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Appendix-11/17

[Appendix 1]

Voluntary Design Guidelines for Designated PET Bottles

Material Evaluation Criteria for Bottles (including Handles)

Revised on March 1, 2011

The Council for PET Bottle Recycling (JAPAN)

Table of Contents 1. Introduction --- Objectives and Backgrounds 2 2. Definition of the “Materials” --- Scope of Application 2 3. Current Situation of Designated PET Bottles 3 4. Basic Requirements 3

A. Food Contact Compliance B. Recycling Processability C. Reutilization Suitability

5. Equipment 3 6. Preparation of the Samples (Recycled and Reference Materials) 3 7. Procedures for Reutilization Suitability Evaluation 4

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 10 9. Making a Report 11 Attached Tables

Attached Table 1 – Procedures for Preparing Test Samples 12 Attached Table 2 – Specifications for Basic Physical Properties

of the Recycled Materials 14 Attached Table 3 – Specifications for the Recycled Materials

for Fiber Application 15 Attached Table 4 – Specifications for the Recycled Materials

for Bottle Application 16 Attached Table 5 – Specifications for the Recycled Materials

for Sheet Application 17

Appendix-12/17

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 1997.

The “Guidelines”, however, were not based on definite evaluation criteria. They exceptionally allowed the use of polycarbonate until the end of March 2000. 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

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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.

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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 Reutilization 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

Evaluation of Basic Physical Properties

Preparation of samples for Application-specific Evaluation

Fiber

Bottle

Sheet

(See Attached Table 1 – Procedures for Preparing Test Samples)

(See Attached Table 2 – Specifications for Physical Properties of the Recycled Materials)

(See Attached Table 1 – Procedures for Preparing Test Samples)

(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)

Preparation of samples for Basic Physical Property Evaluation

Application-specific Evaluation

Appendix-15/17

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 Shape Compare the shape of the flakes with that of the

reference material flakes visually. Appear-

ance Color Compare the color of the flakes with that of the reference

material flakes visually.

Flakes

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.

Intrinsic viscosity retention

Compare IV value for the pellets with that for the 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.

Pellets

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.

Haze Measure the haze of the plate using a haze meter. Appearance Observe for flow marks, sink and other defects.

Plates

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.

Appendix-16/17

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 Evaluation Methods Filtration Observe the increase in filtering pressure with the

passage of time at the specified spinning conditions and filter configuration.

Spinning Count the number of times of yarn breakage, during winding the yarn at the specified speed.

Process- ability

Drawing 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%.

Yarn quality 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.

Physical properties

Dyeability Evaluate uptake rate, dyeing speck and color fastness to light of the dyed circular knit made of the drawn yarn.

Appendix-17/17

2) Equipment and conditions to be used Items Equipment and conditions

Filteration - Equipment Spinning machine (single screw) - Filter configuration #50/#100/#2300-2400/#100 (mesh) - Filtration rate 260 g/cm2/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.

Appendix-18/17

(2) Bottle application

1) Evaluation overview Evaluation Items Evaluation Methods

Injection molding

Mold preforms of approximately 4 mm thick under the standard settings and observe the appearance (for sink, transparency, etc.).

Process- ability

Blow molding

Blow mold the above preforms into bottles under the standard settings and observe the appearance of the bottles (for sink, off-centering, shape, etc.).

Bottle propaties 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.

Appendix-19/17

(3) Sheet application

1) Evaluation overview Evaluation Items Evaluation Methods

Filteration Observe increase in filtering pressure with the passage of time at the specified extruding conditions and filter configuration.

Sheet Forming

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.

Process- ability

Thermo- forming

Mold the sheet into cups and compare the contour and haze with those made from the reference material.

Sheet propaties 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/#750-800/#60 (mesh) - Filtration rate 200 gr/cm2/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.

Appendix-110/17

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.

Number of items that

do not meet the specification Rank

Important Reference

Estimated Impact on Recycling Stream Judgment

AA 0 3 ≥ Almost no impact on current recycling stream

Can be used

A 1 ≥ 3 ≥ Negative impact on recycling stream is expected to be extremely low.

Can be used

B 3 ≥ 5 ≥

Negative impact on recycling stream is expected to be relatively small.

Can be used. Recommended to be improved to A or higher ranks

C 4 ≦ 6 ≦ There is a possibility of having negative impact on current recycling stream.

Must not be used

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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. 7-16 Nihonbashi-Kodemma-cho, Chuo-ku, Tokyo 103-0001, Japan Tel: +81-3-3662-7591 Fax: +81-3-5623-2885

2 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.

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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

↓ Bottle molding

Mold the bottles of intended use.

↓ Crushing

↓ Crushing

Crush the bottles into 8mm mesh flakes.

↓ Flake washing

↓ Flake washing

Immerse the flakes in 1.5% caustic solution at 90°C for 15 minutes.

↓ Rinsing

↓ Rinsing

Rinse the flakes with clean water.

↓ Flakes for the

evaluation ↓

Re-pelletization

↓ Flakes of the

reference material ↓

Re-pelletization

Re-process the flakes into pellets.

(2) Procedures for Preparing Samples for Application-Specific Evaluation

(A) Bottle and Sheet Applications


↓ Bottle molding

↓ Bottle molding

Mold the bottles of intended use.

↓ Crushing

↓ Crushing

Crush the bottles into 8mm mesh flakes.

↓ (Flake washing)

↓ (Flake washing)

Required only if there is a doubt in caustic resistance of the test material.

Common procedure for both bottles and sheet

↓

Flakes for the evaluation

↓ Flakes of the

reference material

(To be used for sheet forming)

Re-pelletization ↓

Re-pelletization ↓

Re-process the flakes into pellets. For bottle application Blending (50%) Blending (50%) Mix the re-processed pellets with the

same amount of virgin PET pellets.

Notes:

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.

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(B) Fiber Application


↓ (Pellet washing)

↓ (Pellet washing)

Required only if there is a doubt in caustic resistance of the test material.

↓ Re-pelletization

↓ Re-pelletization

Re-process the materials into pellets again.

Notes:

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.

Appendix-114/17

Attached Table 2 – Specifications for Basic Physical Properties of the Recycled Materials

(1) Flakes

Evaluation Items Unit Specifications Importance Level Remarks

Shape Equivalent to

the reference material

Reference

Appearance

Color Equivalent to


Reference

In visual comparison with the reference material

Fine powder content % 120 ≥ Important Relative value to the reference material

(2) Pellets and Plates

Evaluation Items Unit Specifications Importance Level Remarks

IV retention % 90 ≦ Important Relative value to the reference material

L (ΔL) 5 ≥ Reference a (Δa) 2 ≥ Reference Color b (Δb) 3 ≥ Important

Difference from the reference material

Haze % 5 ≥ Important Flow marks No flow mark Reference

Appearance Sink No sink Reference Tg °C 70 ≦ Reference Tc1 °C 130 ≦ Reference Tc2 °C 205 ≥ Reference

Thermal property (See Note below) Tm °C 230 ≦ Reference

(plates)

Drying test Agglom-eration No agglomeration

of the pellets 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)

Appendix-115/17

Attached Table 3 – Specifications for the Recycled Materials for Fiber Application

Evaluation Items Evaluation Details Unit Specifications Importance Level Remarks

Filtration Increase in filtration pressure (after three hours of continuous run)

kg/cm2 20 ≥ Important Filter configuration #50/100/2300 - 2400/100

Spinning Yarn breakage at spinning (during three hours of continuous run)

Times 1 ≥ Important 900 g

MDR % 90 ≦ Reference Relative value to the reference material

Process- ability

Drawing Yarn breakage at drawing Times 1 ≥ Important 300 g

Toughness 20 ≦ Important Tf = DT√DE Shrinkage in boiling water % 80 ~ 120 Reference For 30 minutes in

boiling water Thermal shrinkage rate Dry shrinkage

rate % 80 ~ 120 Reference At 100°C for 10 minutes

Color (Δb) 2 ≥ Important Circular knit

Thickness % 80 ~ 120 Reference

Tensile strength % 80 ~ 120 Reference Relative value to the reference material

Tensile elongation % 30 ± 5 Important Setting condition

Yarn quality

Intrinsic viscosity (IV) 0.55 ~ 0.7 Reference

Uptake rate % 90 ≦ Reference Relative value to the reference material Dyeability

Spots No spot Important Dyeing evenness

Physical properties

Dyeability

Color fastness to light Class 4 ≦ Important

Appendix-116/17

Attached Table 4 -- Specifications for the Recycled Materials for Bottle Application

Evaluation Items Evaluation Details Unit Specifications Importance

Level Remarks

Injection molding Appearance of the preforms

Equivalent to the reference

material Important

Appearance of the bottles Equivalent to the reference

material Important

In visual comparison with the reference material

Process- ability Blow

molding Stretching stress % 90 ≦ Reference IV retention % 90 ≦ Reference Acetaldehyde % 110 ≥ Reference

Brimful volume % 1.0 ≥ Important Bottle dimensions Height % 1.5 ≥ Reference

Average wall thickness % 90 ≦ Reference Thickness

distribution Thickness fluctuation % 110 ≥ Reference

Tensile yield strength % 90 ≦ Reference

Fracture point % 90 ≦ Reference

Relative value to the reference material

Color (Δb) 3 ≥ Important Difference from the reference material

Haze % 5 ≥ Important

Drop impact strength Times 1 < Reference 1.2 m in an upright position at 5°C

Bottle properties

Whitening from drop impact No whitening Reference

Drop once from an height of 1.2 m in an upright position at 5°C

Appendix-117/17

Attached Table 5 -- Specifications for the Recycled Materials for Sheet Application

Evaluation Items Evaluation Details Unit Specifications Importance Level Remarks

Filtera- tion

Increase in filtration pressure (after two hour continuous run)

kg/cm2 10 ≥ Important Filter configuration #60/750-800/60

Sink No sink Reference Appearance Flow

marks No flow mark Reference Sheet

Molding Number of fisheyes /m2 2 ≥ Reference 0.5 mm or larger

Contour Equivalent to


Reference

Process- ability

Thermo- forming Test Whitening No whitening Reference

Haze % 3 ≥ Important At 0.3 mm thick

Color(Δb)

2 ≥ Important Difference from the reference material

Impact strength % 85 ≦ Important

Tensile yield strength % 85 ≦ Reference

Fracture point % 85 ≦ Important

Sheet Properties

Tensile modulus % 85 ≦ Reference

Relative value to the reference material