CONFIDENTIAL REPORT Arcoplast, Inc. · ASTM D1308-02 (2013) Testing Method* The second test...

Testing Results Report for ARCOPLAST, INC.

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CONFIDENTIAL REPORT

Arcoplast, Inc.

Prepared By: Avomeen Analytical Services 4840 Venture Drive Ann Arbor, MI 48108 Date: February 14, 2014

http://www.avomeen.com/

Chemical Resistance Testing

Avomeen is a member in good standing of the American Council of Independent Laboratories Avomeen Analytical Services | February 14, 2014| www.avomeen.com | 800-930-5450 P. 2

To: Ghislain Beauregard Arcoplast 1873 Williamstown Drive St. Peters, MO 63376 (636) 978-7781 [email protected]


Thank you for contacting Avomeen Analytical Services for the chemical resistance testing of fiberglass test panels. Following are the results, methodology, and data associated with our analysis of the sample.

Table 1: Sample Description

Avomeen Sample ID Sample Description

011514AR2572 Fiberglass test panels for ISO 2812-4 and ASTM D1308 testing

Executive Summary

The goal of this analysis was perform chemical resistance testing on fiberglass test panels using methods ISO 2812-4:2007 and ASTM D1308-02 (2013) over a period of time to identify at what point failure occurred for each chemical that failed during the previous 72 hour test. The same defects that occurred during the initial 72-hour test occurred after 15 minutes of exposure for 8 of the 13 compounds, including chromic acid (30%), hydrochloric acid (37%), nitric acid (100%), sodium hydroxide (10%), sodium hydroxide (40%), sodium hypochlorite (10-15%), STERIS - Coverage plus NPD, and mustard. The remaining 5 chemicals were tested for exposure periods of 1 hour, 4 hours, and 8 hours until the same defects occurred as seen in the 72-hour test as reported on December 31, 2013. Results for the 4 different exposure times for ISO 2812-4 are expressed in Tables 2-5, and results for ASTM D1308-02 are expressed in Table 9.



Analytical Testing

Initial Observations

The samples were received for analysis on January 15, 2015, and arrived boxed and in foam packaging. Each of the fiberglass test panels consisted of a solid glass/resin matrix panel with a bead of aliphatic urethane finishing compound, both of which were tested. Each of the test panels were approximately 105 mm x 75 mm x 10 mm (L x W x H) with a bead of aliphatic urethane finishing compound across the length of the test panel approximately 8 mm in diameter. A photograph of the test panel samples “As Received” can be found in Figure 1.

Figure 1: Photograph of the fiberglass test panels samples “As Received”

ISO 2812-4:2007 Testing Method* The first test performed on the fiberglass test panels was ISO 2812-4:2007 Paints and varnishes – Determination of resistance to liquids – Part 4: Spotting methods. This part of ISO 2812 specifies spotting methods for determining the chemical resistance of individual layer or multi-layer system of coating materials to the effects of liquid chemicals or products. The panels were tested in triplicate at ambient temperature and humidity, and allowed to condition at ambient temperature and humidity for at least 48 hours before testing. All chemicals listed in Table 2 were applied in volumes of 0.1 mL using a glass pipet to two locations on each test panel at the intersection of the fiberglass gel coat and the sealant using Method A (Horizontal test plane) of the test method. The chemicals were left uncovered on the fiberglass test panels for several different time intervals including: 15 minutes, 1 hour, 4 hours, and 8 hours. Samples were tested until the same failure was observed that was identified in the previous 72 hour test. At the end of the each testing period, the test panels were cleaned off using Kimwipes and deionized water, and then assessed for blistering as specified in ISO 4628-2:2003 and also for any other visible alterations as specified in ISO4628-1:2003. Assessments using these methods were carried out in a well lit room and pictures were taken with both a point-and-shoot camera along with a Dino-Lite Premier digital microscope which allowed for pictures to be taken at 25.7x magnification.



ASTM D1308-02 (2013) Testing Method* The second test performed on the fiberglass test panels was ASTM 2812-02 Standard Test Method for Effect of Household Chemicals on Clear and Pigmented Organic Finished. This was carried out in triplicate using the Open Spot Test method (section 7.3 of ASTM 2812-02) at ambient temperature and relative humidity and test panels were allowed to condition for 48 hours before testing. Approximately 1 mL of mustard was applied to two locations on each test panel at the intersection of the fiberglass gel coat and the sealant and left uncovered. After 15 minutes, the panels were cleaned off with deionized water and a Kimwipe, and then evaluated for any alterations in the surfaces such as discoloration, change in gloss, blistering, softening, and swelling. * The standard methods were deviated from according to customer request. The test panels were left uncovered during the specified testing periods instead of being covered by a watch glass/petri dish. This was done in order to better simulate real conditions (i.e. if hexane was spilled on the fiberglass resin, it would quickly evaporate). If the chemicals were covered, the hexane would stay on the test panel for much longer than it would typically be exposed. Both analyses, ISO 2812-2:2007 and ASTM D1308-02 (2013) were performed by Jon Nezich, Analytical Chemist, and overseen by Dr. Craig Larner, Technical Director. Testing began on February 5, 2014 and was completed on February 7, 2014.

Results and Discussion

ISO 2812-4:2007 Results and Discussion Full results for ISO 2812-4 in Table 2 are expressed using the following specified methods which include: the type of defect; the quantity present (Table 6) and its size (Table 7); the intensity of the change (Table 8). For example, the result for a test panel that experienced discoloration with a quantity rating of 1 (Table 6), a size rating of 4 (Table 7), and an intensity rating of 2 (Table 8), would be expressed as the following: discoloration; degree of discoloration 1(S4); intensity 2. Pictures of each of the test panels tested using chemicals listed in Table 2 for the 15 minute test can be found in Figures 2-37, including a picture of when the chemicals were first applied and a picture of the test panels after they were wiped clean at the end of the specified testing period. Test panels which showed changes in the test surface also have pictures taken using a microscope showing a representative change found on all three of the test panels for that chemical. Pictures of the test panels tested for 1 hour, 4 hours, and 8 hours can be found in Figures 38-52, Figures 53-58, and Figures 59-61, respectively. All test panels showed the same defects in 8 hours or less when compared to the results from the 72 hour test period, although with slightly less intensity. These included chromic acid (10%), chromic acid (30%), hydrochloric acid (37%), BIRKO - FOMACID - 100043, Nitric Acid (10%), nitric acid (100%), sodium hydroxide (10%), sodium hydroxide (40%), sodium hypochlorite (10%), sulfuric acid (30%), STERIS - Coverage plus NPD, and STERIS - SPOR KLENZ. Of these, nitric acid (100%) and sulfuric acid (30%; 8 hour on sealant only) showed blistering, while the rest showed some degree of discoloration or change in gloss. Some of the discolorations were very faint, and seen only under certain lighting, more indicative of a change in gloss/finish. Many of the defects seen were at a lower intensity than seen in the previous 72-hour test, and in order to better distinguish results from the 72 hour test, half increments were used.



Table 2: Results for ISO 2812-4:2007 15 minute testing

Chemical Defects from chemical resistance

testing for glass/resin matrix Defects from chemical resistance

testing for sealant

Chromic Acid (10%) None Discoloration; Degree of

discoloration 2(S2); Intensity 2

Chromic Acid (30%) Change in gloss; Degree of change

in gloss 1(S5); Intensity 0.5 Discoloration; Degree of


Hydrochloric Acid (37%) Discoloration; Degree of

discoloration 1(S5); Intensity 0.5 None

BIRKO - FOMACID - 100043 Change in gloss; Degree of change

in gloss 1(S5); Intensity 1 None

Nitric Acid (10%) None None

Nitric Acid (100%) Blistering; Degree of blistering

5(S3); Intensity 5 Blistering; Degree of blistering 5(S3);

Intensity 5

Sodium Hydroxide (10%) Discoloration; Degree of

discoloration 1(S5); Intensity 1 None

Sodium Hydroxide (40%) Discoloration; Degree of


Sodium Hypochlorite (10-15%) Change in gloss; Degree of change

in gloss 1(S5); Intensity 0.5 None

Sulfuric Acid (30%) Discoloration; Degree of


STERIS - Coverage plus NPD Change in gloss; Degree of change


STERIS - SPOR KLENZ None None



Table 3: Results for ISO 2812-4:2007 1 hour testing



testing for sealant

Chromic Acid (10%) Change in gloss; Degree of change

in gloss 1(S5); Intensity 0.5 Discoloration; Degree of


BIRKO - FOMACID - 100043 Change in gloss; Degree of change

in gloss 1(S5); Intensity 1 Discoloration; Degree of

discoloration 1(S5); Intensity 0.5

Nitric Acid (10%) Discoloration; Degree of

discoloration 1(S5); Intensity 0.5 None



STERIS - SPOR KLENZ Change in gloss; Degree of change





testing for sealant

Nitric Acid (10%) Discoloration; Degree of

discoloration 1(S2); Intensity 1 Discoloration; Degree of







testing for sealant


discoloration 1(S4); Intensity 2 Blistering; Degree of Blistering 1(S5);

Intensity 3



Table 6: Rating scheme for designating the quantity of defects

Rating Quantity of defect

0 None, i.e. no detectable defects

1 Very few, i.e. small, barely significant number of defects

2 Few, i.e. small but significant number of defects

3 Moderate number of defects

4 Considerable number of defects

5 Dense pattern of defects

Table 7: Rating scheme for designating the size of defects

Rating Size of defect

0 Not visible under x10 magnification

1 Only visible under magnification up to x10

2 Just visible with normal corrected vision

3 Clearly visible with normal corrected vision (up to 0.5 mm)

4 0.5 mm to 5 mm

5 Larger than 5 mm

Table 8: Rating scheme for designating the intensity of changes

Rating Intensity of change

0 Unchanged, i.e. no perceptible change

1 Very slight, i.e. just perceptible change

2 Slight, i.e. clearly perceptible change

3 Moderate, i.e. very clearly perceptible change

4 Considerable, i.e. pronounced changed

5 Very marked change



ASTM D1308-02 (2013) Results and Discussion Results for testing using ASTM D1308-02 (2013) can found in Table 9. Pictures of each of the fiberglass test panels tested using reagents listed in Table 9 can be found in Figures 62-66, including a picture of when the mustard was first applied and a picture of the test panels after the panels were wiped clean at the end of the 15 minute testing period. As seen in the difference between Figures 64-66, the yellow discoloration from the mustard decreased significantly when left at ambient temperature and relative humidity for 6 days after the initial assessment. The fiberglass gel panel no longer showed a yellow discoloration after 1 day, and the yellow discoloration on the sealant was reduced in intensity after 1 day, and no longer showed after 6 days.

Table 9: Results for ASTM D1308-02 (2013)

Reagent Defects from chemical resistance testing for

glass/resin matrix

Defects from chemical resistance testing for

sealant

Mustard 1 3

1 = Unaffected = wipes off easily with a damp cloth and mild soap, no color or surface change 2 = Superficial = stain removed easily with water and/or mild abrasive 3 = Considerable = stain not completely removable



Figures

Figure 2: Control fiberglass test panels



Figure 3: Control fiberglass test panel –25.7x magnification



Figure 4: Fiberglass test panels with Chromic Acid (10%) applied for 15 minutes



Figure 5: Fiberglass test panels with Chromic Acid (10%) cleaned off after 15 minute application period



Figure 6: Fiberglass test panels with Chromic Acid (10%) cleaned off after 15 minute application period – magnified

25.7x



Figure 7: Fiberglass test panels with Chromic Acid (30%) applied for 15 minutes



Figure 8: Fiberglass test panels with Chromic Acid (30%) cleaned off after 15 minute application period



Figure 9: Fiberglass test panels with Chromic Acid (30%) cleaned off after 15 minute application period - magnified

25.7x – very faint; arrows point perpendicularly to perimeter of defect



Figure 10: Fiberglass test panels with Hydrochloric Acid (37%) applied for 15 minutes



Figure 11: Fiberglass test panels with Hydrochloric Acid (37%) cleaned off after 15 minute application period



Figure 12: Fiberglass test panels with Hydrochloric Acid (37%) cleaned off after 15 minute application period -

magnified 25.7x – very faint; arrows point perpendicularly to perimeter of defect



Figure 13: Fiberglass test panels with BIRKO - FOMACID-100043 applied for 15 minutes



Figure 14: Fiberglass test panels with BIRKO - FOMACID-100043 cleaned off after 15 minute application period



Figure 15: Fiberglass test panels with BIRKO - FOMACID-100043 cleaned off after 15 minute application period –

magnified 25.7x



Figure 16: Fiberglass test panels with Nitric Acid (10%) applied for 15 minutes



Figure 17: Fiberglass test panels with Nitric Acid (10%) cleaned off after 15 minute application period



Figure 18: Fiberglass test panels with Nitric Acid (100%) applied for 15 minutes



Figure 19: Fiberglass test panels with Nitric Acid (100%) cleaned off after 15 minute application period



Figure 20: Fiberglass test panels with Nitric Acid (100%) cleaned off after 15 minute application period – magnified

25.7x



Figure 21: Fiberglass test panels with Sodium Hydroxide (10%) applied for 15 minutes



Figure 22: Fiberglass test panels with Sodium Hydroxide (10%) cleaned off after 15 minute application period



Figure 23: Fiberglass test panels with Sodium Hydroxide (10%) cleaned off after 15 minute application period –

magnified 25.7x



Figure 24: Fiberglass test panels with Sodium Hydroxide (40%) applied for 15 minutes



Figure 25: Fiberglass test panels with Sodium Hydroxide (40%) cleaned off after 15 minute application period



Figure 26: Fiberglass test panels with Sodium Hydroxide (40%) cleaned off after 15 minute application period –

magnified 25.7x



Figure 27: Fiberglass test panels with Sodium Hypochlorite (10-15%) applied for 15 minutes



Figure 28: Fiberglass test panels with Sodium Hypochlorite (10-15%) cleaned off after 15 minute period



Figure 29: Fiberglass test panels with Sodium Hypochlorite (10-15%) cleaned off after 15 minute application period –




Figure 30: Fiberglass test panels with Sulfuric Acid (30%) applied for 15 minutes



Figure 31: Fiberglass test panels with Sulfuric Acid (30%) cleaned off after 15 minute application period



Figure 32: Fiberglass test panels with Sulfuric Acid (30%) cleaned off after 15 minute application period – magnified

25.7x



Figure 33: Fiberglass test panels with STERIS - Coverage plus NPD applied for 15 minutes



Figure 34: Fiberglass test panels with STERIS - Coverage plus NPD cleaned off after 15 minute application period



Figure 35: Fiberglass test panels with STERIS - Coverage plus NPD cleaned off after 15 minute application period –




Figure 36: Fiberglass test panels with STERIS - SPOR KLENZ applied for 15 minutes



Figure 37: Fiberglass test panels with STERIS - SPOR KLENZ cleaned off after 15 minute application period



Figure 38: Fiberglass test panels with Chromic Acid (10%) applied for 1 hour



Figure 39: Fiberglass test panels with Chromic Acid (10%) cleaned off after 1 hour application period



Figure 40: Fiberglass test panels with Chromic Acid (10%) cleaned off after 1 hour application period – magnified




Figure 41: Fiberglass test panels with BIRKO - FOMACID-100043 applied for 1 hour



Figure 42: Fiberglass test panels with BIRKO - FOMACID-100043 cleaned off after 1 hour application period



Figure 43: Fiberglass test panels with BIRKO - FOMACID-100043 cleaned off after 1 hour application period –

magnified 25.7x – very faint; arrows point to perpendicularly to perimeter of defects



Figure 44: Fiberglass test panels with Nitric Acid (10%) applied for 1 hour



Figure 45: Fiberglass test panels with Nitric Acid (10%) cleaned off after 1 hour application period



Figure 46: Fiberglass test panels with Nitric Acid (10%) cleaned off after 1 hour application period – magnified 25.7x

– very faint; arrows point perpendicularly to perimeter of defect



Figure 47: Fiberglass test panels with Sulfuric Acid (30%) applied for 1 hour



Figure 48: Fiberglass test panels with Sulfuric Acid (30%) cleaned off after 1 hour application period



Figure 49: Fiberglass test panels with Sulfuric Acid (30%) cleaned off after 1 hour application period – magnified




Figure 50: Fiberglass test panels with STERIS - SPOR KLENZ applied for 1 hour



Figure 51: Fiberglass test panels with STERIS - SPOR KLENZ cleaned off after 1 hour application period



Figure 52: Fiberglass test panels with STERIS - SPOR KLENZ cleaned off after 1 hour application period – magnified




Figure 53: Fiberglass test panels with Nitric Acid (10%) applied for 4 hours



Figure 54: Fiberglass test panels with Nitric Acid (10%) cleaned off after 4 hour application period



Figure 55: Fiberglass test panels with Nitric Acid (10%) cleaned off after 4 hour application period – magnified 25.7x

– very faint, arrows point perpendicularly to perimeter of defects



Figure 56: Fiberglass test panels with Sulfuric Acid (30%) applied for 4 hours




25.7x



Figure 59: Fiberglass test panels with Sulfuric Acid (30%) applied for 8 hours




25.7x



Figure 62: Fiberglass test panels with Mustard applied for 15 minutes per ASTM D1308



Figure 63: Fiberglass test panels with Mustard cleaned off after 15 minute application period



Figure 64: Fiberglass test panels with Mustard cleaned off after 15 minute application – close-up; very faint, arrows

point perpendicularly to perimeter of defects



Figure 65: Fiberglass test panels 1 day after initial assessment with Mustard cleaned off after 15 minute application

period per ASTM D1308 – very faint; arrows point perpendicularly to perimeter of defect

Figure 66: Fiberglass test panels 1 day after initial assessment with Mustard cleaned off after 15 minute application

period per ASTM D1308



Wrap Up

Thank you for consulting with Avomeen Analytical Services. If you have any questions regarding this analysis, or if we can be of any further assistance, please call us at (800) 930-5450. Following the receipt of this final report, a final invoice indicating the remaining payment will be sent to you. We will safely and securely dispose of all samples and confidential information in our possession in 30 days, unless otherwise instructed by your company. It has been a pleasure working with you and we look forward to serving you again.

Sincerely, Avomeen Analytical Services

Craig D. Larner Craig D. Larner, Ph.D. Technical Director 800-930-5450 [email protected]

Andrew Kolbert Andrew C. Kolbert, Ph.D., M.T.M. Vice President, Technical Services 800-930-5450 [email protected]

Shri Thanedar Shri Thanedar, Ph.D. CEO/Chief Chemist 800-930-5450 [email protected]

mailto:[email protected]



CONFIDENTIAL REPORT Arcoplast, Inc. · ASTM D1308-02 (2013) Testing Method* The second test...

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