WRAP Large Scale HDPE Recycling Trial Report

Large Scale HDPE Recycling Trial

Project code: MDP006 ISBN: 1-84405-308-3 Research date: Date: February 2007

Front cover photograph:

While steps have been taken to ensure accuracy, WRAP cannot accept responsibility or be held liable to any person for any loss or damage arising out of or in connection with this information being inaccurate, incomplete or misleading. It is the responsibility of the potential user of a material, product or process to consult with the supplier or manufacturer and ascertain whether a particular product or process will satisfy their specific requirements. The listing or featuring of a particular product, process or company does not constitute an endorsement by WRAP and WRAP cannot guarantee the performance of individual products, processes or materials. For more detail, please refer to WRAP’s Terms and Conditions on its web site: www.wrap.org.uk

Published by Waste & Resources The Old Academy Tel: 01295 819 900 Helpline freephone Action Programme 21 Horse Fair Fax: 01295 819 911 0808 100 2040 Banbury, Oxon E-mail: [email protected] OX16 0AH

Large Scale HDPE Recycling Trial 1

Executive summary The development of world leading UK recycling technology allows post-consumer milk bottles to be recycled back into food contact milk bottles. Milk bottles with 30% recycled content perform identically as virgin resin bottles, have been extensively tested and have passed all EU, UK and consumer tests and are currently in production within UK dairies. The revolutionary technology represents the first time post consumer HDPE Milk bottles have been recycled back into Milk Bottles with full food contact status. This achievement is a world first. The process is innovative in the unique separation technology and the decontamination process that it uses. The sorting process exploits a new sensitivity that can identify the homopolymer used in milk bottles apart from the balance of the HDPE bottles in the waste stream. The decontamination technology has demonstrated its efficiency via challenge tests that show it is capable of decontaminating HDPE to a "super-clean" state to meet food packaging standards. The resin and bottles have been tested at industrial scale production and have performed in exactly the same manner as virgin materials and bottles requiring no changes to production equipment beyond the introduction of blending equipment. The milk bottles represent worlds best practice in sustainable milk packaging and will save significant amounts of energy and greenhouses gases and make a major contribution to landfill reduction as the technology spreads through the milk packaging industry. Consumers have positively endorsed the use of recycled content in food packaging.


Contents 1.0 Introduction ............................................................................................................................. 4 2.0 Supply of Baled HDPE............................................................................................................... 4 3.0 Bottle Washing and Grinding Process ...................................................................................... 4

3.1 Washing and Granulating of HDPE Bottles – Process Background.............................................4 3.2 Balestock Material Differentiation..........................................................................................5 3.3 Adhesive Contamination Issues in rHDPE...............................................................................6 3.4 Flake Colour Differences (Batch A / Batch B) .........................................................................7 3.5 Other Key Findings..............................................................................................................9 3.6 Material Balance for the Washing/Grinding Step at Sorepla ...................................................10

4.0 Sorting of rHDPE Flake........................................................................................................... 10 4.1 Flake Sorting Requirements................................................................................................10 4.2 Efficiency of Flake Sorting ..................................................................................................12 4.3 Flake Surface Residue........................................................................................................18

5.0 Extrusion and Decontamination of rHDPE Flake.................................................................... 19 5.1 Material Extrusion & Decontamination .................................................................................19 5.2 Visual Analysis of Recycled HDPE pellets .............................................................................19 5.3 Rheological Results ...........................................................................................................20 5.4 Material Balance after Sorting and Extrusion ........................................................................21 5.5 Overall Material Balance.....................................................................................................21

6.0 Blow Moulding of Milk Bottles................................................................................................ 22 6.1 Processing of Recycled HDPE Pellets into Milk Bottles ...........................................................22 6.2 Blow Moulding Conclusions ................................................................................................22 6.3 Nampak Plastics Evaluation of rHDPE resin ..........................................................................23

6.3.1 Material A - Nampak Blow Moulding Trial Evaluation: ...............................................23 6.3.2 Material B – Nampak Blow Moulding Trial Evaluation................................................23 6.3.3 Nampak Plastics Blow Moulding Evaluation Summary ...............................................24

7.0 Milk Bottle Filling Trials and Tests ......................................................................................... 24 7.1 Visual Analysis of Milk Filled Bottles ....................................................................................25 7.2 Full Scale Commercial Milk Filled Bottles (Chadwell Heath 05-08/12/2006) .............................25 7.3 Full Scale Commercial Milk Filled Bottles (Severnside)...........................................................26

7.3.1 Severnside Audit Trail............................................................................................27 7.3.2 Summary: ............................................................................................................28

7.4 Conclusions from Filling Trials ............................................................................................29 8.0 Milk Bottle Decontamination Analysis ................................................................................... 29

8.1 Fraunhofer IVV Material Testing .........................................................................................29 8.2 Screening of HDPE Recyclates for Migration Relevant Compounds .........................................29 8.3 Screening of rHDPE Milk Bottles for Migration Relevant Compounds.......................................31 8.4 Determination of the Overall Migration from HDPE Milk Bottles (Fraunhofer IVV) ....................34

8.4.1 Overall Migration Results .......................................................................................35 8.4.2 Food Regulatory Assessment .................................................................................35

8.5 Determination of the Specific Migration of Irganox 1076 (Fraunhofer IVV)..............................35 8.5.1 Results of Specific Migration of Irganox 1076 ..........................................................35 8.5.2 Food Regulatory Assessment .................................................................................35

8.6 Overall Migration from Milk Bottles (PIRA International Analysis) ...........................................36 8.7 Migration Studies on Recycled HDPE to be Used for Milk Packaging - PIRA .............................37

8.7.1 Conclusions ..........................................................................................................37 8.8 Recycled HDPE Decontamination Conclusions ......................................................................37

8.8.1 Conclusions from Volatile Screening of HDPE Flake, Pellet and Milk Bottle ..................37 8.8.2 Overall Migration Conclusions.................................................................................38 8.8.3 Specific Migration Conclusions................................................................................39 8.8.4 Decontamination of Recycled HDPE – Key Findings: .................................................39

9.0 Sensory and Bacteriological Test Results .............................................................................. 39 9.1 CCFRA Sensory Test Results...............................................................................................39

9.1.1 CCFRA Findings ....................................................................................................40 9.1.2 Conclusions ..........................................................................................................40

9.2 Reading Scientific Services – Sensory Test Results ...............................................................40


9.2.1 Sensory Evaluation Taint Test: ...............................................................................40 9.2.2 Sensory Evaluation Triangle Tests: .........................................................................41 9.2.3 Conclusions ..........................................................................................................41

9.3 Bacteriological Testing .......................................................................................................41 9.3.1 Conclusions:.........................................................................................................41

9.4 Dairy Crest - RHDPE Bottle Filling and Shelf Life Assessment Report ......................................41 9.4.1 Aims:...................................................................................................................41 9.4.2 Scope: .................................................................................................................41 9.4.3 Methodology: .......................................................................................................42 9.4.4 Results.................................................................................................................42 9.4.5 Summary .............................................................................................................46 9.4.6 Conclusion ...........................................................................................................46

10.0 Legal Assessment of the EU Food Contact Status for Recycled HDPE Milk Bottles............... 47 10.1 Keller and Heckmann Assessment.......................................................................................47 10.2 EU Food Contact Status of Recycled Plastic Materials............................................................47

10.2.1 EU Harmonization .................................................................................................47 10.2.2 Suitable Purity of Recycled Plastics .........................................................................48 10.2.3 Regulation of Recycled Materials in the EU Member States .......................................48 10.2.4 Establishing a Suitable Regulatory Status of Nextek’s Post-Consumer Recycled HDPE Milk Bottles.......................................................................................................................48 10.2.5 Summary of the Food Safety Assessment................................................................50

11.0 Fraunhofer Institute IVV – Expert Opinion on rHDPE Milk Bottles Food Contact Safety....... 50 11.1 Introduction......................................................................................................................50 11.2 Technical Aspects..............................................................................................................50 11.3 Compliance with Food Legislation .......................................................................................51 11.4 Evaluation ........................................................................................................................52

12.0 Project Conclusions................................................................................................................ 52 Appendix 1 Participant Details........................................................................................................... 55 Appendix 2 Screening of HDPE Recyclates for Migration Relevant Compounds................................ 56 Appendix 3 Screening of HDPE Milk Bottles for Migration Relevant Compounds.............................. 73 Appendix 4 Determination of the Overall Migration from HDPE Milk Bottles .................................... 80 Appendix 5 Determination of the Specific Migration of Irganox 1076 .............................................. 83 Appendix 6 PIRA Migration Study...................................................................................................... 86 Appendix 7 Migration Studies on Recycled HDPE for Milk Packaging (PIRA).................................... 91 Appendix 8 Legal Assessment of rHDPE Food Safety in the EU and UK (Keller & Heckmann LLP).. 109 Appendix 9 Fraunhofer IVV Expert Opinion ..................................................................................... 116 Appendix 9 Milk Taint Test Data ...................................................................................................... 121 Appendix 10 Sensory Test Results ................................................................................................... 130 Appendix 11 Milk Filling Trial Protocol............................................................................................. 146 Appendix 12 Dairy Crest Comparison of Virgin and Recycled Bottles APC Results ......................... 152 Appendix 13 Rheological Test Data ................................................................................................. 156 Appendix 14 Variations in Balestock Quality ................................................................................... 158 Appendix 15 Extrusion Mass Balance............................................................................................... 159


1.0 Introduction This project was initiated by WRAP to demonstrate the feasibility of large scale recycling of milk bottles from kerbside collection sources into food grade recycled HDPE resin. Recycling of high density polyethylene (HDPE) milk bottles is highly attractive as it provides a recycled material stream that is rheologically highly consistent with a fairly consistent MFI (Melt Flow Index) of approximately 0.6 g/10min. Furthermore rHDPE resin derived from milk bottles is in high demand as it is unpigmented and provides the most consistent recycled HDPE stream. 2.0 Supply of Baled HDPE The balestock material for the large scale trial was ordered from RECOUP in the UK. The material as ordered was to be manually pre-sorted HDPE, with the specification being for less than 5% coloured HDPE content. RECOUP had obtained the balestock (2 truckloads) from two different suppliers. The balestock on the 1st truckload was primarily made up of milk bottles. It was later discovered that the second truckload was found to contain significantly high levels of coloured HDPE from HC (household cleaning) containers such as detergent, shampoo, cleaning agents and fabric softener type bottles. The effects of this difference in supply had significant consequences for this trial. These are further described in later sections of this report.

Figure 1 Pictures of UK pre-sorted HDPE balestock that was used in this trial. The balestock material was collected in the UK and shipped to a large bottle recycling facility in France Sorepla Industrie S.A for bottle washing and grinding. The process description, a material balance as well as key findings from the washing and grinding stage are described in the following section of this report. 3.0 Bottle Washing and Grinding Process 3.1 Washing and Granulating of HDPE Bottles – Process Background Analysis of balestock at Sorepla revealed that besides milk and juice bottles the HDPE balestock also contained household cleaning containers such as detergent and cleaning agent type bottles which are manufactured from copolymer HDPE. This was particularly the case with the 2nd truckload delivery where bale analysis indicated a 10-20% coloured HDPE content. The first truckload of bales was clearly made up of majority milk bottles. These milk bottles had primarily green, blue and red coloured caps The washing plant based at Sorepla uses the Sorema washing technology and together with the grinding process is based upon a typical industrial recycling process for plastic bottles with a production throughput of 2 tonnes/hr. The bales were broken up using a bale breaker and declumper, passed through vibrating tables and trommels to remove caps and other contaminants. The bottles also contain residues which need to be removed during the grinding and washing step. At Sorepla this involved a whole bottle hot wash as well as flake washing. The bottles were hot-washed and passed through a further trommel to remove labels, caps, fibres and other film type contamination. The post-consumer HDPE bottles were then visually checked and any PET, PVC and non-PE bottles were manually removed from the conveyor belt. Where possible coloured-HDPE bottles were also


removed, however the large percentage (>10%) made it impossible to manually remove these. The balestock also contained large amounts of 5-20L HDPE containers and these had to be manually removed as they had caused a number of conveyor blockages. Aluminium and other tin can contamination was found to be very low and was either manually removed, or removed in the process through trommels or via the Pellenc optical sorting system which automatically rejected any metal contamination. Analysis of this system showed that it was also picking up and rejecting large amounts of milk bottles which contained aluminium foil induction cap seals. At Sorepla the Pellenc sorting system removed many of these bottles. Overall it was had found that significant number of milk bottles had contained the aluminium foil induction cap seals. After visual inspection and manual sorting, the bottles were granulated into flake (5-8mm) and then elutriated to remove fines and plastic film contamination. The flake was then washed to remove residual labels and adhesives as well as milk and other bottle residues. The washed flake was then transferred to a sink-float tank to separate other polymers or contaminants. The flake was then rinsed off, dried and bagged.

Figure 2 Bottle and flake wash chemistry flowchart. 3.2 Balestock Material Differentiation Given the differences in balestock supply a decision was made to classify flake from the 1st truckload as ‘Material A’ and flake from the 2nd truckload as ‘Material B’.

Samples from Material A (1st truckload) had shown that colour content in the final flake product was primarily around 4-6% (w/w). The main colour content was from caps as the coloured flakes were primarily green, blue, followed by red and some whites. The percentage of natural-HDPE flakes that still contained attached labels was found to be as high as 5%. Clean natural HDPE flake was determined to be approximately 90% of the flake product after the hot wash and grinding process at Sorepla. Material from the 2nd truckload had also contained milk bottles but also contained a significantly higher level of household cleaning containers. This was clearly evidenced in flake samples as the coloured HDPE composition had changed to the following colours; white, yellow, orange, light blue, light green, purple and black. These colours are not typically used in the dairy industry and as milk bottle caps are primarily a dark green, blue or red colour. The colour content variation between batch A and batch B is shown in Figures 3 and 4.

Figures 3 Material A – Unsorted Flake Figure 4. Material B – Unsorted Flake

Figures 3 and 4 These pictures provide a visual comparison of the differences between the supply of Material A and Material B.

Bottle Wash

Hot Water Caustic

Flake Wash Hot Water Detergent

Antifoaming Agent

Flotation Tanks

Water Antifoaming Agent

Flake Rinse

Water Antifoaming Agent


Some of the following household cleaning bottles and other type bottles were present in the bales:

Bleach, detergent, shampoo and fabric softener bottles

Industrial and automotive cleaning agent bottles

Weed spray bottles

Motor oil bottles

The HDPE balestock, although manually pre-sorted, also contained between 1-3% of other non-PE bottles such as PET, PVC and PP bottles as well PE film in the form of plastic bags and some Tetra-pak cartons. These bottles and film were being manually removed at Sorepla at a manual sorting conveyor belt. Testing of final HDPE flake samples were found to have on average a PET/PVC contamination of approximately 6.75ppm, but certain samples did show PET/PVC contamination as high as 48ppm. 3.3 Adhesive Contamination Issues in rHDPE Hot melt adhesives can cause a number of major problems during recycling of HDPE. For example some rubber based hot melt adhesives can become blended with HDPE during reprocessing and reduce the mechanical properties of the rHDPE resin. Furthermore adhesives that are not water soluble cause a number of problems during further reprocessing stages and cause darkening of the extruded recyclate. During the trial, it was noticed that specific milk bottles had labels with very strong glues that did not come off during the hot wash. Whilst there were a variety of labels that stayed on the bottles, the following labels were particularly visually prevalent in this balestock: Company & Milk Bottle Details Comments Somerfield Stores Ltd (www.somerfield.co.uk) Semi-skimmed milk

Green labels on these milk bottles were not coming off the bottles during hot wash process.

Nisa Todays Holdings Ltd (www.nisa-todays.com) Nisa Today’s Heritage Fresh Milk

Green labels on these milk bottles were not coming off the bottles during hot wash process.

Welsh Milk Bottles had primarily green but also blue labels. Most labels were not coming off and the hot wash process had problems with removing both green and blue labels.

Kwik Save (www.kwiksave.co.uk)

Bottles had both green and blue labels, which were not coming off the bottles.

Iceland Milk (www.iceland.co.uk)

Green labels on milk bottles not coming off the bottles.

Sainsbury’s British Semi-skimmed milk

Green labels on these bottles were occasionally not coming off. These bottles may have slightly more water soluble glues

Table 1 Details of specific labels that were difficult to remove during this particular trial. The issue with troublesome adhesives and labels will need to be resolved by setting up dialogue about adhesives with the bottle packaging industry. Tests on the washed flake samples had indicated that approximately 1.5-5.5% of the natural HDPE flake still contained labels stuck to the flake after the hot-wash process. It was also discovered that the colours from many of these labels had leached out to a major degree into the wash water, however the polypropylene (PP) labels themselves still remained attached to the flake due to the strong water insoluble adhesives used. Dairy Crest have provided feedback on the labels which were found to be difficult to wash off. These labels were all exclusively PP, some single ply and some laminated. Many of the dairies have been persuaded that PP give better performance in terms of application onto the bottles. The dairy industry requires an adhesive that as very high tack and will cope with wet bottles and a cold damp environment and for this reason a rubber based hot melt adhesive. The hot melt rubber based adhesive is permanent and is therefore very difficult to remove. Paper labels on milk bottles absorb moisture and the washing liquids and as such wash off more easily during the hot-wash process, which then exposes the underlying adhesive to the hot caustic wash and allows for the adhesive to be washed off. The PP labels do not absorb any liquid and as such remain firmly stuck to the flakes. Dairy Crest was advised that the flake sorters would be able to remove the flakes that had stuck labels onto them. Dairy Crest had previously had discussions with milk label suppliers about their adhesives, but were informed that this


style of adhesive is an ‘industry standard’ and that it would be difficult to change this and changing the adhesive could be costly. This feedback corresponds well with what was found during the trial. This is why the flake sorter was set up to specifically remove both coloured flakes as well as flakes with attached colour faded labels. The higher levels of flakes with attached labels had later resulted in increased material loss during the sorting stage. Analysis of the labels that were difficult to remove showed that all were PP and primarily laminated, although some were also single ply.

Figure 5 Examples of difficult to remove labels; aluminium caps and induction seals in caps as well as some labels with leached ink.

Figure 6 Microscopic analysis of individual flakes. When viewed under a microscope a substantial amount of glue residue appears coated in green coloured ink. 3.4 Flake Colour Differences (Batch A / Batch B) As described in earlier section of this report an important finding was determined regarding the levels and source of coloured HDPE within the balestock. This difference had resulted in colour variation within the washed flake


product. Bulk bags of flake that contained significantly higher levels of a coloured-HDPE flake of 10-17% after initial testing of the flake was classified as ‘Material B’. All bulk bags classified as Material B were segregated to be double sorted and extruded separately to Material A. Analysis of Material B flake bulk bags, indicated a more uniform spread of colours. In particular colours such as white, yellow, orange and light purple were more dominant than green, blue, black or red colours. The colour variation was therefore more evenly distributed. The flake also smelled differently and the odour could be described as ‘detergent type smell’. However the important factor was that the surface colour of this flake was significantly cleaner and did not show any of the visible ‘greenish tinge’ of Material A. Another factor that may have contributed to the cleaner flake itself may have been the washing action of the residual detergent from the household cleaning containers. These bottles were primarily detergent bottles, bottles containing cleaning products, bleach bottles, shampoo bottles, etc. Due to the much higher levels and wider spectrum of colours it was decided that it would be necessary to sort this flake twice. The bulk bags that had less coloured flake were primarily from milk bottles, and the coloured flakes consisted of mainly green, blue and red coloured HDPE fragments as would typically be seen on milk bottle caps. Prior to extrusion and decontamination at Erema, this flake had a typically clear milk bottle based odour. The surface colour of the Nat-HPDE flakes themselves were noted to have a green tinge. This was visually observed by comparing the flake surface colour to samples from the previous WRAP trial as well as the flake from Material B in this trial. Visually there was a visible difference between the samples. This material contained approximately 1-5% colour content and hence it was decided that bulk bags with this flake would be sorted once only. The greenish flake surface residue seen in Material A is shown and further discussed in Section 4.2 of this report. A potential reason why Material A flake exhibits a greenish tinge is due to a combination of adhesive removed from labels or antifoam and the inks from labels had washed into the water and then deposited as a thin film on the surface of the flake. The flakes produced from 2nd truckload (Material B) were free of this green tinge possibly due to lower levels of green labels and or possibly due to the extra washing action of residual detergents and cleaning agents from the household cleaning bottles. Whilst the coloured ink from wrap around labels had leached out a lot more easily, many of the single ply or laminated PP labels, which were primarily green, blue with black print, had also lost the printed colour and been leached from the label itself during the hot wash of the whole bottles as well as the flake washing at Sorepla. It may be that the leached colour from the labels may have contaminated the wash water colour and therefore coated the surface of the HDPE flakes. This may not have happened with the flakes from Material B due to the presence of residual detergents and cleaning agents. Due to the colour variation between Material A flake and Material B flake a decision was made to separate the bulk bags for sorting purposes. Therefore it can be concluded that are two label related issues that will require optimization of washing and sorting:

Labels with strong glues that do not dissolve in water and did not come off after the hot wash. Labels where the glue and colour leached out into the hot wash water and built up within the water and

coated the flakes in a thin film of glue and green ink/pigments.

Suggestions for improvements:

Printing inks, particularly those containing heavy metals and pigments that easily leach out need to be avoided.

If stick on labels are needed it is best to use water soluble adhesives instead of hot melt or solvent based adhesives for convenient removal during washing stages

Where possible use wrap around labels or shrink sleeves, as these come off easily during washing and after granulation. During the trial it was discovered that the wrap around labels were the easiest to remove from the bottles, however these labels do not have stable inks and pigments as these leach out during the washing stages. The following pictures show how easily the ink from wrap around labels had leached out. This is clearly shown in Figure 6.


Figure 7 Examples of leached ink from milk bottle labels after a hot wash process. 3.5 Other Key Findings

None of the laboratory tests on flake samples showed any aluminium content, however it was expected that the flake product would contain residual aluminium contamination due to the high level of aluminium foil induction cap seals, as well as ‘aluminium foil caps’ on some flavoured milk bottles and small yoghurt drink bottles. These metal foils would be eventually removed by the extrusion process.

Many of the bottles after the hot wash still contained caps which need to be removed as the caps were

coloured and were approximately 10% (w/w). These caps were not coming off easily during the hot-wash or during the debaling and trommeling processes.

Detergent bottles and other household cleaning containers, although HDPE are also primarily coloured

and as they are made from copolymer HDPE it is preferable that these containers are removed and recycled separately. Due to the high level of coloured household cleaning type bottles in the 2nd truckload bales, it was not physically possible to manually remove many of these at Sorepla and as such the majority were left in the recyclate stream and would need to be removed using the flake sorting system. In an ideal situation an automated bottles sorting system at the recycling plant would have been able to remove the majority of the coloured HDPE bottles and hence leave a much more pure natural HPDE stream. The Sorepla plant did not have whole bottle sorting equipment to specifically remove coloured HDPE bottles.

The balestock also contained large amounts of multi-layer yoghurt drink bottles. Removing the white

multi-layer bottles and flakes is very important as they contain a black coloured barrier middle layer, and this will significantly darken the final pellets during the extrusion step. Multi-layer flakes were identified be an issue for the final product quality and as such information was provided to the flake sorting company so that the flake sorter was optimized to removed them. The multi-layer flake seemed to primarily come from small yoghurt drink bottles and other flavoured milk bottles. These bottles are quite difficult to remove due to their small size. These bottles did not come out through the trommel screen as the openings in the screen were not the right size to remove these bottles. The best method of removing these materials is to optimise the flake sorting equipment to specifically identify ‘whites’ and remove these.

During the washing stage it was noticed that the bales also contained occasional black motor oil HDPE

containers. Where ever possible these were manually removed on the sorting belt, but some may have passed through. It is essential that these containers are removed as even after intensive hot washing in


combination with surfactants, there is still some residual oil left over. During reprocessing, the residual oil could result in strong odour and this may limit the use of the recycled resin.

Flake samples were sieved and tested for residual fines and were found to contain up to 0.125% of

fines. The majority of the flake was ground to a size of 5-7mm.

Figure 8 Examples of aluminium contamination. 3.6 Material Balance for the Washing/Grinding Step at Sorepla The following data on material losses has been provided by Sorepla. Balestock

Weight (Kg)

Moisture in

Balestock (Kg)

Raw Material

Input (Kg)

Heavy Parts Loss

(Kg)

Waste

(Kg)

Fines, Paper (Kg)

Sink Fraction

(Kg)

Final Product

(Kg)

34,220 2,750 31,470 800Kg 300Kg 600Kg 800Kg 28,970Kg 8% 100% 2.5% 1.0% 1.9% 2.5% 92.1%

Table 2 Material balance for the washing and granulating of post-consumer HDPE bottles*. (Source: Sorepla) The above table shows the material balance and associated losses during bottle washing, grinding and flake washing stage. As the table shows, there was also substantial loss due to moisture/liquid present within the bottles in the bales. Sorepla have provided us with feedback that they typically find that most bales contain anywhere between 7-12% moisture/liquid content. During this trial it was found that moisture/liquid within baled bottles was approximately 8%.The above table shows that actual material loss during bottle washing, grinding and flake washing is almost 8%. 4.0 Sorting of rHDPE Flake 4.1 Flake Sorting Requirements Coloured HDPE recyclate is of concern for blow moulding of unpigmented HDPE bottles. In most operations the green colour of rHDPE derived from milk bottles is caused by the incorporation of the caps of the milk bottles into the recycled stream. For this reason it is necessary to utilize colour flake sorters to remove the coloured HDPE cap material. Apart from sorting out coloured caps because of discolouration of the unpigmented natural HDPE, it is also important to remove coloured HDPE bottles. Recycled HDPE homopolymer from dairy bottles can also be mixed with clear and coloured HDPE copolymer containers used in the manufacture of detergent and household cleaning containers, which have a lower melt flow index. It is important to remove the copolymer HDPE bottles due to potential resin discolouration as well due to the mixed resin potentially resulting in lower modulus of the recycled milk bottle resin. The S+S flake sorter system was set up at Erema by the S+S technicians. The initial set-up needed further optimization as there was a need to remove residual label and film fines from the incoming HDPE flake. Thus a basic hydrocyclone air separator was set-up to remove the label film flakes. Once installed, this proved to be an


effective way to remove these residues. A further advantage was that the label film did not build up on the flake sorter screen and infeed tables due to static friction. The following figure shows the settings of the test unit. These optimised settings were found to be the most effective at removing the large levels of colour.

Figures 9 and 10 Figures 9 and 10 show incoming flake from materials A and B. Material A clearly exhibits less colour and the colours shown (green, red and blue) are typical of cap material. Material B shows cap colours but also shows many other coloured flakes from non-milk bottles.

FLAKE SORTING SET-UP

Product: HDPE Delay: 9ms Eject Time: 4ms Filter: 1mm Sensitivity: 50% Vibro Level: 88% Throughput: 600Kg

S+S Spektrum 1000 sorting unit Material Input, Reject and Output Settings of Test Unit

Figure 11 The S+S Separation and Sorting Technology GmbH, flake sorting set-up.

Figure 9. Material A – Unsorted Flake

Figure 10. Material B – Unsorted Flake


4.2 Efficiency of Flake Sorting Analysis was performed on a number of samples for Material A and Material B to ascertain the flake sorting efficiencies at Erema and this data is presented in the following diagrams.

Figure 12 The flake sorting flowchart showing sorting efficiency on Material A flake.

MMaatteerriiaall AA FFllaakkee

Nat-HDPE 91 % Col-HDPE 5.5 %

Labels 3.5 %

MMaatteerriiaall AA FFllaakkee 11sstt PPaassss ‘‘RReejjeeccttss’’

Nat-HDPE 74 %

Col-HDPE 21.5 % Labels 4.5 %

MMaatteerriiaall AA FFllaakkee 11sstt PPaassss ‘‘AAcccceeppttss’’

Nat-HDPE 99.8% Col-HDPE 0.1 %

Labels 0.1 %

1st Pass

EERREEMMAA EExxttrruussiioonn

&& DDeeccoonnttaammiinnaattiioonn

1st RESORT

MMaatteerriiaall AA FFllaakkee 22nndd PPaassss ‘‘AAcccceeppttss’’

Nat-HDPE 99.4 % Col-HDPE 0.3 %

Labels 0.3 % MMaatteerriiaall AA FFllaakkee 11sstt RREESSOORRTT ‘‘RReejjeeccttss’’

Nat-HDPE 63 % Col-HDPE 34 % Labels 3 %

REJECT STREAM Col-HDPE Flake

rHDPE Pellets


Figure 13 Pictorial schematic for Material A sorting and the final pelletised HDPE resin.

Unsorted Flake (Material A)

1st Pass Rejects from Material A

Sorted Flake (Material A)

Final Product after extrusion


Figure 14 The flake sorting flowchart showing sorting efficiency on Material A flake. (The WRAP April 2005 HDPE trial flake contained a coloured HDPE content of around 1.4% and the material after sorting going into the Erema extruder had a colour content of < 100ppm). The figure of 1.4% coloured HDPE content in previous WRAP trial is extremely low and not typical of industrial situations as coloured HDPE fragments from caps alone are normally between 5-10% (w/W) of bottles. During this trial it was found that colour content in manually pre-sorted HDPE balestock can vary from 5% up to 15%, depending the collection scheme and the manual sorting efficiency at the material recycling plants.

MMaatteerriiaall BB FFllaakkee

Nat-HDPE 80 % Col-HDPE 14.5 % Labels 5.5 %

MMaatteerriiaall BB FFllaakkee 11sstt PPaassss ‘‘RReejjeeccttss’’

Nat-HDPE 52%

Col-HDPE 42.5% Labels 5.5 %

MMaatteerriiaall BB FFllaakkee 11sstt PPaassss ‘‘AAcccceeppttss’’

Nat-HDPE 98.2%

Col-HDPE 1% Labels 0.8%

1st Pass SORT

MMaatteerriiaall BB FFllaakkee 22nndd PPaassss ‘‘RReejjeeccttss’’

MMaatteerriiaall BB FFllaakkee 22nndd PPaassss ‘‘AAcccceeppttss’’

Nat-HDPE 99.63 % Col-HDPE 0.25 % Labels 0.12 %

EERREEMMAA EExxttrruussiioonn

&& DDeeccoonnttaammiinnaattiioonn

1st RESORT 2nd Pass Sort



Labels 3.2 %



Labels 0.2 %

2ND RESORT

MMaatteerriiaall BB FFllaakkee 11sstt//22nndd RREESSOORRTT

‘‘RReejjeeccttss’’ Nat-HDPE 55.0 % Col-HDPE 38.5 % Labels 6.5 %

REJECT STREAM Col-HDPE Flake

rHDPE Pellets


Figure 15 Pictorial schematic for Material A sorting and the final pelletised HDPE resin.

Unsorted Flake (Material B)

1st Pass Sort of Material B

Material B 1st Pass Rejects

2nd Pass Sort of Material B

Final product after extrusion.


The following sorting efficiency data analysis was obtained from the S+S testing laboratory on flake inputs into the S+S sorter from flake materials A and B. This is shown in Figures 16 and 17.

Figure 16 Laboratory analysis on material A sorting efficiency. (Source: S+S Separation and Sorting Technology GmbH)


Figure 17 Laboratory analysis on material B sorting efficiency. (Source: S+S Separation and Sorting Technology GmbH).


4.3 Flake Surface Residue A build up of glue and ink type green residue was noticed on pipes conveying flake to the sorter and the ‘glass chute window’ on the sorter itself. The glue and the residue were able to be wiped off with a cloth. Further to that a greenish angel hair type film formed on a number of pipes. Evidence of this phenomena is shown in the following pictures.

Figures 18-23 The figures above show examples of the issues created by excessive glues and the leached ink on the sorting and auxiliary equipment.

Figure 19. Wiping off glue & green ink.

Figure 20. Glue & ink residue wiped from glass

Figure 21. Glue & green ink inside air-classifier

Figure 22. ‘Angel hair film’ removed from pipes.

Figure 23. ‘Angel hair film’ build up in pipes.

Figure 18. Glue & green ink build up on glass.


5.0 Extrusion and Decontamination of rHDPE Flake 5.1 Material Extrusion & Decontamination At Erema after separately extruding the two batches of flake it was finally determined that there were clearly two distinctive types of recycled HDPE flake. The greenish surface tinge of Material A flake had resulted in a light green pellet after extrusion, whereas the extruded HDPE pellets from the cleaner Material B flake had a much lighter natural colour. During the trial at Erema it was not possible to do a 30% rHDPE/virgin blend to check what the final colour of the resin for milk bottles would be as there was no available virgin resin.

Figure 24 The Erema two-step process used for the decontamination and extrusion of post-consumer HDPE flake.

MACHINE PARAMETERS OPERATING CONDITIONS

Temp. KT 80-97 °C Vacuum KT 2-4.5 mbar Aver. dwell time KT 45 min Temp. Reactor RGAT - VS 120-125 °C Vac. Reactor RGAT - VS 0.5-3 mbar Aver. Dwell time RGAT - VS 60 min Screw speed 150 rpm Output 275-325 kg/h Melt temp. 218-221°C Melt pressure 140-170 bar Screens 150 mesh (~ 100µm) Back flush interval 80-120 min

Table 3 Process parameters of the Erema two step process used in this study for decontamination of post-consumer HDPE. The screw design used by Erema for this trial was based upon a special design which, when compared to the barrier screw used for the previous WRAP study had the following unique modifications:

Shallower cut in the feed section

Lower compression-ratio

Includes varying screw-pitches to avoid sudden channel reductions / enlargements

5.2 Visual Analysis of Recycled HDPE pellets A common source of contamination in extruded recycled HDPE pellets is ‘black specs’. These are generally small bits of the polymer or contamination that have been degraded and have become carbonized due to excessive


temperatures or residence time within the extruder. These black specs usually occur due to ‘hang up spots’ within the extruder. Black specs cause major problems when blow moulding natural bottles, where they are visually undesirable and can potentially reduce the containers mechanical properties. Extruded material was analysed by compression moulding it into sheets and examined for black specs but none were found. Flushed material from the Erema filters was analysed and was found to contain some residual PET fines, flakes and some fibrous materials from paper labels. The rHDPE pellet material was filtered using 150µm mesh. Recycling of PCR (Post Consumer Recyclate) HDPE can also lead to the formation of gels during extrusion due to cross-linking, when the stabilizing antioxidants become consumed. The cross-linked regions ‘gels’ can provide stress points which can cause ‘blow outs’ in bottles. Extruded material was compression moulded into sheets and visually analysed for gel formations, however none were discovered. 5.3 Rheological Results The following rheological results were obtained from extruded HDPE samples. More rheological tests will be performed on material samples in the near future.

MFI 190ºC / 2.16Kg

Sample Details

0.61 10:30am 10/07 (Material A) – Tested at Erema 0.62 1:30pm 10/07 (Material A) – Tested at Erema 0.64 5:30pm 10/07 (Material A) – Tested at Erema 0.66 8:00am 11/07 (Material A) – Tested at Erema 0.61 9:30am 11/07 (Material A) – Tested at Erema 0.65 1:30pm 11/07 (Material A) – Tested at Erema 0.65 3:30pm 11/07 (Material A) – Tested at Erema 0.65 8:00am 13/07 (Material A) – Tested at Erema 0.64 Material A (Bag 4) – Tested at London Met Uni 0.64 Material A (Bag 9) – Tested at London Met Uni 0.66 Material A (Bag 17) – Tested at London Met Uni 0.67 Material A (Bag 18) – Tested at London Met Uni 0.64 MFI Average for Material A

0.61 8:00am 12/07 (Material B) – Tested at Erema 0.50 12:00am 12/07 (Material B) – Tested at Erema 0.54 4:00pm 12/07 (Material B) – Tested at Erema 0.58 Material B (Bag 10) – Tested at London Met Uni 0.65 Material B (Bag 11) – Tested at London Met Uni 0.60 Material B (Bag 12) – Tested at London Met Uni 0.60 Material B (Bag 13) – Tested at London Met Uni 0.60 Material B (Bag 14) – Tested at London Met Uni 0.61 Material B (Bag 15) – Tested at London Met Uni 0.64 Material B (Bag 16) – Tested at London Met Uni 0.59 MFI Average for Material B

(Reference Sample: WRAP trial April 2005 MFI = 0.64)

Table 4 Rheological data of HDPE recycled pellets. (Source: Erema/London Metropolitan University) Material A was primarily made up of flake that came from milk bottle balestock and hence the MFI results show a high level of consistency. The MFI average was 0.64 g/10min, this compares favourably with the previous WRAP trial where the MFI of the material was found to be 0.64 g/10min. Material B shows slightly lower MFI results and this may be due to the slightly higher levels of clear copolymer HDPE resin. Full rheological study test results are presented in Appendix D.


5.4 Material Balance after Sorting and Extrusion

INPUT SORTING LOSSES

EXTRUSION LOSSES

OUTPUTS

HDPE Flake

(Kg)

Material Conveying &

Transfer Losses (Kg)

Air Classifier Losses

(Kg)

Melt Filtration Losses

(Kg)

Coloured HDPE Flake

(Kg)

HDPE Pellets

(Kg) 28,970 654 2,100 250 6,713 19,253

Table 5 Mass balance after sorting and extrusion. (Source: Erema) 5.5 Overall Material Balance The following data is preliminary data only, which is being cross-checked and will be further updated.

Material Balance (Efficiency & Losses)

Processing Stages Material Amounts

Step Loss per Stage Cumulative Loss per Stage

(Kg) % % Balestock input 34,220 Moisture and Liquid Loss 2,750 8% Baled HDPE Bottle Input 31,470 Loss of Material (washing/grinding)

2,500 8%

Output of Washed Flake 28,970 15% Sorting - Washed Flake Input 28,970 Material Conveying Losses 654 2% Air Classifier Losses 2,100 7% Rejects - Coloured HDPE Flake 6,713 23% Output of Sorted Flake 19,503 33% Extrusion - Sorted Flake Input 19,503 Melt Filtration Losses 250 1% 1% Output of Pelletised HDPE Resin

19,253

Total Cumulative Loss: 44%

Table 6 The overall process mass balance.


6.0 Blow Moulding of Milk Bottles The blow moulding of milk bottles took place at Nampak Plastics on the 25th of July. The trial involved blow moulding of bottles from Material A and B blended with virgin milk bottle HDPE resin on a single head machine using a 4 pint mould. The bottles were manufactured from a blend of 70% virgin resin / 30% recycled HDPE resin. Some bottles were also manufactured from 100% recycled HDPE resin, using both batch A and B recycled HDPE resin. An initial trial was conducted to produce several hundred bottles. These bottles were then supplied to Dairy Crest for a filling trial and subsequent microbiological and sensory testing.

Figure 25 Blow moulding of milk bottles with 30% of rHDPE content at Nampak Plastics. 6.1 Processing of Recycled HDPE Pellets into Milk Bottles The blow moulding trials resulted in production of bottles containing 30% recycled HDPE content bottles that had similar colour characteristics to the reference bottles (100% virgin). The bottles containing 30% recycled HDPE have also been tested for toploads, brimful capacity, stability, dimensional tests and visual tests and compared to reference 100% virgin bottles. As previously mentioned recycled HDPE Material A pellets, had a greener tinge then Material B pellets. However, when blended with 70% virgin, the bottles were visually similar to the 100% virgin bottles. Bottles produced with a 30% blend of Material B were also visually similar to the 100% virgin reference bottles. Production of bottles from Material A / virgin blend had experienced occasional problems with contamination within the resin. This had resulted in a number of bottles showing streaking and some bottles had also contained small holes or occasionally resulted in blow-outs. The contamination origin is currently being investigated, however it appears to be possibly related to PET fines/flake residue. The PET fines/flakes contamination is believed to have likely come from hang-up spots in material conveying equipment. This issue was found to be related only to the first processed material (e.g. Batch A). There were no bottle processing issues related to the Material B / virgin resin blend. This blend had processed in a similar manner to 100% virgin resin, with very few changes to the machine set-up. The bottles produced did not show any visual or other type defects during the trial production run. 6.2 Blow Moulding Conclusions Bottles were successfully moulded from a 70:30 blend of virgin HDPE to recycled HDPE (Material A and B). The material blend had rheologically behaved in a similar manner to 100% virgin HDPE and the machine set-up did not need to be changed. The rHDPE bottles have also passed all Nampak quality tests such as toploads, brimful capacity, stability and all dimensional and visual tests.


6.3 Nampak Plastics Evaluation of rHDPE resin The following section contains an evaluation report from Nampak Plastics, after a four day commercial trial. The project was run over a four-day period to fully assess the performance of both WRAP grade A and B materials. The main purpose was to assess the process ability and stability of both grades on a standard Uniloy Recip machine designed for HDPE material. The machine designated to the trial was Severnsides SB1 - 4 pint HIS, and was run at a target weight of 41 grams +/- 1.0 with a cycle time of 7.5 seconds. The material was introduced at 30% as per the trial request. The granulator was cleaned down and the machine line was marked up to notify all that the trial was in progress. 6.3.1 Material A - Nampak Blow Moulding Trial Evaluation: The grade “A” trial was run over a period of two days (180,000 containers), and the following observations were made:

A 0.3 – 0.4-gram weight increase was observed in bottles

Noted a slightly reduced die swell from a standard virgin/regrind mix.

Made no changes to the process from our standard running conditions (timers, air pressures or

hydraulics)

Material was very clean, with little or no contamination evident.

Trial reject levels over the total trial period - 2.4%, Nampak reported that the low reject levels could have been attributed to the high emphasis put on the machine with the correct labour in place. However the low reject levels was mainly due to the cleanliness of the material. At the initial start Nampak staff did see a small degree of contamination, which Nampak staff felt was due to the storage of the material (debris on the top of the bag), wooded pallets and the fact that the material was being stored in fabric sacks. 6.3.2 Material B – Nampak Blow Moulding Trial Evaluation The grade “B” trial was run over a period of 14hours (52,000containers), and the following observations were made:

A 0.7 – 1.0-gram weight increase was observed in bottles.

The die swell was slightly decreased again and it was felt that this was due to the material having a

higher density characteristic.

On the commencement of the trial we saw a greater degree of contamination. Whilst it was not enough

to cause holes, we could see gel spots and small contaminants.

During the night shift the operator reported a high percentage of split parisons, and was unable to carry

on processing material. The bag was changed and we saw no further issues. This caused us

approximately 40 minutes of lost production time.

Total trial rejects for the trial period ran at 7.1%.

Figure 26 Commercial blow moulding trials at Nampak Plastics.


6.3.3 Nampak Plastics Blow Moulding Evaluation Summary Whilst both material grades processed well, the preferred material would be grade “A”. Both materials showed very little issues with trimming, processing or problems with weight control. The weights over the period of the whole trial (“A” and “B”) gave a maximum variation of +/- 0.3 grams. The grade “B” as previously stated was not as clean and may be a little more labour demanding (splits parisons). 7.0 Milk Bottle Filling Trials and Tests The first milk bottle filling trials took place at Dairy Crest from the 26th of July to 28th of July at the Totnes site. The filling trials involved filling of milk bottles with the following milk types.

Skim Milk (26/07/06)

Full Cream Milk (27/07/06)

Semi-skim Milk (28/07/06)

Bottles containing blends of recycled HDPE from Batch A and Batch B were filled and sent for external sensory testing. Bottles containing Material A only were filled and set aside for stability/bacteriological testing. A comprehensive testing regime was developed and is presented in Appendix E. The following photographs show the rHDPE milk bottles during the milk filling process.

Figure 27 Milk bottle filling trials at Dairy Crest.


7.1 Visual Analysis of Milk Filled Bottles The milk bottles were filled with several different types of milk to test the effect of milk differences on the visual colour variation of the end product. This is necessary due to the fact that full cream milk has different opacity and hues to skim milk or semi-skim milk. Milk filled bottles had clearly demonstrated that there was no visual colour variation between bottles that contained 30% of recycled HDPE from Batch A or Batch B. The following photographs show that visually there is no difference between samples, A, B and C (the reference bottles).

Figure 28 Comparison of milk filled recycled bottles. Filled bottles were then marked and the following tests were commissioned:

Organoleptic sensory tests by Campden & Chorleywood Food Research Association (CCFRA), Consumer

and Sensory Sciences Department

Organoleptic sensory tests by Reading Scientific Services Ltd

Microbiological / bacteriological tests performed by Eclipse Scientific Group

Shelf life testing by Dairy Crest Ltd

7.2 Full Scale Commercial Milk Filled Bottles (Chadwell Heath 05-08/12/2006) A second market trial was carried out in Chadwell Heath on Marks & Spencer (M&S) standard milk which went into store for a week and was sold out. A total of 78,500 units of 4-pint RHDPE bottles were filled between 4/12 and 8/12 in M&S label (standard English Whole, Semi-skimmed and Skimmed Milk) on a Stork filler at Dairy Crest. These bottles contained 30% recycled content and were sent into store to fulfil M&S demand in order to determine the following:

Do the consumers notice any organoleptic difference between milk in an r-HDPE and milk in a virgin

HDPE bottle?

Do standard milk consumers notice any difference in appearance between a virgin and rHDPE bottle

Is there any difference in performance of a recycled bottle through the supply chain – for example

leakers or cracked bottles at depot / store or in consumers homes

The trial was monitored via M&S consumer complaints data supplied via feedback from M&S. The following table provides a comparison of customer complaints during the trial period this year and a comparison to previous year’s complaints.

This Year’s Complaints Last Year’s Complaints 1 5

The results indicated a 0.6% increase in unit volume and a 80% decrease in complaints. The trial was successful from a filling perspective, although there needed to be significant adjustments made to the filler line due to the distinct differences in dimensions and mouldings of bottles blown at the Severnside site. The dimensional differences from the different sites had resulted in some bottles not being capped and having


suffered damage to the sealing lip. The production was checked for leaking product approx 1 in every 200 / 250 didn’t get capped and suffered damage to the sealing lip. 6 bottles were found in the cold store with mechanical damage from the filler and one bottle was found with a pinhole. Throughout the trial, it had been necessary to adjust the filler settings in order to run with minimal issues, the adjustments made however had reduced excess foaming and damage to the bottle necks stabilised. The dimensional differences between standard Chadwell blown and Severnside rHDPE blown bottles have proven to be significant, and showed the tight tolerances in the milk filling operations.

Figure 29 C Severnside bottles were found to be minutely different in size to the Chadwell bottles. Changes to filler set-up had overcome this slight difference.

Figure 30 Due to this slight difference, there was some initial thread damage to a small number of bottles. This issue was overcome with an optimised filler set-up. In conclusion, there are set up changes that needed to be made to the filler at start and end of production. All the bottles that were damaged under the capping heads didn’t actually get capped so were all rejected. If all bottles supplied to site were from the same moulds then the filler could be engineered to run them successfully but this could not be done for the trial. 7.3 Full Scale Commercial Milk Filled Bottles (Severnside) The final commercial trial took place at the Dairy Crest Severnside site. The trial used bottles that were blown by Nampak Severnside site. The bottles were used for M&S Organic (whole, semi-skimmed and skimmed) milk. All bottles were coded and labelled as containing recycled HDPE ‘(R)’ and each bottle used for this trial was also marked at the base of the bottle. This can be clearly seen in the following pictures.


The trial was very successful in terms of operational filling of the bottles and there were no major issues found with the rHDPE bottles. The rHDPE bottles performed as well as virgin HDPE bottles in all aspects.

Figure 31 Trials at Dairy Crest Severnside site. The above pictures show the (R) marking on milk bottles sent to M&S for sale and customer evaluation. Each milk bottle with a 30%recycled HDPE content was also marked with a punched dot at the base of the bottle. 7.3.1 Severnside Audit Trail Products were filled and boxed at Severnside. Bottles were checked by the DC CSM team in order that a complete audit could be carried out.

Figure 32 C Severnside bottles were found to be minutely different in size to the Chadwell bottles. Changes to filler set-up had overcome this slight difference.


Products were also viewed in Nuneaton (Dairy Crest NDC), M&S Gist depot at Faversham and finally at store overleaf:

Figure 33 C Severnside bottles were found to be minutely different in size to the Chadwell bottles. Changes to filler set-up had overcome this slight difference. The Dairy Crest CSM feedback was found to be invaluable as it allowed DC staff to track the product throughout the complete supply chain

Figure 34 rHDPE bottles (in store) (at home) (proof of purchase)

This Year’s Complaints (DC Severnside) Last Year’s Complaints (DC Severnside) 0 2

The results indicated an 11% increase in unit volume and a 100% decrease in complaints. 7.3.2 Summary: Three milk bottle filling trials have been carried out by Dairy Crest at Totnes, Chadwell Heath and Severnside sites. Some operational difficulties were experienced at Chadwell due to slight bottle size differences. but were overcome by optimising the filling line set up. The finding was that there are very tight tolerances from site to site both in bottle blow moulding and filler set-ups. All trials have now concluded and have been customer complaint results have been signed off technically by M&S. R-HDPE performed comparably to virgin bottles in the supply chain tests.


7.4 Conclusions from Filling Trials The filling trials clearly demonstrated that there were no quality or operational differences when filling milk bottles with recycled HDPE content and 100% virgin HDPE bottles. During the filling trials, one defective bottle was found in the input of bottles sent from Nampak Plastics. The milk bottle filling trials had also clearly demonstrated that there was no significant visual colour variation between bottles containing 30% recycled HDPE (Batch A & B) when compared to filled 100% virgin HDPE milk bottles. Bottles containing 30% recycled HDPE filled with different types of milk such as skim; semi-skim and full-cream milk, did not show any significant colour variation when compared to 100% virgin HDPE milk bottles. Overall feedback from Dairy Crest has indicated that filling of the rHDPE bottles was successful. 8.0 Milk Bottle Decontamination Analysis 8.1 Fraunhofer IVV Material Testing Fraunhofer IVV was commissioned to perform analytical tests on washed flake; super-cleaned extruded pellets, milk bottles. Samples of washed HDPE flake and corresponding extruded pellets of recycled HDPE in tight lid jars were sent to Fraunhofer Institute for testing. Samples were received by the Fraunhofer on the 18th of July. The testing process has involved headspace screening for volatile compounds as well as extraction of the samples and GC screening for medium and non volatile compounds. Bottles from Nampak blow moulding trials were sent to Fraunhofer IVV. All results are compared with virgin HDPE and previous WRAP trial. The following analytical tests were initiated and are described in detail in the following sections of this report:

Screening of HDPE Recyclates for Migration Relevant Compounds

Screening of rHDPE Milk Bottles for Migration Relevant Compounds

Determination of the Overall Migration from HDPE Milk Bottles

Determination of the Specific Migration of Irganox 1076

8.2 Screening of HDPE Recyclates for Migration Relevant Compounds The screening for migration relevant compounds in the post-consumer HDPE material was carried out using headspace gas chromatography by the Fraunhofer Institute for process Engineering and Packaging. The following figures provide typical results obtained from screening tests for migration relevant compounds in the post-consumer recycled HDPE flake and super-cleaned pellets. A comparison to virgin HDPE and previous WRAP trial results is also made. The screening for migration relevant compounds in the post-consumer HDPE materials was carried out using headspace gas chromatography. This method detects substances up to a molecular weight of about 250 g mol-1. The detection limit is in the order of about 1 ppm. The following graphs provide a summary of the headspace test results. Full results of the headspace fingerprints of the investigated recyclate samples are shown in Figure 1 to Figure 37 in Appendix B. Fingerprints of reference samples from the previous study as well as virgin HDPE are given in Figure 38 and Figure 39 in Appendix B. Full details of the screening tests as performed by the Fraunhofer Institute are provided in Appendix B. The evaluation of the results was done only on a qualitative basis. However all samples are analysed in the same way and the fingerprints were plotted in the same scale so that the headspace gas chromatograms can be compared with each other.


Figure 35 Typical headspace gas chromatogram of super-clean HDPE pellets. (Sample - previous WRAP trial).

Figure 36 Typical headspace gas chromatogram of washed HDPE flake. (Sample 2a).

Figure 37 Typical headspace gas chromatogram of super-cleaned HDPE pellet. (Sample 2b)


Figure 38 Typical headspace gas chromatogram of virgin HDPE pellets.

In the flakes samples several polyolefin oligomers could be determined as well as some post-consumer compounds. In the corresponding super-clean pellet samples, the concentrations of these compounds are significantly reduced down to levels below the oligomer concentrations in virgin HDPE. For sample 5a higher amounts of suspicious compounds, which are not typical of HDPE have been detected. However in a second sub-sample, these peaks could not be determined. This indicates, that only some individual flakes are contaminated with higher amounts of compounds that are not related to HDPE. The level of these compounds will be decreased by dilution with non-contaminated HDPE flakes down to lower ppm levels. The super-clean decontamination step further decreases the concentrations in the final product. Due to the fact that most of the detected suspicious compounds are related to flavour and fragrance compounds, Fraunhofer Institute recommended organoleptic tests with milk bottles manufactured from super-clean recycled post-consumer HDPE. 8.3 Screening of rHDPE Milk Bottles for Migration Relevant Compounds The screening for migration relevant compounds in the milk bottles containing 30% super-clean rHDPE material was carried out using headspace gas chromatography by the Fraunhofer Institute for process Engineering and Packaging. The following figures provide results that were obtained from screening tests for migration relevant compounds in HDPE milk bottles manufactured with 30% super-cleaned recycled HDPE pellets. A comparison is made to 100% virgin HDPE milk bottles and milk bottles previous WRAP study1. The screening for volatile migration relevant compounds in the investigated HDPE milk bottles was carried out using headspace gas chromatography. This method detects substances up to a molecular weight of about 250 g mol-1. The detection limit is in the order of about 1 ppm. The headspace fingerprints of the investigated recyclate samples are shown in Figure 36 and Figure 37. Fingerprints of reference samples are shown in Figure 38 and Figure 39 respectively. Full report of the screening tests as performed by the Fraunhofer Institute are provided in Appendix C. Samples tested:

Sample 1: HDPE milk bottles, 4 pint, 30% recyclate, Batch A

Sample 2: HDPE milk bottles, 4 pint, 30% recyclate, Batch B

Sample 3: HDPE milk bottles, 4 pint, 100% virgin HDPE (reference bottle)

Sample 4: HDPE milk bottles, 4 pint, 30% recyclate, WRAP project 2005 (reference bottle)


Results Obtained:

Figure 39 Headspace gas chromatogram of sample 1 (30% Material A)

Figure 40 Headspace gas chromatogram of sample 2 (30% Material B).

Figure 41 Headspace gas chromatogram of sample 3 (100% virgin HDPE).

Samples 1 to 3 have similar headspace fingerprints. The concentrations of the detected compounds are in the reference sample (sample 3, 100% virgin) slightly higher than in the bottles containing recycled HDPE (samples 1 and 2). The bottle from the previous WRAP project (sample 4) has the lowest concentrations, which is however, most probably due to another HDPE virgin pellet quality.


Figure 42 Headspace gas chromatogram of sample 4 (WRAP Project, 2005).

Figures 43 and 44 show the gas chromatograms of the dichloromethane extract of the investigated HDPE milk bottle samples with 30% recyclate. In gas chromatograms of the reference samples are given in Figure 45 and Figure 46 respectively. The internal standards have retention times of 18.4 min (butyl-hydroxyanisol, BHA) and 47.5 min (Tinuvin 234) respectively.

Figure 43 Gas chromatogram of the dichloromethane extract of sample 1 (30% Material A).

Figure 44 Gas chromatogram of the dichloromethane extract of sample 2 (30% Material B).


Figure 45 Gas chromatogram of the dichloromethane extract of sample 3 (100% virgin HDPE).

Figure 46 Gas chromatogram of the dichloromethane extract of sample 4 (WRAP Project, 2005).

All investigated samples have similar fingerprints. The oligomeric pattern, which was determined in the headspace screening was also determined in the extracts. In addition, the polymer additives Irfagos 168 as well as Irganox 1076 were determined. The concentrations of these two additives were in the same concentration range than the virgin milk bottle. Due to the fact that the recyclate containing HDPE milk bottles and the reference bottle manufactured from 100% virgin show no significant differences, it can be expected that also the migration (specific as well as the overall migration) will be in the same range. 8.4 Determination of the Overall Migration from HDPE Milk Bottles (Fraunhofer IVV) The Fraunhofer Institute for Process Engineering and Packaging had performed tests to determine overall migration into aqueous food stimulants from milk bottles manufactured using recycled HDPE. The full report is in Appendix D. The following section of this report gives the results obtained and provides food regulatory assessment. The following samples were supplied for analysis:

Sample 1: HDPE milk bottle, 4 pint, 30% recyclate, Batch A

Sample 2: HDPE milk bottle, 4 pint, 30% recyclate, Batch B

Sample 3: HDPE milk bottle, 4 pint, 100% virgin material (reference)

The test method used was, European Standard EN 1186-9. The test was performed over a period of 10 days at 20°C. The stimulants used were 3% acetic acid and 50% ethanol. The test conditions involved total immersion over a contact area/volume of 0.5dm2/100ml.


8.4.1 Overall Migration Results The following table shows the overall migration test results obtained. The result values given are as mean values.

SAMPLES Overall Migration

3% acetic acid

(mg/dm2)

Overall Migration

50% ethanol

(mg/dm2)

Sample 1 – Batch A (0.0, 0.0, 0.0)

Mean Value = 0.0

(0.0, 0.0, 0.1)

Mean Value = 0.0

Sample 2 – Batch B (0.0,0.0,1.7)

Mean Value = 0.6

(0.0, 0.0,0.0)

Mean Value = 0.0

Sample 3 - Reference (0.0, 0.0)

Mean Value = 0.0

(0.0, 0.4)

Mean Value = 0.2

Table 7 Overall migration test results. 8.4.2 Food Regulatory Assessment The overall migration limit is 10 mg/dm2 contact surface or 60 mg/kg food stimulant. The analytical tolerance of the method used is 2 mg/dm2 for aqueous simulants and for ethanol. Based on the results the Fraunhofer Institute have found that investigated HDPE milk bottles are in compliance with the requirement of the overall migration for milk products as well as for aqueous and acidic types of food for long term storage conditions up to 20°C. 8.5 Determination of the Specific Migration of Irganox 1076 (Fraunhofer IVV) The Fraunhofer Institute for Process Engineering and Packaging had performed tests to determine the specific migration of Irganox 1076 from milk bottles manufactured using recycled HDPE. The full report is in Appendix E. The following section of this report gives the results obtained and provides food regulatory assessment. The following samples were supplied for analysis:

Sample 1: HDPE milk bottle, 4 pint, 30% recyclate, Batch A

Sample 2: HDPE milk bottle, 4 pint, 30% recyclate, Batch B

Sample 3: HDPE milk bottle, 4 pint, 100% virgin material (reference)

The testing method for migration of Irganox 1076 was European Standard 1186-3. The test uses 0.5dm2 of the sample immersed in 110ml 50% ethanol for 10 days at 20°C. Another 0.5dm2 of the sample was immersed in 110ml 3% acetic acid for 10 days at 20°C. Determination of Irganox 1076 was performed in 95% ethanolic migration solution. Irganox 1076 was quantified without further sample preparation using HPLC with UV-detection. In the 3% acetic acid migration solution Irganox 1076 was quantified after dilution with ethanol (0.5ml migration solution + 0.5ml ethanol). The calibration was carried out by external standards. Recovery experiments were performed by spiking the sample. 8.5.1 Results of Specific Migration of Irganox 1076 Irganox 1076 was not detected in the food simulants 95% ethanol and 3% acetic acid. The detection limit for Irganox 1076 in 3% acetic acid was 0.01mg/dm2 and 0.05mg/kg respectively. The detection limit in 50% ethanol was 0.02 mg/dm2 and 0.12 mg/kg, respectively. 8.5.2 Food Regulatory Assessment The specific migration limit for Irganox 1076 is 6mg/kg octadecyl 3-(3,5-di-tert-butyl-4-hydroxyphenyl)-propionate (Irganox 1076, CAS: 2082-79-3) according to the EU Plastics Directive 2002/72/EC las amended by Directive 2005/79/EC. Based on the specific migration tests, Fraunhofer Institute have found that the investigated HDPE milk bottle samples (30% recyclate Batch A, 30% recyclate Batch B and 100% virgin reference) comply with the specific migration limit of Irganox 1076 for milk products as well as for all aqueous and acidic types of food at long term storage conditions at up to 20°C.


8.6 Overall Migration from Milk Bottles (PIRA International Analysis) PIRA International were independently commissioned by Nampak to perform an overall migration test on HDPE bottles manufactured from 100% recycled HDPE (Batch A and B) as well as bottles manufactured using 30% recycled HDPE (Batch A and B). Overall migration was tested by filling, into 50%v/v ethanol; exposure conditions 10 days at 40ºC. After exposure to the simulant under conditions specified, test specimens were removed from contact; the aqueous extract was transferred to a weighed container and evaporated to dryness and constant weight. EN 1186 - 9 - single side contact by filling. 1) 100% recycled material - Batch A Bottles - Test conditions: 10 days at 40°C

Method EN 1186-9 Migration into (50% v/v ethanol) l Replicates mg/kg 1 4.0 2 4.0 3 4.5 Mean result 4.2 Limit 60.0

2) 100% recycled material - Batch B Bottles - Test conditions: 10 days at 40°C

Method EN 1186-9 Migration into (50% v/v ethanol) Replicates mg/kg 1 4.0 2 3.0 3 3.5 Mean result 3.5 Limit 60.0

3) 70% Virgin 30% Batch A recycled resin - Test conditions: 10 days at 40°C


4) 70% Virgin 30% Batch B recycled resin - Test conditions: 10 days at 40°C


The full PIRA report is presented in Appendix F.


8.7 Migration Studies on Recycled HDPE to be Used for Milk Packaging - PIRA The full PIRA report on migration studies from recycled HDPE for use in milk bottle packaging is given in Appendix 7. In summary, the objective of these experiments was to estimate migration of moderately volatile, unidentified substances found to be present in recycled HDPE pellets in a previous study (Report 06A11J0412) to enable a safety assessment to be made. Migration studies were performed on HDPE bottles made from recycled post consumer stock using the food stimulant 50% ethanol v/v in water. The test conditions applied were 10 days at 5°C, representing refrigerated storage at 5°C or below. Additional tests were also conducted using 50% ethanol and exposure conditions of 2 days at 20°C, followed by 5 days at 5°C to allow for a worst case situation where milk may be left out of the fridge at room temperature for a short time. In both cases virgin HDPE control bottles were tested alongside the recycled bottles for comparison. Currently, water is the designated food stimulant for milk, as given in Directive 85/572/EC. However, it is highly likely that 50% ethanol will replace water in the 4th amendment to Directive 2002/72/EC based on experimental findings that migration of substances into milk and other dairy products can be significantly higher than water. The test solutions were extracted with n-heptane and injected for analysis by GCFID. Internal standards were added to the 10 day at 5°C test solutions, prior to solvent extraction, at levels of 2.69 pg/dm2 and 1.62 pg/dm2 (16 ppb and 10 ppb at the EU conventional food packaging ratio of 6dm21kg). The 10 day at 5°C test solutions were also fortified with 0.54 pg/dm2 (3.2 ppb at the EU conventional food packaging ratio of 6dm2/kg). No peaks larger than the internal standards were seen in the recycled bottle extracts that were not also present in the control extracts in both sets of migration tests. The conclusion of these studies is that, although unidentified contaminants are present in the recycled HDPE, there is no detectable migration of individual components into 50% ethanol with a LOD equating to 10 ppb, or better. Considering only the 10 day at 5°C results it can also be judged that migration levels of specific substances into 50% ethanol are below 0.54 µm/dm2 (3.2 ppb at the EU conventional food packaging ratio of 6dm2/kg). This value is below the US FDA threshold of regulation of 0.5 ppb in the diet, after applying the FDA Consumption Factor of 0.13 for HDPE. Taking into account the headspace GC analysis performed by Fraunhofer Institute and the challenge testing, there is now substantial evidence that the use of this batch of recycled HDPE (WRAP A) for the packaging of milk is unlikely to endanger human health. 8.7.1 Conclusions The analytical work in this study provides experimental data showing that there is no detectable migration of substances into 50% ethanol from bottles made from recycled HDPE, in addition to substances that migrate from virgin HDPE. The LOD for the analytical work is judged to be 10 µg/kg (ppb) in solution based upon the responses of three different standards, corresponding to 3 µg/kg (ppb) at the conventional EU food packaging ratio of 6 dm2/kg. Taking into account the headspace GC analysis performed by Fraunhofer Institute and the challenge testing, there is substantial evidence that the use of this batch of recycled HDPE (WRAP A) for the packaging of milk is unlikely to endanger human health. 8.8 Recycled HDPE Decontamination Conclusions 8.8.1 Conclusions from Volatile Screening of HDPE Flake, Pellet and Milk Bottle The Erema decontamination process was found to have removed a wide number of compounds detected in both virgin resin and the HDPE flake. The analytical tests performed by Fraunhofer IVV found that flake samples showed several polyolefin oligomers as well as some post-consumer compounds. When the material input was largely milk bottles, the pellet had the lowest levels of residual of flavour and fragrance compounds (e.g. Material A). The inclusion of household cleaning bottles in the feedstock had resulted in detectable fragrance residues in the finished flake and pellet (Material B). The primary detectable fragrance compound was found to be limonene, however the level of limonene was significantly reduced once the flake had been super-cleaned and extruded by the Erema process. From all the samples tested there was only one sample of flake that showed other fragrance based compounds such as (alpha-pinene, camphene, eucalyptol and isobornylacetate), however further sub-sample tests did not determine these compounds. It can therefore be concluded that only some individual flakes contain these compounds. These findings clearly demonstrate how essential it is for the sorting process to eliminate household cleaning bottles/flakes.


However, it can be stated that the levels of these compounds are further significantly decreased by dilution with non-contaminated milk bottle rHDPE flakes down to very low ppm levels. The Erema super-clean decontamination step further decreases the concentration in the final product. The analytical test results clearly showed that in the corresponding super-clean pellet samples, the concentrations of these compounds were significantly reduced down to levels below the oligomer concentrations in virgin HDPE. The super-cleaning process resulted in recycled HDPE resin that has had a similar analytical fingerprint to the previous WRAP trial material. Analysis of volatile migration relevant compounds had also determined that the concentrations of the detected polyolefinic oligomer compounds in the 100% virgin HDPE reference sample were in fact slightly higher than in the 30% recyclate containing samples of both Material A and B. All bottle samples tested showed similar headspace fingerprints. Milk bottles containing 30% recyclate showed no significant difference when tested for contaminants and compared to 100% virgin HDPE reference bottles. In addition, the concentrations of the antioxidant polymer additives Irfagos 168 as well as Irganox 1076 were determined and were found to be in the same concentration range than the virgin milk bottle. 8.8.2 Overall Migration Conclusions Overall migration test were performed by the Fraunhofer IVV based on the European Standard Test Method – EN 1186-9. Current EU regulation for overall migration into milk products is based on using distilled water at 5°C. EC Directives 2002/72/EC and the UK Plastic Materials and Articles in Contact with Food (England) Regulations 2006 state that the limit for overall migration into milk is 10mg/dm2 contact surface or 60mg/kg of food stimulant for bottles. The Fraunhofer IVV Overall Migration Test Results found that:

30% rHDPE Batch A = 0.0mg/dm2 (3% Acetic Acid, 10 days at 20°C)

30% rHDPE Batch A = 0.0mg/dm2 (3% Acetic Acid, 10 days at 20°C)

30% rHDPE Batch B = 0.6mg/dm2 (3% Acetic Acid, 10 days at 20°C)

30% rHDPE Batch A = 0.0mg/dm2 (50% Ethanol, 10 days at 20°C)

30% rHDPE Batch B = 0.0mg/dm2 (50% Ethanol, 10 days at 20°C)

100% virgin HDPE (reference sample) = 0.0mg/dm2;(3% Acetic Acid, 10 days at 20°C)

0.2mg/dm2 (50% Ethanol, 10 days at 20°C)

These results clearly demonstrate that the overall migration is at extremely low levels even when more aggressive simulants such acetic acid and ethanol are used as opposed to distilled water 5°C. Overall migration test results on bottles containing 100% and 30% recycled HDPE from PIRA International Ltd found that:

100% rHDPE Batch A = 4.2mg/kg (50% Ethanol, 10 days at 40°C)

100% rHDPE Batch B = 3.5mg/kg (50% Ethanol, 10 days at 40°C)

30% rHDPE Batch A = 2.3mg/kg (50% Ethanol, 10 days at 40°C)

30% rHDPE Batch B = 1.2mg/kg (50% Ethanol, 10 days at 40°C)

Whilst there was no intention in this project to produce 100% recycled HDPE bottles for milk bottles, these results show that even when bottles containing 100% recycled HDPE resin are tested at much higher temperatures (e.g. 40°C), the overall migration levels are still extremely low and are significantly below the limit for overall migration into milk is 10mg/dm2 contact surface or 60mg/kg of food stimulant for bottles. The overall migration test results were independently performed by the Fraunhofer Institute and PIRA International. Both tests had independently found that the overall migration was significantly lower than the 60mg/kg limit set by the EU Plastics Directive 2002/72/EC. In conclusion it can be stated that the overall migration test results were found to be significantly lower than the overall migration limit of 10mg/dm2 contact surface or 60mg/kg food stimulant as set out in the EU Plastics Directive 2002/72/EC (lastly amended by Directive 2005/79/EC). The milk bottles containing 30% recycled HDPE resins have been found to be in compliance with the requirements of the overall migration for milk products as well as for all aqueous and acidic types of food for long term storage conditions up to 20°C.


8.8.3 Specific Migration Conclusions Specific migration tests were performed by Fraunhofer IVV based on European Standard Test Method EN 1186-3. This test results obtained clearly demonstrate that HDPE bottles with 30% recycled HDPE content fully comply with the specific migration limit of 6mg/kg of Irganox 1076 as set out in EC No. 2002/72/EC and amendments 2004/1/EC, 2004/19/EC, 2005/79/EC. The analytical tests have clearly shown that the detection for Irganox 1076 in 30% recycled HDPE bottles using 3% Acetic acid for 10 days at 20°C was 0.01mg/dm2 and 0.05mg/kg respectively and in 50% Ethanol for 10 days at 20°C was 0.02mg/dm2 and 0.12mg/kg respectively. This is significantly lower than the EU & UK limit of 6mg/kg. The investigated bottles therefore fully comply with EU Directives for specific migration and re suitable for milk products as well as for all the aqueous and acidic types of food at long term storage conditions at up to 20°C. 8.8.4 Decontamination of Recycled HDPE – Key Findings: Both, Fraunhofer IVV & PIRA overall & specific migration test results show that post-consumer compound migration from rHDPE is very low and complies with all of the current and likely future EU and UK regulations. As was described in previous sections, the tests performed by Fraunhofer IVV used more aggressive simulants, then is currently required. Acetic acid and ethanol are likely to be future regulations. PIRA tests on overall migration used even more aggressive conditions such as higher temperatures and even tested 100% recycled HDPE bottles even though these were never considered for use. However, the results clearly show that even under these conditions using 100% Material A and B, the overall migration was significantly lower than the EU legal requirements of 10mg/dm2 contact surface or 60mg/kg of food stimulant. A further significant development is that Fraunhofer IVV have lodged a submission for the HDPE recycling process and shortly expect to obtained a letter of non-objection from US FDA. This letter would then provide further validity for the use of recycled HDPE for milk bottles. It must also be stated that based on the results obtained from overall and specific migration tests, 30% recycled HDPE bottles produced in this project using the described cleaning and decontamination processes, the bottles satisfy Article 3 of EC Directive 1935/2004 which states that: 1. Materials and articles, including active and intelligent materials and articles, shall be manufactured in compliance with good manufacturing practice so that, under normal or foreseeable conditions of use, they do not transfer their constituents to food in quantities which could: (a) endanger human health; or (b) bring about an unacceptable change in the composition of the food; or (c) bring about a deterioration in the organoleptic characteristics thereof. 2. The labelling, advertising and presentation of a material or article shall not mislead the consumers.

All tests performed in this project clearly demonstrate that the recycled HDPE bottles fully satisfy all of the above described general requirements. This is also the conclusion of PIRA, Fraunhofer IVV and Keller and Heckmann who have all reviewed the relevant test results and have thus confirmed that the use of this batch of rHDPE resin is safe for use with milk bottle packaging. 9.0 Sensory and Bacteriological Test Results Milk filled bottles were sent for organoleptic testing to the Campden & Chorleywood Food Research Association (CCFRA), Consumer and Sensory Sciences Department, and an independent milk taint review was commissioned by Nampak Plastics with Reading Scientific Services Ltd.. The results obtained are discussed in this section of this report. 9.1 CCFRA Sensory Test Results The test by CCFRA panel of taste experts was used to detect any taste differences in milk packaged in bottles manufactured from 100% virgin HDPE (reference sample) and bottles containing recycled HDPE rein (Batch A & B). The panel were not aware of any specific differences in the milk and its packaging. The milk was tested according to the following criteria:


Appearance in Bottle – (Colour tinges; Cream colour; Brightness; Creamy/Thickness)

Odour in Bottle – (Milk/dairy; Sour; Off flavours; Sterilised/UHT)

Odour in Cup – (Milk/dairy; Sour; UHT)

Flavour – (Milk/dairy; Off flavours; Sweetness; Sour)

Aftertaste/Mouthfeel – (Mouthcoating; Milky/Dairy; Acidic; Astringent; Sour)

Nine samples of milk (3 x whole, 3 x semi-skimmed) were submitted to CCFRA for assessment by means of free description (TES-S-011). The objective of the evaluation was to describe the sensory characteristics of the samples at early and late stages of their shelf life against a control sample. This was with regards to any possible tainting from trial bottles, made with 30% PCR recycled HDPE; and to highlight any possible differences. 9.1.1 CCFRA Findings The summary of the Campden & Chorleywood Food research Association study found that there were no major differences in taste between the control sample and Batches A and B. The report states the following conclusions: “There were no major differences between the Control samples and batches A and B for either the Skimmed, Semi-Skimmed and Whole Milk for both assessments.” “Some off flavours were detected across all three milk types. These off flavours, however were also detected in the control samples. There were also several minor differences between the samples but these were not considered to be a concern based on your project objective.” “With regards to appearance there were no major differences detected by the panel during the assessment, however an observation was made with regard to a colour difference between bottles when bottles were placed side by side in the kitchen. It was noted that the control sample across all milk types was very slightly whiter/brighter in appearance.” 9.1.2 Conclusions The sensory test results from CCFRA clearly indicate that there are no major differences in milk taste from bottles containing 30%recycled HDPE and the virgin HDPE reference samples. This finding demonstrates that bottles manufactured with 30% recycled HDPE from Materials A and B are suitable for use as milk bottles as they don’t appear to cause any milk taint. Full results from the Campden & Chorleywood Food research Association study are presented in Appendix I. 9.2 Reading Scientific Services – Sensory Test Results This test was performed to determine whether any off notes could be detected in three samples of plastic bottles, a control and two test samples. The test was to also determine whether any taint was imparted to milk after storing for 72 hours in the same plastic bottles. A taint test was carried out on the plastic bottles and two triangle tests comparing each test sample to the control sample were carried out on the milk. The samples analysed were as follows:

HDPE Bottles Batch –A

HDPE Bottles Batch – B

HDPE Bottles C (Reference)

For the taint test on the plastic bottles, the plastic bottles were cut up into small pieces and a teaspoon of each was placed in a glass vial closed with a lid. Samples were left for two hours prior to evaluation, to enable the headspace to build up in the vial. For the triangle testing, semi skimmed milk was placed in the three types of plastic bottles and left for 72 hours at 5° C. 9.2.1 Sensory Evaluation Taint Test: Control and test samples of the plastic bottles were presented to a panel of ten assessors. Samples were coded with a three digit number and presented in a randomised order to panellists to avoid any bias due to carry over effect. Assessors were asked to smell each of the glass vials and if an off note could be detected, they were asked to rate the intensity of the off odour using a 5 point scale, whereby 0=None and 4=Very Strong. They were further asked to describe the nature of the off odour if any.


9.2.2 Sensory Evaluation Triangle Tests: Control and test samples were compared using the UKAS accredited triangle test procedure RSSL method TM22 based on BS ISO4120:2004. In each of the tests, each assessor received three coded samples, two of which were the same and the third different. Assessors were asked to select the odd sample and to describe the nature of the difference(s) perceived. Twenty-four assessors were used in each test. 9.2.3 Conclusions The results of the taint test on the plastic bottles indicated that very slight off notes were detected in all three samples. No significant differences were found between Batch A , Batch B or reference virgin HDPE bottles. The results of both triangle tests on milk indicated that none of the test samples would impart a flavour change to the milk. The results indicate that both Materials A and B are suitable for use as milk bottles. Full results from the Reading Scientific Services LTD are presented in Appendix G 9.3 Bacteriological Testing The bacteriological testing was performed by Eclipse Scientific Group. Milk filled bottles have been tested for the

following bacteria:

Bacillus cereus

Enterobacteriaceae

Listeria

Pseudomonas

Salmonella

Staphylococcus aureus

Aerobic Colony Count

Thermoduric

9.3.1 Conclusions: Early bacteriological data test results have been found to be satisfactory by Dairy Crest. The data is currently being analysed, however current indications are that all tests have shown no significant difference between bottles containing 30% recycled HDPE and the reference sample bottles. Dairy Crest have found that shelf life for the tested bottles was slightly shorter, however the shelf life results were consistent across all tested samples and it is therefore likely to be related to the initial storage of the samples. Raw test data results from Eclipse Scientific Group is very long and for this reason is not included in this report, however it will be made available upon request. 9.4 Dairy Crest - RHDPE Bottle Filling and Shelf Life Assessment Report 9.4.1 Aims: Post consumer waste polyethylene (milk) bottles, have been collected, flaked, washed and reprocessed. The reprocessed resin was added to virgin resin at a rate of 30% and manufactured into new milk polybottles. Filling trials were necessary to compare the mechanical strength, microbiological standard and sensory quality of these polybottles against polybottles manufactured from 100% virgin resin and filled with fresh pasteurised milk. 9.4.2 Scope: For the filling trials 4-pint milk polybottles were manufactured using 2 discrete batches of recycled resin. Batch A was used for the majority of the trials because although it had a slightly stronger colour there was no distinct odour to the bottles. Batch B had a distinct floral perfume (identified as limonene) so was included only for sensory analysis. The bottles were manufactured by Nampak Plastics in Newport Pagnell and supplied to Dairy Crest at Totnes. Control samples were taken from standard bottle stock. All the bottles were de-boxed by hand onto the de-bagging table and run through the complete filling system from the de-bagging table, through conveyoring, to bottle inverting, filling on a Stork filler and capping with an induction heat seal closure. The labeller was left running for control samples, but turned off for trial bottles, because the bottles had to be left unlabelled for the sensory analysis. Finally the bottles were hand packed into roll containers prior to sorting and boxing for transport to the testing laboratories.


9.4.3 Methodology: Microbiological assess was carried out by Eclipse Scientific in Shropshire using traditional plating methods. A Dairy Crest protocol for assessing new products, packaging and equipment was followed which includes Aerobic plate count (APC) at 30 oC, Bacillus cereus, Enterobacteriaceae, Listeria, Staphylococcus aureus, Pseudomonas, Salmonella and Thermodurics. Testing was carried out in duplicate for the controls and triplicate for the test bottles, on day of production plus 3, 5, 9, 11, 12, 13 and 14. The milk was stored at 8 oC for the duration of the testing. Sensory analysis was carried out by CCFRA in Chipping Campden to identify any odd or unusual flavour or taint characteristics in the milk. A panel of eight trained assessors were asked to independently describe the colour of the milk in the bottle, the odour of each sample as it was opened and when poured into a cup and then to assess the taste of the milk. These assessments were carried out on two occasions. The samples were presented to the assessors under random codes. The milk was stored at 8 oC for the duration. The filling trials were run over three days with a different grade of milk being sampled on each day. Day 1 was skimmed milk, day 2 was whole milk and day 3 was semi-skimmed milk. All samples were held in the dairy’s cold store until day 3 when they were boxed despatched to the testing laboratories by refrigerated courier. 9.4.4 Results To be regarded as acceptable microbiologically results must demonstrate product safety and show no variation between the control samples and test bottles. The clear results at the start of life demonstrate that there was no initial contamination of the product from the test bottles. As expected no pathogenic micro-organisms were detected in either the control samples or the trial bottles throughout life. The following graphs show the APC, Pseudomonas and thermoduric counts.


Whole Milk Shelf Life (Start)

1

10

100

1,000

10,000

100,000

1,000,000

10,000,000

100,000,000

1,000,000,000

9 11 12 13 14DOP

cfu/

ml

WMSC1&2 (APC 30C)

WMST1,2&3 (APC 30C)

WMSC1&2 (Pseudomonas)

WMST1,2&3 (Pseudomonas)

WMSC1&2 (Thermodurics)

WMST1,2&3 (Thermodurics)

Whole Milk Shelf Life (Middle)

1

10

100

1,000

10,000

100,000

1,000,000

10,000,000

100,000,000

1,000,000,000

9 11 12 13 14DOP

cfu/

ml

WMMC1&2 (APC 30C)

WMMT1,2&3 (APC 30C)

WMMC1&2 (Pseudomonas)

WMMT1,2&3 (Pseudomonas)

WMMC1&2 (Thermodurics)

WMMT1,2&3 (Thermodurics)

Whole Milk Shelf Life (End)

1

10

100

1,000

10,000

100,000

1,000,000

10,000,000

100,000,000

1,000,000,000

9 11 12 13 14

DOP

cfu/

ml

WMEC1&2 (APC 30C)

WMET1,2&3 (APC 30C)

WMEC1&2 (Pseudomonas)

WMET1,2&3 (Pseudomonas)

WMEC1&2 (Thermodurics)

WMET1,2&3 (Thermodurics)


Semi-Skimmed Milk Shelf Life (Start)

1

10

100

1,000

10,000

100,000

1,000,000

10,000,000

100,000,000

1,000,000,000

9 11 12 13 14DOP

cfu/

ml

SSSC1&2 (APC 30C)

SSST1,2&3 (APC 30C)

SSSC1&2 (Pseudomonas)

SSST1,2&3 (Pseudomonas)

SSSC1&2 (Thermodurics)

SSST1,2&3 (Thermodurics)

Semi-Skimmed Milk Shelf Life (Middle)

1

10

100

1,000

10,000

100,000

1,000,000

10,000,000

100,000,000

1,000,000,000

9 11 12 13 14DOP

cfu/

ml

SSMC1&2 (APC 30C)

SSMT1,2&3 (APC 30C)

SSMC1&2 (Pseudomonas)

SSMT1,2&3 (Pseudomonas)

SSMC1&2 (Thermodurics)

SSMT1,2&3 (Thermodurics)

Semi-Skimmed Milk Shelf Life (End)

1

10

100

1,000

10,000

100,000

1,000,000

10,000,000

100,000,000

1,000,000,000

9 11 12 13 14DOP

cfu/

ml

SSEC1&2 (APC 30C)

SSET1,2&3 (APC 30C)

SSEC1&2 (Pseudomonas)

SSET1,2&3 (Pseudomonas)

SSEC1&2 (Thermodurics)

SSET1,2&3 (Thermodurics)


Skimmed Milk Shelf Life (Start)

110

1001,000

10,000100,000

1,000,00010,000,000

100,000,0001,000,000,000

9 11 12 13 14

DOP

cfu/

ml

SMSC1&2 (APC 30C)

SMST1,2&3 (APC 30C)

SMSC1&2 (Pseudomonas)

SMST1,2&3 (Pseudomonas)

SMSC1&2 (Thermodurics)

SMST1,2&3 (Thermodurics)

Skimmed Milk Shelf Life (Middle)

110

1001,000

10,000100,000

1,000,00010,000,000

100,000,0001,000,000,000

9 11 12 13 14

DOP

cfu/

ml

SMMC1&2 (APC 30c)

SMMT1,2&3 (APC 30C)

SMMC1&2 (Pseudomonas)

SMMT1,2&3 (Pseudomonas)

SMMC1&2 (Thermodurics)

SMMT1,2&3 (Thermodurics)

Skimmed Milk Shelf Life (End)

1

10

100

1,000

10,000

100,000

1,000,000

10,000,000

100,000,000

1,000,000,000

9 11 12 13 14

DOP

cfu/

ml

SMEC1&2 (APC 30C)

SMET1,2&3 (APC 30C)

SMEC1&2 (Pseudomonas)

SMET1,2&3 (Pseudomonas)

SMEC1&2 (Thermodurics)

SMET1,2&3 (Thermodurics)

The bacteria commonly associated with pasteurised milk (APC, Thermoduric’s, and Pseudomonas), showed expected development through time regardless of bottle type. These are typical for fresh milk stored at 8 oC and do not show any significant differences between the control samples (standard stock polybottles) and the test bottles with 30% PCR. The testing was taken several days beyond normal shelf life in order to establish additional data that could be analysed to strengthen the comparison between the two types of packaging. Statistical analyses of the APC results of the two bottle types demonstrate an excellent correlation (R2 = 0.944, Mean Log difference 0.138).


Control vs Test bottle

y = 0.9034x + 0.5075R2 = 0.9442

0

1

2

3

4

5

6

7

8

9

0 1 2 3 4 5 6 7 8 9

Control (log cfu/g)

Test

bot

tle (l

og c

fu/g

)

Figure 47 Statistical Analysis showing correlation between the control and tests bottles (Source: Dairy Crest). To be regarded as acceptable organoleptically results must show no off flavours or taints and no extraneous odours or taints. The results from CCFRA are attached. Due to the sampling process taste panel assessments were carried out skimmed milk on days 6 and 8, on semi-skimmed on days 4 and 11 and on whole milk on days 5 and 12. 9.4.5 Summary From the microbiological data there is no indication that there is any detrimental effect on the quality of the milk from the use of PCR material. The attached results show that no pathogens or Enterobacteriaceae were found in any of the samples. Graphs show the APC, Pseudomonas and thermoduric counts. These are typical for fresh milk stored at 8 oC and do not show any significant differences between the control samples (standard stock polybottles) and the test bottles with 30% PCR. From the sensory testing there were no major differences between the Control samples and batches A and B. Some off flavours were detected across all three milk types and were also detected in the control samples. Visually, no major differences in appearance were detected by the panel during the assessment, however a slight colour difference could be seen when bottles were placed side by side in the kitchen. It was noted that the control sample across all milk types was very slightly white/brighter in appearance. 9.4.6 Conclusion The microbiological data does not indicate any deterioration in the quality of the milk attributable to the use of PCR material at 30% addition rate. The sensory panel testing also does not indicate any odd flavours / odours in the milk attributable to the use of PCR material. Batch B bottles had a distinct ‘floral’ odour identified as limonene, while this was not identified by the sensory panel it is recommended that this batch of material is not used for further trials without further decontamination.


The colour has been identified as coming from printing inks used on the milk labels (predominantly green from semi-skimmed milk). Further work to amend the flake washing chemistry and with label manufacturers to develop water removable labels that will not leach ink is planned. All analysis work to date confirm that this material meets all current and pending legislation on food contact. A large-scale consumer trial is planned for November 2006. From this trial all consumer complaints will be closely monitored to ensure there are no perceptible differences between milk polybottles manufactured from 100% virgin polymer and those manufactured with 30% PCR added to virgin polymer. 10.0 Legal Assessment of the EU Food Contact Status for Recycled HDPE

Milk Bottles 10.1 Keller and Heckmann Assessment In order to obtain independent legal assessment of the safety of the rHDPE material for food contact applications within the EU and based on current EU regulations Nextek Ltd engaged pre-eminent food contact legal experts Keller & Heckmann to review all test data and provide an independent opinion of the safety of this material for an initial production of 180,000 HDPE milk bottles for marketing and commercial purposes. Keller and Heckmann were informed that the milk bottles are composed of a ratio of 30% recycled resin to 70% virgin HDPE resin. Keller and Heckmann were therefore instructed to focus on the safety of the 30% recycled resin as the virgin resin HDPE grades all currently comply with the EU Plastics Directive (2002/72/EC) and the Framework Regulation (Regulation 1935/2004). In summary, Keller and Heckmann’s conclusion was “based on the information you have provided, namely, considering the data on the recycled post-consumer stock, the recycling process employed, testing data generated by PIRA International and the Fraunhofer Institute, and the implementation of good manufacturing practices, we have no hesitation concluding that the recycled HDPE milk bottles fully comply with the EU Plastics Directive and the general safety requirement under Article 3 of the Framework Regulation and, thus, can be placed and sold in the UK market”. The full Keller and Heckmann food safety opinion report is provided in Appendix 8. The details underlying the above conclusion are discussed more fully in the following sections. This involves an overview on how recycled food-contact materials are presently regulated in the EU. 10.2 EU Food Contact Status of Recycled Plastic Materials 10.2.1 EU Harmonization The EU is currently in the process of harmonizing Member State legislation governing food contact materials. Toward this end, the EU is adopting a series of directives and regulations, which are designed to progressively replace national laws existing in the individual Member States. Products that are subject to EU directives must comply with the applicable Community provisions, while products that are not yet the subject of EU directives must comply with the national legislation in place in the individual Member States of interest, subject to the principle of mutual recognition. The principle of mutual recognition allows for the legal importation and sale in one Member State of products that are legally marketed in another Member State even if the products do not comply with the specific regulatory requirements of the country of import. As interpreted by the European Court of Justice, this means that Member States should allow products that are eligible for mutual recognition to freely circulate within their territory unless they are able to demonstrate, following an appropriate authorization procedure, that this product presents a danger to public health. Presently, there are no directives in the EU that explicitly regulate recycled materials that are intended for use in contact with food. Thus, the same provisions that apply to virgin food contact articles apply equally to articles with recycled content. In this regard, recycled materials must comply with the Framework Regulation (Regulation 1935/2004), which is applicable to all food-contact materials. This Regulation requires that food-contact materials must be manufactured in accordance with good manufacturing practice and not transfer their constituents to food in quantities that could endanger health or bring about an unacceptable change in the composition, taste, or odor to food. Furthermore, recycled materials made entirely of plastic, also must comply with the provisions of the Plastics Directive (Directive 2002/72/EC). The Plastics Directive provides an exhaustive "positive list" of monomers and other starting materials that may be used in the production of food-contact plastics, as well as an incomplete" list of additives that may be used in the production of plastics. Accordingly, monomers used in recycled plastic materials must be listed on the Plastics


Directive, and any additives employed must be identified on the additives list or have a suitable status under the national laws in the Member States of interest. Although there is no Community legislation at this stage with respect to recycled plastics in contact with food, please note that the European Commission is working on a draft Directive that will regulate the use of recycled plastics in contact with food. It is our understanding that the Directive may be adopted in 2007. 10.2.2 Suitable Purity of Recycled Plastics The European Commission has sponsored a study on the criteria necessary to ensure that recycled plastics are suitable for use in contact with food. The study was conducted by the Agro-Industrial Research (AIR) Programme and coordinated by Dr. Lawrence Castle of the United Kingdom's Ministry of Agriculture, Fisheries, and Food (MAFF). The study was accepted by the Commission in January of 1998 (it is commonly referred to as the "AIR Study"). The recommendations that stem from the AIR Study follow the same basic principles set forth in the U.S. Food and Drug Administration's (FDA) Points to Consider for the Use of Recycled Plastics in Food Packaging: Chemistry Considerations (May, 1992). The recommendations concern the nature of the feedstock that is appropriate for recycling into food-contact articles and the use of surrogate testing to demonstrate that the specific recycling process of interest will produce a polymer that is suitably pure for its intended use. With regard to the use of surrogate testing, the view of many regulators in the Community is that this testing is not necessary or appropriate in cases involving chemical recycling, and that companies should ensure the suitability of their chemical recycling process based on an evaluation and determination of what testing is appropriate considering the nature of the particular process involved. We recognize, however, that the recycling process you have described, and will be implemented for HDPE milk bottles, does not constitute "chemical recycling" (tertiary recycling), but rather "physical reprocessing" (secondary recycling). 10.2.3 Regulation of Recycled Materials in the EU Member States In addition to reviewing the requirements of the Framework Regulation and Plastics Directive that are applicable to all materials used in contact with food, one also must review the laws and administrative practices in place in the EU Member States. These laws and practices specify the national requirements that are applicable to demonstrate compliance of recycled materials with the EU requirements, and, principally, the general safety requirements of the EU Framework Regulation. We focus here primarily on the regulatory situation in the U K, as this is where we understand the recycled HDPE milk bottles will be sold. Our research indicates that at least three, and as many as five, of the EU Member States require the filing of an application or petition requesting approval of a recycling process before it may be used to produce food-contact articles. The Member States that require pre-market approval are Austria, Italy, and Spain. (In addition, while not a member of the EU, Norway also requires that recycling processes be approved on a case-by-case basis.) Belgium and France may require an application to be filed for chemical recycling processes with the competent authorities, but this has not been confirmed. The UK has duly implemented the provisions of the EU Plastics Directive. With regard to the Framework Regulation, since this Regulation is directly applicable in the EU Member States, there is no need to transpose its provisions into the UK legal order. We have confirmed with the UK authorities that there is no provision in the UK legislation on food-contact materials that specifically addresses the use of recycled plastics; thus, recycled plastics may be used in food-contact applications in the UK without pre-market authorization, provided the recycled material complies with the general safety standards set forth in the EU Framework Regulation. The responsibility for ensuring that these materials meet this requirement is on the companies manufacturing or using the recycled plastics. Typically, companies will certify that their recycling process is suitable by demonstrating compliance with the AIR study recommendations. Indeed, the regulatory authority in the UK, MAFF, does not typically confirm such suitability even when requested to do so by companies as a voluntary measure. 10.2.4 Establishing a Suitable Regulatory Status of Nextek’s Post-Consumer Recycled HDPE

Milk Bottles The analysis below, concludes, that given the description of recycling procedures, the source of the recyclate material, and the various analytical data provided, that the recycled HDPE milk bottles, given the current regulatory scheme in the EU, fully comply with the EU Plastics Directive (2002/72/EC) and the Framework Regulation (Regulation 1935/2004). The considered recycled HDPE materials (pellets) have been produced during a large scale HDPE recycling trial (Project Code: MDP006) conducted in the UK during the summer of 2006.


The investigated recycling process consists of the following key steps:

Separation of the post-consumer HDPE milk bottles;

Grinding and hot-washing of the bottles;

Removal of labels;

Colour sorting of the ground flake;

Deep-cleaning of the washed flakes and regranulation to pellets

The recycled post-consumer stock for the considered recycled HDPE pellets was primarily sourced from HDPE milk bottles. The material was manually pre-sorted, with a specification of less than 5% coloured HDPE content. The main conclusions, based on the data generated d d g this trial, are as follows:

The sorting and processing of the flakes into decontaminated pellets was realized with the input material

to the extruded material being greater than 99.4% clear HDPE.

The decontamination process removed a wide number of compounds detected in both virgin resin and in

the HDPE flakes.

Analytical tests of flake samples showed several polyolefin oligomers. In the corresponding pellets

samples, the concentration of these compounds were significantly reduced down to levels below the

oligomers concentration in the virgin HDPE.

Overall migration test results from recycled HDPE milk bottles, performed independently by the

Fraunhofer Institute and PIRA Intemational, were found to be significantly lower than the overall

migration limit of 10 mg/dm2 contact surface or 60 mg/kg food simulant as set out in the EU Plastics

Directive 2002/72/EC (lastly amended by Directive 2005/79/EC). The milk bottles containing 30%

recycled HDPE resins were found to be in compliance with the requirements of the overall migration for

milk products, as well as for all aqueous and acidic types of food for long-term storage conditions up to

20°C.

The investigated HDPE bottles with 30% recycled HDPE content comply with the specific migration limit

of 6 mg/kg of Irganox I076 for milk products, as well as for all the aqueous and acidic types of food at

long-term storage conditions at up to 20°C.

In addition to the above mentioned data, PIRA Intemational has estimated migration of moderately volatile, unidentified substances found to be present in recycled HDPE pellets. These unidentified substances were detected by extraction of the HDPE pellets with severe solvents. By assuming 100% transfer to food, it was calculated that one of the largest components seen was at a level that equated to 50 ppb in food. Therefore it was required to establish if these components actually migrate into food to determine the safety of the recycled material. For this purpose, migration testing was performed by PIRA International on HDPE bottles made from recycled post-consumer stock using the food simulant 50% ethanol v/v in water. The test conditions applied were 10 days at S°C, representing refrigerated storage at S°C or below. Additional tests were also conducted using 50% ethanol and exposure conditions of 2 days at 20°C, followed by 5 days at 5OC to allow for a worst case situation where milk may be left out of the refrigerator at room temperature for a short period of time. In both cases, virgin HDPE control bottles were tested alongside the recycled bottles for comparison. The analytical work in the PIRA study provides experimental data showing that there is no detectable migration of additional substances into 50% ethanol from bottles made from 100% recycled HDPE, when compared to substances that migrate from virgin HDPE. The limit of detection (LOD) for the analytical work was judged by PIRA to be 10 µg/kg, or 10 ppb, in solution based upon the responses of three different standards, corresponding to 3 µg/kg, or 3 ppb, at the conventional EU food packaging ratio of 6 dm2/kg. As discussed above, although the EU does not have specific regulations in place for recycled materials used in food-contact applications, other than the fact that the material must comply with the Framework Regulation, and the monomers and additives used in the underlying resin must comply with the Plastics Directive, the current understanding of how the EU intends to regulate recycled materials used in food-contact applications in the future is that the requirements may be very similar to the U.S. Food and Drug Administrator's FDA Threshold


of Regulation approach, i.e., compounds present in the recycled material should be present in the diet at levels no greater than 0.5 ppb. (See, Guidance for Industry: Use of Recycled Plastics in Food Packaging: Chemistry Considerations, August 2006). Based on the migration testing performed by PIRA, K&H concluded that the potential dietary exposure to any compounds that may migrate from the recycled HDPE milk bottles will be below 0.5 ppb. It is important to reiterate that, based on the testing generated by PIRA, it was determined that there are no additional compounds migrating from the recycled HDPE milk bottles as compared to virgin HDPE. One quantitative way to calculate that dietary exposure will be below 0.5 ppb is by utilizing FDA's consumption factor (CF) of 0.13 for HDPE. This is, indeed, a very conservative CF to employ here as 0.13 represents the percent of an individual's daily diet, albeit in the United States, that packages food in all types of HDPE packaging. This is, of course, a gross exaggeration here, as Nextek's application is limited to HDPE milk bottles and for a very limited quantity of production. Applying the 0.13 CF to the LOD of 3 ppb, one can conclude that the dietary exposure would be 0.13 x 3 ppb, or 0.39 ppb. However, for the above reasons, the actual dietary exposure would be expected to be far less." Furthermore, the PIRA testing was performed on 100% recycled material; since Nextek's HDPE recycled milk bottles will only have a 30% recycled content, we can consider the results obtained by PIRA to exaggerate migration when compared to the commercial application. Thus, another reason to conclude that the expected dietary exposure under actual commercial conditions will be well below the 0.5 ppb dietary threshold discussed above. K&H concluded that the PIRA testing, in addition to the analytical work performed by the Fraunhofer Institute on both volatile and non volatile compounds (Fraunhofer Project No PN4436106 reported above), demonstrate that the recycled post-consumer stock used to blow HDPE milk bottles, at a ration of 30% recycled resin to 70% virgin material, is safe and suitable for marketing under the intended conditions of use. 10.2.5 Summary of the Food Safety Assessment In summary, based on the above, K&H state that “we have no hesitation in concluding that the 30% recycled post-consumer resin, sourced from HDPE milk bottles, may be used as intended in the manufacture of some 180,000 HDPE milk bottles to be sold in the UK, and that such use can be said to comply fully with the framework Regulation 1935/2004 and the Plastics Directive 2002/72/EC, provided that the recycling process described above is implemented, and provided good manufacturing practices are followed throughout the recycling process and subsequent manufacture of the recycled HDPE milk bottles”. 11.0 Fraunhofer Institute IVV – Expert Opinion on rHDPE Milk Bottles Food

Contact Safety The original full version opinion is presented in Appendix 9. The following section summarises the key opinions and conclusions determined by the Fraunhofer Institute. 11.1 Introduction Within a publicly financed project, a super clean recycling process for the closed loop recycling of post-consumer HDPE milk bottles has been developed. The project included the determination of typical contamination levels in recollected milk bottles, a challenge test according to the principles recommended by FDA and European Guidelines in order to investigate whether the output material is suitable for re-use in packaging materials with direct food contact as well as a quality assurance concept. 11.2 Technical Aspects The investigated recycling process consists of the following key steps:

Separation of the post-consumer natural HDPE milk bottles;

Grinding and hot-washing of the bottles, removal of labels

Colour sorting of the ground flakes

Deep-cleaning of the washed flakes and regranulation to pellets

The envisaged recycling concept for the post-consumer milk bottles involves the following state-of-the-art

technologies:

Sorting of the milk bottles with RTT technology (or similar)

Washing of the ground flakes with the SOREMA technology (or similar)

Colour sorting with the Morgensen technology (or similar)


Super-cleaning on the basis of flakes using Erema technology (or similar)

The results of the aforementioned project were as follows:

The washed and ground flakes made from post-consumer HDPE milk bottles had a good homogeneity. In total, samples from approx 24,000 to 30,000 individual “post-consumer” HDPE milk bottles were examined. Hints for misuse for storage of household chemicals were not found. The probability of a milk bottle contaminated with a substance foreign to HPDE or beverages could end up in the flow of recycled material is hence below or far below of 0.003%

Predominant compounds in conventionally recycled (not-super recycled) hot washed flake samples are unsaturated oligomers, which can be also be determined in virgin HDPE pellet samples used for milk bottle production. In addition, the flavour compound limonene, the degradation product of antioxidant additives di-tert-butylphenol as well as low amounts of saturated oligomers were determined in higher concentrations in the post-consumer samples in comparison to virgin HDPE. However, the overall concentrations in conventionally recycled samples were of similar or lower concentration ranges in comparison to virgin HDPE.

The contamination with other HDPE untypical compounds were rare and are in most cases related to non-milk bottles, which made up <2.1% of the input material of the recycling process in the aforementioned study. Due to the dilution of non-milk bottles with excess of (non-contaminated) milk bottles during washing, the maximum concentration of HDPE untypical compounds in the recycling feed-stream can be estimated to about 100ppm to 150ppm. Increasing the sorting efficiency will decrease maximum concentrations significantly.

The “super-clean” recycling process brought all detectable substances down to concentration levels that are lower or equivalent to that of virgin HDPE. In particular, small molecules, which have a higher migration potential due to their high rate of diffusion, were removed from the polymer most effectively. For that reason, general potential migration from recyclate containing milk bottles is not greater than from milk bottles made exclusively of virgin HDPE. However, limonene, the flavouring compound, was detected even after the “super-clean” recycling process. The concentration of limonene was in the range of that of typical HDPE oligomers.

Compared to virgin HDPE, the results for the overall migration from the recyclate containing milk bottles (recyclate amount 100%, 50%, 30%) showed no cause for concern, even under worst-case conditions (e.g. 1dm2 contact area with 100ml 95% ethanol (total immersion) for 10 days at 20°C). The specific migration of selected reference components was below the analytical detection limit of 10µg dm-2.

In the organoleptic tests, test bottles with recyclate amounts of 100%, 50% and 30% show no significant off-odour or off-taste in comparison to the reference bottles manufactured form 100% virgin HDPE. The test conditions of the organoleptic tests (bottles filled with tap water, stored for 10 days at 8°C) can be considered as worst case for fresh milk.

Filling trials under real filling conditions conducted under the responsibility of Dairy Crest show no significant differences between virgin milk bottles and recyclate containing bottles up to a recyclate containing content of 100%.

11.3 Compliance with Food Legislation Current food legislation in Europe does not include or prohibit the use of recyclates in materials for food contact applications. As, however there are still no relevant Europe wide regulations, national guidelines remain in legal force. However the requirements of Article 3 of the European Regulation 1935/2004 must be met. Accordingly, materials and products must be manufactured in such a way that under their intended or foreseeable application conditions no components are released into foods in quantities which: “endanger human health or bring about an unacceptable change in the composition of the food, or bring about a deterioration in the organoleptic characteristics thereof”. Analogous to packaging made exclusively from virgin material, the company that introduces the packaging into the marketplace is responsible for ensuring compliance with food legislation. In the USA, the Food and Drug Administration (FDA), working in collaboration with industry, has published recommendations on the use of recyclates in direct with foods. There, the specific evaluation criterion used is the so-called “threshold-of-regulation” concept which is based on comprehensive assessment of toxicological data. According to this concept, the migration of substances – even potentially unknown substances – from the packaging material into food is negligible small provided a limit value of 0.5ppb for each individual substance in the daily diet is not exceeded. Using so-called “consumption factors” (CF), the maximum migration which


corresponds to 0.5ppb in the daily diet, is calculated depending on the particular polymer by the respective fraction of the polymer in the total food packaging material. The CF for HDPE is 0.13. In accordance with this concept, this means that the maximum tolerable migration is 3.8ppb. The introduction of a similar concept in Europe is still being discussed in the European Commission. In addition, an expert committee of the “International Life Science Institute” (ILSI) has dealt with the subject of recyclate use and has published recommendations. 11.4 Evaluation The quality assurance of “post-consumer” polymers for food contact applications is carried out in accordance with the recommendations mentioned in section 3 and considers the following aspects:

Monitoring of the starting materials and recycling logistics (feedstock control)

Monitoring the cleaning efficiency of the “super-clean” recycling process

Analytical quality control of the starting material for the “super-clean” recycling process and also the

recyclate.

The starting material for the recycling process is post-consumer milk bottles from curbside collections. The bottles were separated from non-milk HDPE bottles by an efficient sorting technology. The sorting efficiency was tested to be >97.9% using only the sorting technology and >99% with additional hand picking. In addition it is expected that the sorting efficiency will increase with further development of the separation technology as well as with further training of the software in the industrial scale plant. Therefore foreign polymers from non-food applications can virtually wholly be excluded from entering the recycling chain. As a result, effective feedstock control was carried out. The cleaning efficiency of the recycling process was generally verified by carrying out a so-called “challenge test”. The cleaning efficiency of the recycling technology used for the feasibility study was determined as part of a publicly funded project. The “challenge test” was carried out in accordance with the guidelines of the ILSI, BfR and EU. The cleaning efficiencies for different contaminants are hence known. In our opinion these values should be satisfactory for the decontamination of “post-consumer” HDPE milk bottle flakes, when taking the maximum initial contamination levels into account. Part of the aforementioned study was also the development of a quality assurance method for monitoring migratable substances. Provided that Nextek will implement such a quality assurance method (or a similar method) into the recycling process, the routine quality control of the output material of the recycling process the routine quality control of the output material of the recycling process is established. Finally, taking the above conclusions considerations on HDPE recycling into account, then we come to the conclusion that the analytical results demonstrate that the super-clean recycling process, when including sorting, washing and deep cleaning with vacuum and high temperature as performed in the aforementioned project, is suitable for the recycling of post-consumer HDPE bottles for direct food contact applications where the food contact applications where the food contact application is fresh milk bottling and where consequently only relative short contact times at relative low temperatures (storage in refrigerator) would reduce migration rates compared to normal room temperature applications. Further on, for technical reasons, the output material from the super-clean recycling process will be reused for direct food contact applications for HDPE milk bottles only up to 50% recyclate content, which again implicates a safety factor in relation to the migration potential. As a consequence of all considerations and results, the Fraunhofer IVV had requested on behalf of Nextek Ltd an opinion letter from the American Food and Drug Administration (FDA) for the application of fresh milk bottling up to a recyclate content in the HDPE container of 50%. At the time of writing the evaluation of this petition is still in progress at the FDA 12.0 Project Conclusions FEEDSTOCK SUPPLY, WASHING, SORTING:

The quality of the final resin product is significantly influenced by the composition of the feedstock, the type of labels and method of printing and the washing chemistry used.

The quality of the final resin product is significantly influenced by the composition of the feedstock, the type of labels and method of printing and the washing chemistry used.


The variation in the feedstock has meant that non-milk bottles were included in the wash trials, which resulted in two types of flake and pellet quality.

The sorting and processing of the flake into decontaminated pellet progressed efficiently with the input material to the extruder being >99.4% clear HDPE for all of the input material.

PROCESS MASS BALANCE:

Preliminary data currently shows that material losses overall were 44%. However 23% of the 44% loss was related due to the high levels of coloured HDPE within the bales. The loss would be expected to be approximately 5% if the colour levels were similar to the previous WRAP trials.

The overall process efficiency for the material was 66%.

DECONTAMINATION OF RECYCLED HDPE:

The decontamination process removed a wide number of compounds detected in both virgin resin and the HDPE flake.

The super-cleaning process resulted in a resin that has had a similar analytical fingerprint to the previous WRAP trial material.

Analysis of volatile migration relevant compounds had determined that the concentrations of the detected compounds in the 100% virgin HDPE reference sample were slightly higher than in the recyclate containing samples (30% Material A / B).

When the material input was largely milk bottles, the pellet had the lowest levels of residual of flavour and fragrance compounds (Material A).

The inclusion of household cleaning bottles resulted in detectable fragrance residues in the finished flake and pellet (Material B).

Analytical tests of flake samples showed several polyolefin oligomers as well as some post-consumer compounds. In the corresponding super-clean pellet samples, the concentrations of these compounds were significantly reduced down to levels below the oligomer concentrations in virgin HDPE.

One sample of flake (5a) showed compounds such as (alpha-pinene, camphene, eucalyptol and isobornylacetate), however a second sub-sample test did not determine these compounds. This indicates that only some individual flakes contain these compounds but this level is decreased by dilution with non-contaminated rHDPE flakes down to very low ppm levels. The super-clean decontamination step further decreases the concentration in the final product.

The primary detectable fragrance compound was found to be limonene, however the level of limonene was significantly reduced once the flake had been super-cleaned and extruded by the Erema process.

Overall migration test results were independently performed by the Fraunhofer Institute and PIRA International. Both tests had independently found that the overall migration was significantly lower than the 60mg/kg limit set by the EU Plastics Directive 2002/72/EC.

Overall migration test results were found to be significantly lower than the overall migration limit of 10mg/dm2 contact surface or 60mg/kg food stimulant as set out in the EU Plastics Directive 2002/72/EC (lastly amended by Directive 2005/79/EC). The milk bottles containing 30% recycled HDPE resins have been found to be in compliance with the requirements of the overall migration for milk products as well as for all aqueous and acidic types of food for long term storage conditions up to 20°C.

The investigated bottles HDPE bottles with 30% recycled HDPE content comply with the specific migration limit of 6mg/kg of Irganox 1076 for milk products as well as for all the aqueous and acidic types of food at long term storage conditions at up to 20°C.

BLOW MOULDING TRIALS:

Bottles were successfully moulded from a 70:30 blend of virgin HDPE to recycled HDPE (Material A and B). The material blend had rheologically behaved in a similar manner to 100% virgin HDPE and the machine set-up did not need to be changed.

It was discovered that a number of bottles manufactured from the Virgin HDPE / Material A showed visual defects such as streaking due to solid particles and in a few bottles this had resulted in bottles with holes or bottle blow-outs.

Nampak Plastics have evaluated the material through extensive blow moulding trials and have signed off on the suitability of this resin for blow moulding of milk bottles.

MILK FILLING TRIALS:

The milk bottle filling trials clearly demonstrated that there was no visual colour variation between bottles containing 30% recycled HDPE (Batch A & B) when compared to filled 100% virgin HDPE milk bottles.


Filling bottles containing 30% recycled HDPE with different types of milk such as skim; semi-skim and full-cream milk did not result in colour variation when compared to 100% virgin HDPE milk bottles.

SENSORY TEST RESULTS:

CCFRA found that there were no major differences between the control samples and milk bottles containing batches A and B of recyclate for either the Skimmed, Semi-Skimmed and Whole Milk for both assessments.

CCFRA noted that some off flavours were detected across all three milk types. These off flavours, however were also detected in the control samples. There were also several minor differences between the samples but these were not considered to be a concern based on the project objective.

CCFRA also found that there were no major differences detected by the panel during the assessment in regards to the appearance, however, an observation was made that the control sample across all milk types were very slightly whiter/brighter in appearance.

A further independent report on ‘plastic bottles and triangle test on milk stored in plastic bottles’ by Reading Scientific Services Ltd found that the results of the taint test on the plastic bottles indicated that very slight off notes were detected in all three samples. The results of both triangle tests on milk indicated that none of the test samples would impart a flavour change to the milk.

EU and UK FOOD CONTACT SAFETY TECHNICAL & LEGAL ASSESSMENT: Fraunhofer Institute have tested the rHDPE and assessed it against all EU and UK regulations and have

found it to fully comply with all regulations and therefore safe for use in milk bottles. PIRA International have further tested the material and analysed any potential for migration into food or

milk and have concluded that this batch of material is safe to use PIRA found that there is no detectable migration of substances into 50% ethanol from bottles made from recycled HDPE, in addition to substances that migrate from virgin HDPE. The LOD for the analytical work is judged to be 10 µg/kg (ppb) in solution based upon the responses of three different standards, corresponding to 3 µg/kg (ppb) at the conventional EU food packaging ratio of 6 dm2/kg. Taking into account the headspace GC analysis performed by Fraunhofer Institute and the challenge testing, there is substantial evidence that the use of this batch of recycled HDPE (WRAP A) for the packaging of milk is unlikely to endanger human health.

A fully comprehensive legal assessment of the recycling process and the current batch of rHDPE resin was undertaken by Keller & Heckmann.

In summary, K&H state that “we have no hesitation in concluding that the 30% recycled post-consumer resin, sourced from HDPE milk bottles, may be used as intended in the manufacture of some 180,000 HDPE milk bottles to be sold in the UK, and that such use can be said to comply fully with the framework Regulation 1935/2004 and the Plastics Directive 2002/72/EC, provided that the recycling process described above is implemented, and provided good manufacturing practices are followed throughout the recycling process and subsequent manufacture of the recycled HDPE milk bottles”.

A submission to obtain a letter of non-objection for the safety of this process and material has also been made to the US FDA. The submission is currently under review.


Appendix 1 Participant Details NEXTEK Limited 221 Westbourne Park Rd, London, W11 1EA, UK www.nextek.org Prof Edward Kosior, Managing Director Mob: +44 (0)7981 277 561 Email: [email protected] Robert Dvorak, Project Manager Email: [email protected]

WRAP The Old Academy 21 Horse Fair, Banbury, Oxon OX16 0AH, UK www.wrap.org.uk Dr. Paul Davidson, Plastics Technology Manager Tel: +44 (0) 1295 819913,[email protected] Olwen Cox, Materials Project Officer Tel: +44 (0) 1295 819900, [email protected]

Dairy Crest Limited Technical Development Centre Crudgington, Telford, Shropshire TF6 6HY, UK www.dairycrest.co.uk Ms Lesley Moody Senior Development Technologist – Packaging Tel: +44 (0) 1952 653150 email: [email protected]

NAMPAK Plastic Europe Limited Jenna Way, Interchange Park, Newport Pagnell, Bucks, MK16 9QJ, UK www.eu.nampak.com Graham Hadfield Technical Manager Tel: +44 (0)1908 611554 email:[email protected]

Fraunhofer Institute for Process Engineering and Packaging (IVV) Giggenhauser Str 35 85354 Freising, Germany Dr. Frank Welle, Product Safety Manager Tel: +49 (0)8161 491 724 email: [email protected]

Food Standards Agency Aviation House 125 Kingsway, London WC2B 6NH Mr. Richard Sinclair Tel: +44 (0)2072 768 514 email: [email protected]

EREMA Engineering Recycling Maschinen und Anlagen Freindorf-Unterfeldstr.3, P.O.B 38 A-4052 Ansfelden/Linz, AUSTRIA Tel.: +43 732 3190 - 144 Fax: +43 732 3190 – 6344 www.erema.at Mr. Manfred Hackl, CEO, [email protected] Mr. Georg Weigerstorfer, Manager Process Engineering [email protected] Mr. Gilbert Netter, Manager Project Department, [email protected]

S+S Separation and Sorting Technology GmbH Regener Strasse 130 D-94513 Schoenberg / Germany Web: www.se-so-tec.com Mr. Peter Mayer (Sales Manager Recycling Technology) Phone +49 (0)8554 308-121 Fax +49 (0)8554 308-22325 email: [email protected]

RECOUP Services Ltd 1 Metro Centre Welbeck Way Woodston Peterborough PE2 7UH www.recoup.org John Simmons, (Director) Tel: +44 (0)1733 390021 email: [email protected]

SOREMA / PREVIERO Via dei Platani 11 22040 Alzate Brianza, Como, Italy Mr. Dario Previero General Manager Tel: + 39 (0) 31 619 224 email: [email protected]


Appendix 2 Screening of HDPE Recyclates for Migration Relevant Compounds The screening for migration relevant compounds in the post-consumer HDPE material was carried out using headspace gas chromatography by the Fraunhofer Institute for process Engineering and Packaging. The following data provides results obtained from screening tests for migration relevant compounds in the post-consumer recycled HDPE pellets.


















Appendix 3 Screening of HDPE Milk Bottles for Migration Relevant Compounds








Appendix 4 Determination of the Overall Migration from HDPE Milk Bottles




Appendix 5 Determination of the Specific Migration of Irganox 1076




Appendix 6 PIRA Migration Study The following report presents migration study results on bottles containing 30% recycled HDPE (Batch A & Batch B). The report was independently commissioned by Nampak Plastics and the testing was performed by PIRA International.






Appendix 7 Migration Studies on Recycled HDPE for Milk Packaging (PIRA)



















Appendix 8 Legal Assessment of rHDPE Food Safety in the EU and UK (Keller & Heckmann LLP)








Appendix 9 Fraunhofer IVV Expert Opinion






Appendix 9 Milk Taint Test Data The following report represents results obtained from a milk taint study commissioned by Nampak Plastics. The study was performed by Reading Scientific Services and its objective was to determine whether any off notes could be detected in the bottles containing recycled HDPE (Batch A & B) and virgin HDPE reference sample bottle










Appendix 10 Sensory Test Results The following tables provide results obtained from day 12 sensory tests.

















Appendix 11 Milk Filling Trial Protocol The following data shows the milk filling trial testing details. The tests were performed on a total of 315 bottles.







Appendix 12 Dairy Crest Comparison of Virgin and Recycled Bottles APC Results

Control Test bottle

Sample CFU/ml CFU/ml 0 0 0 0 25,500 32,167 3,375,000 1,581,667 15,650,000 17,450,000 36,750,000 60,000,000

Whole Milk Start

18,750,000 35,833,333

0 0 0 0 31,500 36,000 1,617,500 3,806,667 17,575,000 13,816,667 19,500,000 42,000,000

Whole Milk Middle

24,750,000 77,333,333

0 0 0 0 30,500 29,500 3,420,000 1,566,667 15,800,000 16,750,000

18,500,000 48,500,000

Whole Milk End

29,250,000 57,166,667

0 0 0 0 382,500 421,667 10,150,000 8,183,333 17,000,000 45,166,667 22,250,000 35,500,000

Semi Skimmed Start

15,425,000 98,500,000

0 0 0 0 345,000 491,667 7,050,000 9,616,667 23,750,000 53,833,333 19,250,000 35,333,333

Semi Skimmed Middle

22,750,000 86,666,667

Comparison between Standard and Recycled bottles APC Results


0 0 0 5 212,500 160,000 11,100,000 9,153,333 23,750,000 44,166,667 21,750,000 46,500,000

Semi Skimmed End

22,000,000 51,833,333 0 0 0 0 11,000 19,333 235,000 453,333 7,850,000 1,678,333 8,850,000 18,766,667

Skimmed Milk Start Control

19,500,000 19,166,667 0 0 0 0 21,250 24,833 250,000 291,667 3,250,000 2,185,000 6,425,000 23,033,333

Skimmed Milk Middle Control

34,000,000 43,333,333 0 0 0 0 18,000 16,667 277,500 365,000 7,400,000 2,920,000 8,650,000 15,900,000

Skimmed Milk End Control

39,500,000 31,666,667


Control vs Test bottle

y = 0.9034x + 0.5075R2 = 0.9442

0

1

2

3

4

5

6

7

8

9

0 1 2 3 4 5 6 7 8 9

Control (log cfu/g)

Test

bot

tle (l

og c

fu/g

)

SUMMARY OUTPUT

Regression Statistics

Multiple R 0.971695642 R Square 0.94419242 Adjusted R Square 0.94283126 Standard Error 0.259584907 Observations 43 ANOVA

df SS MS F Significance FRegression 1 46.74229737 46.74229737 693.667229 2.58217E-27Residual 41 2.762757288 0.067384324 Total 42 49.50505466

Coefficients Standard Error

t Stat P-value

Intercept 0.507517126 0.23250786 2.182795565 0.034832629 X Variable 1 0.90338469 0.034300238 26.33756308 2.58217E-27 Lower 95% Upper 95% Lower 95.0% Upper 95.0%

0.037957718 0.977076534 0.037957718 0.9770765340.834113916 0.972655465 0.834113916 0.972655465


t-Test: Paired Two Sample for Means

Control Test Mean log difference Mean 6.541798726 6.679636775 0.137838049 Variance 1.178691778 1.363688917 Observations 43 43 Pearson Correlation 0.971695642 Hypothesized Mean Difference 0 df 42 t Stat -3.225839486 P(T<=t) one-tail 0.001217486 t Critical one-tail 1.681951289 P(T<=t) two-tail 0.002434973 t Critical two-tail 2.018082341


Appendix 13 Rheological Test Data

Melt Flow Rate Analysis

HDPE Samples

Report No. 2036 Client:

Nextek Ltd 221, Westbourne Park Road London W11 1EA

Attention: Robert Dvorak Edward Kosier

Reported by: Anna Arkhireeva

Date of report: 14 August 2006

1. INTRODUCTION At the request of Mr Edward Kosier of Nextek Ltd, the Melt Flow Rate was determined for 11 polymer samples.

2. ANALYSIS and RESULTS Measurements were carried out using a standard Davenport melt flow indexer equipped with a Eurotherm temperature controller in accordance with BS EN ISO 1133:2000 BS2782-7: Method 720A at 1900C using the weight of 2.16 kg. The tests were performed at 23-240C, at ca. 40% humidity.

Table 1. MFR results for HDPE samples

Sample Identification MFR (g/10min) Mean (g/10min) A/Bag 4

0.64 0.64 0.65 0.64 0.65

0.64

A/Bag 9

0.63 0.64 0.64 0.64 0.65

0.64

A/Bag 17

0.66 0.66 0.66 0.66 0.67

0.66

0.66 0.67


A/Bag 18 0.68 0.68 0.68

0.67

B/Bag 10

0.57 0.58 0.58 0.58 0.58

0.58

B/Bag 11

0.65 0.65 0.65 0.66 0.65

0.65

B/Bag 12

0.59 0.59 0.59 0.60 0.61

0.60

B/Bag 13

0.59 0.61 0.60 0.60 0.61

0.60

B/Bag 14

0.59 0.60 0.60 0.61 0.61

0.60

B/Bag 15

0.60 0.61 0.60 0.61 0.61

0.61

B/Bag 16

0.64 0.64 0.64 0.64 0.64

0.64

Reported by Anna Arkhireeva London Metropolitan University


Appendix 14 Variations in Balestock Quality RECOUP have provided the following explanation for the differences found in colour content and feedstock variation between the two batches. This clearly shows that well specified and consistent feedstock supply is key to the final product quality and colour. The variation in balestock was unknown to Nextek Ltd, at the time of supply. “As for the supplies of material, we did obtain them from two different sources to give you an option to see the material that you would typically find available from collection schemes. The vast majority of material will have been collected from the domestic waste stream and may include a small supply from any commercial sources that they may have locally. The material will have been sorted in their facilities and should comply with the levels of contamination in our bale specification which, generally, they do, but occasionally we do find a site goes over the recommended level just as you may find sites that are well under the contamination level. If you have any figures and photos of this contamination, I will speak to the site concerned”. “As some general information, each scheme will be set up slightly differently. Some may ask the public to separate their plastic bottles into collection banks and may specifically ask for one collection bank just to contain a specific type of bottle, i.e. Milk Bottles. This can mean that bottles are baled direct from how they are sorted by the public with just a quick inspection from staff who take out whatever bottles are not required so there is often little contamination in these bales as there is usually less to take out. Other schemes may have them all collected in one collection bank whilst other schemes may include their plastic bottle collections in their kerbside collection box/bag/bin where there will be other items besides plastic bottles collected together (i.e. paper, card, steel/aluminium cans, textiles, glass, etc.). The levels of contamination will also depend on the quantity of material through a plant, the manning levels, staff training and the supervision of staff so I would expect that contamination levels may vary from time to time between loads even within the same facility”.


Appendix 15 Extrusion Mass Balance The following table provides the full material break down after extrusion at Erema.

BAG No: MATERIAL A (Kg)

MATERIAL B(Kg)

REJECTED Col-HDPE FLAKE

1 1171 2 1030 3 930 4 1086 5 1100 6 1085 7 1126 8 1143 9 1129 10 1147 11 1071 12 1058 13 1205 14 1085 15 1020 16 954 17 1142 18 771 19 20 764 21 570 22 786 23 778 24 558 25 360 26 747 27 690 28 763 29 697.5

Amount Produced: 11,713 Kg 7,540 Kg 6,713.5 Kg Total Weight of

Pelletised Resin: 19,253 Kg

TOTAL WEIGHT

25,966.5 Kg

Final Mass Balance after Sorting and Extrusion (Source: Erema)

Written by: Edward Kosior and Robert Dvorak NEXTEK Ltd 221 Westbourne Park Rd W11 1EA London, U.K. http://www.nextek.org

Published by Waste & Resources The Old Academy Tel: 01295 819 900 Helpline freephone Action Programme 21 Horse Fair Fax: 01295 819 911 0808 100 2040 Banbury, Oxon E-mail: [email protected] OX16 0AH www.wrap.org.uk

Documents

WRAP Large Scale HDPE Recycling Trial Report