ASTM D 6400: Determing Aerobic Biodegradation of Plastic Materials Under Controlled Composting Conditions

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TEL: 831-724-5422

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ASTM D 6400
Determing Aerobic Biodegradation of Plastic
Materials Under Controlled Composting Conditions

Work Order #:
0020396-01

Report Prepared For:


Aseem Das
World Centric
2121 Staunton Court
Palo Alto, CA 94306

Tested By:
Soil Control lab
42 Hangar Way
Watsonville, CA 95076
U.S.A.
phone: 831-724-5422
www.compostlab.com

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Table of Contents
Page #
Section 1.) Summary of Test Results 3

Section 2.) Preliminary Test, Part I - Heavy Metals 5

Section 3.) Prelimary Test, Part II - Ash, Thickness, 6


and Summary of FTIR & Biobased Testing

Section 4.) Results of Disintegration & Plant Growth Studies 7

Section 5.) Results of Biodegradability 8

Appendix A - Test Method Description 10

Appendix B - Information on the Inoculum Used 12

Appendix C - QC Evaluation of Batch 13

Appendix D - Raw Data from Biodegradation Study 14

Appendix E - Pictures of Disintegration Study 21

Appendix F - FTIR Report (sub-contracted) 32

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Account #: 5991
Date Reported: October 1, 2010
Aseem Das
World Centric
2121 Staunton Court
Palo Alto, CA 94306

Summary of Results from Compostability Testing


Product Tested: Sample Product Box Custom, 100 KN-PS-6, Knives
Thickness of Material: The thickest portion of the material is 2.68 mm

Summary of Results: The product met all the requirements to be considered "compostable"
as judged by the United States standard ASTM D 6400.

Description of requirements to pass ASTM D 6400:


To be considered “compostable” by either ASTM D 6400 the product must demonstrate
the three following items:
1.) Disintegration
• After starting with the product cut to 2cm lengths, in 12 twelve weeks of
composting under laboratory controlled composting conditions 90% of the
product must pass a 2mm sieve.
2.) Biodegradation
• 60% of the organic carbon must be converted to carbon dioxide by the
end of the test period, when compared to the positive control (cellulose).
3.) No Adverse Effects on the Quality of the Compost
• Plant Growth
The germination rate and the plant biomass of the sample composts shall
be no less than 90 % that of the corresponding blank composts for two
different plant species following OECD Guideline 208 with the
modifications found in Annex E of EN 13432.
• Heavy Metals - see the table on the following page for levels that are
acceptable based on geographical region.

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Table 1: Acceptable Levels of Heavy Metals based on Geographical Region


Limits for US Limits for Canada Limits for Europe Limits for Japan
Analyte (ppm) (ppm) (ppm) (ppm)
Arsenic (As) 21.5 37.5 5 5
Cadmium (Cd) 19.5 10 0.5 0.5
Copper (Cu) 750 NA 50 60
Lead (Pb) 150 250 50 10
Mercury (Hg) 8.5 2.5 0.5 0.2
Nickel (Ni) 210 90 25 30
Selenium (Se) 50 7 0.75 NA
Zinc (Zn) 1400 925 150 180
Cobalt (Co) NA 75 NA NA
Chromium (Cr) NA NA 50 50
Molybdenum (Mo) NA 10 1 NA
Fluorine (F) 100 100 100 NA
Notes:
Metal limits for US are 50% of those proscribed by CFR 503.13 Table 3 (per ASTM 6400 requirements).
Metal limits for Canada are 50% of those proscribed in Table II of “Standards for Metals in Fertilizers and Supplements”.
Fluorine level is consistent with EU regulations.

Results for this product:


Disintegration - Passed
• 92% of the sample passed the 2mm sieve after 12 weeks of composting
Biodegradation - Passed
• It took 119 days for 69% of the organic carbon in the material being tested to be converted
to carbon dioxide when compared to the positive control (cellulose), thus meeting the standard of 60%.
• ASTM D 6868 & EN 13432 standards require 90% biodegradation - it took 140 days for 93% of the
organic carbon in the material being tested to be converted to carbon dioxide when compared to the
positive control (cellulose), thus meeting the standard of 90%.
• End of test - the testing was stopped after 175 days, the cumulative carbon dioxide production was 103%.
No Adverse Effects on Compost Quality - Passed
• Plant Growth Study - Passed. Corn showed 100% emergence and 112% biomass; cucumber showed 99%
emergence and 93% biomass.

• Heavy Metals - The heavy metals results meet the standards for the US, Canada, Europe, and Japan.

Sincerely,

Mike Galloway
Lab Director
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Heavy Metals Concentration


Product Name: Sample Product Box Custom, 100 KN-PS-6, Knives
Portion of Product Analyzed: Whole Sample

Results
mg/Kg Reporting Pass or Fail of Standards by Region
Analyte dry weight Limit US Canada Europe Japan
Arsenic (As) ND 0.5 Pass Pass Pass Pass
Cadmium (Cd) ND 0.5 Pass Pass Pass Pass
Copper (Cu) ND 0.5 Pass NA* Pass Pass
Lead (Pb) ND 0.5 Pass Pass Pass Pass
Mercury (Hg) ND 0.2 Pass Pass Pass Pass
Nickel (Ni) ND 0.5 Pass Pass Pass Pass
Selenium (Se) ND 0.5 Pass Pass Pass NA*
Zinc (Zn) 7.4 0.5 Pass Pass Pass Pass
Cobalt (Co) ND 0.5 NA* Pass NA* NA*
Chromium (Cr) ND 0.5 NA* NA* Pass Pass
Molybdenum (Mo) ND 0.5 NA* Pass Pass NA*
Fluorine (F) ND 10 Pass Pass Pass NA*

The analyses above were conducted in-house by Soil Control Lab using the following methods.
As & Se - Digestion EPA 3050B, Analysis EPA Method 6020 (ICPMS)
Cd, Cu, Pb, Ni, Zn, Co, Cr, & Mo Digestion EPA 3050B, Analysis EPA Method 6010 (ICP-AES)
Mercury (Hg) by EPA 7471 (Cold Vapor)
Fluorine (F) by EPA 300.0 (IC)

Also, please note: The criteria for Pass/Fail for each region are listed in the "Summary of Results from"
"Compostability Testing" Section of the Report (earlier in this report).

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Date Reported: October 1, 2010

Preliminary Tests, Part II - FTIR, Ash, Thickness


(and Biobased if tested)
Product Name: Sample Product Box Custom, 100 KN-PS-6, Knives

Layer/Material:
Ash Content: 29.3%
Thickness: 2.68 mm
FTIR Summary (Full FTIR Report Attached in Appendix F): The following is a quote from the report
"In our opinion, the spectrum for Sample A verifies that the Cutlery is composed of a modified bio-
polyester. Talc was also found to be in the compostion. the cutlery spectrum matches closely to that
of Nature Works PLA."

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Disintegration Study

Product Name: Sample Product Box Custom, 100 KN-PS-6, Knives


Portion of Product Analyzed: Whole product broken down in 2cm x 2cm squares

% Passing
Week 2mm sieve Criteria Pass/Fail

12 92 greater than 90 % Pass

Pictures of the disintegration study can be found in Appendix E.

Plant Growth Study


Portion of Product Analyzed: Whole product after it had been put through the disintegration test

Plant Species % Emgerence % Biomass Pass/Fail

Cucumber 25% compost 99 93 Pass


50% compost 96 72 NA*
Corn 25% compost 100 112 Pass
50% compost 95 88 NA*

*It should be noted that both plant species were affected at the higher concentrations of the compost,
but at the 25% compost concentration the plants did fine. This is typical of what we tend to see.

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Biodegradation Study

Product Name: Sample Product Box Custom, 100 KN-PS-6, Knives


Number of layers/material tested for above mentioned product: 1

Layer/Material Number 1 of 1
Layer/Material Analyzed: Whole Sample

Amount of Carbon Converted to Carbon Dioxide


(as compared to cellulose as the positive control)

Day % Converted to CO2

0 0
7 -2
14 1
21 0
28 0
35 -1
49 4
56 3
63 10
70 15
77 24
84 27
91 35
98 44
105 54
119 69
126 81
133 88
140 93
147 96
154 97
161 99
168 101
175 103

Please see following page for a graph of the results.

Pg. 8
% of Organic Carbon Converted to Carbon
Dioxide as Compared to Cellulose
Whole Sample
110
100
90
% Biodegradation

80
70
60
50
40
30
20
10
0
0

14

28

42

56

70

84

98

112

126

140

154

168
Days
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Description of Test Procedure


Description of the Equipment Used:
A temperature controlled incubator capable of holding it's temperature at 58°C ± 2°C over the entire length
of the test procedure. Cylinderical composting vessels that have a capacity of 7.5 liters each. The
containers are sectioned into two parts using a porous pad so that the top section has a volume of 6 liters.
One liter of water is placed in the bottom section and the test material in the top. Carbon dioxide free air is
bubbled through the water to saturate the air with water, then through the porous pad, into the main test
chamber, then out of the top.

Description of the Test Procedure (how we executed ASTM D 5338) :

Inoculum: A suitable 3 month old stable compost from the Monterey District composting facility is used for
the inoculum. The compost is sieved through a 9.5mm sieve and then mixed. When we are ready to use it,
we add ammonium chloride so that the C/N ration is less than 15 plus the appropriate volume of water to
adjust the moisture content to 50%.
Disintegration Test: The "Disintegration Testing" and the "Biodegradation Testing" are tested separately,
but in the same incubator. For the disintegration test we conduct ASTM D 5338 without the CO2 trapping
componento the method. We start off with 200g of 2cm X 2cm squares of the product being tested and
add it to 1200g of compost and put the mixture in the composting vessels as described in the "Equipment"
section above. The mixture is composted for 12 weeks at 58°C ± 2°C. The composting vessel is shaken
weekly to mix the sample & compost and to prevent extensive channelling, provide uniform attack on the
test specimen, and provide an even distribution of moisture. Any observations made by the analyst are
recorded, such as "material starting to appear grainy & brittle". Also, pictures are taken at key times to
visually document the products progress during the study. At the end of 12 weeks material is emptied from
the composting vessels and screened through a 2mm sieve. In order to pass this test, no more than 10%
of the original dry weight of the product can be retained on the sieve.

Biodegradation Test: The biodegradation testing has to be conducted in triplicate on each of the
following: 1.) the sample (100g of sample + 600g dry weight of compost), 2.) positive control (100g of
cellulose + 600g dry weight of compost), 3.) negative control (100g of polyethylene + 600g dry weight of
compost), 4.) blank (600g dry weight of compost). The moisture content of the mixtures is adjusted to
50%, then they are put into the composting vessels as described in "Equipment" above. The composting
vessels are placed in the incubator at 58°C ± 2°C. The CO2 free air is then connected and adjusted so
that the flow rate is between 150 and 200 ml per minute. The gases exiting the test chambers are plumbed
to a solenoid valve which is controlled to divert air for 2 minutes out of every 2 hours. These diverted
gases flow into 1 liter adsorption units containing a known volume of 1N sodium hydroxide to adsorb the
carbon dioxide being produced in the vessels (for the remainder to the 2 hours the exhaust is simply
vented to the room).
The sodium hydroxide is periodically titrated to measure the CO2 production; our standard days for the
titration are 3, 7, 14, and every 7 days after that. We titrate to pH 8.5 with 0.5N HCl after adding BaCl2 to
precipitate the carbonates formed by the CO2. Fresh 1N sodium hydroxide is placed in the absorption
units and the whole process is repeated. The testing is carried out until the CO2 production from both the
sample and the positive control have plateaued up to a maximum of 180 days.
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Description of Test Procedure (continued)

Plant Growth Study:


The pots used were cups with clear plastic covers, which holds in moisture, thus reducing the need to
water which could lead to leaching of phytotoxins out of the material being tested.
Several dilutions are made by diluting the sample with vermiculite; the same dilutions are also conducted
on the positive control (cellulose). The dilutions are necessary because compost is not a good a potting
mix due to excess salts and excess nutrients. Triplicates of each dilution were made and all were
seeded. The highest concentration of the control that produced healthy plants was used for interpreting
the results. The method that this is based off of is OECD Guideline 208 with the modifications found in
Annex E of EN 13432.
The method is the same for all seeds except Farm Lawn which is described in the next paragraph. Seeds
are counted when planted and percent germination is determined using percent germination of the control
as 100 percent. The average height of healthy plants is used to determine biomass.
Farm Lawn (this species is not always used): A half gram (500mg) of seed was planted into each cup. A
plant density scale was developed using 0, 100, 200, 300, 400, and 500 mg of seeds in a series of cups
and given an index of 0, 1, 2, 3, 4, 5 respectively to be used in determining percent germination. The
index value of the control is considered 100 percent germination when determining the index of the
sample. Biomass is based on average height of healthy plants.

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Description of Inoculum Used


Inoculum: A suitable 3 month old stable compost from the Monterey District composting facility was
used for the inoculum. The compost was sieved through a 9.5mm sieve and then mixed. Before using it,
we added ammonium chloride so that the C/N ration was approximately 15 plus the appropriate volume of
water to adjust the moisture content to 50%.

pH at start of tests = 7.4

pH at end of tests = 7.3

% dry solids = 37%, but adjusted to 50% for test

% volatile solids = 45% on a dry weight basis

Total Nitrogen = 1.4% on a dry weight basis, but added 8 grams of NH4Cl to each composting
vessel/reactor (containing 600g dry weight of compost) to lower C/N ratio to 15.

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Evaluation of QC Criteria for the Analytical Batch


Carbon Dioxide production of the inoculum for the first 10 days:
Our result = 60mg (suggested range is 50-150mg)

At day 45 cellulose must have converted 70% or more of it's carbon to CO2 and the standard
deviation of the % converted at the end of the test must be below 20%
Our result = 72.4% at 45 days, 82.5% at the end, and a standard deviation of 5.0%

At the end of the test the pH of the compost + sample material must be greater than 7.0.
Our results = 7.3

Incubator must be maintained at 58 deg C +/- 2 deg C.


Temperature was maintained within limits through out the testing.

Satisfactory appearance, odor, & moisture content must be maintained in all composting vessels.
We were able to accomplish this throughout the study.

Pg. 13
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Carbon Dioxide Production from Inoculum


Measured production (gm) Cumulative production (gm)
Day Reactor 1 Reactor 2 Reactor 3 Day Reactor 1 Reactor 2 Reactor 3
0 0.00 0.00 0.00 0 0 0 0
7 41.45 39.64 43.19 7 41 40 43
14 23.71 29.28 27.11 14 65 69 70
21 2.71 9.62 6.26 21 68 79 77
28 2.22 1.02 2.47 28 70 80 79
35 3.28 2.61 2.77 35 73 82 82
49 9.87 8.70 4.77 49 83 91 87
56 3.08 2.91 0.93 56 86 94 88
63 4.87 3.43 5.03 63 91 97 93
70 4.11 3.66 2.87 70 95 101 95
77 4.18 3.94 4.18 77 99 105 100
84 4.11 3.66 2.87 84 104 108 102
91 5.22 3.54 3.92 91 109 112 106
98 5.27 4.53 5.38 98 114 117 112
105 4.51 3.05 5.45 105 119 120 117
119 9.04 5.53 8.42 119 128 125 126
126 5.03 3.28 3.87 126 133 128 130
133 5.08 3.46 4.59 133 138 132 134
140 4.15 2.72 -2.43 140 142 135 132
147 3.61 2.52 3.68 147 145 137 135
154 3.68 2.45 3.65 154 149 140 139
161 6.21 4.99 1.34 161 155 145 140
168 3.52 3.91 3.28 168 159 148 144
175 2.53 2.25 3.36 175 161 151 147

Cumulative Production of CO2 by Inoculum

180

160

140
CO2 Production (gm)

120

100 Series1
Series2
80 Series3

60

40

20

0
0 10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190
Day

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Carbon Dioxide Production from Inoculum plus Cellulose


Measured production (gm) Cumulative production (gm)
Day Reactor 1 Reactor 2 Reactor 3 Day Reactor 1 Reactor 2 Reactor 3
0 0.00 0.00 0.00 0 0 0 0
7 121.77 109.36 112.70 7 122 109 113
14 54.77 46.35 50.68 14 177 156 163
21 14.09 9.81 14.65 21 191 166 178
28 8.11 4.83 4.40 28 199 170 182
35 6.99 4.85 4.06 35 206 175 186
49 10.74 9.02 7.05 49 216 184 194
56 2.63 2.26 1.92 56 219 186 195
63 6.45 5.59 5.87 63 226 192 201
70 4.23 4.74 5.78 70 230 197 207
77 5.10 5.80 4.31 77 235 203 211
84 4.80 5.47 4.66 84 240 208 216
91 7.92 7.69 7.25 91 248 216 223
98 9.49 9.21 9.13 98 257 225 232
105 3.71 3.60 3.96 105 261 229 236
119 12.53 6.59 12.73 119 273 235 249
126 3.58 1.22 2.90 126 277 236 252
133 3.14 1.21 2.58 133 280 238 255
140 2.84 1.74 2.48 140 283 239 257
147 3.83 3.36 3.62 147 287 243 261
154 5.16 3.87 4.97 154 292 247 266
161 5.58 3.99 5.05 161 297 251 271
168 4.96 4.70 4.43 168 302 255 275
175 3.20 3.53 3.34 175 306 259 279

Cumulative Production of CO2 by Inoculum plus Cellulose

350

300

250
CO2 Production (gm)

200 Reactor 1
Reactor 2
150 Reactor 3

100

50

0
0 10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190
Day

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Date Reported: October 1, 2010

Carbon Dioxide Production from Inoculum plus Test Material


Measured production (gm) Cumulative production (gm)
Day Reactor 1 Reactor 2 Reactor 3 Day Reactor 1 Reactor 2 Reactor 3
0 0.00 0.00 0.00 0 0 0 0
7 39.81 39.55 40.65 7 40 40 41
14 25.83 29.21 31.13 14 66 69 72
21 2.66 4.52 9.16 21 68 73 81
28 1.17 1.06 2.76 28 69 74 84
35 3.14 2.81 1.98 35 73 77 86
49 6.98 13.20 14.80 49 80 90 100
56 1.67 3.01 1.09 56 81 93 102
63 6.76 13.34 10.90 63 88 107 112
70 8.12 9.56 8.48 70 96 116 121
77 14.71 10.38 12.79 77 111 127 134
84 7.21 8.30 4.69 84 118 135 138
91 12.95 9.87 14.80 91 131 145 153
98 17.36 12.72 15.21 98 148 158 168
105 15.55 12.85 15.87 105 164 170 184
119 24.75 22.21 25.44 119 189 193 210
126 10.27 25.49 12.24 126 199 218 222
133 8.07 9.03 11.44 133 207 227 233
140 6.12 7.00 8.77 140 213 234 242
147 5.36 5.94 6.91 147 218 240 249
154 6.32 5.72 6.18 154 225 246 255
161 5.14 5.51 8.20 161 230 251 263
168 6.31 6.73 6.21 168 236 258 270
175 5.44 5.45 6.19 175 242 263 276

Cumulative Production of CO2 by Inoculum plus Test Material

300

250
CO2 Production (gm)

200

Reactor 1
150 Reactor 2
Reactor 3

100

50

0
0 10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190
Day

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Carbon Dioxide Production from Inoculum plus Polyethylene


Measured production (gm) Cumulative production (gm)
Day Reactor 1 Reactor 2 Reactor 3 Day Reactor 1 Reactor 2 Reactor 3
0 0.00 0.00 0.00 0 0 0 0
7 41.45 39.64 43.19 7 41 40 43
14 23.71 29.28 27.11 14 65 69 70
21 2.71 9.62 6.26 21 68 79 77
28 2.22 1.02 2.47 28 70 80 79
35 3.28 2.61 2.77 35 73 82 82
49 9.87 8.70 4.77 49 83 91 87
56 3.08 2.91 0.93 56 86 94 88
63 4.87 3.43 5.03 63 91 97 93
70 4.11 9.56 2.87 70 95 107 95
77 4.18 3.94 4.18 77 99 111 100
84 4.11 3.66 2.87 84 104 114 102
91 5.22 3.54 3.92 91 109 118 106
98 5.27 4.53 5.38 98 114 122 112
105 4.51 3.05 5.45 105 119 125 117
119 9.04 5.53 8.42 119 128 131 126
126 5.03 3.28 3.87 126 133 134 130
133 5.08 3.46 4.59 133 138 138 134
140 4.15 2.72 -2.43 140 142 140 132
147 3.61 2.52 3.68 147 145 143 135
154 3.68 2.45 3.65 154 149 145 139
161 6.21 4.99 1.34 161 155 150 140
168 3.52 3.91 3.28 168 159 154 144
175 2.53 2.25 3.36 175 161 157 147

Cumulative Production of CO2 by Inoculum plus Polyethylene

180

160

140
CO2 Production (gm)

120

100 Reactor 1
Reactor 2
80 Reactor 3

60

40

20

0
0 10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190
Day

Pg. 17
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Mean Cumulative Carbon Dioxide Production in Reactors


Cumulative production (gm)
Day Cellulose Sample Polyethylene Enoculum
0 0 0 0 0
7 115 40 41 41
14 165 69 68 68
21 178 74 74 74
28 184 76 76 76
35 189 78 79 79
49 198 90 87 87
56 200 92 89 89
63 206 102 94 94
70 211 111 99 97
77 216 124 103 101
84 221 130 107 105
91 229 143 111 109
98 238 158 116 114
105 242 173 120 118
119 253 197 128 126
126 255 213 132 130
133 257 223 137 135
140 260 230 138 136
147 263 236 141 139
154 268 242 145 143
161 273 248 149 147
168 278 255 152 150
175 281 260 155 153

Mean Cumulative Carbon Dioxide Production in Reactors

300

250
CO2 Production (gm)

200
Cellulose
Sample
150
Polyethylene
Enoculum
100

50

0
0 10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190
Day

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Cumulative Carbon as C Converted to Carbon Dioxide (mean)


Cumulative Production (gm) Cumulative Production( % of Organic C)
Day Cellulose Sample Polyethylene Day Cellulose Sample Polyethylene
0 0.00 0.00 0.00 0 0 0 0
7 19.96 -0.39 0.00 7 48 -1 0
14 26.48 0.16 0.00 14 63 0 0
21 28.29 -0.04 0.00 21 68 0 0
28 29.35 -0.11 0.00 28 70 0 0
35 30.00 -0.18 0.00 35 72 -1 0
49 30.32 0.88 0.00 49 73 3 0
56 30.31 0.78 0.00 56 73 2 0
63 30.72 2.38 0.00 63 74 7 0
70 31.10 3.79 0.54 70 74 11 1
77 31.36 6.12 0.54 77 75 18 1
84 31.75 6.99 0.54 84 76 21 1
91 32.68 9.25 0.54 91 78 27 1
98 33.83 11.99 0.54 98 81 35 1
105 33.67 14.83 0.54 105 81 44 1
119 34.47 19.33 0.54 119 82 57 1
126 34.07 22.58 0.54 126 82 66 1
133 33.50 23.98 0.54 133 80 71 1
140 33.74 25.57 0.54 140 81 75 1
147 33.84 26.34 0.54 147 81 77 1
154 34.22 27.10 0.54 154 82 80 1
161 34.41 27.67 0.54 161 82 81 1
168 34.72 28.45 0.54 168 83 84 1
175 34.89 29.26 0.54 175 83 86 1

Cumulative Carbon Converted to Carbon Dioxide as % of Organic C

100

90

80
CO2 Production (gm)

70

60
Cellulose
50 Sample
Polyethylene
40

30

20

10

0
0 10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190
Day

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Mean Oxygen Consumption in Reactors


Oxygen Consumption (grams per day)
Day Cellulose Sample Polyethylene Inoculum
0 0 0 0 0
7 11.91 4.16 4.30 4.30
14 5.26 2.98 2.77 2.77
21 1.33 0.57 0.64 0.64
28 0.60 0.17 0.20 0.20
35 0.55 0.27 0.30 0.30
49 0.46 0.61 0.40 0.40
56 0.24 0.20 0.24 0.24
63 0.62 1.07 0.46 0.46
70 0.51 0.91 0.57 0.37
77 0.53 1.31 0.43 0.43
84 0.52 0.70 0.37 0.37
91 0.79 1.30 0.44 0.44
98 0.96 1.57 0.53 0.53
105 0.39 1.53 0.45 0.45
119 0.55 1.25 0.40 0.40
126 0.27 1.66 0.42 0.42
133 0.24 0.99 0.45 0.45
140 0.24 0.76 0.15 0.15
147 0.37 0.63 0.34 0.34
154 0.49 0.63 0.34 0.34
161 0.51 0.65 0.43 0.43
168 0.49 0.67 0.37 0.37
175 0.35 0.59 0.28 0.28
175 0.00 0.00 0.00 0.00

Mean Oxygen Consumption in Reactors

14

12
O2 consumption (gram per day)

10

Cellulose
8
Sample
Polyethylene
6
Inoculum
4

0
0 10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190
Day

Pg. 20
TEL: 831-724-5422
FAX: 831-724-3188

Work Order: 0020396-01


Account #: 5991
Date Reported: October 1, 2010

Description of the Pictures


Picture 1 - Product as it was submitted to us

Picture 2 - Disintegration Study at end (12 weeks)

Picture 3 - Plant Growth Study (Corn) - Sample at 25% concentation

Picture 4 - Plant Growth Study (Corn) - Control at 25% concentation

Picture 5 - Plant Growth Study (Corn) - Sample at 50% concentation

Picture 6 - Plant Growth Study (Corn) - Control at 50% concentation

Picture 7 - Plant Growth Study (Cucumber) - Sample at 25% concentation

Picture 8 - Plant Growth Study (Cucumber) - Control at 25% concentation

Picture 9 - Plant Growth Study (Cucumber) - Sample at 50% concentation

Picture 10 - Plant Growth Study (Cucumber) - Control at 50% concentation

Pg. 21
pg. 22
pg. 23
pg. 24
pg. 25
pg. 26
pg. 27
pg. 28
pg. 29
pg. 30
pg. 31
CONFIDENTIAL! LABORATORY REPORT Advanced
Not to be released
without appropriate
IMaterials
authorization! Center, Inc.
125 Swanson Street Ottawa, IL. 61350 (815)433-1495 Fax (815) 433-1795

To: Soil Control Lab Date: March 17, 2010


Frank Shields Project: 10P1084 FTIR/Ash/DSC
PO#: 1144

Purpose:
Evaluate one (1) sample for material composition using FTIR infrared spectrometry and DSC Differential Scanning
Calorimeter. An ash test was also conducted on the sample.

Sample Identification: Source:


A. SCL-0020396 "Cutlery - Knives" Soil Control Lab

Conclusions:
In our opinion, the analysis of the Cutlery shows the major components to be a modified bio-polyester. The
filler in the cutlery appears to be talc.

Results:
The FTIR transmission spectra for the samples were obtained to ID the material composition evaluated of the
samples and are attached for reference.

In our opinion, the spectrum for Sample A verifies that the Cutlery is composed of a modified bio-polyester. Talc
was also found to be in the composition. The cutlery spectrum matches closely to that of Nature Works PLA.

The DSC analysis showed that the cutlery material had a major absorption peak at 157.97° C. This implies that
polypropylene, polyethylene or polystyrene are not present.

Ash testing shows an inorganic residue of 28.81% by weight on Sample A as received.

Discussion / Experimental:
Sample A was evaluated using an FTIR transmission infrared spectrometer fitted with an ATR accessory, Perkin
Elmer Spectrum 100. The DSC analysis was conducted using a Perkin Elmer DSC Series Seven Thermal Analyzer
upgraded with a Temperature Programmer Interface for Perkin Elmer. The ash test of the material was run using a
crucible, controlled pre burning and final heating at 650 Celsius in a Thermolyne 6000 Muffle Furnace.

GregJGeil j
Environmental Scientist
Attachments: FTIR Spectra, DSC Graph

pg. 32
100.0

1264.32
95 _
3676.72

90 2997.46 2855 69
-

2924.84
85 _

80
1454.57

75 _
1384.23

%T 70 _

65

60

55

1183.62

50 _ 1749.05

45 _

42.0 _
4000.0 3000 2000 1500 1000 650.0
cm-1
c:\pel_data\spectra\13190.sp - 10P1084-Soil Control Lab-SCL-0020396-"Cutlery-Knife"

pg. 33
23.4
4000.0 3000 2000 1500 1000 650.0
cm-1
c:\pel_data\spectra\13190.sp - 10P1084-Soil Control Lab-SCL-0020396-"Cutlery-Knife"
c:\pel_data\spectra\polylactic acid.sp - Nature Works 4042D - 30.0 mil

pg. 34
99.0

95.

90

85
3675.82

80

75 _

70 _

65

60 _

%T 55.

50 _

45

40,

35

30 _

668.13
25 _

20 991.17

13.0
4000.0 3000 2000 1500 1000 650.0
cm-1
c:\pel_data\spectra\13190b.sp - 10P1084-Soil Control Lab-SCL-0020396 Cutlery Ash

pg. 35
Advanced Materials Center, Inc
File Name: 10P1084.DSC Operator: GGG
Size: 4.00 Date: 03/02/2010
DSC Desc. 1 : 10P1084-Soil Control Lab-SCL-0020396-Knife Time: 13:55:26
Desc. 2 : Instrument: DSC 7

30

157.97 C
25

18.68J/C

20

141.99 C

1 15
I

<D 10
I

Seg Start End Heat Hold Gas


Temp Temp Rate Time
1 25 200 20 0 Nitrogen
Sample Rate: 1 sec

20 40 60 80 100 120 140 160 180 200


Temperature (C)
Printed(3/2/2010 2:25:33 PM) Program(Version 4.2.109) pg. 36

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