ASTM D 6400: Determing Aerobic Biodegradation of Plastic Materials Under Controlled Composting Conditions
ASTM D 6400: Determing Aerobic Biodegradation of Plastic Materials Under Controlled Composting Conditions
ASTM D 6400: Determing Aerobic Biodegradation of Plastic Materials Under Controlled Composting Conditions
FAX: 831-724-3188
ASTM D 6400
Determing Aerobic Biodegradation of Plastic
Materials Under Controlled Composting Conditions
Work Order #:
0020396-01
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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TEL: 831-724-5422
FAX: 831-724-3188
Table of Contents
Page #
Section 1.) Summary of Test Results 3
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FAX: 831-724-3188
Summary of Results: The product met all the requirements to be considered "compostable"
as judged by the United States standard ASTM D 6400.
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FAX: 831-724-3188
• 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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TEL: 831-724-5422
FAX: 831-724-3188
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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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
% Passing
Week 2mm sieve Criteria Pass/Fail
*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
Layer/Material Number 1 of 1
Layer/Material Analyzed: Whole Sample
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
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% 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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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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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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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
Satisfactory appearance, odor, & moisture content must be maintained in all composting vessels.
We were able to accomplish this throughout the study.
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Work Order: 0020396-01
Account #: 5991
Date Reported: October 1, 2010
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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Work Order: 0020396-01
Account #: 5991
Date Reported: October 1, 2010
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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Work Order: 0020396-01
Account #: 5991
Date Reported: October 1, 2010
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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Work Order: 0020396-01
Account #: 5991
Date Reported: October 1, 2010
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
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Work Order: 0020396-01
Account #: 5991
Date Reported: October 1, 2010
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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Work Order: 0020396-01
Account #: 5991
Date Reported: October 1, 2010
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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Work Order: 0020396-01
Account #: 5991
Date Reported: October 1, 2010
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
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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
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.
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.
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