`
`Association of PostconsumerPlastic Recyclers
`1001 G Street, NW, Suite 500,
`Washington D.C. 20001
`
`www.plasticsrecycling.org
`
`Champions for Change
`Applications Guidance for Innovations
`“HDPE Bottles Applications Guidance Document”
`
`The Association of Post Consumer Plastic Recyclers (APR) recognizes that packaging innovation
`drives the growth of bottles available for recycling and that growth in the supply of these bottles
`is essential to the well being of the plastic bottle recycling industry. APR also recognizesthat
`some innovations maycreate bottles that present technical challenges for recycling. This
`documentrepresents a tool to help the innovator understand the approximate effect of the
`innovation on high density polyethylene (HDPE)plastic bottle recycling processes.
`
`The APR encourages Innovators to perform comprehensive recycle evaluation studies on new
`innovation materials intended to be introduced into the HDPEbottle stream. This Applications
`Guidance Documentdescribes the protocols to be followed to evaluate the mechanical
`recyclability of the following Innovation materials that are intended to be madeinto or
`incorporated onto HDPEbottles:
`
`AwARwnr
`
`HDPEResins
`Additives
`Coatings
`Labels
`Adhesives
`Multilayer resins
`
`In particular, a comprehensive recycling evaluation is accomplished by following a step-wise
`process involving the evaluations of the innovation using Testing Protocols that have been
`developed by APR. APR recognizes accomplishmentand allows upon petition for the Innovator
`to publicize that they have completed each step. The steps include:
`
`STEP 1
`
`1.00 CRITICAL GUIDANCE DOCUMENT
`1.10 Resins, Additives, Coatings, Labels, Adhesives and Multilayer Resins
`Evaluation Protocol, Critical Guidance
`
`Approved by APR Board May 13, 2009
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`Page 1 of 11
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`Edition I
`
`EPL LIMITED EX1019
`U.S. Patent No. 10,889,093
`
`EPL LIMITED EX1019
`U.S. Patent No. 10,889,093
`
`

`

`STEP2
`
`2.00 APPLICATIONS GUIDANCE DOCUMENT
`2.10 Bottle-To-Bottle Evaluation, (BtB)
`
`Upon the completion ofall parts of STEP 2, meeting or exceedingall of the strictest guidance,
`APR would considera petition for full Recycling Guidance Recognition.
`
`The screening tool referred to above in STEP 1 as the HDPECritical Guidance document (CGD)
`is intended to help identify possible technical challenges that a new Innovation might create for
`the HDPErecycle stream. An Innovatoris requested to first test an innovation material following
`the CDG before proceeding to STEP 2 and the more extensive Bottle-to-Bottle evaluation.
`
`Whencoupling the CGD screening protocol with a Bottle-to-End-Use evaluation, it is necessary
`to increase the quantity of the Control and Innovation materials used in the CGDprotocolto
`producesufficient material for making the finaltest bottles
`
`The guidance contained in this document doesnot include time as a variable. Innovations which
`include timeas a factor will require additional considerations.
`
`THIS DOCUMENTIS NOT A SPECIFICATION AND DOES NOT IMPLYIN ITS
`
`DEFINITIONS, PROCEDURES, OR VALUES FITNESS FOR USE, MARKET
`
`ACCEPTABILITY, SAFETY, OR ANY GUARANTEE OR WARRANTY. MEETING
`THESE GUIDELINES DOES NOT OBLIGATE APR MEMBERSTO BUY BOTTLES
`CONTAINING THE INNOVATION.
`
`Moreover,the inability of an innovation to meet specified values does not imply recycling failure,
`but should be a clear messagethat significant technical challenges might exist under certain
`circumstances and mitigation of the issue may be needed to avoid degrading the value of the
`stream of recyclable bottles.
`
`THE FOLLOWING PROTOCOLS DO NOT PURPORT TO ADDRESS ALL OF THE
`
`SAFETY ISSUES, IF ANY, ASSOCIATED WITH THEIR USE.
`IT 1S THE
`RESPONSIBILITY OF THE USER TO ESTABLISH APPROPRIATE SAFETYAND
`HEALTH PRACTICES AND DETERMINE THE APPLICABILITY OF REGULATORY
`LIMITATIONS PRIOR TO USE.
`
`1.0 CRITICAL GUIDANCE DOCUMENT(CGD)
`Introduction
`The CGDis intendedto be a screening tool that can be used by Innovators to gain a quick
`understanding on the impact of their innovation on the HDPErecycle stream before proceeding to
`the more extensive Bottle-to-Bottle Protocol and other end use protocols. While the CGD
`protocol is designed as a recycle screening protocol, the material that has been processedin the
`CGDstudy can then be usedasthe starting material to continue the recycle evaluation through a
`Bottle-to-Bottle study.
`
`Testing Procedures
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`

`The procedures needed for performing the tests called for in the recycling protocols are listed
`below:
`
`Color (ASTM D6290)
`Melt Index (ASTM D1238)
`Density (ASTM D1505, ASTMD792,or equivalent)
`Melt filtration
`% polypropylene in HDPE (ASTM D7399)
`
`Testing Protocols
`The detailed protocols to be followed are listed below andare describedin detail in this
`document.
`
`e
`
`1.10 Resin, Additives, Coatings, Labels, Adhesives, and Multilayer Resins, Critical
`Guidance
`
`ControlResins
`The virgin control resins that can be selected for use following the CGDare listed below. The
`Innovator is requested to select a Control resin based uponits intended end-use application. These
`resins are to be used to make both the Control flake and the Innovation bottle flake that will
`contain the additive, coating, label, adhesive or multilayer resin for the recycle study.
`
`Homo Polymer HDPE
`Chevron Phillips Marlex® EHM 6007
`Dow UNIVAL™ DMDH-6400 NT 7
`Exxon-Mobil Paxon™ HDPE AD60-007
`
`Copolymer HDPE
`Chevron Phillips Marlex® HHM 5502BN
`Chevron Phillips Marlex® 9505H
`Dow UNIVAL™ DMDA-6230 NT 7
`Dow UNIVAL™ DMDA-6200 NT 7
`ExxonMobil Paxon™ HDPE AB50-003
`
`Labels and Adhesives
`If the innovation does not involve labels or adhesives, and if it can be correctly argued that labels
`and adhesives have no impact on the innovation,
`the innovation samples can be made and
`processed without the presence of labels or adhesives.
`
`1.10 Resins, Additives, Coatings, Labels, Adhesives and Multilayer Resins Evaluation
`Protocol, CRITICAL GUIDANCE
`
`Background
`The control bottles required for this test must be made from one of the APR-namedcontrolresins.
`The bottles can be supplied from commercial sources or blown as a separate test set and do not
`
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`

`have to be of any special design or size. The additive, coating, label, adhesive or multilayer resin
`to be evaluated should be incorporated into or onto bottles made using the same control resin.
`
`Resins, Additives, Coatings, Labels Adhesives, and Multilayer Resins Test Protocol
`Forall extrusion and molding steps, the process should first be established on the Control resin
`and then used without changes for the innovation materials. Any required processing changes for
`the innovation material content samples should be documented and reported. It is recognized that
`minor process changes may be needed andthese will not be considered significant when judging
`the innovation materials suitability for recycling.
`
`Resins, Additives, Coatings, Labels, Adhesives, and Multilayer Resins
`
`Evaluation Flow Schematic
`HDPE Resins, Additives, Coatings, Labels, Adhesives and Multilayer Resin Protocol
`GENERAL APPLICATIONS GUIDANCE
`
`Contro! Bottles
`
`Innovation Bottles
`
`
`
`elutriate
`
`Grind, Elutriate
`
`
`
`Grind, Elutriate
`
`Wash, sink/float, air dry,
`
`Wash, sink/float, air dry,
`
`elutriate
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`Bottle-to-Bottle
`Bottle-to-Bottle
`
`
`Sample Blends
`Sample Blends
`
`
`
`Sample F
`Sample E
`Sample D
`
`
`
`50% Sample C2
`50%Sample B2
`50% Sample A2
`
`50%Control
`50%Control
`50%Control
`
`
`pellets
`pellets
`pellets
`
`
`
`
`Bottle Blowing
`Bottle Blowing
`Bottle Blowing
`
`
`Sample F4
`Sample D4
`Sample E4
`
`
`
`Bottle Testing,
`Bottle Testing,
`
`
`Evaluation
`Evaluation
`
`Bottle-to-Bottle
`Sample Blends
`
`Bottle Testing,
`Evaluation
`
`
`
`
`
`Melt blend
`
` Melt blend
`Sample F and
`
`
`test Sample J5
`
`H5 molding for
`molding for
`
`stress crack
`stress crack
`
`
`
`
`Control and Innovation/Variant Bottle Manufacture
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`

`1. Control bottles should be made from one of the namedresins listed in the APR Bottle
`Recycle Evaluation Protocol. The Innovation bottles should be made with this same resin
`incorporating the resin, additive, coating or multilayer resin at the intended use level.
`
`Flake Preparation
`The Reclaim Processing Test Protocol is to include butis not limited to the following:
`1. The Control bottles and Innovation bottles should be dry-ground to nominal %” to %”
`size flake.
`2. Air elutriate to removelight fractions with one pass and with less than 2% loss set for
`the Control Flake. (Note: This step may be eliminated if these samples are wet ground.
`If omitted, more innovation failures may occur.)
`3. Wash in highly agitated water at least 60° C for 10 to 15 minutes. Water may contain
`surfactants and have a pH of 12 to 13. Report wash solution composition.
`Specific gravity separation in water of materials with density greater than 1.0.
`Skim off and collect any material that is floating after the wash.
`Air-dry flakes with no heat or vacuum
`A secondair elutriation to removelight fractions with one pass and with less than 2%
`loss set for the Control Flake may be carried out on the dried washed flake
`
`raws
`
`Extrude, including meltfiltration, to produce product pellets as below.
`
`Sample Blending
`Washed flake from number6 or 7 above will be used to make the required Samples.
`1. Prepare samples AO and I0 above. Air dry AO and10 at room temperature for 24 hours, no
`vacuum or heat applied either as number6 aboveor after number 7 above.
`2. Create the following three test blends from the washedflake for study:
`Sample Al:
`100% Control Material, AO
`0% Innovation Material, I0
`Sample B1:
`75% Control Material, AO
`25% Innovation Material, I0
`Sample C1:
`50% Control Material, AO
`50% Innovation Material, 10
`3. Measure volatiles on flakes. For 10 grams of air-dried flake Samples Al, B1, and Cl
`exposed to 160°C for 10 minutes,
`
`Guidelines comparing Samples B1 and C1 to Control Al
`a. Less than 0.2% absolute difference after exposure for Samples B1 and C1 compared to
`Sample Al, Use moisture analyzerfor measurement.
`
`Extrusion/Pelletization
`1. Dry samples Al, B1 and C1 at no more than 150 F for 10 minutes before extrusion.
`2. Extrude under conditions determined by the control sample, Sample A1, using a
`40/150/40 meshscreen pack.
`3. Pelletize each of the sample blends, giving each its second melt history. Make Sample A2
`from flake blend Al, Sample B2 from flake blend B1 and Sample C2 from flake blend C1.
`
`Guidelines comparing Samples B2 and C2 to Control A2
`a. No more than 10% higher pressure required on extrusion ofthe Innovation Samples B2
`and C2 compared to the Control Sample A2 after 30 minutes ofextrusion.
`b. The extrusion rate should be at least 500 gm/cm’ per hour.
`c. No additional fuming, smoking or odors should be noticed when extruding the
`Innovation Samples comparedto the Control.
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`d. No build up on screen
`e. Resin pellets orflakes should not stick together during drying.
`
`Pellet evaluation
`1. Measure volatiles on pellets after extrusion.
`For 10 grams of air-dried pellets Samples A2, B2, and C2 exposed to 160°C for 10
`minutes.
`Guidelines comparing Samples B2 and C2 to Control A2
`a. Less than 0.1% absolute difference after exposure for Samples B2 and C2 compared to
`Sample A2. Use moisture analyzerfor measurement.
`
`2. Measure melt index for samples A2, B2, and C2
`Guidelines
`a. For copolymer HDPE, 0.2 to 0.7 gm/10 minutes, Samples A2, B2, and C2
`b. For homopolymer HDPE, 0.2 to 0.9 gm/10 minutes, Samples A2, B2, and C2
`
`3. Measure density for samples A2, B2, and C2
`Guidelines
`a. For copolymer and homopolymer HDPE, Samples B2 and C2 are +/- 0.010 gm/cm?
`compared to Sample A2. C2 alwaysless than 0.995 gm/cm3.
`
`4. Measure percentage polypropylene for samples B2, and C2
`Guidelines
`a. For copolymer and homopolymer HDPE, Samples B2 and C2 are less than 2%
`polypropylene (totalpercentpolypropylene in innovation bottles less than 4%).
`
`Plaque Molding (natural homopolymer)
`1. Dry samples A2, B2, and C2 at no more than 150 F for 10 minutes before extrusion.
`2.
`Injection mold 3mm plaques from the control Sample A2 first. Then mold 3mm plaques
`from Samples B2 and C2 under identical conditions if possible to form plaque samples
`A3, B3, and C3. If the processing conditions need to be changed, then these changes must
`be documented and reported.
`Guidelines comparing Samples B2 and C2 to Control A2 or comparing Samples B3 and C3 to
`Control A3
`a. 3mm Plaque Colorfor Sample Plaques A3, B3 and C3 or Pellets A2, B2, and C2.
`i, For natural HDPE, L* should be >63 for Samples A3 and C3 or Samples A2 and
`C2
`a* greater than -4.5for Samples A3 and C3 or Samples A2 and C2
`b* less than 13 for Samples A3 and C3 or Samples A2 and C2
`NOTE:color can be measured on plaquesorpellets
`
`li,
`iii.
`
`NOTE: This completes the Critical Guidance Document requirements. If a Bottle-to-Bottle
`study is beingperformed, then continue with thefollowing steps.
`
`2.0 APPLICATIONS GUIDANCE
`2.10 Bottle-to-Bottle Protocol (BtB)
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`The Bottle-to-Bottle evaluation program is designed to show processing and bottle performance
`differences between a control material and that control material containing recycle-content
`Innovation material. It is a generally comparative study that does notrely on the final blown
`bottles meeting absolute performancecriteria other than minimumslisted.
`
`Since the Bottle-to-Bottle program is designed to use a one quart generic monolayer motoroil
`bottle the optimal study will be one wherethe initial control resin selected for use in the Critical
`Guidance Documentscreening will be selected from the list of APR-named control HDPEresins.
`The Control homopolymervirgin resin called for in Step 1 below ideally would be identical to the
`Critical Guidance Documentcontrolresin.It is recognized that if the Innovation being studied in
`the Critical Guidance Documentis a copolymerresin or an additive incorporated into a
`copolymerresin, it may not be ideal for motor oil bottle performance. Howeverthis non-base
`material can still be blended with a control (selected from the table above) to begin the Bottle-to-
`Bottle evaluation. Whenthisis the case,it is important to recognize that the resulting control
`bottles and Innovation recycle-content bottles may not perform ideally in all ofthe tests. Since the
`bottle test performanceof the Innovation recycle-content bottles will be compared to the control
`bottles, it will still be possible to judge the Innovation's compatibility for the recycle stream if the
`bottle test criteria are met. Because the non control materials are currently found in the recycle
`stream, it can be presumed then any new material similar to these that does not result in
`significant differences in recycle-content bottle performanceare, therefore, also expected to be
`compatible.
`
`1. Create the following test blends of Samples A2, B2 and C2 by blending each at 50% with
`the Control virgin resin pellets.
`Sample D: 50% Virgin HDPEcontrol resin pellets + 50% Sample A2. (0% innovation)
`Sample E: 50% Virgin HDPEcontrolresin pellets + 50% Sample B2. (25% innovation)
`
`Sample F: 50% Virgin HDPE controlresin pellets + 50% Sample C2. (50% innovation)
`
`Examination One: Blow Molding of Bottles
`The blends of Samples D, E and F should be blow molded into one quart straight-wall generic
`base monolayer “motor oil bottles”. The cross-section can be rectangular or square. The bottom
`comers should have radii as small as commercial motor oil bottles. Bottle height should be
`typically for one quart motor oil bottles. Neck may be offset. The bottle must weigh 50 + 5
`grams.
`
`Control Sample D Resin should be blown first and followed by Samples E and F each blown
`under the identical conditions used for Sample D if possible. If the processing conditions need to
`be changed, then these changes must be documented andreported.
`
`Guidelines comparing Samples E and F to Control Sample D
`a. There should be no significant differences required when processing Samples E and F
`compared to Control Sample D. Small differences in blow moldsettings are acceptable.
`b. A reduction in performance of bottles made from Samples E and F should not exceed
`the specified test limits when compared to Sample D bottlesfor thefollowingtests:
`
`i. Visual inspection for surface defects including ‘orange peel’ and other surface
`roughness
`i. Bottle integrity
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`

`i. Bottle height
`iii. Bottle weight
`iv. Capacity
`v. Top load
`vi. Drop impact
`vii. Stress crack resistance
`viii. Fouling on tooling
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`Bottle Test Guideline Criteria
`
`
`Test
`Appearance
`
`Guidance
`Measurement
`Visual defects including surface} No more than whatseen for.
`roughness
`Control D4 bottles, minimum
`10 bottles.
`
`
`No more than what seen for
`Examination for incomplete
`Bottle Integrity
`bottles, blowouts or pinholes or|Control D4 bottles, minimum
`parison curling or excessive die|10 bottles.
`lines or excessive flash or weak
`weld line or bottle warping, or
`
`incomplete pinch off
`Height
`
`
`+ 5% of Control D4
`
`Bottle Dimensions
`
`
`Thickness
`Shoulder
`0.012 inch minimum thickness
`Top, mid, bottom side wall
`0.012 inch minimum thickness
`
`Total Bottle Weight
`
`+ 5% of Control D4
`
`Staircase
`
`Top Load
`
`No more than 5% decrease
`from Control D4
`
`
`ASTM D2659
`
`Drop Impact Mean failure height per ASTM|Noless than “95% mean
`
`D2463, procedure B, Bruceton|failure height vs. Control D4
`
`Noneobservedvs. control for
`Deposits on tooling
`Additional observation
`
`two hours of bottle making
`
`Examination Two: Stress Crack Testing
`Stress cracking is an important issue for bottles which might hold various liquids. Testing bottles
`themselves for stress crack performance can easily becomea test of the method rather than a test
`of material because of how sensitive the outcome can be to how a bottle is made. For that reason
`testing is done per ASTM D 1693in the latest version. A test sample must be prepared for the
`Condition B (nominal 1.50 inches x 0.50 inches x 0.075 inches, or 38mm x 13 mm x 1.90 mm)
`and notched (nominal 0.013 deep, or 0.35 mm deep) and tested at 122°F (50°C) in the same
`solution of 10 to 100% by volumeof Igepal CO-630 in waterfor all specimens.
`
`Samples D, E, and F should be prepared with melt blended pellets to assure the same heat history
`as a bottle and to assure homogeneity of the test specimen. Specimens prepared may, per ASTM
`1693, be compression moldedor injection molded, but injection molding is preferred. Note the
`manneroftest specimen preparation. Specimens should be notched per ASTM D 1693 Condition
`
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`

`B. Such samples are now Control Sample G (made from Control Sample D), Sample H (made
`from blend Sample E), and Sample J (made from blend Sample F).
`
`Innovation test results are after a specific number of hours of exposure, the hours to achieve 50%
`failure for the controls.
`
`Guidelines comparing Samples H and J to Control Sample G
`a. A minimum of 20 test specimens must be examined for each sample composition. 30 or
`more specimens for each sample, the same number of specimens for each sample, is
`suggested.
`b. Per ASTM D 1693, condition specimens for at least 40, no more than 96 hours before
`testing.
`c. Per the ASTM D 1693, 3.1.2, failure is defined as “any crack visible to an observer with
`normal eyesight”.
`a. Calculate the 50% failure rate timefor the Control SampleGeitheras the timefor halfof
`the initial control specimenstofail or graphically per ASTMD 1693 Appendix.
`e. Either by count of specimens or graphically find the failure rate (number of samples
`failed/‘numberof initial samples) for Samples H and J at the time for 50% failure rate of
`the control Sample Gfoundin d. above..
`Ff. The rate offailures difference for Samples H or J compared to Sample G (control) shall
`be no greater than 10 percentage points.
`i. Thefailure ratefor Control Sample G should be 50% from d. above.
`ii. Failure rate difference is calculated as (number ofSample Jfailures/number of
`Sample J specimens) - (number of Sample Gfailures/number ofSample G
`specimens) to be equalto or less than 0.10 to be acceptable. This would allow two
`additionalfailuresfor the innovation sample more than control sample when 20 test
`specimensare usedfor each sample and three additionalfailuresfor the innovation
`sample more than the control when 30 test specimens are usedfor each sample.
`
`Conclusion
`A Resin, Additive, Coating, Label, Adhesive or Multilayer resin that meetsall of the abovetest
`criteria for the Sample C (50% innovation) and Sample F (25% innovation) and Sample J (25%
`innovation) would be considered technically compatible in the average reclaimer process for
`bottle making when introduced into the HDPE bottle recycle stream. The Innovation material
`maystill be considered technically suitable for bottle making if the Sample F test criteria are not
`all met but all of the Sample C and Sample E and SampleH test criteria are met and the
`Innovation material under evaluation is not expected to be present in the recycle stream at the
`25% innovation concentration of Sample F, even in localized recycling environments. If most, but
`notall, of the abovetest criteria are met for Samples C and F andJ, further explanation or testing
`may be required to demonstrate technically compatibility for recycling.
`
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`Appendix A
`Controlresins
`
`All Data shownin this table has been taken from what are believed to be current resin data sheets.
`density
`flow rate
`ESC
`gm/cm® gm/10 min
`hours
`0.964
`0.65
`15
`0.961
`0.80
`20
`
`ASTM D1693, Condition B
`ASTM D 1693
`
`mer Resin Listing
`
`ASTM D1693, Condition B
`
`0.963
`
`0.73
`
`10
`
`ASTM D1693, Condition B
`
`ASTM D1693, Condition B
`ASTM D1693, Condition B
`ASTM D1693, Condition B
`ASTM D1693, Condition B
`
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