apr’s statement of rationale for the study · 2016-08-26 · apr’s statement of rationale for...

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APR’s Statement of Rationale for the Study

APR, the Association of Postconsumer Plastic Recyclers, funded this study, on the materials used for shrink sleeve labels used on PET containers. APR retained the services of Plastics Forming Enterprises LLC, Amherst, NH; a recognized expert independent testing laboratory. This statement from APR details the situation perceived relative to shrink sleeve labels on PET and the examinations needed.

Shrink sleeve labels have historically caused serious disruption in PET bottle recycling. Outside of these studies, opaque full sleeve labels may make proper identification of bottle sidewall resin difficult for near infrared-based sorting machines. Shrink sleeve labels can bind tightly around PET bottles in a pre-wash unit operation, resulting in the label not being removed by mechanical separation of loose labels. Sleeve label flakes that sink during a recycler’s sink/float separation step may not separate efficiently by air elutriation. Those non-separating label flakes are associated with two very significant negative effects: clumping of low melting resins which foul the PET dryers, and carryover of the label colorants to the PET product.

Carryover of colorants depends on the inks used and is not part of this test design, but is a critical issue for PET recyclers. Color carryover, exhibited in the test design by measuring label material not separated from PET flake, is expected to negate any material’s compatibility exhibited by a non-PET resin material because of expected PET product discoloration. Additionally, thin-walled PET water bottle sidewall flakes having particle weights similar to flakes of sleeve labels make air elutriation separation inefficient, unless high levels of PET removal and subsequent economic loss are acceptable.

APR divides this study into two sections. Study 1 examines how much residual label material will remain with the PET flakes after the recycling process; additionally, it investigates the effects of residual label resins on PET properties. The APR processing definition of unit operations and feeds, reflect the special challenges faced when PET recyclers confront sleeve labels. These challenges include a high, but realistic, level of thin-walled PET water bottles and a simulation of pre-wash, resulting in no first elutriation after grinding. The level of water bottles used reflects the situation faced by PET recyclers as thin-walled water bottles represent a significant share of the bottles collected in the postconsumer stream for recycling. The APR test plan calls for only un-inked labels to be investigated so the effects seen would be for the polymeric materials and not the choice of inks or label decoration.

http://postconsumer1.ipower.com/�

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Study 2 examines the deliberate spiking of PET with materials often used for labels and for other packaging uses that may be collected with PET containers. The data generated is useful to assess the effects of the inclusion of packages made of non-PET materials with PET packages when there is no separation done in the processing. As such, the regression curves can be used to estimate the concentration of specific non-PET resins in PET. Study 2 does not include any evaluation of the ability of a recycling process to remove the non-PET material or effects other than color and haze.

APR has identified the shrink sleeve labels on PET bottles as a significant problem to the effective growth and stability for the recycling of postconsumer PET containers. In our opinion, this study analytically clarifies the reality that recyclers confront when trying to effectively recycle PET containers with shrink sleeve labels and explains why many recyclers remove these bottles from their processing stream whenever they are detected. APR, however, recognizes the popularity of the full bottle, shrink sleeve design and challenges the plastic packaging industry to find a material type for shrink sleeve labels that is compatible with domestic recycling.

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Association of Postconsumer Plastic Recyclers

Shrink Label Learning Protocol

Study 1 and Study 2

Conclusion/Summary Lessons Learned

Recommendations

Plastics Forming Enterprises, LLC Plastics Consulting, Research and Engineering

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Executive Summary

The Study 1 was conducted with unprinted labels to determine how much residual label material would be with PET after recycling processing and to investigate the effects of residual label resins on PET properties. None of the sleeve labels examined was found fully satisfactory with regard to material effects while a polypropylene wrap around label, typical of commercial use, was found satisfactory. Those label materials that lead to excessive clumping likely would be even more problematic for color carryover effects if the labels had been printed. PVC labels performed so poorly that they should not be considered for PET containers. The results for the cavitated PETG sample examined were unexpectedly poor. All labels that sink in water are expected to be very problematic for PET recycling when decorated. Only floating sleeve labels show promise of meeting the label materials needs for avoiding very serious problems in the PET recycling process. The testing protocol called for a 50% loading of light weight water bottles and omitted an elutriation after wet grinding. These process definitions created a shift in the expected results due to the lower removal efficiency of the shrink labels at the process conditions required to meet the yield loss guidelines for elutriation. Study 2, the spiking of PET with various materials showed that low levels of polyolefin’s create high levels of haze, stressing the need for quantitative separations of polyolefin’s from PET in the recycling process. Other materials showed less color and haze effects at low concentration. No clumping tests were performed and the effects of the label inks were not included.

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Estimated PPM Conclusions and Summary The labels processed through both, the study 1 & 2 Shrink Sleeve Label Learning Protocol have been compared to predict the range of ppm in study 1 final production plaque.

The ppm range estimate for shrink sleeve labels that are olefin based are determined by the study 2 correlation equation calculated for haze. It was determined that there is a consistency when evaluating a non-linear curve for the haze value when comparing the olefin label materials.

The ppm range estimate for shrink sleeve labels that are non-olefin based are determined by the study 2 correlation equation calculated for b*. It was determined that there is a consistency when evaluating a linear curve for the b* value when comparing the non-olefin label materials.

Study 1 - Visual Estimated % and PPM Estimated Label %

Removed by Only Wash and Sink/Float

Estimated Label % Removed Only by

Air Separation Total % of Label

Removed

CTRL Label (OPP) 74.36% 18.80% 93.16%

A (OPS) 46.58% 17.81% 64.38%

B (PETG) 2.86% 5.71% 8.57%

C (PETG Cav.) 11.96% 53.26% 65.22%

D (PVC) 29.73% 24.32% 54.05%

E (LD-PET) 76.09% 18.48% 94.57%

Study 1 & 2 – PPM Comparison Study 1 - Visually Estimated

Residual After Processing and Oven Cooked, PPM

Study 2 - Color Correlation Estimated PPM

CTRL Label (OPP) 1,500 ppm 25-225 ppm

A (OPS) 11,000 ppm 9,000-12,000 ppm

B (PETG) 37,000 ppm **

C (PETG Cav.) 9,500 ppm - - -

D (PVC) 19,000 ppm 14,000-17,000 ppm

E (LD-PET) 1,700 ppm 200-400 ppm **Study 2 – Neat PETG addition has so little affect on PET color it cannot produce a confident regression/correlation

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APR Shrink Label Learning Protocol

“Lessons Learned” The study is designed to yield information on the impact that residual remaining shrink label materials have on bottle flake after recycle processing. Some of the items that were observed by PFE during the course of the testing are noted below:

• After completion of testing, it was evident that none of the sleeve labels tested warranted any positive remarks about overall performance. All materials have flaws in the various facets of Shrink Sleeve Label testing.

• Bulk density of flake from water bottles effect the buoyancy of the PET and whether some labels float. • The olefin based labels will have much higher removal efficiency but low residual amounts can create

noticeable haze. • The non-olefin based labels such as PETG – OPS – PVC, and PLA by similar specific gravity, will

have lower removal efficiency and will create sticking, clumping and color problems from bleeding inks and inks carried over with the label.

• The control label made from non-shrink OPP substrate and demonstrated the best performance. • Cavitated films should be able to separate easier and have higher removal efficiency, however, the

cavitated PETG film tested did not demonstrate the ability to float or have low color effect. • Printed Labels should be expected to affect the color relative to the removal efficiency of the process.

APR Shrink Label Learning Protocol Recommendations

After reviewing the data and test results, PFE proposed recommendations for further study of the shrink label effect. PFE suggests selecting 3 to 4 label materials which represent the current market or innovative materials breaking into the market and conduct a study to determine the following:

1) Effect of the same ink system on each label 2) Develop a clumping or sticking test protocol 3) Review varying water bottle spiking levels. The 50% water bottle inclusion was done to

represent a “worst, but realistic case”. 4) Create a Sleeve Label Film Development Project

a. Examine the value of Perforated Sleeve for self-ripping during pre-wash b. Target development of a Polyolefin that meets economic and functional needs for

sleeve labels c. Examine Cavitated/Foamed materials that float in water after hot washing

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Recycle Evaluation

Study 1


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Study 1 Table of Contents

Page # Processing Conclusions and Summary 3 Discussion of Process Summary 4 Proposed Learning Protocol for PET Bottles Containing Shrink Labels 5 Objectives, Materials and Equipment 6 Material Information 7 Pilot Scale Wash System 8 Air Separation 9

Yield Loss of PET % Oven Tested Samples (Incoming, Washed, and After Processing) 10-12 Floatable Dye Test 13 Intrinsic Viscosity 14 Plaque Color Data 15 White and Black Background (Order of L*, b*, and Haze) 16 Plaque L* and a* Value Graphs 17 Plaque b* and Haze* Value Graphs 18 Specific Testing 19

Sink / Float (500g) Bulk Density Oven Bake Test (No load on flakes) 20

Study 1 – Storyboard 21 Glossary 22

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Study 1 Processing Conclusions and Summary

The control and 6 label variables faced consistent lab scale processing. We conclude the following:

• Clumping percentages below 5% for this testing procedure are considered favorable because of the results for the regularly accepted OPP wrap-around labels. These values are based on the separation achieved for 50% intended labeled bottle ground with 50% unlabeled water bottle defined as test sample.

• 500 grams sink/float results above 80% floating are considered favorable in our opinion. These values are based on 100% intended labeled bottle ground.

• Haze requirements, per the APR PET Critical Guidance for bottles, are less than 9.5% should not be a problem. Haze between 9.5% and 14% needs study and haze over 14% is likely noticeable. These criteria are absolute and not relative so that their use should not depend on the percent of labeled bottle examined. We conclude the APR Critical Guidance for haze for PET bottles is appropriate for this study. The un-inked cavitated PETG label, the un-inked PVC label, and the un-inked LD-PET label all far exceeded the limit for haze.

• Δb* per the APR PET Critical Guidance requirements is for 50% concentration of added material: Δb* less than 1.5 should not be a problem, Δb* between 1.5 and 5.5 needs study, and Δb* over 5.5 is unsuitable for many applications. Due to this study not being the same concentration condition as the Critical Guidance Document with the level of added material not being deliberately 50% and the use of “less than 3 Δb*” being utilized in other APR guidance for testing of 100% undiluted samples, we conclude the acceptance criteria should be ‘less than 3 Δb*’ to be considered favorable for the material. Test results showed un-inked OPS label, un-inked cavitated PETG label, and un-inked PVC label exceeded the ∆b* criteria. Inked labels that sink in water are expected to further create unacceptable color results.

• For clear PET, L*greater than 82 is the APR Critical Guidance requirement. We conclude the tables for favorable vs. less favorable should be based on the APR criteria. Test results showed un-inked cavitated PETG label and un-inked PVC label exceeded the L* criteria.

The ability to determine an acceptable material can only be decided by the importance of one attribute over another. Therefore, it is inconclusive as to an unequivocal preferred sleeve material choice of those examined. The table included below is based on 5 selected criteria, green for favorable values and pink for less favorable values. Processing the material, as evidenced by clumping behavior, is as important as are the color and haze. All five values are critical to finding the acceptable material for Shrink Sleeve Labels. The reader should note this examination is only for un-inked labels and that inking or decorating labels can create additional negative results.

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Shrink Label Assessment

PLEASE NOTE the pink and green do not represent a complete pass or a fail parameter. The values have the possibility to change when ink are applied for both the floatable labels and the sinkable labels. It is suggested that selected labels be processed with inks that have passed a bleeding label protocol to understand the impact of inks on shrink sleeve labels. Knowing how the label material will react in the processing conditions specified per the study 1 learning protocol, it is evident the inks will be required to evaluate when approving a shrink sleeve label. The results for PVC labels are so uniformly outside of the range of acceptable that PVC labels should not be used for PET bottles, as the APR Design for Recyclability Guidelines state.

% Clumping (Oven Baked)

500G Sink/Float % Floatable Haze b* L*

CTRL Label (OPP) 3.25% 99.07% 8.66 3.04 87.66

A (OPS) 25.90% 4.90% 8.98 6.68 86.85

B (PETG) 22.77% 0.00% 8.54 4.42 87.93

C (PETG Cav.) 18.99% 0.40% 84.62 16.53 75.11

D (PVC) 8.44% 0.00% 51.24 72.92 54.08

E (LD-PET ) 28.47% 83.13% 19.07 5.58 85.83

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Study 1 Discussion of Process Summary

The APR-funded this project on quantifying removal efficiency and the consequences of residual shrink sleeve labels on PET flake. The project leads us to be able to make verifiable decisions on the criteria for the ideal shrink sleeve label substrate without ink.

Shrink sleeves are good in that there are no adhesives involved to get a label to stay on a bottle. Having an adhesive added to the variables can create potential problems. The full bottle labels are less than desirable in that they can confuse auto sort machines and pose a removal problem.

The popularity of full sleeve labels on bottles with products that are either not meant to be visible or need some UV light protection means that the market will probably not be seeing fewer such labels. The APR realizes the need to be more specific on what is acceptable and recommended.

The objective was to process a control and a control with a known wrap label. Additionally, five shrink sleeve label substrates were chosen to determine the removal and effects of removal per the APR shrink label learning protocol.

This testing protocol included a 50% loading of light weight water bottles. The grinding process was managed so the labeled or unlabeled intended bottle to water bottle material was ground together and essentially blended in the grinder. The addition of water bottles created a unique situation that posed some complications in the removal efficiency of the shrink labels at the process conditions required to meet the guidelines.

After grinding, the materials were then processed through the wash and rinse procedure. The floatable retains were collected at three separate times and weighed accordingly. It was during this process that some concerns arose. The control of 50% intended non-labeled bottled to 50% water bottles by weight produced more floatables than expected. The material that floated was dominantly water bottle material. The thin wall water bottles had the tendency to float due to air pockets created in the curled flake. A small sample of each floatable was processed through a dye test that all label materials reacted to with the exception of the OPP control label. The washed flake for all samples was also tested by baking it at a 450°F temp for 60 minutes to determine a visual removal.

The material following the wash was air dried for 48 hours and then submitted to the elutriation procedure. The equipment was calibrated with 2% +/- .5% carryover of PET flake with removed label material for the control. There was a reduction in air speed necessary from the typical PET CSD control bottle calibration. The reason for reduction in air speed was due to the wall thickness of the thin wall water bottle with unacceptably high carryover of the thin water bottle material if the air speed were not reduced.

After all samples finished the elutriation step the heavies from all samples were also evaluated by baking it at a 450°F temp for 60 minutes to determine a visual removal. Material was then desiccant dried and extruded into pellets and crystallized. IV data was completed at this time. The PET IV for samples with PVC contamination where decidedly lower, proving that PVC contamination degrades polymers.

The pellets, for each sample were processed into a plaque. The L*, a*, b*, and haze data was completed at this time. Materials that were repeated in study 2 had a calibration that was used to determine the ppm left in the material. The PETG Cavitated is the only material that was not also processed in Study 2 and would be valuable to be repeated to verify/determine the ppm in Study 1.

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Proposed Learning Protocol for PET Borttles Containing Shrink Labels

Decorated Undecorated APR Non-APR APR Non-APRShrink Wrap Shrink Wrap Control Intended Control Intended Control Control Label Label Bottle Resin Bottle Resin Water Bottle Resin Water Bottle Resin

Bleeding Control Intended Control Intended Control ControlLabel Test Bottles Bottles Water Bottles Water Bottles

Measure IV Measure IV Measure IV Me Measure IV

APR Quick APR QuickCorrect Color Test Color TestProblem No YesInk

Select Select Yes No Another No Another

Resin Resin

Float / Sink Yes

Unlabeled Control Shink Label Grind Evaluation TestIntended Bottles Intended Bottles 500g Measure % Floating Label

Bottle Blending

Bulk Density Control Sample Test Sample Bulk DensityMeasurement 50% w/w Unlabeled Control 50% w/w Shrink Label Measurement

Intended Flake Intended FlakeAPR Oven 50% w/w Unlabeled Water 50% w/w Unlabeled Water APR OvenBake Test Bottle Flake Bottle Flake Bake TestWeight % Clumps Weight % Clumps

Grind Grind

Proceed directly to APR WashSink/Float Elutriate to get on initial study. If on completion Elutriate at Sink/FloatAir Elutriated 2.0% Lights the guidelines are not met, then Control Air ElutriatedLights Removal the study will need to be re- Setting LightsRecord Floatable wgt. Record wgt. Removed peated with this 1st elutriation Record wgt. Removed Record Floatable wgt.

step now included.

Skim Floatables APR Hot APR Hot Skim FloatablesDry/Weigh Caustic Wash Caustic Wash Dry/WeighRecord Measure % Label

Skim Floatables Water Float/Sink Water Float/Sink Skim FloatablesDry/Weigh Test #1 Test #1 Dry/WeighRecord Measure % Label

Skim Floatables Water Float/Sink Water Float/Sink Skim FloatablesDry/Weigh Test #2 Test #2 Dry/WeighRecord Measure % Label

Air Dry Air Dry Estimate %Flake Flake Label Remaining

Sink/Float Elutriate to get Elutriate under Control Sink/FloatAir Elutriated 2.0% Lights Sample conditions Air ElutriatedLights Removal, Weigh Removal, Weigh LightsRecord Floatable wgt.

Extrude/Pelletize Extrude/PelletizeCrystallize CrystallizeMeasure IV Measure IV

Plaque Molding Plaque Molding

Measure: Measure:IV, L*, b*/Haze IV, L*, b*/HazeBlack Specks Black Specks

Deltab*<3

Delta b*<3

Pass/

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Study 1

A Study of PET Bottles Containing Shrink Labels from Different Substrate Materials Objectives:

Quantifying removal efficiency and consequences of residuals for shrink sleeve labels on PET bottles.

Obtain data to help APR form an opinion on current shrink label substrate materials. Use the learnings as the basis for a long-term, on-going shrink label innovation test protocol

Materials:

Thin walled Water Bottles without Label Intended bottles without shrink label applied Intended bottles with wrap label :

• Control Label - OPP Intended bottles with shrink label:

• Label A - OPS • Label B - PETG • Label C – PETG Cavitated • Label D - PVC • Label E - LD-PET

Equipment:

Recycle System - Pilot Plant Wash System - Convection Ovens (Surface Drying) - Kice Elutriator - Grinder with 3/8” Screen - Desiccant Dryer - Arburg Injection Machine with a 3MM plaque mold - Konica Minolta CM-3600d spectrophotometer

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Material Information

Label % Label to Intended

Bottle* CTRL Label - OPP 4.11% Label A - OPS 5.54% Label B - PETG 7.14% Label C - PETG (Cav.) 4.95% Label D- PVC 7.39% Label E - LD-PET 5.67%

*%Label to intended bottle is defined as grams of label divided by grams of bottle plus label. Each undecorated test label variable is a 50/50 blend of, Water bottle (835 bottles) 8” Tall label applied to Intended bottle (250 bottles).

Label Call Out Type Weight (grams)

Thickness (inches)

Density (g/cm3)

CTRL

Water Bottle

& 10.900

0.004

Intended Bottle

38.160

0.022

CTRL Label - OPP

A – OPS

Wrap around OPP Label

Shrink OPS Label

1.634

2.239

0.015

0.002

0.957

1.153

B - PETG

C – PETG Cav.

D - PVC

E – LD-PET

Shrink PETG Label

Shrink PETG Cavitated Label

Shrink PVC Label

Shrink LD-PET Label

2.932

1.989

3.047

2.295

0.002

0.002

0.002

0.002

1.348

1.089

1.298

0.950

Water Bottle Intended Bottle

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Pilot Scale Wash System

Caustic Wash: The flakes are exposed to a caustic wash solution of 0.3% by weight Triton X-l00 (6.0 gms or 5.7 m1 per 2,000 ml water) and 1.0% by weight caustic (20 gms NaOH per 2,000 ml water) at 185°F (85° C). Wash was highly agitated (880 rpm) at 88 + 2°C for 15 minutes.

Rinse: Flakes are drained of caustic wash solution and rinsed with room temperature water with agitation in order to remove the caustic solution.

Sink/Float: Floatables were removed at three different times. Floatables were skimmed off during the wash, after material had settled, and as well as after the rinse and agitated sink float process.

Drying: Flakes were ambient air dried with no heat or vacuum.

Wash and Rinse Water Photographs

314 Study 1 Control

Wash and Rinse Water

314 Study 1 Label CTRL, A, B, C, D, & E

Process water- Same appearance for all labels Wash and Rinse Water

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Air Separation

The elutriation steps found in the Critical Guidance Document Protocol following bottle grinding have been eliminated in this protocol to make this study simulate the air separation done for a wet grinding of bottles. The process set-up is for one pass to remove light fractions.

• The air flow was set up based on the control materials to be within, 2.0 + 0.5% of PET flakes are

removed as “lights”.

• The total lights for control and test samples were recorded and % listed in chart below.

• The PET flake was visually examined for the presence of label film residue and noted approximate percentage with a cooked sample.

The standard air flow rate was reduced to meet the 2.0% ± 0.5% specification. This was caused by the lower bulk density of the materials at 50% Intended bottle and 50% thin wall water bottles

Yield Loss of PET %

CTRL

No Label CTRL Label

(OPP) Floatable - Yield Loss 0.55% 2.11% Elutriation - Yield Loss 2.43% 4.22% Total Yield Loss 2.98% 6.33%

A

(OPS) B (PETG) C

(PETG Cav.) D

(PVC) E

(LD-PET) Floatable - Yield Loss 2.69% 0.65% 0.88% 1.50% 3.42% Elutriation - Yield Loss 4.49% 4.60% 5.21% 3.66% 3.48% Total Yield Loss 7.18% 5.25% 6.10% 5.15% 6.90%

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Oven Tested Samples Incoming, Washed, and After Processing

All cooked samples: Dry flake is cooked at 450°F for 60 minutes. Temperatures and time was tested, final time and temp was adequate. Due to the labels having no inks, labels blended with PET flake making it hard to distinguish until heated or stained.

314 – Study 1 Control Label (OPP Wrap)

Incoming Cooked at 450°F for 1 hour

314 – Study 1 Control Label (OPP Wrap)

Washed Cooked at 450°F for 1 hour

314 – Study 1 Control Label (OPP Wrap) Washed and Air Separated Cooked at 450°F for 1 hour

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LD PET LD PET LD PET

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314 – Study 1 Floatable Dye Test

Dye Test was added to determine the amount of thin wall water bottle flake that floated with label materials through the wash processing. The purpose was to distinguish the label from the thin wall water bottle. This test revealed labels that typically do not float were present in the floatable material. The nature of the thin wall water bottle caused it to curl during the processing. This allowed the flake to trap air and grab labels eventually pulling them to the surface.

All dyed samples were submitted to a chemical dye test for 15 minutes. All labels with the exception of the

OPP control label did not absorbed the dye, see pictures below.

CTRL Label - OPP Label A - OPS

Label B – PETG Label C – PETG Cavitated

Label D - PVC Label E – LD-PET

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Intrinsic Viscosity

The incoming intended bottles and water bottles were measured for intrinsic viscosity to get a starting value by using the weight average calculation. After processing was completed, the crystallized pellets for each variable were measured for intrinsic viscosity in order to evaluate any significant drops in the IV when compared to the control.

Incoming bottle IVs:

Pellet IVs:

Plaque IVs:

Black Specks over 0.015 Inches Within 3 mm Plaques (3879 sq. mm per plaque, 50 plaques examined for each label)

Intended Water Calculated IV 0.754 0.730 0.742

CTRL 0.724

CTRL – OPP A – OPS B – PETG C – PETG Cav. D – PVC E – LD-PET 0.727 0.733 0.727 0.726 0.532 0.726

CTRL 0.669

CTRL – OPP A – OPS B – PETG C – PETG Cav. D – PVC E – LD-PET 0.683 0.669 0.658 0.680 0.354 0.622

CTRL 0

CTRL – OPP A – OPS B – PETG C – PETG Cav. D – PVC E – LD-PET 5 4 3 8 18 8

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PLAQUE COLOR DATA

Plastics Forming Enterprises, LLC Project: APR Shrink Label

Equipment: Konica Minolta CM-3600d

Conditions: CIE Lab, 10 degrees, D65

Run # Description

L * Values

a* Values

b* Values

L* Average

a* Average

b* Average Haze

Haze Average

CTRL 50 IB / 50 WB

87.84 -0.71 3.61

88.70 -0.47 2.91

8.58

8.59 87.93 -0.63 3.43 8.4 89.86 -0.15 2.02 8.97 89.96 -0.16 1.93 8.68 87.93 -0.68 3.54 8.34

CTRL - Label

OPP Wrap Label

87.7 -0.8 4.26

87.66 -0.76 3.04

8.89

8.66 87.93 -0.63 3.43 8.4 89.86 -0.15 2.02 8.97 89.96 -0.16 1.93 8.68 87.93 -0.68 3.54 8.34

314 - A OPS Shrink Label

86.85 -0.88 6.61

86.85 -0.89 6.68

8.96

8.98 86.83 -0.88 6.64 8.96 86.84 -0.9 6.65 9 86.81 -0.92 6.94 8.9 86.91 -0.87 6.57 9.09

314 - B PETG Shrink Label

87.9 -0.7 4.42

87.93 -0.72 4.42

8.59

8.54 87.89 -0.7 4.43 8.62 88.01 -0.76 4.4 8.44 87.91 -0.72 4.43 8.55 87.92 -0.7 4.41 8.52

314 - C PETG Cavitated Shrink Label

74.84 0.98 16.76

75.11 0.90 16.53

84.86

84.62 76.16 0.66 15.24 83.73 74.82 0.95 16.9 84.89 74.84 0.96 16.93 84.8 74.89 0.94 16.81 84.8

314 - D PVC Shrink Label

51.98 28.97 73.52

54.08 26.89 72.92

49.19

51.24 52.91 28.43 73.38 49.23 55.95 24.59 72.29 54.06 55.42 25.69 72.78 52.01 54.15 26.78 72.65 51.73

314 - E LD-PET Shrink Label

85.81 -0.45 5.47

85.83 -0.50 5.58

19.25

19.07 85.78 -0.46 5.55 19.14 85.83 -0.54 5.68 19.05 85.85 -0.53 5.67 19.01 85.88 -0.5 5.51 18.9

The color data for each label material represents randomly selected plaque samples from the same population of material.

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White and Black Background

Plaque Photos in Order of L*, b*, and Haze

CTRL Label – OPP (Wrap Label) 314 B - PETG (Shrink Label) 314 A – OPS (Shrink Label) 314 E – LD-PET (Shrink Label) 314 – C PETG Cav. (Shrink Label) 314 – D PVC (Shrink Label)

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Plaque L* and a* Value Graphs

88.704 87.656 86.848 87.926

75.11

54.082

85.83

0

10

20

30

40

50

60

70

80

90

100

L

L*

CTRL1

CTRL2

OPS

PETG

PETG-Cav.

PVC

LDPE-Comp.

-0.466 -0.758 -0.89 -0.716

0.898

26.892

-0.496

-5

0

5

10

15

20

25

30

a

a*

CTRL1

CTRL2

OPS

PETG

PETG-Cav.

PVC

LDPE-Comp.

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Plaque b* and Haze* Value Graphs

2.906 3.040 6.682 4.418

16.528

72.924

5.576

0

10

20

30

40

50

60

70

80

b

b*

CTRL1 CTRL2 OPS PETG PETG-Cav. PVC LDPE-Comp.

8.594 8.660 8.982 8.544

84.616

51.244

19.07

0

10

20

30

40

50

60

70

80

90

haze

Haze

CTRL1

CTRL2

OPS

PETG

PETG-Cav.

PVC

LDPE-Comp.

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Specific Testing

Sink / Float (500g) This test is performed with 500 grams of 100% ground Intended bottles with wrap and/or shrink labels (No thin wall water bottle flake included). This does not represent the recycled process used in study 1 and therefore demonstrates further the affect of grinding/washing/rinsing and sink/floating from a separate test of the intended bottle with the label only. The unwashed flake material is added to 2L of room temperature water with 0.3% surfactant. The results are shown as percent removed from initial weight and actual weight of floating material.

Material CTRL OPP A - OPS B - PETG C - PETG CAV. D - PVC E – LD-PET Total Weight of Intended

Bottle with Label 500 500 500 500 500 500 Total Weight of Label 21.500 29.337 38.422 26.056 39.924 30.065

Total Floatables 21.300 1.450 0.000 0.104 0.000 19.266 Label Removal Efficiency 99.070% 4.943% 0.000% 0.398% 0.000% 83.131%

The data shows that the majority of label content was removed in the sink / float process for CTRL Label OPP, and E. All other labels show labels will not be removed in wash process.

Bulk Density The bulk density was measured just before the material was processed through the wash system.

Run Number Mass lbs/ft3 g/cm3 Water Bottle Flake 610 12.65 0.203 Intended Bottle Flake 1115 23.12 0.370 CTRL – OPP 870 18.04 0.289 A – OPS 865 17.94 0.287 B – PETG 755 15.66 0.251 C – PETG Cav. 760 15.76 0.252 D – PVC 655 13.58 0.217 E – LD-PET 770 15.97 0.256

LD PET

Page | 21

Oven Bake Test (No load on flakes)

This study is performed in order to understand the tendency of labels to become sticky when heated which can cause agglomeration and clumping of flakes. Each label sample subjected to an oven temperature of 208°C (406°F) for a period of 90 minutes per APR Protocol for Oven Baking PET Flake. After the flakes cooled from the oven, each sample was sorted by hand to remove any flake clumps and then weighed and calculated as a percentage of the total weight of the sample.

Percentage of clumps sample:

Run Number % of Clumps CTRL – OPP 3.25% A – OPS 25.90% B – PETG 22.77% C – PETG Cav. 18.99% D – PVC 8.44% E – LD-PET 28.47%

LD PET

Page | 22

Study 1 – Storyboard

Page | 23

Study 1 Glossary

• a* - this is the unit of measurement in regards to how red or green an object is.

• Agglomeration - term used to describe the potential of label materials to melt at low temperatures and

essentially create clumps of flake materials.

• b* - this is the unit of measurement in regards to how yellow or blue an object is.

• Bulk Density – a measurement of the amount of volume materials occupy

• Caustic – a chemical used in the wash process, specifically, Sodium Hydroxide (NaOH).

• CNTLLabel – Nomenclature for OPP wrap label used as a control

• Elutriation – a term used to describe the process of removing light fractions from non-PET. Also

known as Air Separation.

• IB – acronym for Intended Bottle

• Inherent Viscosity (IV) – this is the measurement of the molecular weight of PET

• L* - this is the unit of measurement in regards to how white or black an object is.

• LD-PET – Low Density PET structure with additional layers of confidential materials

• OLEFIN – Polyolefin material

• OLEFIN MD – Polyolefin ROLL FED

• OPP – Orientated Polypropylene

• OPP MD – Oreintated Polypropylene ROLL FED

• OPS – Orientated Polystyrene

• PETG – Polyethylene terephthalate with glycol modification

• PETG Cavitated – a foamed version of PETG

• PLA – Polylactic acid

• PVC – Polyvinyl Chloride

• Surfactant – a chemical (detergent) used in the wash process

• WB – acronym for Water Bottle

Page | 1



Spiking Evaluation Study 2

Objectives:

Determine the impact of known amounts of a control wrap label and various shrink label materials in a control mixture of water bottle flake and Intended bottle flake. Create a calibration curve for each material.

Materials:

Thin walled water bottles without label Intended bottles without shrink label applied Control wrap label OPP Shrink label materials: OPS, PETG, PLA, PVC, OPP MD (Roll Fed), OLEFIN MDO (Roll Fed),

LD-PET Equipment:

3/8” Grinder and 1/4” Wiley Mill grinder Arburg Injection Press with a 3mm plaque cavity mold Walton/Stout Desiccant Dryer VAPOR PRO CT-3100 Moisture Analyzer Konica Minolta CM-3600d Spectrophotometer


Page | 2

Table of Contents Procedure…………………………………………………………….. 3 Summary and Conclusion…………………………………………… 3-4 Calibration Curve All Variables up to 1,000ppm………………… 5 - 7 Non-Olefin Materials Calibration Curve up to 25,000ppm………. 8 - 10 Olefin Materials Calibration Curve up to 5,000ppm………………11 - 13 Study 2 Storyboard Photograph……………………………………. 14

APPENDIX: Color Data Control OPP ………………………………….………….…15 OPS………………………………………………….….….. 16

PETG………………………………………………….…... 17 PLA…………………………………………………….….. 18

PVC……………………………………………………….. 19 OPP MD……………………………………………….……20

Olefin MDO…..………………………………………..…... 21 LD-PET ……….…………………………………………. ..22

Page | 3

Procedure

The study is designed to yield information on the impact that residual remaining shrink label materials will have on the discoloration and haze generation when the PET material is molded into 3mm thick plaques. The results can be used to produce a calibration graph of ppm content vs. transmission color, L*, b* and haze.

• Grind water bottles and intended bottles, no labels applied, and make 50:50 weight blend of control flake.

• Create master batch of pellets at 10,000 ppm through extrusion and pelletization. • Create blends at 0, 50, 250, 500 and 1,000 ppm using master batch pellets and control flake. • Desiccant dry the blends to achieve a moisture below 50 ppm. • To give the material a second heat history, mold the pellet blends into 3mm plaques. • Plot the L*, b* and haze results for each test sample over the range of spiked concentrations to create the

calibration curve for each shrink label material in PET.

Summary The reader must remember that this study is for undecorated, uninked label material and does not reflect the full impact of these materials on recycling. Further, the reader must remember that the spiking is intentional and the observations cited do not reflect the removal efficiency of any recycling process. Study 1 presents the residuals seen for the various label materials. These data are meant for calibration, not decision making on the suitability of any material choice.

• The CONTROL Label for this study was an OPP wrap label currently used in the market today. The OPP MD contained in this report is a shrink label specific material and is not identical to the control.

• L* color values for OPS and PETG labels do not fluctuate significantly with the deliberate increase of parts per million to 1,000 ppm. The OPP label has the most significant decrease in L* value showing that it becomes less clear as the parts per million are deliberately increased.

• The b* values for OPS and PETG show little change as parts per million are deliberately increased. These results are only for uncolored polymer samples, not decorated labels. The most noticeable increase in b* value comes from the PVC label which has a significant jump in yellowness as parts per million are deliberately increased.

• Haze values for undecorated, deliberately spiked neat OPS, PETG and PVC have very minimal increase with low parts per million. The OPP, Olefin MDO and LD-PET labels have a large impact on the % haze reading at low level parts per million starting at 250 ppm. The observation about polyolefins hazing PET is known in the industry and reason for process emphasis on removal of such labels.

Page | 4

Conclusion

The reader is cautioned to remember that these results are for the deliberate spiking of certain materials into PET that is subsequently made into plaques. The conclusions are only about material effects at low concentrations and are not an endorsement or representation of how a decorated label would perform in a recycling process. The effects of residuals of just undecorated materials are given in Study 1.

• The non-polyolefin and polyolefin-based neat materials are displayed separately in the graphical analysis of this report. This is because of the major differences of impact on color at certain concentrations between the base materials. Olefin based material have more tendency to impact materials at lower levels while non-olefins show more impact at higher concentrations for the deliberate spiking. The concentrations examined do not reflect the removal efficiency possible for any label material or reflect the impact of retained colorants and inks.

• The data for the calibration curves shows that L* values for neat PETG and OPS reveal very little impact while higher levels of neat PLA, LD-PET and PVC had a moderate effect, leaving OPP with the most noticeable impact for deliberate spiking of undecorated material. Clumping effects are not included and such effects for decorated/inked labels are expected to be severe for L*.

• The b* data again shows neat PETG and OPS having little impact for the deliberate spiking of undecorated material. Neat PLA, LD-PET and OPP had a moderate effect while PVC had a large impact with high b* values. Clumping effects are not included and such effects for decorated/inked labels are expected to be severe for b*.

• The percent haze data revealed increases for all materials with higher level ppm content due to deliberate spiking. Neat materials that showed slow to steady increases were the OPS, PETG and PVC, while the LD-PET and OPP show large increases in haze with low level ppm content. Clumping effects are not included and such effects for decorated/inked labels are expected to be severe for haze

• Due to the differences between polyolefin and non-polyolefin materials it has been determined that focusing on using the % Haze for polyolefin based labels and b* values for non-polyolefin based labels to correlate the approximate parts per million content should be the most reliable analysis when only undecorated label materials are being examined.

Page | 5

Calibration Curve Data 0 – 1000 ppm All Variables

*Concentrations of label content were limited due to experimental integrity. *The color data for each label material represents randomly selected plaque samples from the same population of material.

MaterialCNTLLabelLDPEOLEFINOPPOPSPETGPLAPVC

Plot of Fitted Model

Conc. (ppm)

L*

0 0.2 0.4 0.6 0.8 1(X 1000)

82

84

86

88

90

LD PET

Page | 6


*Concentrations of label content were limited due to experimental integrity. *The color data for each material represents randomly selected plaque samples from the same population of material.



Conc. (ppm)

b*

0 0.2 0.4 0.6 0.8 1(X 1000)

0

3

6

9

12

15

LD PET

Page | 7


*Concentrations of label content were limited due to experimental integrity. *The color data for each material represents randomly selected plaque samples from the same population of material.



Conc. (ppm)

Haz

e

0 0.2 0.4 0.6 0.8 1(X 1000)

0

10

20

30

40

50

LD PET

Page | 8

Calibration Curve Data Non-Olefin Materials (L*)

*The color data for each material represents randomly selected plaque samples from the same population of material.

Plot of Fitted Model -- L* vs Conc Misc Labels

Misc Label Conc (ppm)

L V

alue

PETG

0 5 10 15 20 25(X 1000)

65

70

75

80

85

90 OPS

PVCPLA

P&PA

Page | 9

Calibration Curve Data Non-Olefin Materials (b*)


Plot of Fitted Model -- b* vs Conc Misc. Labels


bValu

es

PVC

0 0.2 0.4 0.6 0.8 1(X 10000)

0

10

20

30

40

50

60

PLA

OPSPETG

P&PA

Page | 10

Calibration Curve Data

Non-Olefin Materials (Haze)


Plot of Fitted Model -- Haze vs Conc Misc. Labels


Haze

PETG

0 5 10 15 20 25(X 1000)

010203040506070

PLA

PVC

OPS

P&PA

Page | 11

Calibration Curve Data Olefin Materials (L*)


Plot of Fitted Model-- L* vs Conc. Olifins

Olifin Conc. (ppm)

L V

alue

LDPE

0 1 2 3 4 5(X 1000)

65

70

75

80

85

90

OLEFIN

CNTL Label

OPP

P&PA

Olefins

Olefins

LD PET

Page | 12

Calibration Curve Data Olefin Materials (b*)


Plot of Fitted Model-- b* vs Conc. Olifins

Olifin Conc. (ppm)

bValu

es

LDPE

0 1 2 3 4 5(X 1000)

0

3

6

9

12

15

18

CNTL LabelOPP

OLEFIN

P&PA

Olefins

Olefins

LD PET

Page | 13

Calibration Curve Data Olefin Materials (Haze)


Plot of Fitted Model-- Haze vs Conc. Olifins

Olifin Conc. (ppm)

Haze

LDPE

0 1 2 3 4 5(X 1000)

0

20

40

60

80

100

P&PA

OPPOLEFIN

CNTL Label

Olefins

Olefins

LD PET

Page | 14

Study 2 Storyboard Photo

Page | 15

APPENDIX: Color Data

Calibration Curve Color Data 50 – 5000 ppm CTRL Label

Run # Description L *

Values a*

Values b*

Values L*

Average a*

Average b*

Average Haze Haze

Average

CTRL 0 ppm

88.88 -0.66 2.83

89.15 -0.65 2.78

8.86

8.52 88.95 -0.65 2.78 9.03 89.18 -0.63 2.74 9.04 89.32 -0.67 2.77 7.81 89.41 -0.64 2.76 7.88

CTRL 50 ppm

89.62 -0.71 3.02

89.34 -0.70 3.02

8.22

8.65 89.48 -0.66 2.80 8.13 89.24 -0.71 3.12 9.05 89.18 -0.70 3.09 8.78 89.18 -0.70 3.06 9.08

CTRL 250 ppm

88.08 -0.66 3.32

88.03 -0.65 3.34

14.70

14.53 88.05 -0.64 3.28 14.33 88.03 -0.65 3.32 14.09 88.04 -0.65 3.33 14.22 87.94 -0.66 3.47 15.29

CTRL 500 ppm

86.76 -0.55 4.36

87.15 -0.61 4.10

20.23

18.44 87.31 -0.60 3.95 17.36 87.15 -0.62 4.09 18.71 87.29 -0.62 4.03 17.69 87.23 -0.65 4.08 18.19

CTRL 1000 ppm

84.42 -0.54 5.87

84.69 -0.54 5.60

36.97

36.18 84.75 -0.54 5.58 35.23 84.99 -0.50 5.21 34.66 84.89 -0.61 5.45 38.64 84.40 -0.49 5.87 35.39

CTRL 5000 ppm

69.64 0.87 14.43

69.99 0.86 14.41

86.55

85.88 69.86 0.83 14.68 85.99 70.20 0.88 14.47 86.29 70.09 0.87 14.22 85.66 70.17 0.83 14.27 84.92

Page | 16

Calibration Curve Data 50 – 15000 ppm

OPS Label


Values a*

Values b*

Values L*

Average a*

Average b*

Average Haze Haze

Average

CTRL 0 ppm

88.88 -0.66 2.83

89.15 -0.65 2.78

8.86

8.52 88.95 -0.65 2.78 9.03 89.18 -0.63 2.74 9.04 89.32 -0.67 2.77 7.81 89.41 -0.64 2.76 7.88

314-1 50 ppm

88.89 -0.70 2.95

88.86 -0.69 2.92

8.01

8.03 88.86 -0.73 2.98 7.99 88.86 -0.67 2.86 8.03 88.83 -0.66 2.86 8.00 88.88 -0.69 2.93 8.14

314-1 250 ppm

88.77 -0.68 2.96

88.78 -0.68 2.95

8.04

7.96 88.76 -0.67 2.90 7.96 88.82 -0.68 2.93 7.84 88.74 -0.69 2.99 8.05 88.79 -0.70 2.96 7.93

314-1 500 ppm

88.76 -0.69 3.04

88.76 -0.69 3.04

8.10

8.15 88.76 -0.69 3.03 8.19 88.77 -0.68 3.01 8.12 88.74 -0.69 3.03 8.16 88.76 -0.70 3.08 8.19

314-1 1000 ppm

88.75 -0.69 3.18

88.76 -0.70 3.18

8.10

8.10 88.65 -0.67 3.22 8.65 88.80 -0.69 3.14 7.86 88.79 -0.70 3.16 7.90 88.79 -0.73 3.20 7.99

314-1 5000 ppm

87.79 -0.87 4.24

87.80 -0.84 4.20

8.35

8.24 87.87 -0.90 4.68 8.02 87.99 -0.79 3.76 8.32 87.66 -0.83 4.32 8.22 87.69 -0.81 4.02 8.28

314-1 15000 ppm

87.06 -1.12 5.67

87.09 -1.14 5.69

11.70

11.37 87.08 -1.14 5.72 11.27 87.08 -1.14 5.73 11.39 87.10 -1.14 5.66 11.24 87.11 -1.14 5.65 11.25

Page | 17

Calibration Curve Data 50 – 25000 ppm

PETG Label


Values a*

Values b*

Values L*

Average a*

Average b*

Average Haze Haze

Average

CTRL 0 ppm

88.88 -0.66 2.83

89.15 -0.65 2.78

8.86

8.52 88.95 -0.65 2.78 9.03 89.18 -0.63 2.74 9.04 89.32 -0.67 2.77 7.81 89.41 -0.64 2.76 7.88

314-2 50 ppm

88.28 -0.85 3.73

88.23 -0.83 3.72

7.72

7.94 88.30 -0.85 3.69 7.65 88.20 -0.84 3.75 8.11 88.26 -0.81 3.68 7.83 88.13 -0.81 3.73 8.37

314-2 250 ppm

88.17 -0.76 3.66

88.18 -0.76 3.65

7.90

7.89 88.17 -0.74 3.61 7.90 88.17 -0.75 3.63 7.92 88.20 -0.78 3.67 7.86 88.19 -0.78 3.67 7.85

314-2 500 ppm

88.19 -0.74 3.51

88.19 -0.74 3.53

7.92

7.96 88.19 -0.73 3.51 7.91 88.18 -0.75 3.52 7.98 88.20 -0.75 3.53 7.95 88.18 -0.75 3.57 8.04

314-2 1000 ppm

88.18 -0.92 4.05

88.21 -0.85 3.82

7.94

7.89 88.25 -0.77 3.58 7.86 88.17 -0.88 3.99 7.86 88.22 -0.86 3.81 7.87 88.22 -0.80 3.69 7.94

314-2 10000 ppm

87.80 -0.92 4.61

87.81 -0.91 4.58

9.48

9.46 87.82 -0.90 4.59 9.46 87.82 -0.91 4.58 9.37 87.82 -0.92 4.54 9.49 87.80 -0.89 4.57 9.50

314-2 25000 ppm

87.38 -0.80 4.90

87.46 -0.84 4.89

11.84

11.45 87.38 -0.81 4.88 11.86 87.40 -0.80 4.89 11.93 87.54 -0.81 4.85 11.39 87.59 -0.99 4.94 10.23

Page | 18

Calibration Curve Data 50 – 5000 ppm PLA Label


Values a*

Values b*

Values L*

Average a*

Average b*

Average Haze Haze

Average

CTRL 0 ppm

88.88 -0.66 2.83

89.15 -0.65 2.78

8.86

8.52 88.95 -0.65 2.78 9.03 89.18 -0.63 2.74 9.04 89.32 -0.67 2.77 7.81 89.41 -0.64 2.76 7.88

314-3 50 ppm

88.10 -0.79 4.00

88.10 -0.76 3.76

10.09

9.14 88.06 -0.68 3.45 8.54 88.14 -0.77 3.70 9.18 88.04 -0.78 3.85 9.73 88.15 -0.80 3.80 8.16

314-3 250 ppm

87.81 -0.65 4.03

87.75 -0.67 4.12

9.75

11.33 87.91 -0.66 4.03 9.40 87.56 -0.69 4.37 15.05 87.76 -0.67 4.08 10.54 87.73 -0.68 4.10 11.91

314-3 500 ppm

88.00 -0.54 4.10

88.02 -0.54 4.07

8.43

8.60 87.99 -0.53 4.12 8.45 88.46 -0.53 3.65 8.09 87.67 -0.55 4.38 9.18 87.98 -0.55 4.10 8.83

314-3 1000 ppm

85.45 -0.28 6.97

85.40 -0.29 7.08

13.27

13.60 85.20 -0.27 7.48 14.86 85.36 -0.28 6.79 12.03 85.63 -0.32 6.86 13.56 85.38 -0.28 7.29 14.26

314-3 5000 ppm

69.28 1.90 13.73

69.20 1.90 13.79

56.35

56.79 69.23 1.93 13.86 56.43 69.05 1.86 13.59 58.12 69.19 1.93 13.88 56.87 69.27 1.90 13.88 56.18

Page | 19

Calibration Curve Data 50 – 10000 ppm PVC Label


Values a*

Values b*

Values L*

Average a*

Average b*

Average Haze Haze

Average

CTRL 0 ppm

88.88 -0.66 2.83

89.15 -0.65 2.78

8.86

8.52 88.95 -0.65 2.78 9.03 89.18 -0.63 2.74 9.04 89.32 -0.67 2.77 7.81 89.41 -0.64 2.76 7.88

314-4 50 ppm

88.26 -0.59 3.34

88.18 -0.61 3.55

8.25

8.24 88.28 -0.67 3.53 8.18 88.14 -0.59 3.65 8.11 88.11 -0.60 3.75 8.34 88.13 -0.59 3.47 8.30

314-4 250 ppm

87.53 -0.37 5.19

87.55 -0.35 5.29

8.03

7.99 87.53 -0.35 5.34 8.00 87.54 -0.34 5.34 7.99 87.58 -0.35 5.30 7.95 87.56 -0.35 5.26 8.00

314-4 500 ppm

86.68 -0.01 7.31

86.71 -0.01 7.24

8.31

8.34 86.73 -0.01 7.21 8.16 86.75 -0.02 7.16 8.33 86.62 0.02 7.38 8.42 86.77 -0.04 7.16 8.48

314-4 1000 ppm

85.12 0.39 11.68

85.19 0.39 11.75

9.37

8.96 85.18 0.39 12.01 8.65 85.24 0.41 11.72 8.62 85.27 0.39 11.72 8.85 85.16 0.36 11.60 9.33

314-4 10000 ppm

65.75 16.52 51.48

66.22 15.83 50.72

20.60

22.00 65.74 16.54 51.47 21.24 66.07 16.06 50.90 22.32 65.77 16.22 51.06 22.76 67.75 13.83 48.68 23.09

Page | 20

Calibration Curve Data 50 – 5000 ppm OPP Label


Values a*

Values b*

Values L*

Average a*

Average b*

Average Haze Haze

Average

CTRL 0 ppm

88.88 -0.66 2.83

89.15 -0.65 2.78

8.86

8.52 88.95 -0.65 2.78 9.03 89.18 -0.63 2.74 9.04 89.32 -0.67 2.77 7.81 89.41 -0.64 2.76 7.88

314-5 50 ppm

87.93 -0.65 3.38

87.94 -0.65 3.36

10.04

10.01 87.97 -0.63 3.28 9.88 87.94 -0.66 3.40 9.91 87.97 -0.66 3.32 9.95 87.90 -0.65 3.40 10.29

314-5 250 ppm

87.01 -0.57 3.79

87.05 -0.60 3.78

16.21

16.81 87.07 -0.59 3.77 16.31 87.07 -0.59 3.78 17.00 87.01 -0.60 3.83 17.04 87.07 -0.64 3.75 17.50

314-5 500 ppm

85.07 -0.56 5.49

85.72 -0.54 4.95

24.85

22.33 85.83 -0.52 4.90 22.09 85.85 -0.53 4.84 22.17 85.90 -0.56 4.80 21.21 85.96 -0.55 4.72 21.34

314-5 1000 ppm

82.74 -0.43 6.60

82.34 -0.43 7.11

43.15

45.53 82.25 -0.42 7.21 46.78 82.25 -0.43 7.22 46.15 82.37 -0.44 7.15 45.36 82.07 -0.41 7.35 46.19

314-5 5000 ppm

79.95 -0.07 11.80

79.90 -0.12 11.99

86.89

86.56 80.16 -0.24 12.29 86.45 79.92 -0.13 12.25 86.77 79.61 -0.11 11.72 85.83 79.87 -0.06 11.91 86.85

Page | 21

Calibration Curve Data 50 – 5000 ppm Olefin MD Label


Values a*

Values b*

Values L*

Average a*

Average b*

Average Haze Haze

Average

CTRL 0 ppm

88.88 -0.66 2.83

89.15 -0.65 2.78

8.86

8.52 88.95 -0.65 2.78 9.03 89.18 -0.63 2.74 9.04 89.32 -0.67 2.77 7.81 89.41 -0.64 2.76 7.88

314-6 50 ppm

88.27 -0.69 3.28

87.98 -0.66 3.52

9.65

11.74 88.20 -0.69 3.36 10.20 87.64 -0.63 3.80 14.01 87.67 -0.62 3.78 14.07 88.14 -0.65 3.36 10.76

314-6 250 ppm

87.59 -0.63 4.10

87.34 -0.66 4.35

19.97

19.00 86.89 -0.67 4.79 20.36 87.22 -0.68 4.49 19.04 87.55 -0.65 4.12 17.34 87.43 -0.65 4.24 18.28

314-6 500 ppm

87.23 -0.60 4.49

87.26 -0.60 4.47

25.79

26.23 87.25 -0.57 4.42 27.27 87.23 -0.58 4.53 27.67 87.28 -0.62 4.45 25.13 87.30 -0.61 4.45 25.30

314-6 1000 ppm

86.32 -0.48 5.25

86.40 -0.49 5.15

40.25

39.13 86.43 -0.50 5.14 39.30 86.46 -0.50 5.15 37.68 86.38 -0.47 5.05 39.23 86.43 -0.49 5.15 39.20

314-6 5000 ppm

81.37 -0.36 10.45

80.00 -0.63 11.30

82.92

85.43 80.07 -0.26 12.70 86.14 80.24 -0.12 11.90 86.30 78.00 -2.17 9.25 86.30 80.34 -0.26 12.21 85.48

Page | 22

Calibration Curve Data 50 – 5000 ppm LD-PET Label


Values a*

Values b*

Values L*

Average a*

Average b*

Average Haze Haze

Average

CTRL 0 ppm

88.88 -0.66 2.83

89.15 -0.65 2.78

8.86

8.52 88.95 -0.65 2.78 9.03 89.18 -0.63 2.74 9.04 89.32 -0.67 2.77 7.81 89.41 -0.64 2.76 7.88

314-7 50 ppm

88.15 -0.66 3.30

88.10 -0.65 3.33

10.29

10.44 88.01 -0.64 3.31 10.74 88.13 -0.65 3.35 10.17 88.10 -0.66 3.34 10.52 88.11 -0.66 3.34 10.48

314-7 250 ppm

87.23 -0.62 3.90

87.44 -0.81 4.61

21.68

18.68 87.89 -0.63 3.63 15.37 87.44 -0.93 5.33 18.75 87.34 -0.84 4.79 18.47 87.32 -1.05 5.41 19.14

314-7 500 ppm

86.77 -0.67 4.43

86.77 -0.74 4.78

31.20

31.54 86.82 -0.69 4.50 31.19 86.78 -0.72 4.77 31.57 86.73 -0.88 5.07 30.97 86.77 -0.76 5.14 32.77

314-7 1000 ppm

85.06 -0.59 5.47

85.05 -0.58 5.56

43.88

44.27 84.97 -0.57 5.52 45.56 84.90 -0.59 5.54 46.24 85.15 -0.58 5.45 44.87 85.17 -0.58 5.80 40.80

314-7 5000 ppm

67.72 1.18 16.07

67.72 1.17 16.20

89.73

89.68 67.73 1.20 16.14 89.74 67.69 1.18 16.29 89.63 67.73 1.15 16.23 89.66 67.74 1.16 16.28 89.66

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Study 2 Glossary

• a* - this is the unit of measurement in regards to how red or green an object is.

• b* - this is the unit of measurement in regards to how yellow or blue an object is.

• CNTLLabel – Nomenclature for OPP wrap label used as a control

• IB – acronym for Intended Bottle

• L* - this is the unit of measurement in regards to how white or black an object is.

• LD-PET – Low Density PET structure with additional layers of confidential materials

• OLEFIN – Polyolefin material

• OLEFIN MD – Polyolefin ROLL FED

• OPP – Orientated Polypropylene

• OPP MD – Oreintated Polypropylene ROLL FED

• OPS – Orientated Polystyrene

• PETG – Polyethylene terephthalate with glycol modification

• PETG Cavitated – a foamed version of PETG

• PLA – Polylactic acid

• PVC – Polyvinyl Chloride

apr’s statement of rationale for the study · 2016-08-26 · apr’s statement of rationale for...

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