.
March 2007
FTIR Equipment
FTIR: Fourier Transform Infrared Spectrometer for Material ID
March 2007
Close-up of FTIR
This photo shows the top of the FTIR. The sample would be placed where you can see the circle. An anvil, located in the center of the open gate, is used to compress non-liquid samples against a diamond ATR top plate. The top plate is located inside the light grey circle centered under the open gate.
March 2007
Simplistic Attenuated Total Reflectance Process
Sample
ATR Crystal
IR Light To Detector
IR Light From Source
March 2007
March 2007
Quality Control
A spectral scan of a reference material can be generated and stored in a spectral search database. A stored reference scan will allow all future material spectra to be compared back to the same earlier scan. The objective is to look for material differences. Differences noted in a newly generated spectral scan could indicate a change in processing or a possible contamination of the polymer.
March 2007
Polymer Contamination
FTIR spectral subtractions can be used to look for contamination in polymers. The amount of contamination that can be detected depends on the polymers involved. Contamination involving polymers with very different infrared spectra can be detected at a level of about 1-2%. Contamination involving polymers with similar infrared spectra may not show up at even the 10% level.
March 2007
Limitations of Computerized Searches
Computer programs are very helpful for comparing unknown spectral scans to those of known materials, but computer selected matches can be misleading. Small spectral databases, polymer blends, fillers, certain types of additives, and sample contamination can cause computerized search programs to suggest inappropriate matches.
March 2007
Film Thickness (a.k.a. Gage)
Drop Dial Gauge ASTM D6988 Apparatus A

Techniques For Measuring Film Dimensions
ASTM D6988 - Standard Guide for Determination of Thickness of Plastic Film Test Specimens
Apparatus AManually Operated Thickness Gauge Apparatus BAutomatically Operated Thickness Gauge Apparatus CManually Operated Thickness Gauge with Linear Optical Encoder Apparatus DAutomatically Operated Thickness Gauge with Digital Display
ASTM D5947 - Standard Test Methods for Physical Dimensions of Solid Plastics Specimens
This is an actual test method unlike ASTM D6988 which is a guide. References four different types of measuring devices that can be used. References five different test methods that can be used. Film test methods typically refer to ASTM D5947 stating which technique is to be used for measuring the test specimens for that particular test. For example: ASTM D882 (Tensile Properties of Films) requires Method C of ASTM D5947 to be used for measuring thickness of tensile strips.
March 2007
Common Units of Thickness Measurements For Films
Micron (m) = one millionth of a meter Inch (in. or ) Mil (one thousandth of an inch) Millimeter (mm)
1m = 0.000039in = 0.039mil = 0.001mm
March 2007
Coefficient of Friction

Test method ASTM D1894 Moving sled with stationary plane, or Stationary sled with moving plane Sled = 2.5 x 2.5
Foam wrapped 0.25 g/cm3 nominal foam density Sled weight = 200 5 grams
Stationary plane of suitable size to allow sled to be pulled sufficient distance (4 x 10 minimum) Test speed = 6.0 in/min
March 2007
Coefficient of Friction
Pulley Monofilament
Stationary Substrate
Moving Sled
March 2007
Coefficient of Friction (Important Considerations)
Condition of surfaces
Dust Grease Fingerprints
Slip Agents
Blooming Action
Direction of pull
Machine direction Transverse direction
Foam Pad
Density (0.25 g/cm3) Pressure to compress (12.5 psi at 25% compression)
Level base Technique

Consistency between technicians Consistency during test
Total weight of sled

200 5 grams
Coefficient of Friction Calculations
Static Coefficient of Friction = Initial force to initiate sled movement divided by sled weight. Kinetic Coefficient of Friction = Mean force over five inch distance divided by sled weight.
March 2007
Static COF
March 2007
Surface Energy

Test method ASTM D5946 Uses a Contact Angle Goniometer for measuring water droplet angle Adhesion of various materials to film Inks Paints Clear Coats Film surfaces are often treated to increase adhesion properties. Wetting out versus beading up
Wetting out - the spreading of a liquid over a surface
Contact angle can be related to a films ability to accept and retain inks, coating, adhesives, etc. Important Considerations Static Charge Specimens should not be handled in the measurement area Water Quality Cleanliness of glass substrate Droplet angle measurement interpretation
March 2007
Goniometer For Measuring Contact Angle
Magnifier
Syringe
Test Strip
March 2007
Contact Angle Water Droplet
March 2007
Specific Gravity and Density

Specific Gravity is the ratio of the weight of a given
volume of sample to that of an equal volume of water at a specific temperature.
Temperature normally 23.0C Specific Gravity =Dry Wt / (Dry Wt Wet Wt) Dry Wt = Apparent Weight in Air Wet Wt = Apparent Weight in Water
Density (g/cm3) = Specific Gravity x 0.9976
March 2007
Dry Weight Measurement
March 2007
Wet Weight Measurement
March 2007
Permeability

Water Vapor Transmission (Test Method ASTM E96)
Manual weight technique
Water Vapor Transmission (Test Method ASTM F1249)

Instrumented technique using modulated infrared sensor
Oxygen Transmission (Test Method ASTM D3985)

Instrumented technique using a coulometric sensor
March 2007
Water Vapor Transmission (ASTM E96)
Water Vapor Transmission (Test Method ASTM E96) Manual weight technique Procedure A Desiccant method at 23C Procedure B Water method at 23C Procedure BW Inverted Water method at 23C Procedure C Desiccant method at 32C Procedure D Water method at 32C Procedure E Desiccant method at 38C Water Vapor Permeance the time rate of water vapor tramsmission through unit area of material. The average permeability is expressed as follows: Average Permeability (g/Pasm) Water Vapor Transmission rate the steady water vapor flow in unit time through unit area of a material. The Water Vapor Transmission is expressed as follows: Water Vapor Transmission (g/hrm)
ASTM E96 Test Dish Assembly

Test Dish Gasket / Seal Specimen
March 2007
Water Vapor Transmission (ASTM F1249)

Dry chamber separated from wet chamber by the barrier material Dry chamber and the wet chamber make up a diffusion cell in which the test film is sealed. Water vapor diffusing through the film mixes with the gas in the dry chamber Carried to a pressure-modulated infrared sensor. Sensor measures the fraction of infrared energy absorbed to produce electrical signal. The amplitude is compared to a calibration film of known water vapor transmission rate. Information is then used to calculate the rate at which moisture is transmitted through the material being tested.
March 2007
Oxygen Transmission Rate

Test Method: ASTM D3985 Oxygen gas transmission rate is determined after the sample has equilibrated in a dry test environment. Specimen is mounted in apparatus and acts as a sealed semi-barrier One chamber purged by nitrogen and the other contains oxygen. As oxygen gas permeates through the film, the nitrogen carrier gas it transports it to the detector. Electrical current is generated which allows for measurement of oxygen flowing into the detector per unit time. Oxygen permeance (PO2) = mol/(m2sPa) Oxygen transmission rate (O2GTR) = mol/(m2s)
March 2007
Equipment for measuring gas permeation rates
slide provided by
Flow thru technology
Test gas Diffusion cell
To vent
Test film
Test film
Carrier gas
To the detector
slide provided by
Testing a formed bag

Entire assembly in either the atmosphere or controlled environment
( BAG )
Package mounting fixture
slide provided by
Blocking Load of Plastic Films

Test Method ASTM D3354 Blocking = unwanted adhesion Force required to separate two pieces of film blocked together Procedure A: Modified Balance Technique
Utilizes a two-pan balance and water titrator
Procedure B: Universal Tester / Load Cell Technique

Technique used by Intertek PTL 5.0mm/min 4 x 4 aluminum blocks to wrap film around
Load in grams
March 2007
Blocking Apparatus (ASTM D3354 Procedure B)
Load Cell
Mounting Blocks
Film Specimens
March 2007
Electrical Properties of Film

Dielectric Strength Dielectric Constant / Dissipation Factor Volume Resistivity and Surface Resistivity
March 2007
Dielectric Strength

Test Method: ASTM D149 Alternating current with a frequency of 60Hz Opposing Electrodes
0.25, 1.0 and 2.0 diameter are common. 2.0 is typical for film specimens.
Dielectric Breakdown Voltage the potential difference at which dielectric failure occurs on a material located between two electrodes. Dielectric Strength the voltage gradient at which dielectric failure of the insulating material occurs. Method A: Short-time Test Voltage increase at a rate to produce breakdown within 10 to 20 seconds. (Most common method) 500 Volts per second is a common rate Method B: Step-by-Step Test Voltage applied in steps and held at each step for a duration until breakdown occurs. Breakdown should occur in four to ten steps. Method C: Slow Rate-of-Rise Test Typical rate of applied voltage is between 1 and 100 Volts per second.
March 2007
Typical Film Set-up (Dielectric Strength)
Voltage In
Electrodes Specimen
Ground
March 2007
Dielectric Strength
Air Oil
March 2007
Dielectric Constant / Dissipation Factor

Test Method ASTM D150 Dielectric Constant (Relative Permittivity)
A measure of the ability of an insulator to store electrical energy Specimen capacitance divided by the air capacitance using the same electrode configuration
Dissipation Factor (Loss Index)

Measures the inefficiency of an electrical insulating material. The ratio of the power dissipated in the test material to the power applied
March 2007
DC/DF Equipment
Electrodes
March 2007
Surface & Volume Resistivity

Test Method: ASTM D257 Surface Resistance - the resistance to leakage current along the
surface of an insulating material. Surface Resistivity the surface resistance multiplied by the ratio of specimen surface dimensions which transforms the measured resistance to that obtained if the electrodes had formed the opposite sides of a square. Units = ohms (per square) or /square
Volume resistance - the resistance to leakage current through the body of an insulating
material. Volume Resistivity the volume resistance multiplied by the ratio of specimen volume dimensions which transforms the measured resistance to that resistance obtained if the electrodes had formed the opposite sides of a cube. Units = ohms-cm or -cm
The higher the surface/volume resistivity, the lower the leakage current and the less
conductive the material is.
March 2007
Surface & Volume Resistivity Equipment
Electrodes
March 2007
Differential Scanning Calorimetry
Test Method: ASTM D3418 Used for material identification, locate transitions, crystallinity Transition temperatures of polymers / properties of interest
Tm (melting point)
10C/min
Tg (glass transition temperature)
20C/min
Hm - the amount of energy in joules/gram a sample absorbs while melting Tc - the temperature at which a polymer crystallizes upon heating Hc - the amount of energy in joules/gram a sample releases while crystallizing.
March 2007
Differential Scanning Calorimetry
March 2007
Differential Scanning Calorimetry (Perkin Elmer DSC-7)
March 2007
DSC Sample and Reference Heads
March 2007
Thermogravimetric Analysis

Test Method: ASTM E1131 Measure resin content vs. filler content
March 2007
TGA Scan
March 2007
Coefficient of Thermal Expansion

Test Method: ASTM E831 Thermal Expansion by Thermal Mechanical Analyzer
March 2007
Thermomechanical Analyzer
Measurement Probe Specimen Cooling/Heating Chamber
March 2007
Film Specimen in TMA Holder
March 2007
CTE Graph
March 2007
Dynamic Mechanical Analysis (DMA)
Environmental Chamber
Specimen Clamp Test Specimen
March 2007
Dynamic Mechanical Analysis - Tension

Test Method ASTM D5024 (Tension) Measure stiffness as a function of temperature Detect transitions like glass transition and other molecular movements Quality Control Failure Analysis Application Specific Studies
Shrink Wrap - Axial force changes with temperature
Elastic or Storage modulus E1 - Elastic Component of the polymer. stiffness Loss Modulus E11 - The viscous or dissipative component of the polymer. Energy lost to friction and internal motions Tan Delta ratio of E11 to E1 relative degree of damping of the material. How efficiently a material loses energy to molecular rearrangements and internal friction
March 2007
DMA Plot Of A Nylon Polymer
10
10
0.14 Temp = 78C

Point A
Rubbery Plateau
0.12
0.1
10
tan_delta ( []
) G" ( [Pa]
from E Plateau Curve G'Tg Rubbery (half height) Point C
0.08
E11
G' ( [Pa]
0.06
E1
108 0.04
0.02
Point B
10 7 -150.0
Temp = -62C 0.0

-100.0 -50.0 0.0 50.0 100.0 150.0 200.0
250.0
Tem p [C]
March 2007
Flammability Testing

Test Method: UL 94VTM (Very Thin Materials) Vertical Burning Test Specimens tested after conditioning at 23C/50% RH Specimens tested after conditioning at 70C for 168 hours in an air circulating oven Test specimens are wrapped around a 12.7mm mandrel and clamped and hung vertically from one end. 20mm flame height Flame applied 10mm below specimen for three seconds Flame Ratings
VTM-0 VTM-1 VTM-2
UL 94 VTM
Specimen
Flaming
Burner
March 2007
Oxygen Index Testing

Test Method: ASTM D2863 Measures the minimum oxygen concentration to support candle-like combustion
March 2007
Accelerated Weathering
(Left) Q-Panel QUV/se Tester used for UV-A&B, Condensation Exposure of Plastics, Paints and related coatings. (Right) Atlas Electric Ci4000 Xenon Arc Weatherometer for ASTM G155, SAE J1960 SAE 1885.
March 2007
Example of how the weather can effect a polymer
The polymer on the left contains a UV Stabilizer. The polymer on the right does not. Notice the severe discoloration, loss of gloss and degradation
March 2007
Optical Testing
Color (ASTM E308, ASTM D6290) Ultra-Violet and Visible (UV/VIS) light absorption or transmission Refractive Index (ASTM D542) Gloss (ASTM D523) Haze & Luminous Transmittance (ASTM D1003) Yellowness Index (ASTM E313)
March 2007
Case Study
United States Postal Service USPS-T-3204 Outlines procedures for testing polywrap film used to enclose flat mail pieces
that are destined for automated sorting operations. Film Thickness (ASTM D374)
Thickness must be greater than 0.001
Tensile Modulus (ASTM D882)

1% Secant Modulus in MD must be greater than 40,000 psi 1% Secant Modulus in TD must be greater than 50,000 psi
Haze & Luminous Transmittance (ASTM D1003)

Haze must be less than 70%
Coefficient of Friction (ASTM D1894)

Film on Film must fall between 0.20 and 0.55 Film on Metal must be less than 0.45
Blocking Resistance (ASTM D3354)

Must be less than 15 grams of force
Static Electrification (ASTM D4470)

Must be less than 2.0 kilovolts
Testlopedia (Comprehensive Test Descriptions)
Testlopedia,
Free encyclopedia of
plastics tests on www.ptli.com Intertek PTLs index of plastics testing facilitates: Search by test type View test equipment used at Intertek PTL Determine appropriate scope & sample size

Polymer Film Testing

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Polymer Film Testing (Techniques and Analysis)

Oil, Chemicals and Agri (Caleb Brett Division)

Industries That Commonly Use Polymer Films

Oil, Chemicals and Agri (Caleb Brett Division)

Organizations for Test Standards

Oil, Chemicals and Agri (Caleb Brett Division)