TECHNOLOGY ASSESSMENTEcoPure

Biodegradation-Promoting Additive System

A scientifically documentable assessment of the EcoPure biodegradation

technology: test methods, results and most likely biodegradation mechanism

EcoPure Technology Assessment

CE TECH CONSULTING, INC. (www.ce-technologies.com)

Resin and Compound Development and Specification Material/colorant/additive qualification, specification, etc. Raw material cost reduction/material substitution State-of-the-art resins, elastomers, fillers, additives, etc.

Product Design, Development and Performance Testing Product benchmarking and competitive/new product performance testing Product design and engineering through affiliation with Trendscape, LLC Tooling engineering and design through affiliation with APAC Sourcing

Material Analysis Failure analysis/forensic analysis Reverse engineering

Resin/colorant/additive Sourcing Global energy/resin market analysis and reporting Raw material purchasing guidance Identification of sources of lower cost materials

Auxiliary Services Expert witness Patent review/estate preparation M&A assessments

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EcoPure Technology Assessment

CE TECH CONSULTING, INC. (www.ce-technologies.com)Partial Client Listing

Consumer Product Companies NewellRubbermaid (Rubbermaid; Sanford; Levellor; Graco) Kimberly Clark WearEver AnchorHocking ClearChoice The Onecare Company Home Products International

Industrial Product Companies Colson Caster/Colson Plastics/RC Tenn Rehrig International Macro Plastics Otto Environmental Systems Hilex Poly Co.

Investment Banking/Venture Capital Angelo, Gordon & Co. Alix Partners Protostar Partners

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Resin Majors ConnectionsExxonMobilINEOSChevron PhillipsMA HollandLyondellBasell

Technology Center ConnectionsGA Tech Research Institute (GTRI)Southwest Research Institute (SwRI)

EcoPure Technology Assessment

Charles J. Lancelot, PhD (Princeton University; 1971)

CE Tech Consulting, Inc; Founder and General PartnerSpecialize in materials technology, including commodity and engineering

plastics and processes as well as thermoplastic and other rubbers; polymer material testing;resin sourcing; competitive analysis; failure analysis.

Ansell International, Protective Prod. Div.; VP of Technology and Business Development Global R&D reposnsibility for a $300MM industrial glove and protective

apparel business. Increased new product sales from 4% of total sales in 1994 to 15% by 1996.

Rubbermaid Comm. Prod. Inc. Director, Technology and Bus. Dev.; Waste Systems R&D responsibility for an overall $110MM annual business volume, and

accountable for the generation of $10-12MM in sales of new plastic products annually; more than doubled new product sales in 1995 over the prior year.Director, Materials and Process Technology; responsible for new products

and cost reductions; implemented a closed-loop LLDPE recycling business.

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TECHNOLOGY ASSESSMENTEcoPure

What is EcoPure and how does it differ from other available technologies.

EcoPure is a Unique Additive for Conventional Resins

EcoPure is not a new, biochemically synthesized polymer like PLA or the PHA (eg: Mirel) series where:

Part performance, especially toughness, is not always at desired levels. Despite claims, repeated microwavability is tenuous at best. The full Life Cycle Inventory (LCI) it is not as favorable as is that of PP. Must be recycled in a separate stream; PLA now has its own number: 10. More expensive and heavier (density >1.2 vs. PP at 0.905 and HDPE at 0.95-0.96).

EcoPure is not an oxo-biodegradation- or uv degradation-promoting additive that initiates a chemical pre-decomposition of the host resin to species that can be subsequently biologically attacked, but that:

Can kick off prematurely, limiting part shelf life and in-use performance, and as such, Can affect the recyclability of parts when they enter the recycle stream. Typically incorporate transition metals or other catalysts that may not be environmentally

friendly.

EcoPure is not a starch-based additive or blended resin system that is partially biodegradable, but that

Most often degrade certain resin physical properties; products are typically very brittle. Can only be processed with great difficulty; difficult to avoid scorching. Most often are very moisture sensitive further aggravating processing problems and

creating difficulties in use. Can affect the recyclability of the product in the recycle stream.

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EcoPure is a Unique Additive for Conventional Resins

EcoPure is an additive that does not modify the conventional base resin to which it is added:

It is a proprietary blend of organic compounds that are melt-compounded into a masterbatch carrier resin, which is then pelletized.

The masterbatch is subsequently melt-blended into the final base resin (PE; PP; PS; PET) by the enduser in manufacturing the biodegradable product.

Base resin and product retain all of their original properties and shelf life. Recyclability of the part is completely unaffected; recycling number remains the same.

EcoPure initiates and promotes solely a biodegradation process, and does so only in the presence of microorganisms.

polymer alteration only commences when the material is exposed to an active biomass in a moist environment, such as in an active landfill.

In a landfill, the EcoPure blend causes three things to happen: Renders the hydrophobic (water-repellent) base resin much more hydrophyllic,

facilitating the formation and intimate adhesion of a moisture-borne biofilm. Attracts and initiates the growth of microorganisms within the biofilm that can

acclimatize to the base polymer as the primary nutrient source. Promotes the active and vigorous growth of the adapted microorganisms.

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EcoPure Technology Assessment: Approach

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ASTM D5511-11 Anaerobic Digestion Test

This method determines the degree of anaerobic biodegradation of plastic materials in a high-solids anaerobic environment.

High solids conditions are usually considered to be greater than 20% solids. The test sample is exposed to a methanogenic inoculum cultivated from a

wastewater treatment facilitys anaerobic digesters operating on household waste. The digester test conditions remain static.

This test method involves measuring the volume of carbon dioxide (CO2) and methane (CH4) evolved over time from the biodegradable test sample relative to a positive control (typically cellulose), a negative control (typically the same resin lacking the EcoPure additive), and the inoculum alone.

At the conclusion of the test, the remaining solid test sample mass and control sample masses are determined by weight.

This method is considered an accelerated representation with respect to a typical active landfill environment.

EcoPure Technology Assessment: Approach

ASTM D5511-02 Anaerobic Digestion Test

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ASTM D5511-02 Results: LLDPE/LDPE Blend

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ASTM D5511-02 Results: Extruded PS Foam

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ASTM D5511-02 Results: Extruded PS Foam

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The digesters were allowed to continue running under incubation for three additional weeks, after which the sample residues were harvested for cleaning and residual mass determination.

The residual mass data below confirm the gas evolution data but also reflect the additional degradation that had occurred to the time of residue harvest, in that the average residue mass loss was 9.07% vs. 5.09% degradation as measured by gas evolution.

These weights could be lower limits since it is probably impossible to remove 100% of the adhered biomass.

ASTM D5511-02 Results: PETE

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ASTM D5511-02 Results: Polypropylene (PP)

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Positive Control PP

GPC Cut

TECHNOLOGY ASSESSMENTEcoPure

Perform a standard laboratory analytical technique to probe for

actual macromolecular degradation: Gel Permeation

Chromatography (GPC)

Independent Confirmation: Gel Permeation Chromatography (GPC)

Plastic materials are composed of an array of long-chain polymer molecules of varying length. In general, the longer the chains, the tougher the plastic.

Cutting the chain lengths will degrade the plastic. This can happen by the action of excessive heat during product manufacture or use, by the action of air or sunlight unless properly stabilized, and normally in certain plastics only, by the action of microorganisms.

There are several analytical techniques used to look for cutting of the long chains. These are frequently used in forensic analysis of product failure, competitive material or product analysis, etc.

One technique actually separates the chains by length in solution and gives measures of these lengths and the distribution of the various lengths. It is called Gel Permeation Chromatography (GPC).

GPC depends on the selective entrapment of polymer molecules in the micropores present in the gel particles in a column. As the polymer solution passes down the column, the individual molecular chains get stuck more or less deeply in the micropores depending on their size, the smaller the deeper. The longer chains pass by and are eluted first, and so on to the shortest chains which get out last.

The result is a bell-shaped curve showing the distribution of chain lengths, which is mathematically analyzed and the molecular weight ranges reported.

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Independent Confirmation: Gel Permeation Chromatography (GPC)

The bell-shaped curve gives you the number of chains (Ni) of each length (or weight) (Mi) in the array of polymer molecules. What is reported is: Number average molecular weight (Mn): divide the total weight of the sample by the

total number of the molecules. Mn = NiMi/Ni Weight average molecular weight (Mw): calculate weight fraction Wi = NiMi/NiMi

Then Mw = WiMi. Molecular weight distribution (MWD) = Mw/Mn; breadth of bell curve.

When polypropylene (PP) treated with Eco-Pure was examined by GPC both before and after exposure to the conditions of the ASTM D5511-02 test after45 days (p.14), both Mn and Mw were reduced by 40%, and the MWD was broadened. This indicates that polymer degradation has occurred through the action of the microorganisms, and that it has occurred on chains of all lengths in the original plastic material matrix.

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PP with EcoPureExposed to D-5511

PP with EcoPureNot exposed to

D-5511

Independent Confirmation: Gel Permeation Chromatography (GPC)

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TECHNOLOGY ASSESSMENTEcoPure

The likeliest mechanisms by which EcoPure is achieving

significant polymer biodegradation.

A General View of the Workings of EcoPure

As mentioned above (p. 7), our understanding is that in a landfill or other biomass-containing environment, the EcoPure blend causes three things to happen:

Renders the hydrophobic (water-repellent) base resin much more hydrophyllic, facilitating the formation and intimate adhesion of a moisture-borne biofilm.

Attracts and initiates the growth of microorganisms within the biofilm that can acclimatize to the base polymer as the primary nutrient source.

Promotes the active and vigorous growth of the adapted microorganisms.

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A General View of the Workings of EcoPure

Renders the hydrophobic (water-repellent) base resin much more hydrophyllic, facilitating the formation and intimate adhesion of a moisture-borne biofilm. Close adhesion of a biofilm to the substrate in many cases is a pre-

requisite to microorganism acclimatization; mobility throughout the polymer is also a factor.

Virtually all plastic resin surfaces are by their nature hydrophobic; this is particularly true of polyolefins, to which very little of anything adheres without some form of pre-treatment (corona; flame; etc.)

EcoPure functions much as a surface-active agent in rendering the resin hydrophyllic, and being also hygroscopic in nature, retains moisture, promoting the approach and adhesion of a moisture-borne biofilm composed of the micro-organisms present in biologically active landfills, composters, etc.

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A General View of the Workings of EcoPure

Attracts and initiates the growth of microorganisms within the biofilm that can acclimatize to the base polymer as the primary nutrient source.

Largely aerobic environment near landfill surface; largely anaerobic down deeper. Moisture is essential of course.

Likeliest points of attack on hydrocarbon polymers are at or near the chain ends, as they are sterically accessible. Resins such as PP and PE are in a fully saturated (reduced) state; review of the literature indicates that an enzymatically-catalyzed oxidation process is occurring, placing olefinic, aldehyde, ketone, carboxylate or similar functionality in place. This can happen aerobically as well as anaerobically in the presence of a chemical oxygen source (alcohols, acids, etc.).

The literature also suggests that polystyrene degrades as well via oxidative attack and ring opening of the benzene rings in the polymer.

In heteropolymers, enzymatically catalyzed hydrolysis will most likely occur first at the ester (polyesters) or amide (polyamides) linkages to start a more general process.

In any event, most likely a syntrophic environment is established, requiring the establishment of multiple strains of acclimatized bacteria to accomplish these complex chemical steps.

Elements of EcoPure appear to attract and promote the establishment of such syntrophic biomass venues that eventually acclimatize to the resin as the primary and/or sole nutrient source.

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A General View of the Workings of EcoPure

Promotes the active and vigorous growth of the adapted microorganisms, through a bacterial communication process known as quorum sensing.

Quorum sensing involves the regulation of gene expression in response to fluctuations in cell-population density. Quorum sensing bacteria produce and release chemical signal molecules (auto-inducers) that increase in concentration as a function of cell density. The detection of a minimal threshold stimulatory concentration of an autoinducer leads to an alteration in gene expression. Although the nature of the chemical signals, the signal relay mechanisms, and the target genes controlled by bacterial quorum sensing systems differ, in every case the ability to communicate with one another allows bacteria to coordinate the gene expression, and therefore the behavior, of the entire community.It would certainly appear that the adapted biomass that has begun to thrive on the EcoPure-treated polymer system then multiplies more rapidly by a process such as quorum sensing .

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ASTM D5511-02 Results: Polypropylene (PP)

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Positive Control PP

GPC Cut

SUMMARY

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EcoPure is an additive that does not modify the conventional base resin to which it is added. The latter retains all its original properties and shelf life.

EcoPure is a proprietary blend of organic compounds that are melt-compounded into a masterbatch carrier resin, which is then pelletized.

EcoPure initiates and promotes solely a biodegradation process, and does so only in the presence of microorganisms.

Testing in a high-solids anaerobic environment (ASTM D5511 test) has shown up to 37% conversion of the total carbon in polypropylene (PP) to methane and CO2in 90 days and a 40% reduction in molecular weight as measured by GPC after 45 days.

EcoPure renders normally water-repellent polymers more hydrophyllic, attracting and promoting the intimate adhesion of the prerequisite biofilm.

The additive system then facilitates the growth of syntrophic colonies of diverse microorganisms that degrade hydrocarbon polymers through an enzymatically-catalyzed oxidative process (PP; PE) as well as by oxidative ring-opening (PS).