Voluntary Design Guidelines for Designated PET Bottles Appendix 1 Appendix 1-1 : Material Evaluation Criteria for Bottles (including Handles)

Transcription

1 Voluntary Design Guidelines for Designated PET Bottles Appendix 1 Appendix 1-1 : Material Evaluation Criteria for Bottles (including Handles) Revised on May 22, 2015 The Council for PET Bottle Recycling (JAPAN) Table of Contents 1. Introduction --- Objectives and Backgrounds...P2 2. Definition of the Materials --- Scope of Application.P2 3. Current Situation of Designated PET Bottles P3 4. Basic Requirements...P3 A. Food Contact Compliance B. Recycling Processability C. Recycling Suitability 5. Equipment..P3 6. Preparation of the Samples (Recycled and Reference Materials)..P4 7. Procedures for Recycling Suitability Evaluation...P4 7-A. Evaluation of Basic Physical Properties 7-B. Application-specific Evaluation (1) Fiber application (2) Bottle application (3) Sheet application 8. Judgment of Evaluation Results..P10 9. Making a Report..P11 Attached Tables Attached Table 1 Procedures for Preparing Test Samples P12 Attached Table 2 Specifications for Basic Physical Properties of the Recycled Materials P14 Attached Table 3 Specifications for the Recycled Materials for Fiber Application P15 Attached Table 4 Specifications for the Recycled Materials for Bottle Application...P16 Attached Table 5 Specifications for the Recycled Materials for Sheet Application P17 1/25

2 1. Introduction --- Objective and Backgrounds This document is prepared as an appendix to Voluntary Design Guidelines for Designated PET Bottles (these Guidelines ) by The Council for PET Bottle Recycling (the Council). It prescribes properties (including hygienic safety) of the materials required from the viewpoint of recycling and methods for evaluating recyclability of the materials used for the bodies of the designated PET bottles for soft drinks, alcoholic beverages and specified seasonings which are sold in Japan. The companies such as manufacturers, dealers and importers that are planning to use the designated PET bottles incorporating the materials other than PET are responsible for conducting evaluation in accordance with these Criteria. <Backgrounds> The Council issued the Voluntary Design Guidelines for Type II Designated PET Bottles in April 1995 and put it into practice. It was revised in 1998, in line with the Law for Promotion of Sorted Collection and Recycling of Containers and Packaging (the Container and Package Recycling Law ) came into effect and collection and recycling of post consumer PET bottles started in April The Guidelines, however, were not based on definite evaluation criteria. They exceptionally allowed the use of polycarbonate until the end of March For the use of polyarylate, aromatic polyamide and polyethylene naphthalate (PEN), which were also exceptionally allowed to be used, the limitation of use was described as within the range of not causing problems on the recycling stream. The Council conducted the evaluations of those three resins, namely polyarylate, aromatic polyamide and PEN to investigate the acceptable range of the contents for recycling to fiber, bottles and sheet, and then established Material Evaluation Criteria, with which classification of the effects on quality of the recycled products is possible. In the last (2001) version of the Guidelines the list of materials exceptionally allowed to be used was removed. Those Criteria set out guidelines for evaluation methods and specifications by which the concerned companies should confirm in determining the limit content of other resins mixed or multi-layered with PET and in determining the type and composition of PET copolymers. In this version, the Criteria are retitled Material Evaluation Criteria for Bottles (including Handles) and mainly the scope of application is revised. Other sections remain almost unchanged. These Criteria may evolve according to the progress and change in recycling technologies, and also with changes of social circumstances. 2. Definition of the Materials ---Scope of Application The term Materials for Bottles in these Guidelines and these Criteria specifies all the materials composing bodies of the designated PET bottles. (See Bottles in Attached Table List of Basic Standards of these Guidelines.) They include 1) other resins multi-layered with PET, 2) other resins, additives or PET copolymers blended with PET, 3) coatings, etc. Coloring of the bottle bodies, usage of base cups and direct printing except for date and/or production coding for designated PET bottles have been prohibited. The companies* that are planning to use PET bottles incorporating new materials as 1), 2), or 3) above are requested to conduct evaluation on the basis of these Criteria and verify the absence of problems in the recycling stream. * The companies include manufacturers of the resins, the additives and the bottles, bottle 2/25

3 users such as beverages, food and filling companies, the dealers and the importers. 3. Current Situation of Designated PET bottles Currently, almost all the designated PET bottles in the market comply with these Guidelines and Criteria. For example, the use of barrier enhanced PET bottles which are 1) multi-layered with other resins than PET, 2) blended with other resins and/or additives, 3) coated bottles etc. has increased recently and only those evaluated on the basis of these Criteria, reported to the Council and confirmed to comply with these Guidelines have been put on the market. Although member companies of the Council have converted colored bottles, which have been prohibited, to colorless ones at a rate of 100%, there still remain very small amount of colored bottles in the market. As they trouble reclaimers by increasing labor for sorting and lowering the value of the recycled materials as contaminant, the Council is asked strongly to stick more closely to the Guidelines. The Council is continuously requesting the manufacturers, the dealers and the importers for conversion to colorless bottlers. 4. Basic Requirements The designated PET bottles incorporating new materials should meet the requirements A through C below: A. Food Contact Compliance * The bottles should be compliant with the Standards and Criteria for Foods and Additives (Ministry of Health and Welfare Notification No. 370) set forth in accordance with the Food Sanitation Act. * All the materials used should be compliant with the voluntary standards set by the Japan Hygienic Olefin and Styrene Plastics Association or with the U.S. FDA regulations, or the absence of hygiene and safety problems is verified on the responsibility of the bottle manufacturer, the material supplier or the company commercializing the bottles. * In case recycled materials are employed in the designated PET bottles, the users of the materials and/or the bottles are responsible for confirming hygienic safety of the materials. B. Recycling Processability There should not be discoloration, quality change or deterioration when the material is immersed in 1.5% caustic solution at 85 to 90 C for 15 minutes. C. Reutilization Suitability The recycled materials should meet the specifications for fiber, sheet and bottle applications when evaluated in accordance with the methods prescribed in these Criteria. 5. Equipment Since the purpose of the evaluation is to confirm that the materials to be evaluated will give no significant impact on current recycling stream, it would be desirable to use industrial recycling equipment. However, if there is any difficulty in conducting the evaluation with industrial equipment, laboratory equipment may be used as a substitute. In such a case, the equipment and condition used have to be those give similar results with those used in actual recycling facilities in terms of processability and product quality. 3/25

4 6. Preparation of the Samples (Recycled and Reference Materials) The samples of the recycled materials should be prepared from the flakes obtained by crushing the bottles to be evaluated in an appropriate manner for each end-application. The type of the bottles to be evaluated should be, in principle, that for the intended application (e.g. the new material system intended for soy sauce application should be molded into soy sauce bottles). The procedures for preparing the samples are shown in Attached Table 1 Procedures for Preparing Test Samples. The reference sample should be prepared from the same bottles containing only PET. 7. Procedures for Recycling Suitability Evaluation The evaluation is comprised of basic physical properties and the application-specific properties. The former is the properties required for reclaimed flakes, while the latter is those required for end application products. The recycled materials should be evaluated for use of three applications i.e. fiber, bottle and sheet, as most of the recycled materials are used in these categories currently. [Evaluation Flowchart] Bottles to be evaluated Preparation of samples for Basic Physical Property Evaluation Evaluation of Basic Physical Properties (See Attached Table 1 Procedures for Preparing Test Samples) (See Attached Table 2 Specifications for Physical Properties of the Recycled Materials) Preparation of samples for Application-specific Evaluation (See Attached Table 1 Procedures for Preparing Test Samples) Application-specific Evaluation Fiber Bottle Sheet (See Attached Table 3 Specifications for the Recycled Materials for Fiber Application) (See Attached Table 4 Specifications for the Recycled Materials for Bottle Application) (See Attached Table 5 Specifications for the Recycled Materials for Sheet Application) 4/25

5 7-A. Evaluation of Basic Physical Properties The evaluation should be carried out on the flakes and the pellets prepared in accordance with Attached Table 1 (1) Procedures for Preparing Test Samples for Basic Physical Properties, and injection molded plates of 3 mm thick made from the pellets. (1) Evaluation Overview Evaluation Items Evaluation Methods Flakes Appearance Shape Compare the shape of the flakes with that of the reference material flakes visually. Color Compare the color of the flakes with that of the reference material flakes visually. Fine powder generation Sift the flakes using 50-mesh sieve and compare the amount of the fine powder generated during crushing with that of the reference material. Pellets Intrinsic viscosity Compare IV value for the pellets with that for the retention reference material pellets. Color Measure the differences of L, a, and b values between the pellets of the sample and those of the reference material with color measuring equipment. Drying test Place 200 g of the recycled pellets that have been crystallized at 130 C for 60 minutes in a cylindrical tube of 80 mm diameter, apply a load of 10 kg, and introduce flowing nitrogen gas heated up to 150 C into the tube for three hours. Then, observe agglomeration of the pellets. Plates Haze Measure the haze of the plate using a haze meter. Appearance Observe for flow marks, sink and other defects. Thermal Property Measure glass transition temperature (Tg), crystallizing temperature at heating (Tc1), melting temperature (Tm) and crystallizing temperature at cooling (Tc2) for samples from the plate with a differential scanning calorimeter (DSC*). * DSC conditions: Heating rate: 10 C/min (Tg, Tc1, Tm) Keep at 300 C for three minutes Cooling rate: 10 C/min (Tc2) (2) Specifications See Attached Table 2 Specifications for Basic Physical Properties of the Recycled Materials. 5/25

6 7-B. Application-specific Evaluation The evaluation should be carried out for applications of fiber, bottles and sheet, as most of the recycled material is used in these three categories currently. (1) Fiber application 1) Evaluation Overview Evaluation Items Process- Filtration ability Physical properties Spinning Drawing Yarn quality Dyeability Evaluation Methods Observe the increase in filtering pressure with the passage of time at the specified spinning conditions and filter configuration. Count the number of times of yarn breakage, during winding the yarn at the specified speed. Measure the maximum draw ratio (MDR) when drawing the yarn. Count the number of times of yarn breakage when the yarn is drawn to a elongation of 30±5%. Measure thickness (dtex) and intrinsic viscosity (IV) for the undrawn yarn. Measure thickness (dtex), tensile strength, thermal shrinkage rate and toughness for the drawn yarn. Measure the color (L, a, b) of circular knit made of the drawn yarn. Evaluate uptake rate, dyeing speck and color fastness to light of the dyed circular knit made of the drawn yarn. 6/25

7 2) Equipment and conditions to be used Items Equipment and conditions Filteration - Equipment Spinning machine (single screw) - Filter configuration #50/#100/# /#100 (mesh) - Filtration rate 260 g/cm 2 /hr - Spinning temperature 280 to 285 C - Testing time 3 hours Spinning - Equipment Spinning machine (single screw) - Winding rate 700 m/minute - Undrawn yarn thickness 70±2 dtex/8 filaments (equivalent to nine dtex/filament) Drawing - Equipment Drawing machine - Hot roller temperature 80 C - Hot plate temperature 150 C - Elongation 30±5% - Draw ratio 3 to 4 times (to be set based on elongation factor) - Drawing rate 600 m/minute - Drawn yarn thickness 17 to 22 dtex/8 filaments (equivalent to 2.2 dtex/filament) Dyeing - Equipment Circular knitting machine, miniature color dyeing machine, thermo setter etc. - Refining Treat the circular knit at 60 to 70 for 20 minutes with standard chemicals and auxiliaries at a bath ratio of 1:30 to 1:50. - Pre-setting at 150 to 200 C, for 30 to 60 seconds - Dyeing Treat the circular knit with blue disperse dye for polyester (such as Dianix Blue and Resoline Blue) and auxiliaries at a bath ratio of 1:30 to 1:50 at 130 C for 30 minutes. - Reduction cleaning Treat the circular knit with standard reducing agents and auxiliaries at a bath ratio of 1:30 to 1:50 at 70 to 80 C for 20 minutes. - Final setting at 160 C for 30 to 60 seconds Color fastness to light (To be carried out in accordance with the procedures specified in JIS L-0842) - Equipment UV fade meter - Irradiation at 63 C for 20 hours 3) Specifications See Attached Table 3 Specifications for the Recycled Materials for Fiber Application. 7/25

8 (2) Bottle application 1) Evaluation overview Evaluation Items Process- Injection ability molding Bottle propaties Blow molding Evaluation Methods Mold preforms of approximately 4 mm thick under the standard settings and observe the appearance (for sink, transparency, etc.). Blow mold the above preforms into bottles under the standard settings and observe the appearance of the bottles (for sink, off-centering, shape, etc.). Evaluate propaties of the bottles including IV retention, acetaldehyde content, bottle dimensions, material distribution, tensile strength, color-b, haze, drop impact strength and whitening from drop impact. 2) Equipment and conditions to be used Items Equipment and conditions Injection molding - Equipment Injection molding machine - Mold Preform molds for 500 to 1,500 ml bottles (molds with two or more cavities are recommended.) - Melt temperature 280 to 300 C (setting) - Molding conditions To be set using the reference material - Testing time 3 hours Stretching blow molding - Equipment Stretch blow molding machine - Mold Blow molds for 500 to 1,500 ml bottles - Molding conditions To be set using the reference material 3) Specifications See Attached Table 4 -- Specifications for the Recycled Materials for Bottle Application. 8/25

9 (3) Sheet application 1) Evaluation overview Evaluation Items Process- Filteration ability Sheet propaties Sheet Forming Thermoforming Evaluation Methods Observe increase in filtering pressure with the passage of time at the specified extruding conditions and filter configuration. Form a sheet of 0.30±0.02 mm thick, and observe the appearance to check for sink, flow marks and other defects, and count the number of fisheyes. Mold the sheet into cups and compare the contour and haze with those made from the reference material. Evaluate propaties of the sheet including IV value, transparency (haze), color, impact strength, tensile yield strength, fracture point and tensile modulus. 2) Equipment and conditions to be used Items Equipment and conditions Filteration - Equipment Extruder - Filter configuration #60/# /#60 (mesh) - Filtration rate 200 gr/cm 2 /hr - Melt temperature 280 to 290 C - Testing time 120 minutes Sheet Forming - Equipment Sheet forming machine - Melt temperature 280 to 290 C (standard condition for PET) - Sheet thickness 0.30±0.02 mm - Sheet width 250 mm or wider Thermoforming - Equipment Air pressure or vacuum thermoformer - Forming temperature 90 to 100 C (standard condition for PET) - Mold diameter 80 to 100 mmφor equivalent (rectangular or circular) - Draw ratio 0.5 or more - Number of molds Two or more rows in the widthwise direction 3) Specifications See Attached Table 5 Specifications for the Recycled Materials for Sheet Application. 9/25

10 8. Judgment of Evaluation Results Evaluation items are classified as either Important or Reference depending on the level of importance (see Attached Tables 2 through 5). The results are, in principle, judged with relative values to the reference material except for certain items which are judged with absolute values. The judgment of evaluation results should be made as follows. Rank Number of items that do not meet the specification Important Reference AA 0 3 A 1 3 B 3 5 C 4 6 Estimated Impact on Recycling Stream Almost no impact on current recycling stream Negative impact on recycling stream is expected to be extremely low. Negative impact on recycling stream is expected to be relatively small. There is a possibility of having negative impact on current recycling stream. Judgment Can be used Can be used Can be used. Recommended to be improved to A or higher ranks Must not be used 10/25

11 9 Making a Report As it is essential to understand the materials used in PET bottles correctly in order to ensure smooth recycling, submission of a report on the evaluation results to The Council for PET Bottle Recycling is requested prior to putting the bottles incorporating newly developed materials on the market. The report should include the information listed below: 1 Submit to: The Council For PET Bottle Recycling 2F, Nikkei Build Nihonbashi-Kodemma-cho, Chuo-ku, Tokyo , Japan Tel: Fax: Format: A4 size, stapled lengthwise on the left 3 Information to be included (1) Submitter and the date of submission (2) Material name (tradename and/or substance name) (3) Manufacturer of the material (4) Intended use and limitations (such as soy sauce, CSD applications etc.) (5) Method of use (such as monolayer, blend, multi-layer, coating, etc.) (6) Upper limit of the content of the material that complies with these Criteria. (7) Documents verifying compliance with hygienic standards (such as the Food Sanitation Act, US FDA regulations and voluntary standards) (8) Evaluation results of recycling processability performed based on these Criteria (9) Evaluation results of reutilization suitability performed based on these Criteria (10) Brief information about the fiber, the bottles and the sheet used for the evaluation Material name (2) and/or the manufacturer (3) are not always required to be specified as it may result in disclosure of intellectual properties. 11/25

12 Attached Table 1 Procedures for Preparing Test Samples (1) Procedures for Preparing Samples for Basic Physical Property Evaluation Test Material Reference Material Remarks Test Materials Pure PET Use the PET of the same grade. Bottle molding Crushing Flake washing Rinsing Flakes for the evaluation Re-pelletization Bottle molding Crushing Flake washing Rinsing Flakes of the reference material Re-pelletization Mold the bottles of intended use. Crush the bottles into 8mm mesh flakes. Immerse the flakes in 1.5% caustic solution at 90 C for 15 minutes. Rinse the flakes with clean water. Re-process the flakes into pellets. (2) Procedures for Preparing Samples for Application-Specific Evaluation (A) Bottle and Sheet Applications Common procedure for both bottles and sheet For bottle application Notes: Test Material Reference Material Remarks Test Materials Pure PET Use the PET of the same grade. Bottle molding Bottle molding Mold the bottles of intended use. Crush the bottles into 8mm mesh Crushing Crushing flakes. Required only if there is a doubt in (Flake washing) (Flake washing) caustic resistance of the test material. Flakes for the Flakes of the (To be used for sheet forming) evaluation reference material Re-pelletization Re-pelletization Re-process the flakes into pellets. Blending (50%) Blending (50%) Mix the re-processed pellets with the same amount of virgin PET pellets. 1) As it is generally difficult to mold bottles normally with 100% recycled material, use 50/50 mixture of the recycled material and virgin PET in the evaluation for bottle application. 2) For sheet application, the evaluation may be conducted with the re-pelletized materials. The caution against IV dropping during the re-pelletizatin process would be necessary. 12/25

13 (B) Fiber Application Test Material Reference Material Remarks Test Materials Pure PET Use the PET of the same grade. (Pellet washing) Re-pelletization Notes: (Pellet washing) Re-pelletization Required only if there is a doubt in caustic resistance of the test material. Re-process the materials into pellets again. 1) It was found in preliminary investigations that contamination that occurs during the process of preparing test samples makes the evaluation difficult when a laboratory spinning machine is used. The test material, therefore, may be melt processed directly into pellets of mixture of starting materials to simulate the effect of thermal history, skipping the process of bottle molding, crushing and flake washing. 2) In the evaluation of the recycled materials to be processed into fiber, the effect of the IV value cannot be ignored. It is, therefore, important to re-pelletize the materials under conditions in which the IV value becomes between 0.55 and 0.70 dl/g. 13/25

14 Attached Table 2 Specifications for Basic Physical Properties of the Recycled Materials (1) Flakes Evaluation Items Unit Specifications Appearance Shape Color Equivalent to the reference material Equivalent to the reference material Importance Level Reference Reference Fine powder content % 120 Important Remarks In visual comparison with the reference material Relative value to the reference material (2) Pellets and Plates Evaluation Items Unit Specifications Importance Level IV retention % 90 Important L (ΔL) 5 Reference Color a (Δa) 2 Reference b (Δb) 3 Important Haze % 5 Important Flow Appearance marks No flow mark Reference Sink No sink Reference Tg C 70 Reference Thermal property Tc1 C 130 Reference (See Note Tc2 C 205 Reference below) Tm C 230 Reference Drying test Agglomeration of the pellets No agglomeration Important Note: DSC conditions: Heating rate: 10 C /min (Tg, Tc1, Tm) Keep at 300 C for three minutes Cooling rate: 10 C /min (Tc2) Remarks Relative value to the reference material Difference from the reference material (plates) 14/25

15 Attached Table 3 Specifications for the Recycled Materials for Fiber Application Evaluation Items Evaluation Details Unit Specifications Processability Physical properties Filtration Spinning Drawing Yarn quality Dyeability Increase in filtration pressure (after three hours of continuous run) Yarn breakage at spinning (during three hours of continuous run) Importance Level kg/cm 2 20 Important Times 1 Important 900 g MDR % 90 Reference Yarn breakage at drawing Times 1 Important 300 g Remarks Filter configuration #50/100/ /100 Relative value to the reference material Toughness 20 Important Tf = DT DE Shrinkage in For 30 minutes in Thermal % 80 ~ 120 Reference boiling water boiling water shrinkage rate % 80 ~ 120 Reference Dry shrinkage rate At 100 C for 10 minutes Color (Δb) 2 Important Circular knit Thickness % 80 ~ 120 Reference Relative value to the Tensile strength % 80 ~ 120 Reference reference material Tensile elongation % 30 ± 5 Important Setting condition Intrinsic viscosity (IV) 0.55 ~ 0.7 Reference Dyeability Uptake rate % 90 Reference Relative value to the reference material Spots No spot Important Dyeing evenness Color fastness to light Class 4 Important 15/25

16 Attached Table 4 -- Specifications for the Recycled Materials for Bottle Application Evaluation Items Evaluation Details Unit Specifications Processability Injection molding Blow molding Bottle properties Appearance of the preforms Appearance of the bottles Equivalent to the reference material Equivalent to the reference material Importance Level Important Important Stretching stress % 90 Reference IV retention % 90 Reference Acetaldehyde % 110 Reference Bottle Brimful volume % 1.0 Important dimensions Height % 1.5 Reference Average wall Thickness thickness % 90 Reference distribution Thickness fluctuation % 110 Reference Tensile yield strength % 90 Reference Fracture point % 90 Reference Color (Δb) 3 Important Haze % 5 Important Drop impact strength Times 1 < Reference Whitening from drop impact No whitening Reference Remarks In visual comparison with the reference material Relative value to the reference material Difference from the reference material 1.2 m in an upright position at 5 C Drop once from an height of 1.2 m in an upright position at 5 C 16/25

17 Attached Table 5 -- Specifications for the Recycled Materials for Sheet Application Evaluation Items Evaluation Details Unit Specifications Importance Level Increase in filtration Filterapressure (after two hour tion continuous run) kg/cm 2 10 Important Sink No sink Reference Processability Sheet Molding Thermoforming Test Sheet Properties Remarks Filter configuration #60/ /60 Appearance Flow marks No flow mark Reference Number of fisheyes /m 2 2 Reference 0.5 mm or larger Equivalent to Contour the reference Reference material Whitening No whitening Reference Haze % 3 Important At 0.3 mm thick Difference from Color(Δb) 2 Important the reference material Impact strength % 85 Important Tensile yield strength % 85 Reference Relative value to the reference Fracture point % 85 Important material Tensile modulus % 85 Reference 17/25

18 Voluntary Design Guidelines for Designated PET Bottles Appendix 1 Appendix1-2: Bottle-to-Bottle (BtoB) Evaluation Criteria May 22, 2015 The Council for PET Bottle Recycling (JAPAN) Table of Contents 1. Introduction --- Objectives and Backgrounds P19 2. Basic Requirements P19 A. Food Contact Compliance B. Recycling Processability C. Recycling Suitability 3. Recyclability Evaluation Methods.P20 4. Review of Guidelines.P20 5. BtoB Evaluation Methods..P21 6. BtoB Evaluation Criteria P22 Attached Tables Attached Table 6 : Procedures for Preparing Test Samples for BtoB Recycling Suitability Test.. P23 Attached Table 7 : Criteria for BtoB Recycling Suitability...P25 18/25

19 1. Introduction --- Objectives and Backgrounds The Basic Law for Establishing a Recycling-based Society has clarified the priority of activities (in order): reduce, reuse, recycle, recover energy and dispose of waste appropriately. Producers, vendors and importers are giving the highest priority to reducing materials when supplying PET bottles to the market, and they are implementing voluntary action plans that define targets for lightweighting. To ensure lightweighting does not impact product shelf life and convenience for the consumer, they are developing multilayer, blending and coating technologies that use functional materials other than PET. In light of development of these new technologies and to promote recycling of PET bottles in Japan, new guidelines have been added to promote bottle-to-bottle (BtoB) recycling using mechanical recycling of advanced horizontal recycling methods. 2. Basic Requirements The designated PET bottles incorporating new materials should meet the following basic requirements as addition to the requirements listed in Appendix 1-1:Material Evaluation Criteria for Bottles (including Handles). A. Food Contact Compliance Materials should be compliant with the Guidelines for the Use of Recycled Plastic Materials in Equipment and Packaging for Food, dated April 27, 2012 and established by the Ministry of Health, Labour and Welfare. In addition, there should be no hazardous substances generated in the BtoB decontamination process or the filling process when using chemical or electron beam (EB) irradiation for sterilization B. Recycling Processability There should be no discoloration, quality change or deterioration caused in the BtoB process. C. Recycling Suitability Materials should meet the criteria when evaluated in accordance with the attached test methods for BtoB recycling. Processing conditions should not vary significantly when mold preforms and bottles. Note: The following points apply when material separation is possible using any indication, any sorting equipment and/or visual hand sorting. (1) When new separation equipment is developed and recyclers install it, evaluations can be carried out on samples after sorting with the newly developed separation equipment. (2) When recyclers can carry out additional separation by visual and hand sorting with any package identification, those sorting can be used for preparing evaluation samples, which have been blended with new material. 19/25

20 3. Recyclability Evaluation Method Evaluations of BtoB recycling suitability is to evaluate the physical properties required for BtoB recycled products. Bottles to be evaluated Preparation of samples for Basic Physical Property Evaluation Evaluation of Basic Physical Properties Preparation of samples (See Attached Table 1 (1) Procedures for Preparing Test Samples for Basic Physical Property) (See Attached Table 2 Criteria for Basic Physical Property Evaluation) (See Attached Table 1 (2) Procedures for Preparing Test Samples for Recyclability) Fiber (See Attached Table 3 Specifications for the Recycled Materials for Fiber Application) Evaluation for each Bottle (See Attached Table 4 Specifications for the Recycled Materials for Bottle Application) Sheet (See Attached Table 5 Specifications for the Recycled Materials for Sheet Application) Evaluation of BtoB recycling suitability Preparation of test samples for BtoB recycling suitability test (See Attached Table 6 Procedures for Preparing Test Samples for BtoB Recycling Suitability Test) Evaluation of BtoB recycling suitability (See Attached Table 7 Specifications for BtoB Recycling Suitability) 4. Review of Guidelines BtoB recycling is an area that is significant technological development, so these evaluation criteria will be reviewed and amended as required. 20/25

21 5. BtoB Evaluation Methods (1) Evaluation Overview Evaluation Items Evaluation Methods BtoB processed pellets IV Color Measure and compare IV value for the pellets with that for the reference material pellets. Measure L*, a* and b* values using the reflection method. Use the equivalent of a D65 fluorescent lamp as the light source in the measurement apparatus. Plates Color Measure L*, a* and b* values of a 3-mm thick plate in the thickness direction using the transmission method, and find the difference between it and the reference material. Use the equivalent of a D65 fluorescent lamp as the light source in the measurement apparatus. Haze With a haze meter, measure a 3-mm thick plate using a method that complies with the JIS K 7136 standard. (2) Evaluation Overview Evaluation Items BtoB processing test - Recommended equipment - Testing time - Sample weight - Heating condition - Degree of vacuum Injection molding - Equipment - Injection plate - Injection temp. Evaluation Methods -To use 20L rotary evaporator with oil bath heater -Maintain material at 205 C or higher for 7 hrs or longer kg or more -No unevenness in thermal history of material -1 torr or less ; inert gas flow method is also acceptable -Injection molding machine with chilled mold -3 mm thickness -280 to 300 C (as set value) 21/25

22 6. BtoB Evaluation Criteria Evaluation criteria are judged on Required evaluation items. The results are, in principle, judged with relative values to the reference material except some items which are judged with absolute values. The judgment of evaluation results should be made as follows. Rank Evaluation result of required item Judgment A All Required items are ranked A Can be used B C All Required items are ranked B or higher Required items include one or more items ranked C Can be used for only 3 years from the date of accreditation. However, this limitation does not apply if fully Rank A results are provided after improvements. Must not be used Even if materials, which have been accepted in existing guidelines, are ranked B or C in this Appendix 1-2:BtoB Evaluation Criteria, they can be used for only five years from the date of this revision. However, this limitation does not apply if fully Rank A results are provided after improvements. 22/25

23 Attached Table 6 Procedures for Preparing Test Samples for BtoB Recycling Suitability Test (1) Procedure for Preparing Flake Test Samples Test Material Reference Remarks Material Test Material PET only Use the same grade PET resin for bottle as reference. Bottle molding Bottle molding Mold the bottles of intended use. Crushing Crushing Crush the bottles into flakes 8mm in size or less. (Flake washing) (Flake washing) Wash the flakes if necessary. Immerse the flakes in 1.5% caustic solution at 90 C for 15 minutes. Rinsing Rinsing Rinse the flakes with clean water. Draining Flakes for the evaluation Draining Flakes of the reference material Remove attached water by air drying at 50 C for 3 hours. Execute pneumatic separation if necessary. (Refer to the following table) Pneumatic separation: Overview, Equipment and Test Conditions Evaluation Evaluation Methods Items Pneumatic Choose pneumatic separation condition which achieves 5% loss or less separation for flakes of the reference material in (1) of Attached Table 6. conditions If possible, measure contamination removal ratio. Pneumatic Recommendation: Model CFS-150 separator by ACO Co., Ltd. separator (2) Procedure for Preparing Re-pelletized Test Samples Test Material Reference Material Flakes for the evaluation Re-pelletizati on Crystallization and drying Blending Re-pelletization Flakes of the reference material Crystallization and drying Blending Re-pelletization Remarks Use flakes prepared in (1) of Attached Table 6 after pneumatic separation. Use rinsed and water drained flakes, if the separation is not used. Recommended: 140 C for 4 hours Blend flakes with the same weight of virgin PET pellets. Use a single-screw extruder or co-rotating twin-screw extruder. 23/25

24 (3) Procedure for Preparing Test Samples for BtoB Processing Evaluation Test Material Reference Material Remarks Re-pelletized test Re-pelletized Use pellets prepared in (2) of Attached Table 6. material reference BtoB processing Plate molding Crystallization and drying Solid state polymerization material Crystallization and drying Solid state polymerization Recommended: 140 C for 4 hours 205 C or higher for 7 hours or longer Mold 3mm thickness plates at C 24/25

25 Attached Table 7 Criteria for BtoB Recycling Suitability BtoB Processability Evaluation Items Unit Criteria Importance Level BtoB L * processed pellets a * Injection molding plates b * IV increase % Rank A : 90, 120 Rank C : 90>, 120< Flow marks Rank A: No flow mark Rank C: Flow mark Sink Rank A : No sink Rank C : Sink Haze % Rank A : 5 Rank C : 5< L * Include in report Include in report Include in report Required Required Required Required Include in report Remarks Difference from the reference material (ΔIVs/ΔIVr) a * Include in report b * ΔL * Δa * Δb * Rank A : 12 Rank C : 12< Rank A : 2 Rank B : 2<Δb * 5 Rank C : 5< Required Include in report Difference from the reference material Include in report Difference from the reference material Required Difference from the reference material ΔIVs: Variation between IV of test material before and after solid state polymerization. ΔIVr: Variation between IV of reference material before and after solid state polymerization. Note: Include the following information in reports when executed the pneumatic separation. Evaluation Items Unit Criteria Importance Level Remarks Pneumatic separation Yield % 95 Include in report Only when executed pneumatic separation Contamin ation removal % Include in report Only when measureable 25/25