Laboratory Test Results Evaluating Resimac Reischem ... · ASTM D4541-09 ; Pull-Off Adhesion ....

March 15, 2016

3 – 2221 41 Ave NE, Calgary, AB Canada +1 403 514 2334 [email protected]

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Laboratory Test Results

Evaluating Resimac Reischem 512UCEN Epoxy Coating System

per ISO 2812-1:2007, Chemical Immersion

Prepared for:

Dalco Services Inc 152 Petrolia Dr. Red Deer, AB

T4E 1B4

Prepared by: _________________________

Jason Hartt, B.Sc. Laboratory Manager

Approved by: ________________________

Yasir Idlibi, Ph. D. President

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Test results in this report relate only to the samples tested.

Specific samples tested are given in Section 3.0 of this report.

Revision Level Reason for Revision Date A1 Initial Release March 4, 2016 A2 Change the name of the coating March 15, 2016

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Use or disclosure of data is subject to restrictions on the title page of this ADANAC Global Testing & Inspection document. of 20

Table of Contents

Section Page

1.0 Scope .................................................................................................................................... 4

2.0 Testing Criteria .................................................................................................................... 4

3.0 Samples Received / Application & Inspection .................................................................... 5

4.0 Sample Preparation & Selection .......................................................................................... 5

5.0 Test Results .......................................................................................................................... 6

5.1 Chemical Immersion ........................................................................................................ 6

5.2 Pull-Off Adhesion Results.............................................................................................. 15

5.3 EIS Test Results ............................................................................................................. 20

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List of Tables Page

Table 1 – Samples Received ....................................................................................................................... 5 Table 2 – Summary of Chemical Immersion Results, 6% Hydrochloric Acid (ISO 2812-1:2007) ........... 6 Table 3 – Summary of Chemical Immersion Results, 6% Sodium Hydroxide (ISO 2812-1:2007) ........... 7 Table 4 – Summary of Chemical Resistance Results, 50/50 Water/Bitumen (ISO 2812-1:2007) ............. 9 Table 5 – Summary of Chemical Resistance Results, 15% Sodium Hydroxide (ISO 2812-1:2007) ....... 10 Table 6 – Summary of Chemical Resistance Results, 4% Citric Acid (ISO 2812-1:2007) ...................... 12 Table 7 – Summary of Chemical Resistance Results, 6% Sodium Hypochlorite (ISO 2812-1:2007) ..... 13 Table 8 –Summary of Pull-Off Adhesion (ASTM D4541-09) on Treated Samples ................................ 15 Table 9 –Summary of Pull-Off Adhesion (ASTM D4541-09) on Treated Samples, Continued .............. 16

List of Figures Page

Figure 1 – Pre-Test and Post-Test Samples of 6% Hydrochloric Acid Immersion .................................... 8 Figure 2 – Pre-Test and Post-Test Samples of 6% Sodium Hydroxide Immersion .................................... 8 Figure 3 – Pre-Test and Post-Test Samples of 50/50 Water/Bitumen Immersion .................................... 11 Figure 4 – Pre-Test and Post-Test Samples of 15% Sodium Hydroxide Immersion ................................ 11 Figure 5 – Pre-Test and Post-Test Samples of 4% Citric Acid Immersion .............................................. 14 Figure 6 – Pre-Test and Post-Test Samples of 6% Sodium Hypochlorite Immersion .............................. 14 Figure 7 –Pre-Test Pull-Off Adhesion ...................................................................................................... 17 Figure 8 –Post-Test Pull-Off Adhesion, 6% Hydrochloric Acid Immersion ............................................ 17 Figure 9 –Post-Test Pull-Off Adhesion, 6% Sodium Hydroxide Immersion ........................................... 17 Figure 10 –Post-Test Pull-Off Adhesion, 50/50 Water/Bitumen Immersion ........................................... 18 Figure 11 –Post-Test Pull-Off Adhesion, 15% Sodium Hydroxide Immersion ....................................... 18 Figure 12 –Post-Test Pull-Off Adhesion, 4% Citric Acid Immersion ...................................................... 18 Figure 13 –Post-Test Pull-Off Adhesion, 6% Sodium Hypochlorite Immersion ..................................... 19 Figure 14 –Graph of EIS Data on Pre-Test and Post-Test Immersion Samples ....................................... 20

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1.0 SCOPE

To evaluate Resimac Reischem 512UCEN Epoxy coating system per ISO 2812-1:2007 using test

conditions outlined in Section 2.

2.0 TESTING CRITERIA

Testing was performed on the supplied coating using the following methods:

Test Method Test Description Test Conditions Test Start Date

ISO 2812-1:2007, Method A

Immersion Testing, Single Phase Liquid

6% Hydrochloric Acid, 90°C for 30 days January 20, 2016

6% Sodium Hydroxide, 90°C for 30 days January 20, 2016

50% Produced Water & 50% Bitumen, 90°C for 30 days January 20, 2016

15% Sodium Hydroxide, 90°C for 30 days January 20, 2016

4% Citric Acid, 90°C for 30 days January 20, 2016

6% Sodium Hypochlorite, 90°C for 30 days January 25, 2016

Electrochemical Spectroscopy (EIS)

Impedance Determination 21°C, 3% NaCl, 0.01Hz February 19, 2016

ASTM D4541-09 Pull-Off Adhesion

21°C, Positest AT-A, 14 mm Dolly, 100 psi/sec Ramp Rate, Two Component Quick-Set Epoxy

February 22, 2016

TEST MODIFICATIONS

Chemical immersion testing per ISO 2812-1:2007 was tested using client selected chemicals.

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3.0 SAMPLES RECEIVED / APPLICATION & INSPECTION

The following is the list of samples received:

Table 1 – Samples Received

Name or Designation of Coating (If Known)

Number of Samples Received

Size of Samples Date Received Condition

Resimac Reischem 512UCEN Epoxy Dark Grey 22 2" x 5" x 1/4" 11-Dec-15 Fair

All test panels were prepared and supplied by Dalco Services Inc. for testing. Surface profile and

coating application were not inspected by ADANAC Global Testing & Inspection. No applicator

quality control notes were supplied.

4.0 SAMPLE PREPARATION & SELECTION

No sample preparation was required other than normal test procedures.

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5.0 TEST RESULTS

5.1 Chemical Immersion Table 2 – Summary of Chemical Immersion Results, 6% Hydrochloric Acid (ISO 2812-1:2007)

Sample #

Testing Phase

Dry Film Thickness1

(mil) Adhesion2 Blistering3 Colour4

(Change) Cracking

(Y/N) Rusting5

1 Pre-Test 36.3/51.5/41.7 8/6 None Grey N S10/G10/P10

Post Test 38.5/47.6/42.3 10/10 None Sv N S10/G10/P10


Post Test 34.7/44.2/39.3 6/6 F#2 Sv N S10/G10/P10



NOTES:

N/A – Not Applicable N/T – Not Tested Test temperature is set to (90±3)°C. 1 Film thickness measurement per ASTM D7091-13. Rating is Low/High/Average of at least five measurements. 2 Adhesion per ASTM D6677-07(2012). Rating is the value of both points of the X-cut. 3 Blistering evaluation per ASTM D714-02(2009). 4 Colour change evaluation per NACE TM0185-2006, Section 5.3.1. 5 Rusting evaluation per ASTM D610-08(2012).

Rating Key Colour Change (NACE TM0185-2006)

Adhesion (ASTM D6677-07(2012))

Rating: N Sl M Sv

Description: No change Slight change Moderate change Severe change

Rating: 10 8 6 4 2 0

Description: Extremely difficult to remove; ≤ 0.8 mm fragments Difficult to remove; 1.6 to 3.2 mm fragments Somewhat difficult to remove; 3.2 to 6.3 mm fragments Light pressure to remove; ≥ 6.3 mm fragments Easily removed or peeled; ≥ 6.3 mm fragments Easily peeled as one piece; ≥ 6.3 mm fragments

Blistering (ASTM D714-02(2009))

Rusting (ASTM D610-08(2012))

Size: #2 Large #4 Medium #6 Small #8 Very Small #10 None

Frequency: Dense D Medium Dense MD Medium M Few F None N

Rating: 10 9 8 7 6 5 4 3 2 1 0

Area: <0.01% 0.01% – 0.03% 0.03 – 0.1% 0.1– 0.3% 0.3 – 1.0% 1.0 – 3.0% 3.0 – 10.0% 10.0 – 16.0% 16.0 – 33.0% 33.0 – 50.0% >50%

Spot – S / General – G / PinPoint - P

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Table 3 – Summary of Chemical Immersion Results, 6% Sodium Hydroxide (ISO 2812-1:2007)

Sample #

Testing Phase

Dry Film Thickness1


(Change) Cracking

(Y/N) Rusting5


Post Test 36.3/40.6/38.4 10/10 M#6A N N S10/G10/P10


Post Test 33.9/40.6/37.6 10/10 None N N S10/G10/P10



NOTES:

N/A – Not Applicable N/T – Not Tested Test temperature is set to (90±3)°C. 1 Film thickness measurement per ASTM D7091-13. Rating is Low/High/Average of at least five measurements. 2 Adhesion per ASTM D6677-07(2012). Rating is the value of both points of the X-cut. 3 Blistering evaluation per ASTM D714-02(2009). 4 Colour change evaluation per NACE TM0185-2006, Section 5.3.1. 5 Rusting evaluation per ASTM D610-08(2012). A Blisters are only located in the upper portion of the sample.



Rating: N Sl M Sv


Rating: 10 8 6 4 2 0






Rating: 10 9 8 7 6 5 4 3 2 1 0

Area: <0.01% 0.01% – 0.03% 0.03 – 0.1% 0.1– 0.3% 0.3 – 1.0% 1.0 – 3.0% 3.0 – 10.0% 10.0 – 16.0% 16.0 – 33.0% 33.0 – 50.0% >50%


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Pre-Test Post Test

Figure 1 – Pre-Test and Post-Test Samples of 6% Hydrochloric Acid Immersion

Pre-Test Post Test

Figure 2 – Pre-Test and Post-Test Samples of 6% Sodium Hydroxide Immersion

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Table 4 – Summary of Chemical Resistance Results, 50/50 Water/Bitumen (ISO 2812-1:2007)

Sample #

Testing Phase

Dry Film Thickness1


(Change) Cracking

(Y/N) Rusting5


Post Test 23.2/36.2/29.2 8/8 None N NA S10/G10/P10


Post Test 24.6/40.6/31.5 8/8 None N NA S10/G10/P10



NOTES:

N/A – Not Applicable N/T – Not Tested Test temperature is set to (90±3)°C. 1 Film thickness measurement per ASTM D7091-13. Rating is Low/High/Average of at least five measurements. 2 Adhesion per ASTM D6677-07(2012). Rating is the value of both points of the X-cut. 3 Blistering evaluation per ASTM D714-02(2009). 4 Colour change evaluation per NACE TM0185-2006, Section 5.3.1. 5 Rusting evaluation per ASTM D610-08(2012). A Samples show general checking effect.



Rating: N Sl M Sv


Rating: 10 8 6 4 2 0






Rating: 10 9 8 7 6 5 4 3 2 1 0

Area: <0.01% 0.01% – 0.03% 0.03 – 0.1% 0.1– 0.3% 0.3 – 1.0% 1.0 – 3.0% 3.0 – 10.0% 10.0 – 16.0% 16.0 – 33.0% 33.0 – 50.0% >50%


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Table 5 – Summary of Chemical Resistance Results, 15% Sodium Hydroxide (ISO 2812-1:2007)

Sample #

Testing Phase

Dry Film Thickness1


(Change) Cracking

(Y/N) Rusting5


Post Test 36.3/41.6/39.1 10/10 M#6A N N S10/G10/P10


Post Test 31.1/40.2/35.0 6/6 M#6B N N S10/G10/P10


Post Test 30.4/37.4/34.0 6/6 F#6B N N S10/G10/P10

NOTES:

N/A – Not Applicable N/T – Not Tested Test temperature is set to (90±3)°C. 1 Film thickness measurement per ASTM D7091-13. Rating is Low/High/Average of at least five measurements. 2 Adhesion per ASTM D6677-07(2012). Rating is the value of both points of the X-cut. 3 Blistering evaluation per ASTM D714-02(2009). 4 Colour change evaluation per NACE TM0185-2006, Section 5.3.1. 5 Rusting evaluation per ASTM D610-08(2012). A Blisters are only located in the lower half of the sample. B Blisters are only located in the upper half of the sample.



Rating: N Sl M Sv


Rating: 10 8 6 4 2 0






Rating: 10 9 8 7 6 5 4 3 2 1 0

Area: <0.01% 0.01% – 0.03% 0.03 – 0.1% 0.1– 0.3% 0.3 – 1.0% 1.0 – 3.0% 3.0 – 10.0% 10.0 – 16.0% 16.0 – 33.0% 33.0 – 50.0% >50%


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Pre-Test Post Test

Figure 3 – Pre-Test and Post-Test Samples of 50/50 Water/Bitumen Immersion

Pre-Test Post Test

Figure 4 – Pre-Test and Post-Test Samples of 15% Sodium Hydroxide Immersion

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Table 6 – Summary of Chemical Resistance Results, 4% Citric Acid (ISO 2812-1:2007)

Sample #

Testing Phase

Dry Film Thickness1


(Change) Cracking

(Y/N) Rusting5







NOTES:




Rating: N Sl M Sv


Rating: 10 8 6 4 2 0






Rating: 10 9 8 7 6 5 4 3 2 1 0

Area: <0.01% 0.01% – 0.03% 0.03 – 0.1% 0.1– 0.3% 0.3 – 1.0% 1.0 – 3.0% 3.0 – 10.0% 10.0 – 16.0% 16.0 – 33.0% 33.0 – 50.0% >50%


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Table 7 – Summary of Chemical Resistance Results, 6% Sodium Hypochlorite (ISO 2812-1:2007)

Sample #

Testing Phase

Dry Film Thickness1


(Change) Cracking

(Y/N) Rusting5


Post Test 28.3/43.3/36.3 8/8 None M N S10/G10/P10





NOTES:




Rating: N Sl M Sv


Rating: 10 8 6 4 2 0






Rating: 10 9 8 7 6 5 4 3 2 1 0

Area: <0.01% 0.01% – 0.03% 0.03 – 0.1% 0.1– 0.3% 0.3 – 1.0% 1.0 – 3.0% 3.0 – 10.0% 10.0 – 16.0% 16.0 – 33.0% 33.0 – 50.0% >50%


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Pre-Test Post Test

Figure 5 – Pre-Test and Post-Test Samples of 4% Citric Acid Immersion

Pre-Test Post Test

Figure 6 – Pre-Test and Post-Test Samples of 6% Sodium Hypochlorite Immersion

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5.2 Pull-Off Adhesion Results Table 8 –Summary of Pull-Off Adhesion (ASTM D4541-09) on Treated Samples

Immersion Media

Sample #

Testing Phase

Test Site #

Pull-Off Value (psi)

Failure Mode Type

Coating Acceptable1 (Pass/Fail)

None 19 Pre-Test 1 3022 100% Glue N/A 2 3090 100% Glue N/A 3 1722 100% Glue N/A

6% HCl

1 Post-Test 1 1660 100% Glue N/A 2 1734 100% Glue N/A



6% NaOH




50/50 Water/

Bitumen




NOTES: N/A – Not Applicable Test Temperature: 23.2°C Test Relative Humidity: 15% 1 There is no Pass/Fail criterion unless otherwise specified by client. Failure Mode Rating Key – (estimate to the nearest 5%) A – Substrate, % amount B – Layer one, % amount C – Layer two, % amount etc Layer failure – A/B, B/C, etc, % amount GF - Glue failure, % amount

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Table 9 –Summary of Pull-Off Adhesion (ASTM D4541-09) on Treated Samples, Continued

Immersion Media

Sample #

Testing Phase

Test Site #

Pull-Off Value (psi)

Failure Mode Type

Coating Acceptable1 (Pass/Fail)

15% NaOH




4% Citric Acid




6% NaOCl




NOTES: N/A – Not Applicable Test Temperature: 23.2°C Test Relative Humidity: 15% 1 There is no Pass/Fail criterion unless otherwise specified by client. Failure Mode Rating Key – (estimate to the nearest 5%) A – Substrate, % amount B – Layer one, % amount C – Layer two, % amount etc Layer failure – A/B, B/C, etc, % amount GF - Glue failure, % amount

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Sample #19

Figure 7 –Pre-Test Pull-Off Adhesion

Sample #1 Sample #2 Sample #3

Figure 8 –Post-Test Pull-Off Adhesion, 6% Hydrochloric Acid Immersion


Figure 9 –Post-Test Pull-Off Adhesion, 6% Sodium Hydroxide Immersion

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Figure 10 –Post-Test Pull-Off Adhesion, 50/50 Water/Bitumen Immersion


Figure 11 –Post-Test Pull-Off Adhesion, 15% Sodium Hydroxide Immersion


Figure 12 –Post-Test Pull-Off Adhesion, 4% Citric Acid Immersion

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Figure 13 –Post-Test Pull-Off Adhesion, 6% Sodium Hypochlorite Immersion

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5.3 EIS Test Results

Figure 14 –Graph of EIS Data on Pre-Test and Post-Test Immersion Samples

Laboratory Test Results Evaluating Resimac Reischem ... · ASTM D4541-09 ; Pull-Off Adhesion ....

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