Date: 7 October 2024

Report: 18823/002

Test Report:
• Compositional Analysis:
o Elemental Content: Determination of Prodegradant Catalysts

• Accelerated Ageing Studies:

o Polymer Oxidation During Accelerated Ageing:
▪ Thermal Stability
▪ Thermal Degradation, Following Initial UV Exposure

Test Reference: 18823 Altacoppo Ind. e Com. de Produtos Descartaveis Ltda.

Product Tested: PP/Internal Recycled Plastic PP Cups - for hot drinks

Prepared for: Altacoppo Ind. e Com. de Produtos Descartaveis Ltda.

Prepared by: Yasmine Benjelloun, Junior Scientist

Symphony Environmental Ltd, Product Testing Laboratory

6 Elstree Gate, Elstree Way, Borehamwood WD6 1JD

Telephone: +44 (0)20 8207 5900

[email protected]
www.symphonyenvironmental.com

Registered in England Number 2967867- Address as above.

A wholly owned subsidiary of Symphony Environmental Technologies Plc.
 18823 Altacoppo Ind. e Com. de Produtos Descartaveis Ltda.

TEST REPORT

1.0 AIMS

• To evaluate the presence of prodegradant catalysts in the PP/Internal Recycled Plastic PP Cups - for
hot drinks samples by determination of the prodegradant catalyst metal cations by X-ray fluorescence
(XRF) spectroscopy.

• To evaluate the stability and degradation behaviour of the PP/Internal Recycled Plastic PP Cups - for
hot drinks samples by means of accelerated laboratory ageing techniques, while monitoring extent of
polymer oxidation by infrared (IR) spectroscopy as a function of time.

2.0 SAMPLE DETAILS

Samples Provided by: Altacoppo Ind. e Com. de Produtos Descartaveis Ltda.

Product Type: PP/Internal Recycled Plastic PP Cups - for hot drinks
Date Received: 05/09/2024

Table 1: Sample Details

SEPTL Sample ID Client Reference Polymer Type Prodegradant Additive
PP/Internal Recycled
18823/9373 RES062 - 1 None
Plastic
PP/Internal Recycled
18823/9374 RES062 - 2 0.5% d2w 93390/C
Plastic
Table 1 is based solely on information provided by the client.

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3.0 RESULTS & CONCLUSIONS

3.1 Compositional Analysis

3.1.1 Determination of Prodegradant Catalysts

The presence of prodegradant catalysts in each sample is confirmed by determination of the prodegradant
catalyst metal cations by energy-dispersive X-ray fluorescence (XRF) spectroscopy.

The prodegradant catalyst content result, as determined by X-ray fluorescence (XRF) spectroscopy, is
given in Table 2.

Table 2: Determination of Prodegradant Catalyst

Sample ID Spectrum Ref. Prodegradant Content
18823/9373 212014/3193 Not Detected
18823/9374 212014/3194 Prodegradant Present, Less Than Effective Concentration

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3.2 Accelerated Ageing

3.2.1 Thermal Stability

The real-time stability of polymer products stored at ambient temperatures and protected from extended
exposure to sunlight is evaluated over shorter period of time in the laboratory by monitoring stability and
degradation during thermal ageing at elevated temperatures according to ASTM D5510.

Polymer stability and degradation is evaluated by determination of polymer oxidation by infrared

spectroscopy in accordance with ISO 10640. The increase in magnitude of features of the infra-red spectra
corresponding to the carbonyl products of polymer oxidation, is recorded as carbonyl optical density. The
period of accelerated thermal ageing where no significant increase in carbonyl optical density (Table 5) is
observed is considered to be representative of the real-time period of product stability in storage
conditions.

Samples 18823/9373 demonstrated no significant oxidation during the accelerated stability test (Table
3/Figure 1). This result is consistent with the sample having undergone no significant degradation.

The absence of degradation in the sample for the duration of this test confirms that the product is stable
in dark conditions, at ambient temperatures for an initial life period corresponding to the product life.

Sample 18823/9374 demonstrated a significant increase in carbonyl optical density measurement at the
conclusion of the test (Table 3/Figure 1). This result is consistent with the sample having undergone
significant degradation.

The observation of degradation of the sample shows that the product is not stable to thermal ageing. This
indicates that the product is vulnerable to premature degradation.

The use of product formulation designed provide a greater extent of stabilisation will be likely to extend
the shelf-life of this product.

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Table 3: Carbonyl Optical Density During Accelerated Thermal Ageing

ΔCarbonyl Optical Density (IR Abs 1714 cm-1/Thickness)
Accelerated Ageing Time (AAT)
18823/9373 18823/9374
0 hrs 0.0000 0.0000
42 hrs 0.0000 0.0000
71 hrs 0.0000 0.0000
234 hrs 0.0000 0.0003
336 hrs 0.0001 0.0009
405 hrs 0.0000 0.0016
500 hrs 0.0001 0.0028
525 hrs 0.0000 0.0031
573 hrs 0.0001 0.0041

Figure 1: Carbonyl Optical Density During Accelerated Thermal Ageing

0.0500

0.0450

0.0400
IR Abs 1714 cm-1/Sample Thickness (µm)

0.0350
ΔCarbonyl Optical Density

0.0300

0.0250

0.0200

0.0150

0.0100

0.0050

0.0000

-0.0050
0 hrs 100 hrs 200 hrs 300 hrs 400 hrs 500 hrs 600 hrs 700 hrs
Thermal Ageing | Accelerated Ageing Time (AAT)

18823/9373 18823/9374 Spontaneous Embrittlement (COD = 0.01, 1x/100)

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3.2.2 Thermal Degradation, Following Initial UV Exposure

Polymer degradation in dark conditions, following initial exposure to sunlight is evaluated in a shorter
period of time in the laboratory by monitoring degradation during accelerated fluorescent UV ageing in
accordance with ASTM D5208 followed by thermal ageing at elevated temperatures according to ASTM
D5510.

Polymer degradation is evaluated by determination of polymer oxidation by infrared spectroscopy in

accordance with ISO 10640. The increase in magnitude of features of the infra-red spectra corresponding
to the carbonyl products of polymer oxidation, is recorded as carbonyl optical density. An increase in
carbonyl optical density of 0.0100 corresponds to a >95% reduction in mechanical properties and is
therefore considered indicative of advanced degradation as such to bring about spontaneous
embrittlement (Table 5). The rate of degradation is evaluated and compared by monitoring carbonyl optical
density as a function of ageing time.

3.2.2.1 48 hours Initial UV Exposure

The samples were initially exposed to constant fluorescent UV ageing for a period of 48 hours. The
samples were then exposed to accelerated thermal ageing in dark conditions.

A carbonyl optical density value of ≥0.0100 is consistent with oxidation and molecular weight reduction of
the polymer film sufficient to bring about a substantial reduction in mechanical properties (Table 5), this
together with an observation of spontaneous embrittlement of the sample is sufficient to confirm an
absolute elongation at break of 5% or less, according to ASTM D3826.

Sample 18823/9373 demonstrated no significant increase in carbonyl optical density throughout the test
(Table 4/Figure 2). This result is consistent with this sample having undergone no significant degradation.

Sample 18823/9374 demonstrated a significant increase in carbonyl optical density (Table 4/Figure 2).
This result is consistent with this sample having undergone significant degradation. However, the sample
failed to meet the degradation endpoint (carbonyl optical density value of ≥0.0100) indicative of advanced
degradation.

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Table 4: Carbonyl Optical Density During Accelerated Thermal Ageing, Following 48 hours Initial UV Exposure
ΔCarbonyl Optical Density (IR Abs 1714 cm-1/Thickness)
Accelerated Ageing Time (AAT) Exposure
18823/9373 18823/9374
0 hrs 0.0000 0.0000
UV
48 hrs 0.0002 0.0009
94 hrs 0.0000 0.0039
168 hrs 0.0002 0.0071
263 hrs 0.0001 0.0086
Thermal
336 hrs 0.0002 0.0080
387 hrs 0.0001 0.0086
436 hrs 0.0002 0.0087

Figure 2: Carbonyl Optical Density During Accelerated Thermal Ageing, Following 48 hours Initial UV Exposure
0.0500

0.0450

0.0400
IR Abs 1714 cm-1/Sample Thickness (µm)

0.0350
ΔCarbonyl Optical Density

0.0300

0.0250

0.0200

0.0150

0.0100

0.0050

0.0000

-0.0050
0 hrs 100 hrs 200 hrs 300 hrs 400 hrs 500 hrs 600 hrs 700 hrs
UV + Thermal Ageing | Accelerated Ageing Time (AAT)
18823/9373 18823/9374
End of UV Exp. (48 hrs) Spontaneous Embrittlement (COD = 0.01, 1x/100)

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4.0 TEST METHODOLOGY

4.1 FT-IR Spectroscopy

4.1.1 Polymer Oxidation

For determination of polymer oxidation, the infrared (IR) spectra are recorded by transmission, in
accordance with ISO 10640 using a Thermo Scientific Nicolet iS10 Fourier transform infrared (FT-IR)
Spectrometer fitted with a transmission accessory. Spectra are collected across the range 650 to 4,000
cm-1, ≥16 scans, with a resolution of 4 cm-1.

4.1.1.1 Carbonyl Optical Density Calculation

The extent of oxidation is reported as the carbonyl optical density, a function of the net increase in infrared
carbonyl (C=O) absorbance at 1714 cm-1 during ageing, per unit of the path length (sample thickness in
µm):

𝐼𝑅 𝐴𝑏𝑠1714 𝑐𝑚−1
Equation 1: 𝐶𝑎𝑟𝑏𝑜𝑛𝑦𝑙 𝑂𝑝𝑡𝑖𝑐𝑎𝑙 𝐷𝑒𝑛𝑠𝑖𝑡𝑦 = 𝑇ℎ𝑖𝑐𝑘𝑛𝑒𝑠𝑠 (µ𝑚)

4.1.1.1.1 Extent of Oxidation, Interpretation of Carbonyl Optical Density

The carbonyl optical density value may be interpreted to indicate the approximate extent of degradation
of polyolefin films, according to Table 5.

Table 5: Carbonyl Optical Density, Indicated Extent of Degradation

Carbonyl Optical Density Extent of Degradation

0.000 No significant degradation

0.001 ~50% reduction in mechanical properties (EaB)

Spontaneous Embrittlement,
0.010
~>95% reduction in mechanical properties (EaB)

≥0.030 Significant Biodegradability

4.2 XRF Spectroscopy

The XRF spectrum of each unaged sample is recorded using a Bruker S2 Puma Series 2 benchtop
spectrometer in air over 120 s live time, using an Ag X-ray anode and graphene window detector, with a
40.00 kV voltage, automatic current settings (300 kcps), and a 500.0 µm aluminium filter. Film samples
were prepared in 38 mm diameter HDPE XRF sample cups and the total thickness made up to ~200 µm
with 36 mm discs cut from the bulk material using a James Heal 230/10 sample cutter.

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4.2.1 Determination of Prodegradant Catalyst

The concentration of prodegradant catalyst metal cations is quantified by correlation with a calibration of
validated reference samples.

4.3 Accelerated Ageing Exposure

4.3.1 Sample Preparation/Holders

35 x 90 mm film samples were cut using a scalpel and secured in a sample holder with four exposure
windows.

4.3.2 Thickness Determination

The thickness of the sample material is determined before ageing using a digital electronic micrometer, in
not less than four random locations across the test sample and the average value recorded.

4.3.3 Accelerated Thermal Ageing

Thermal ageing of the samples was carried out in a Memmert UFE 600 fan assisted oven at a temperature
of 70ºC in accordance with ASTM D5510 Procedure B: Forced Ventilation Oven.

4.3.3.1 Thermal Stability Real Time Exposure Prediction

The real-time period (RT) at ambient temperature (TRT) represented by accelerated ageing time (AAT) at
elevated accelerated ageing temperature (TAA) is predicted in accordance with ASTM F1980 using the
relationship outlined in Equation 2.

The calculation is performed using an anticipated average storage exposure temperature (TRT) of 30°C
and a conservative ageing factor (Q10) of 2.

𝑅𝑇
Equation 2: 𝐴𝐴𝑇 =
𝑄10 [(𝑇𝐴𝐴−𝑇𝑅𝑇 )/10]

4.3.4 Accelerated Fluorescent UV Ageing

Samples were exposed to ultraviolet radiation in accordance with ASTM D5208 in a Q Panel QUV/se test
apparatus fitted with UVA 340 lamps, set to a black panel temperature of 50ºC and irradiance of 0.78
W/m2/nm @ 340 nm.

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5.0 REPORT HISTORY

Date Report Ref. Author Comments

Previous Version
10/09/2024 18823/001 YB Prodegradant content report

Current Version – this report supersedes all previous versions

07/10/2024 18823/002 YB Added accelerated ageing data

6.0 REPORT AUTHORISATION

Author: Digitally signed by Yasmine Benjelloun

DN: cn=Yasmine Benjelloun, o=Symphony
Yasmine Benjelloun Environmental Ltd., ou=Junior Scientist ,
BSc (Hons) [email protected], c=GB
Junior Scientist Date: 2024.10.07 10:25:55 +01'00'

The information presented in this report is based on the material tested. Performance of finished products depends on their formulation, the
conditions under which, and length of time for which the additives and finished product is stored, and on the method of manufacture of the finished
product, and the heat, light, stress, and other conditions to which the finished product is exposed. Nothing in this report constitutes or implies a
license to use Symphony's intellectual property.

Declaration of Authenticity

Unless otherwise stated in writing, this document is issued by Symphony Environmental Ltd. This report is prepared solely for the use of the
client(s) named in this document. As the author or a co-author of this document, I (we) declare that this report has been composed and authorised
by myself (ourselves) and is an original document. All information and results herein are correct at the time of publication to the best of our
knowledge. Under no circumstance shall any alterations be made to this document, and this document shall not be reproduced in full or in part.

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