Biodegradable Testing Badger Sunscreens

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OECD 301B Ready/Ultimate

Biodegradability Assessment
Date of Final Report: April 27, 2011
Total Number of Pages: 9
Report Prepared For: Report Prepared By:

Autumn Harp Inc. RespirTek, Inc.
26 Thompson Drive 12450 Shortcut Rd. Bldg F
Essex Junction, VT 05452 Biloxi, MS 39532
802-857-4703 228-392-7977
RespirTek, Inc. 12450 Shortcut Road Bldg. F, Biloxi, MS 39532 www.respirtek.com

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Project ID: AUT-2283

Date: April 27, 2011
Quality Assurance Unit Statement
The purpose of the Quality Assurance Unit is to monitor the conduct and reporting of
laboratory studies. Enclosed is the final report data for project ID AUT-2283. All
analyses were conducted following procedures set forth by the environmental laboratory
accreditation program standards. Quality assurance systems and quality control criteria
have been reviewed for the data collected, either internally or externally by one of
RespirTek’s affiliate laboratories, and the data review generated the following response:
QA/QC criteria met for all analyses
James Radich, M.S. ChE

Interim CEO &
Vice President/Research
RespirTek, Inc.
Phone: (228) 392-7977
Fax: (228) 392-7838
www.respirtek.com
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Report on Ready/Ultimate Biodegradability Test
Client – Autumn Harp Inc.

Test Product – 93-263 SPF 30 Lightly Scented Sunscreen, 93-261 SPF 30 Sunstick
Ready/Ultimate Biodegradability Test
April 27, 2011
Laboratory
Testing as presented in this report was conducted by RespirTek, Inc (RespirTek). The
testing facility is located at 12450 Shortcut Rd., Bldg F, Biloxi, MS 39532.
Sample Receipt
The sample was received on November 23, 2010 at the RespirTek testing facility. The
package received from Fedex contained 2 small clear glass jars. One sample was
labeled “93-263 SPF 30 Lightly Scented Sunscreen.” The other sample was labeled “93-
261 SPF 30 Sunstick.” Samples were at ambient temperature in good condition with no
evidence of damage or contamination. No temperature preservation was required.
Inoculum Collection and Conditioning

The inoculum was collected from a local wastewater treatment facility treating
predominantly domestic sewage. The facility is the Escawtapa POTW, and inoculum
was collected on January 27, 2011. Following collection, the inoculum was immediately
transported to the testing facility and was aerated with CO2-free air.
Summary of Method
The study commenced on February 2, 2011 and continued for 69 days. The purpose of
the study was to determine if the test products would meet requirements for
Ready/Ultimate Biodegradability per the OECD 301B test method. The OECD 301B
method is normally a 28 day test for Ready Biodegradability but may be extended if the
test material has not reached a plateau in biodegradation. In such cases, the extended
study becomes one strictly for Ultimate Biodegradability determination within the larger
class of Inherent Biodegradability tests.
OECD 301B biodegradability testing monitors the degree of activity of microorganisms

exposed to a material that is being tested for a biodegradable status. In the test, if the
microorganisms recognize the material as a food source, then an increase in biological
activity is observed through data collection specifically designed to assess biological
conversion of organic carbon to inorganic carbon. If the material is not a recognizable
food source or is toxic or inhibitory, then there is no measurable increase in biological
activity or, in some cases, there is a marked decrease in activity relative to a
biodegradable control.
The following test vessels were prepared and analyzed for the study: Blank Control,
Test Products, and Positive Control. Reactors were setup in duplicate for statistical
validation of results, and a total of 30 sampling events were executed.
The Test Products and Positive Control are analyzed for total organic carbon prior to
study initiation to determine appropriate dilutions that yield a concentration of organic
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carbon of 10-20 mg//L per method requirements. The organic carbon contributions for
each test reactor are included in the data appendices attached to this report.
Analytical testing was conducted as follows:
Carbon Analyzer: High Sensitivity Shimadzu TOCvch

TIC Analysis Employed: Aqueous Phase pH > 10 via NaOH; Inorganic Carbon via
TOCvch
Results
Based on the testing conducted in accordance with the specified method, test product
93-263 SPF 30 Lightly Scented Sunscreen achieved 61.70% biodegradation after 69
days of testing. The product met method requirements for Ultimate Biodegradability
classification. The test product 93-261 SPF 30 Sunstick achieved 69.16%
biodegradation after 56 days of testing. The product met method requirements for
Ultimate Biodegradability classification.
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Project Number: AUT-2283

Final Report Date: April 27, 2011
Project Initiation Date: February 1, 2011
Test Method: OECD 301B CO2 Evolution Test
Test Chemicals Biodegradation Classification

93-263, SPF 30 Lightly Scented Sunscreen 61.70% Ultimate
93-261, SPF 30 Sunstick 69.16% Ultimate
Prepared for Autumn Harp Inc.
Prepared by RespirTek, Inc.

12450 Shortcut Road
Building F
Biloxi, MS 39532
The enclosed data relates only to those samples received by the laboratory.
This report shall not be reproduced, except in full, without written approval of the laboratory.
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Analytical
Positive TOC 20.00 mg/L
Sunscreen - A TOC 19.63 mg/L
Sunscreen - B TOC 19.91 mg/L
Positive ThCO2 220.00 mg

Sunscreen - A ThCO2 215.93 mg Test Compound 93-263, SPF 30 Lightly Scented Sunscreen
Sunscreen - B ThCO2 219.01 mg Positive Control Dextrose: PC
Calculations Incubation Temperature: 23°C
TIC (mg/L)
Day 0 Day 2 Day 5 Day 7 Day 9 Day 12 Day 15 Day 17 Day 19 Day 21 Day 23 Day 26 Day 28 Day 30 Day 33 Day 35 Day 37 Day 40 Day 42 Day 44 Day 47 Day 49 Day 51 Day 54 Day 56 Day 58 Day 61 Day 63 Day 65 Day 68 Day 69
Blank-1 0 14.180 21.07 10.87 9.66 11.52 11.27 9.09 9.17 8.37 8.08 10.26 7.09 8.95 10.77 7.80 11.97 9.52 9.11 10.93 10.39 6.76 6.52 8.21 7.24 7.05 8.90 5.12 8.77 7.38 32.31
Blank-2 0 13.630 16.63 14.02 7.83 10.73 11.18 8.28 8.38 8.87 7.82 9.29 6.44 4.77 10.07 7.92 11.77 10.92 8.92 8.61 9.35 6.79 8.19 8.98 7.32 6.94 9.04 4.70 8.77 7.73 29.98
PC-1 0 102.2 104.50 56.28 27.67 24.49 18.10 14.33 11.69 11.45 9.48 12.73 8.77 7.74 14.19 5.15 11.52 12.61 12.31 9.10 13.43 9.67 9.70 10.31 6.88 N/A N/A N/A N/A N/A N/A
PC-2 0 95.0 110.80 62.21 24.04 19.78 15.95 11.93 10.98 6.40 9.04 13.22 8.58 8.19 10.02 4.42 10.89 9.86 9.07 8.81 10.62 8.57 7.58 8.47 7.42 N/A N/A N/A N/A N/A N/A
TC-1 0 18.32 22.90 21.82 15.95 18.79 19.48 15.30 12.24 11.05 11.09 16.54 12.77 11.56 15.34 5.92 12.67 15.96 14.05 13.71 13.92 13.12 11.98 13.04 10.10 10.84 12.91 10.01 15.19 13.29 37.34
TC-2 0 24.51 33.82 40.30 36.13 40.84 38.34 25.60 16.92 17.88 12.66 20.40 11.62 11.12 13.75 4.21 8.83 10.54 10.82 9.98 13.74 9.50 9.28 8.83 8.00 12.47 10.81 7.06 10.58 9.66 32.88
Total CO2 (mg)

Blank-1 N/A 10.41 15.47 7.98 7.09 8.46 8.27 6.67 6.73 6.14 5.93 7.53 5.21 6.57 7.91 5.72 8.79 6.99 6.69 8.02 7.63 4.96 4.78 6.03 5.31 5.17 6.54 3.76 6.44 5.42 23.72
Blank-2 N/A 10.00 12.21 10.29 5.74 7.88 8.21 6.08 6.15 6.51 5.74 6.82 4.73 3.50 7.39 5.81 8.64 8.02 6.55 6.32 6.86 4.99 6.01 6.59 5.38 5.09 6.64 3.45 6.44 5.67 22.00
PC-1 N/A 75.01 76.70 41.31 20.31 17.98 13.29 10.52 8.58 8.40 6.96 9.34 6.44 5.68 10.42 3.78 8.46 9.26 9.04 6.68 9.86 7.10 7.12 7.57 5.05 N/A N/A N/A N/A N/A N/A
TC-1 N/A 13.45 16.81 16.02 11.71 13.79 14.30 11.23 8.98 8.11 8.14 12.14 9.37 8.49 11.26 4.35 9.30 11.71 10.31 10.06 10.22 9.63 8.79 9.57 7.41 7.96 9.48 7.35 11.15 9.75 27.40
TC-2 N/A 17.99 24.82 29.58 26.52 29.98 28.14 18.79 12.42 13.12 9.29 14.97 8.53 8.16 10.09 3.09 6.48 7.74 7.94 7.33 10.09 6.97 6.81 6.48 5.87 9.15 7.93 5.18 7.77 7.09 24.13
Cumulative CO2 (mg)***

Blank-1 N/A 10.4 25.9 33.9 40.9 49.4 57.7 64.3 71.1 77.2 83.1 90.7 95.9 102.5 110.4 116.1 124.9 131.9 138.5 146.6 154.2 159.2 163.9 170.0 175.3 180.5 187.0 190.7 197.2 202.6 226.3
Blank-2 N/A 10.0 22.2 32.5 38.2 46.1 54.3 60.4 66.6 73.1 78.8 85.6 90.4 93.9 101.2 107.1 115.7 123.7 130.3 136.6 143.4 148.4 154.4 161.0 166.4 171.5 178.1 181.6 188.0 193.7 215.7
TC-1 N/A 13.4 30.3 46.3 58.0 71.8 86.1 97.3 106.3 114.4 122.5 134.7 144.0 152.5 163.8 168.1 177.4 189.2 199.5 209.5 219.7 229.4 238.2 247.7 255.2 263.1 272.6 279.9 291.1 300.8 328.2
TC-2 N/A 18.0 42.8 72.4 98.9 128.9 157.0 175.8 188.2 201.4 210.7 225.6 234.2 242.3 252.4 255.5 262.0 269.7 277.7 285.0 295.1 302.1 308.9 315.3 321.2 330.4 338.3 343.5 351.3 358.3 382.5
Percent Biodegradation (%)

TC-1 N/A 1.50 2.88 6.06 8.51 11.12 13.93 16.17 17.35 18.18 19.25 21.54 23.59 25.18 26.86 26.20 26.47 28.42 30.13 31.47 32.85 35.00 36.58 38.09 39.05 40.35 41.69 43.43 45.61 47.56 49.67
TC-2 N/A 3.55 8.57 17.91 27.09 37.04 46.13 51.80 54.53 57.63 59.21 62.77 64.40 65.83 66.94 65.72 64.70 64.81 65.42 65.49 66.78 67.70 68.34 68.42 68.66 70.50 71.11 71.84 72.44 73.15 73.73
PC Average 0.00 28.26 57.89 73.51 79.21 82.89 84.82 86.31 87.16 87.26 87.70 88.77 89.40 89.77 90.33 89.31 89.09 89.43 89.99 89.71 90.43 91.22 91.65 91.91 91.87 N/A N/A N/A N/A N/A N/A
TC Average 0.00 2.53 5.72 11.99 17.80 24.08 30.03 33.99 35.94 37.91 39.23 42.16 43.99 45.51 46.90 45.96 45.59 46.62 47.77 48.48 49.82 51.35 52.46 53.25 53.85 55.43 56.40 57.63 59.03 60.35 61.70
Standard Deviation
PC N/A 5.06 4.45 4.19 2.57 3.33 1.52 1.70 0.50 3.57 0.31 0.35 0.13 0.31 2.95 0.52 0.45 1.94 2.29 0.21 1.99 0.78 1.49 1.30 0.39 N/A N/A N/A N/A N/A N/A
TC N/A 4.38 7.72 13.07 14.27 15.59 13.34 7.28 3.31 4.83 1.11 2.73 0.81 0.31 1.12 1.21 2.71 3.83 2.28 2.64 0.13 2.56 1.91 2.98 1.48 1.15 1.48 2.09 3.26 2.57 3.15
Blank N/A 0.39 3.14 2.23 1.30 0.56 0.06 0.57 0.56 0.35 0.18 0.68 0.46 2.96 0.49 0.09 0.14 0.99 0.14 1.64 0.74 0.02 1.18 0.54 0.06 0.08 0.10 0.30 0.00 0.25 1.65
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Sunscreen OECD 301B Ready/Ultimate Assessment

100
90
80
70
% Biodegradation
60
93-263, SPF 30
Lightly Scented
Sunscreen
50
Positive Control
40
Ten Day Window

30
20
10
0
0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75
Time (days)
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Analytical
Positive TOC 20.00 mg/L
Sunstick - A TOC 19.81 mg/L
Sunstick - B TOC 19.69 mg/L
Positive ThCO2 220.00 mg

Sunstick - A ThCO2 217.91 mg Test Compound 93-261, SPF 30 Sunstick
Sunstick - B ThCO2 216.59 mg Positive Control Dextrose: PC
Calculations Incubation Temperature: 23°C
TIC (mg/L)
Day 0 Day 2 Day 5 Day 7 Day 9 Day 12 Day 15 Day 17 Day 19 Day 21 Day 23 Day 26 Day 28 Day 30 Day 33 Day 35 Day 37 Day 40 Day 42 Day 44 Day 47 Day 49 Day 51 Day 54 Day 56
Blank-1 0 14.180 21.07 10.87 9.66 11.52 11.27 9.09 9.17 8.37 8.08 10.26 7.09 8.95 10.77 7.80 11.97 9.52 9.11 10.93 10.39 6.76 6.52 8.21 16.62
Blank-2 0 13.630 16.63 14.02 7.83 10.73 11.18 8.28 8.38 8.87 7.82 9.29 6.44 4.77 10.07 7.92 11.77 10.92 8.92 8.61 9.35 6.79 8.19 8.98 12.84
PC-1 0 102.2 104.50 56.28 27.67 24.49 18.10 14.33 11.69 11.45 9.48 12.73 8.77 7.74 14.19 5.15 11.52 12.61 12.31 9.10 13.43 9.67 9.70 10.31 6.88
PC-2 0 95.0 110.80 62.21 24.04 19.78 15.95 11.93 10.98 6.40 9.04 13.22 8.58 8.19 10.02 4.42 10.89 9.86 9.07 8.81 10.62 8.57 7.58 8.47 7.42
TC-1 0 14.13 25.95 21.76 19.03 37.54 37.52 24.80 17.91 16.84 12.10 15.35 12.48 12.08 16.04 10.54 12.05 14.16 10.47 11.35 13.10 10.35 10.00 9.57 35.70
TC-2 0 14.12 37.45 40.51 32.21 36.19 27.30 18.35 15.00 19.38 14.36 18.92 12.29 5.23 12.54 8.80 12.87 16.12 14.95 11.99 19.49 14.61 13.02 13.99 39.17
Total CO2 (mg)

Blank-1 N/A 10.41 15.47 7.98 7.09 8.46 8.27 6.67 6.73 6.14 5.93 7.53 5.21 6.57 7.91 5.72 8.79 6.99 6.69 8.02 7.63 4.96 4.78 6.03 12.20
Blank-2 N/A 10.00 12.21 10.29 5.74 7.88 8.21 6.08 6.15 6.51 5.74 6.82 4.73 3.50 7.39 5.81 8.64 8.02 6.55 6.32 6.86 4.99 6.01 6.59 9.43
PC-1 N/A 75.01 76.70 41.31 20.31 17.98 13.29 10.52 8.58 8.40 6.96 9.34 6.44 5.68 10.42 3.78 8.46 9.26 9.04 6.68 9.86 7.10 7.12 7.57 5.05
PC-2 N/A 69.76 81.33 45.66 17.65 14.52 11.71 8.76 8.06 4.70 6.64 9.70 6.30 6.01 7.35 3.24 7.99 7.24 6.66 6.47 7.80 6.29 5.57 6.21 5.45
TC-1 N/A 10.37 19.05 15.97 13.97 27.55 27.54 18.20 13.15 12.36 8.88 11.27 9.16 8.87 11.77 7.74 8.84 10.39 7.68 8.33 9.62 7.60 7.34 7.02 26.20
TC-2 N/A 10.36 27.49 29.73 23.64 26.56 20.04 13.47 11.01 14.22 10.54 13.89 9.02 3.84 9.20 6.46 9.45 11.83 10.97 8.80 14.31 10.72 9.56 10.27 28.75
Cumulative CO2 (mg)***

Blank-1 N/A 10.4 25.9 33.9 40.9 49.4 57.7 64.3 71.1 77.2 83.1 90.7 95.9 102.5 110.4 116.1 124.9 131.9 138.5 146.6 154.2 159.2 163.9 170.0 182.2
Blank-2 N/A 10.0 22.2 32.5 38.2 46.1 54.3 60.4 66.6 73.1 78.8 85.6 90.4 93.9 101.2 107.1 115.7 123.7 130.3 136.6 143.4 148.4 154.4 161.0 170.5
PC-1 N/A 75.0 151.7 193.0 213.3 231.3 244.6 255.1 263.7 272.1 279.1 288.4 294.8 300.5 310.9 314.7 323.2 332.4 341.5 348.2 358.0 365.1 372.2 379.8 384.8
PC-2 N/A 69.8 151.1 196.7 214.4 228.9 240.6 249.4 257.4 262.1 268.8 278.5 284.8 290.8 298.1 301.4 309.4 316.6 323.3 329.7 337.5 343.8 349.4 355.6 361.0
TC-1 N/A 10.4 29.4 45.4 59.4 86.9 114.5 132.7 145.8 158.2 167.0 178.3 187.5 196.3 208.1 215.8 224.7 235.1 242.8 251.1 260.7 268.3 275.7 282.7 308.9
TC-2 N/A 10.4 37.9 67.6 91.2 117.8 137.8 151.3 162.3 176.5 187.1 201.0 210.0 213.8 223.0 229.5 238.9 250.8 261.7 270.5 284.8 295.6 305.1 315.4 344.2
Percent Biodegradation (%)

PC-1 N/A 29.46 58.03 72.66 78.97 83.43 85.73 87.61 88.58 89.53 90.04 91.02 91.69 91.99 93.25 92.34 92.23 93.02 94.12 93.90 95.09 96.05 96.84 97.41 94.79
PC-2 N/A 27.07 57.75 74.35 79.45 82.34 83.92 85.00 85.74 85.00 85.36 86.51 87.11 87.56 87.42 86.28 85.95 85.83 85.85 85.53 85.78 86.38 86.46 86.41 83.97
TC-1 N/A 0.08 2.47 5.60 9.07 17.97 26.83 32.25 35.33 38.10 39.50 41.37 43.30 45.06 46.95 47.85 47.91 49.24 49.73 50.26 51.35 52.56 53.45 53.78 60.84
TC-2 N/A 0.07 6.38 15.89 23.84 32.33 37.78 41.06 43.17 46.81 48.98 52.08 53.96 53.41 54.12 54.44 54.78 56.78 58.79 59.55 62.81 65.46 67.38 69.21 77.49
PC Average 0.00 28.26 57.89 73.51 79.21 82.89 84.82 86.31 87.16 87.26 87.70 88.77 89.40 89.77 90.33 89.31 89.09 89.43 89.99 89.71 90.43 91.22 91.65 91.91 89.38
TC Average 0.00 0.07 4.42 10.75 16.46 25.15 32.30 36.65 39.25 42.46 44.24 46.73 48.63 49.23 50.54 51.15 51.35 53.01 54.26 54.90 57.08 59.01 60.41 61.49 69.16
Standard Deviation
PC N/A 5.06 4.45 4.19 2.57 3.33 1.52 1.70 0.50 3.57 0.31 0.35 0.13 0.31 2.95 0.52 0.45 1.94 2.29 0.21 1.99 0.78 1.49 1.30 0.39
TC N/A 0.01 8.13 13.26 9.32 0.95 7.23 4.56 2.06 1.80 1.60 2.52 0.13 4.84 2.47 1.23 0.58 1.39 3.17 0.45 4.52 3.01 2.14 3.13 2.46
Blank N/A 0.39 3.14 2.23 1.30 0.56 0.06 0.57 0.56 0.35 0.18 0.68 0.46 2.96 0.49 0.09 0.14 0.99 0.14 1.64 0.74 0.02 1.18 0.54 2.67
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SunStick OECD Ready/Ultimate Assessment

100
90
80
70
% Biodegradation
60
50
93-261, SPF 30 Sunstick
Positive Control
40 Ten Day Window
30
20
10
0
0 5 10 15 20 25 30 35 40 45 50 55 60
Time (days)

Biodegradable Testing Badger Sunscreens

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1 of 9

OECD 301B Ready/Ultimate

Date of Final Report: April 27, 2011

Total Number of Pages: 9

Report Prepared For: Report Prepared By:

RespirTek, Inc. 12450 Shortcut Road Bldg. F, Biloxi, MS 39532 www.respirtek.com

Project ID: AUT-2283

QA/QC criteria met for all analyses

James Radich, M.S. ChE

Report on Ready/Ultimate Biodegradability Test

Client – Autumn Harp Inc.

Inoculum Collection and Conditioning

OECD 301B biodegradability testing monitors the degree of activity of microorganisms

Analytical testing was conducted as follows:

Carbon Analyzer: High Sensitivity Shimadzu TOCvch

Project Number: AUT-2283

Test Chemicals Biodegradation Classification

Prepared for Autumn Harp Inc.

Prepared by RespirTek, Inc.

Positive ThCO2 220.00 mg

Calculations Incubation Temperature: 23°C

Total CO2 (mg)

Cumulative CO2 (mg)***

Percent Biodegradation (%)

Sunscreen OECD 301B Ready/Ultimate Assessment

Ten Day Window

Positive ThCO2 220.00 mg

Calculations Incubation Temperature: 23°C

Total CO2 (mg)

Cumulative CO2 (mg)***

Percent Biodegradation (%)

SunStick OECD Ready/Ultimate Assessment

40 Ten Day Window

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