Chemical Injection Mandrel Testing Report
Shell Offshore, Inc.
Attendees:
Steve Terrebonne, Roy Adams, Shell Deepwater Production
Barry C. Ellis, Seal-Tite® International
Enterra Chemical Injection Mandrel
Preheat, Inc.
Shawn Higganbotham, McMurry - Macco
This report is designed to explain the effects that were encountered when a trial application of Seal-Tite® sealant was applied to the chemical injection mandrel. The following test was performed at NOVA Technology Corporation's Lafayette facility on October 23, 1998.
The following is a sequential chain of events:
1. Mandrel was pre-heated to 150 degrees using Pre Heat, Inc. of Broussard, Louisiana.
2. Check valves on mandrel were removed to allow the installation of an altered fitting into the inlet port of the valve. (This fitting was a 1/2" NPT Nipple that was cut across the threads using a shop saw and then installed with a 1/2" collar.)
3. The check valves along with a supply line from a nitrogen source were installed. (At this time McMurry installed a spring loaded 2,000 psi internal valve Macco to simulate a back pressure from FTP/flow tubingpressure.) The manifold provided by FMC was used to simulate sub-surface fittings and restrictions that may be encountered in this system.
4. The nitrogen source was opened and an immediate leak was detectable at start up on the altered fitting.
5. The severity of the leak we created was very severe and it was doubtful that we could repair that large of a leak path. We proceeded with the test to show the effects of a severe leak in a chemical injection system.
6. We proceeded to pump MB 525 through the leak path to insure that the flow stream was clean and unobstructed. No pressure build-up was encountered at the pump.
7. We then mixed a solution of Seal-Tite® and MB 525 and pumped this solution into the leak path and attempted to seal the leak.
8. The severity of this leak did not allow us to seal the leak in this altered fitting.
9. The decision to replace the altered fitting with one that would leak without alteration was made to show the effects of Seal-Tite® sealing a leak.
10. A 1/2" NPT fitting was installed hand tight and then backed out two turns to allow a noticeable leak path when nitrogen was applied.
11. When nitrogen was applied to this fitting a very noticeable leak occurred.
12. When the pump was engaged using Seal-Tite® to pump into the leak path an immediate sealing of the leak occurred.
13. After the leak was repaired and pressure increased to 2,000 psi the internal valve opened allowing excess sealant to flow out into the tubing cavity.
14. A pressure test was done for 90 minutes against the 2,000 psi internal valve and no leak was found.
15. The internal valve was removed and a dummy valve was installed to allow increased pressure to be applied to 5,000 psi.
16. At 5,000 psi the Walther coupling provided by FMC started leaking and we were forced to reduce our pressure to 2,500 psi and monitor for leaks.
17. No leaks were found and the 2,000 psi internal valve was reinstalled and a flush procedure was applied to insure the chemical injection system was unobstructed and reusable. Upon inspection on the system it was discovered that the integrity of the Seal-Tite® seal was intact and the chemical injection system was unobstructed and usable.
18. The 2,000 psi internal valve was taken to McMurry Macco for inspection and reports indicate that the valve although had residual sealant was not affected or damaged in any way.
19. The manifold provided by FMC did not show any signs of residue in any of its components.
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Subsurface Safety ValveTesting Report
Pemex
Summary
At the Well Services Department of Pemex, Seal-Tite® cured a simulated severe leak in a subsurface safety valve. After curing the leak, Pemex was able to cycle the test valve repeatedly to verify that the valve was fully functional.
After the successful shop test, a leaking installed SCSSV was selected to verify the shop results in the field. The selected SCSSV was of a different manufacturer and type. The high viscosity oil used to maintain the valve open was displaced and sealant injected into the control line. Over a brief period of time, the leak was cured to a pressure of 5000 psi. After verifying the functionality of the valve, the pressure was reduced to the operating pressure of 3200 psi and the valve tied back into the main hydraulic control panel.
Cost Savings
As documented by Pemex, the typical repair cost for changing a leaking SCSSV is over US $243,000. Seal Tite was able to cure both the simulated SCSSV leak and the existing field SCSSV leak for a fraction of the cost of Pemex's typical repair cost.
Pemex SPE Paper
The results of Pemex's field and shop evaluation of the Seal-Tite® pressure activated sealant can be found in SPE Paper No. 59026. The paper is entitled, "Leak Sealant in Hydraulic Systems Minimizes Maintenance Costs in Offshore Wells". Miguel A. Mendoza and Javier Hernandez of Pemex prepared the SPE paper.
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Subsurface Safety Valve Testing Report
Petrobras
Summary
Petrobras personnel created simulated severe leaks in both wireline and tubing retrievable subsurface safety valves to test the ability of Seal-Tite® to cure the leaks using Seal-Tite's pressure activated sealant. Using procedures identical to procedures used in the field, the Seal-Tite® engineer was able to cure each simulated leak. Videos of the tests are included on Seal-Tite's CD-ROM. The Seal-Tite® seal was able to hold constant pressure at the maximum design pressure of 5,000 psi for the test components. The valves were fully functional after curing the leaks with the Seal-Tite® sealant. After dismantling the equipment, the Petrobras personnel verified that the sealant caused no adverse effects to any of the components.
Testing Procedures
The purpose of this testing was to determine the ability of the Seal-Tite® pressure activated sealant to cure simulated severe leaks in wireline and tubing retrievable subsurface safety valves. The tests were performed at Petrobras' facility in December, 1999.
Tubing Retrievable Valve
Petrobras removed the O-ring from the piston that activates the flapper valve. The O-ring is the primary seal for the piston. The secondary guide ring remained as the only sealing surface on the piston. The leak rate through the piston was 60 liters per hour.
Wireline Retrievable Valve
A grinder was used to severely damage both sets of V-packing on a wireline retrievable subsurface safety valve. The leak rate through the damaged V-packing was in excess of 80 liters per hour.
Leak Sealing Procedure
Initially, in each case, after creating the simulated leak paths, a flow of hydraulic fluid was established through the simulated leaks to verify the leak rates and the severity of each leak.
To duplicate the conditions of a typical hydraulic system, the sealant was pumped from the Seal-Tite® injection system through a simulated system of multiple valves and lengthy umbilical lines before being tied into the test valves.
For each valve, once the leak had been verified, the Seal-Tite® pressure activated sealant was injected. As the seal was established by the sealant polymerization process, the operation of the valve was monitored. For both valves, when the seal was able to withstand a pressure of 1500 to 2000 psi, the valve opened normally. Thereafter, the seal was allowed to cure for a brief period and the pressure was raised to the full operational pressure of 5000 psi. As a final test, the valves were cycled over ten times to verify that the full operation capabilities of the valves were maintained. Petrobras was able to cycle the valves with no loss of hydraulic fluid; thus, proving that the leaks were cured and the valves were fully operational.
Analysis of Dismantled Equipment
After the tests were concluded, the equipment was dismantled and examined. As reported by the testing personnel, the liquid sealant polymerized into a rubber-like substance within the damaged areas resulting in effective leak stoppage. The sealant was effective in curing the leaks in both the unsealed piston and the damaged V-packing. In each instance, the testing personnel found that the components were easily disassembled. No seizing between components occurred due to the presence of the polymerized Seal-Tite® sealant in the leak paths. Additionally, the Seal-Tite® sealant did not cause any damage to any of the test components.
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Umbilical Line Testing Report
Petrobras
Summary
Petrobras provided a damaged section of umbilical line to test the ability of Seal-Tite® to cure umbilical leaks using Seal-Tite's pressure activated sealant. Using procedures identical to procedures used in the field, the Seal-Tite® engineer was able to cure each simulated leak. The Seal-Tite® seal was able to hold constant pressure at the maximum design pressure of 5,000 psi until the end fitting of the umbilical failed and blew out. The Petrobras personnel verified that the sealant did not plug the umbilical line or any fittings.
Testing Procedures
The purpose of this testing was to determine the ability of the Seal-Tite® pressure activated sealant to cure simulated severe leaks in the fittings, connections and hose of an umbilical line. The line was weak and worn from prior use. The tests were performed at Petrobras' facility in December, 1999.
A hole was made in the umbilical using a 1/16 inch nail. A JIC connection was damaged. Due to the poor quality of the worn umbilical and fittings, it was expected that other leaks would appear.
Leak Sealing Procedure
As soon as HW525 fluid was pumped through the umbilical, leaks appeared through the nail hole and through the JIC connection. After the leaks were established, the sealant was pumped into the umbilical. As the injection pressure reached 1800 psi, the leak through the nail hole was sealed. As the injection pressure reached 2000 psi, three additional leaks appeared in the umbilical line. As additional sealant was pumped, the leak in the JIC connection was cured. By cycling the injection pressure between 1000 psi and 2500 psi, the leak rates were reduced and, after a few minutes, the remaining three leaks were cured. As pressure was increased to 3000 psi, a new leak appeared. Although the pressure dropped to 2000 psi, by continuing to pump sealant, the new leak was cured in less than ten minutes. As pressure was increased to 4500 psi, the last leak reappeared, but was quickly re-cured. Once all leaks were cured, the pressure was raised to 5000 psi. With the pressure stable at 5000 psi and all leaks cured, the end fitting of the umbilical line failed and catastrophically failed. No further test could be performed on the umbilical line due to the end fitting failure.
Analysis of the Umbilical Line
After the tests were concluded, the umbilical line and fittings were examined. As reported by the testing personnel, the liquid sealant polymerized and cured the leaks without plugging the umbilical line or fittings. Fluid was still able to flow through the umbilical line and out of the end of the line.
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Service Companies
Wellhead and Hanger Testing Report
Major Wellhead Manufacturer
Summary
Personnel from a major wellhead manufacturer created simulated severe leaks in wellhead components to test the ability of Seal-Tite® to cure the leaks using Seal-Tite's pressure activated sealant. Using procedures identical to procedures used in the field, the Seal-Tite® technician was able to cure each simulated
leak. The Seal-Tite® seal was able to hold pressure at the maximum design pressures of the test components. The test equipment included wellheads and other components rated at various pressures up to 15,000 psi. After dismantling the equipment, the manufacturer's personnel were unable to find that the sealant caused any adverse effects to any of the test components.
Testing Procedures
The purpose of this testing was to determine the ability of the Seal-Tite® pressure activated sealant to cure simulated severe leaks in wellhead hangers and other components. The tests were performed at the manufacturer's facility on August 19/20, 1999.
Manufacturer's personnel damaged seals and seal profiles to create leak that were at least as severe as is typically experienced in the field. A grinder was used to create the damage to the components.
Tested Wellhead Components
1. 7 1/16 Tubing Hanger-15,000 psi.
2. 13 5/8 Casing Hanger-3,000 psi. (w/ primary plate and tubing spool) (13 5/8 x 9 5/8)
3. 9 inch tubing head for storage well-5,000 psi.
Leak Sealing Procedure
Initially, in each case, after creating the simulated leak path, a flow of nitrogen was established through the simulated leak. The flow of nitrogen verified the severity of each leak.
The Seal-Tite® proprietary injection system was tied into the test port of the wellhead. Sealant was injected into nitrogen stream and pumped into the test port. Injection was regulated to establish a differential pressure of 500 psi to 1800 psi through the leak path.
The differential pressure through the leak caused the sealant to polymerize in the leak path. As resistance to the pumping indicated formation of a seal, the pumping rate was reduced with pumping continuing until a seal of the leak was established at the maximum allowed working pressures of the test components (3,000
psi/5,000 psi/15,000 psi). Once the maximum allowed working pressures was reached, sealant pumping was stopped and the seal allowed to cure. The Seal-Tite® injection system was rigged down.
After curing the seal, nitrogen alone was used to cycle pressure between zero pressure and the maximum allowed working pressures of the test components. By cycling the pressure using nitrogen, the manufacturer's personnel attempted to breach the Seal-Tite® seal and cause the leaks to reappear. Despite the cycling of pressure, the leaks did not reappear.
As a last step in the testing, a successful Bubble Test was performed on the 7 1/16 Tubing Hanger to the maximum allowed working pressure of 15,000 psi.
Analysis of Dismantled Equipment
After the tests were concluded, the equipment was dismantled and examined.
As reported by the testing personnel, the liquid sealant polymerized into a rubber-like substance within the damaged areas resulting in effective leak stoppage. The sealant was effective in both elastomer O-rings and metal to metal seals.
In each instance, the testing personnel found that the components were easily disassembled. No seizing between components occurred due to the presence of the polymerized Seal-Tite® sealant in the leak paths. Additionally, the Seal-Tite® sealant did not cause any damage to any of the test components.
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Subsea Control Valve Testing Report
Major Valve Manufacturer
Background
An operating company was experiencing a leak in a subsea control valve in the Gulf of Mexico. To verify that Seal-Tite® could cure the leak, the operator asked a major valve manufacturer in Houston to reproduce the leak and test the ability of Seal-Tite® to cure the simulated leak.
Test Procedures
A simulated leak was created in an identical subsea control valve by crimping the metal-to-metal seal that was the suspected source of the leak. The severity of the leak was verified by pumping nitrogen through the damaged valve while the valve was suspended in a vat of water. As shown on the video of the testing, the water roiled from the large quantity of escaping gas.
Once the leak had been verified, the Seal-Tite® pressure activated sealant was injected. A seal was quickly established by the sealant polymerization process. Thereafter, the seal was allowed to cure for a brief period and the pressure was raised to the full operational pressure of 5000 psi. To show the strength of the seal, the pressure on the valve was increased to 7000 psi. As a final test, the valve was cycled to verify that the full operation capabilities of the valve were maintained. The engineers were able to cycle the valve with no loss of hydraulic fluid; thus, proving that the leak was cured and the valve was fully operational.
Results
The simulated leak was cured and the Seal-Tite® seal was able to withstand a pressure of 7000 psi (2000 psi over normal working pressure).
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Subsea SCSSV Control Circuit Testing Report
Independent Oil Company and a Major Equipment Manufacturer
Background
An operating company was experiencing a leak in a subsea SCSSV control valve in the North Sea. Working with a major equipment manufacturer, the operator constructed a test assembly consisting of the components of the subsea SSSV control system including a tree cap, xmas tree, the subsea tree SSSV control circuit and an umbilical line. The operator wanted to verify that Seal-Tite® could cure the field leak without plugging vital components.
Tree Pressure Drop Test
One objective of the test was to ascertain the pressure drop occurring across a subsea control circuit at different flow rates. Seal-Tite® sealant was pumped through the test assembly at flow rates from 1.5 liters per minute to 4.0 liters per minute. The tubing hanger SSSV poppet (at the bottom of the tubing hanger) was left open to simulate a parted control line.
Pressure drops up to 320 psi were experienced in the test assembly at a flow rate of 4.0 liters per minute. Even at a pressure drop of 320 psi, no polymerization of the sealant was experienced in the test assembly. The sealant did not clog any components of the test assembly,
Seal-Tite® Sealant Test
Another objective of the test was to simulate a control line leak and attempt to seal the leak using Seal-Tite® pressure activated sealant. The first simulated leak was approximately 20 liters per minute and was created by cutting through the threads of an NPT blanking plug at the end of the control line. This leak was beyond the capabilities of the Seal-Tite® sealant.
The second simulated leak was created by loosening the NPT blanking plug at the end of the control line. The leak rate of 0.75 liters per minute at 2,000 psi was established through the leaking NTP plug. The sealant was pumped through the test assembly to the leaking NTP plug.
Within thirty minutes of commencing pumping of the sealant, the leak rate was noticeably diminished. Within one hour, the leak was sealed and the control line was holding 2,000 psi. After a brief curing time, the pressure was increased to 4,000 psi and remained stable through the end of the testing.
Conclusions
At pressure drops below 320 psi, the Seal-Tite® sealant will not plug any of the components of a subsea SSSV control circuit. The Seal-Tite® sealant is able to cure leaks of up to 0.75 liters per minute at 2,000 psi and establish a seal that is sufficient to hold at a pressure of 4,000 psi.
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Independent Testing
Filter Test-Gly-Flo
C.D.A. and Associates, Inc.
Analytical and Corrosion Services
P.O. Box 51641 Lafayette, La. 70505
Office 318-237-2342
Fax 318-237-8982
March 22, 1999
Test Report by Cedric D. Adams
Re: Report Number 990029
Specialized testing of Seal-Tite® sealant and HW-525
The following tests have been conducted to certify the capabilities and compatibility of the Seal-Tite® Gly-Flo sealant. The sealant was received by C.D.A. and Associates, Inc. as a field strength compound. The compound is referred to as Gly-Flo. The Gly-Flo mixture was reported to be 50 percent Seal-Tite® sealant and 50 percent HW-525.
Discussion of Test Results
The results of the individual tests are attached at the end of this report.
A. HW-525 Compatibility Test
The Seal-Tite® sealant was received already mixed into HW-525, therefore, to determine the compatibility of the Seal-Tite® sealant with HW-525, the Gly-Flo compound which had the appearance of a pink liquid suspension was centrifuged at 1,500 rpm for 5 minutes. The results indicated a minor separation at the top of the centrifuge tube of 10 % of the total volume. The separated liquid was a clear pink. The bottom of the tube contained 1.3 % white particles. The remaining liquid was stable.
The HW-525 compatibility test results are included in Attachment A.
B. Thermal Test
Thermal tests were performed at -1 °C (30 °F), 24 o C (75 o F), and 66 °C (150°F) to determine if the Gly-Flo and the HW-525 were stable at these various temperatures. The samples were inspected visually at 24 hours, at 48 hours, and at 72 hours. The results indicate that very little separation occurs in the HW-525 material or Gly-Flo material at -1 o C and at 24 o C.
At 66 o C, the HW-525 liquid turned green and had slight separation at the top. At 66 o C, significant separation occurs in the Gly-Flo material. Samples of each of the Gly-Flo layers were extracted and separately observed. The top layer was a clear dark pink liquid. The middle layer was an opaque pink liquid. The bottom layer was light pink liquid. Although each layer was a different color, the three layers seemed to have similar flow characteristics. Solids were not observed in any of the layers. The sample was briefly agitated using 50 shakes and the layering disappeared. The mixed liquid had the same general characteristics as the original sample of Gly-Flo.
The visual results of this test for the Gly-Flo material are shown in Figures 1, 2, 3, and 4. These figures show the samples at the start of the test, at 24 hours, at 48 hours, and at 72 hours. The same test was conducted on the HW-525 material. Figures 5, 6, 7, and 8 show the progress of HW-525 material at each time interval.
The thermal test results are included in Attachment B.
C. Viscosity Tests
The viscosity of the HW-525 and the Gly-Flo sealant were run at temperatures of -1° C (30 °F), 24 °C (75 °F), and 66 °C (150 °F). The viscosity values were reported in centipoise (cP) using a Fann model 39 viscometer, which was equipped with a temperature probe. The results indicated that the temperature did not significantly affect the viscosity of these liquids. The viscosity of the HW-525 ranged from 2.0 cP at 66 o C to 3.0 cP at -1 o C. These values were slightly less than the viscosity of the Gly-Flo, which was approximately 10.5 cP at all temperatures.
The viscosity test results are included in Attachment C.
D. Sea Water Compatibility Test
The Gly-Flo and the HW-525 were mixed 50/50 by volume into a synthetic seawater brine with a chloride content of approximately 35,000 mg/l. To determine the compatibility of the compounds with seawater the sample mixtures allowed to stand at room temperature for three days. The bottles were inspected at 24-hour intervals. Figures 9, 10, 11, and 12 show the samples at initial mix, at 24 hours, at 48 hours, and at 72 hours. The HW-525 became hazy immediately after mixing with the seawater. In Figure 10, it was clear that the HW-525 separated into two layers during the first 24 hours. The top 10% was a dark hazy blue while the remaining liquid was a clear light blue. The Gly-Flo in seawater showed a slight separation after 48 hours. The separation was at the top and was approximately 2 % of the total volume.
The sea water compatibility report is included in Attachment D.
E. Nylon Compatibility Test
Two samples of nylon were measured for thickness and weighed. One sample was immersed in the Gly-Flo and the second was immersed in HW-525. The samples were maintained at a temperature of 66 °C (150°F) for seventy-two (72) hours. After the 72-hour period the samples were again measured and weighed. The sample, which had been immersed in Gly-Flo, had a slight yellow tint. The sample had increased in weight from 1.8884 grams to 2.0332 grams or 7.7 %. The thickness of the sample had increased from 0.126 inches to 0.128 inches or 1.6 %. The sample, which had been immersed in HW-525, had a blue tint. The sample had increased in weight from 1.7991 grams to 1.9520 grams or 8.5 %. The thickness of the sample had increased from 0.126 inches to 0.129 inches or 2.4 %. There did not appear to be any changes in the mechanical integrity of the nylon samples. The nylon samples at the start of the test are shown in Figure 13. The samples at the end of the test are shown in Figure 14.
The test results are included in Attachment E.
F. Elastomer Compatibility Test
Samples of 90d elastomer were measured, weighed, and immersed in samples of the Gly-Flo and the HW-525. The samples were stored at a temperature of 66 °C (150°F) for seventy-two (72) hours. The elastomer samples were removed at the end of the test and again measured and weighed. The samples were also inspected for mechanical integrity. The results indicate that the elastomer sample immersed in the HW-525 increased slightly in diameter and weight. The weight increase from 0.5336 grams to 0.5573 grams represents an increase of 4.4 %. The diameter increase was from 0.101 inches to 0.102 inches or less than 1 %. The elastomer sample immersed in the Gly-Flo had no increase in diameter and an increase in weight from 0.4557 grams to 0.4635 grams or 1.7 %. The test conditions did not appear to affect the integrity of the two samples. The elastomer samples at the end of the test are shown in Figure 15.
The elastomer compatibility test results are included in Attachment F.
G. Bacterial Action Test
An active sulfate reducing bacteria culture (1,000,000 colonies/ml) was used for this test. The culture media, which contained the bacteria, was mixed 50/50 by volume with sterile water, HW-525, and Gly-Flo. The mixtures were allowed to stand at 35 o C (95 o F) for 2 hours. Standard serial dilutions were then made to six (6) bottles deep. The culture media was 3 % NaCl brine. The bottles were placed in an incubator at 35 o C (95 o F). The bottles were inspected for bacterial growth after seventy-two (72) hours. At the end of the 72 hour period, all test bottles had positive results. These results would indicate that neither the HW-525 nor the Gly-Flo is a deterrent to bacterial growth. The culture bottles at the end of the test are shown in Figure 16.
The bacteria test report is included in Attachment G.
H. Corrosion Test
Coupon samples of 316 stainless steel, 4140 carbon steel, 1045 carbon steel, and 15-5 ph stainless steel were measured, weighed, and immersed in Gly-Flo and in HW-525 at a temperature of 66 °C (150°F) for seventy-two (72) hours. The coupons were then processed as per NACE standard RP-07. The general corrosion rate was calculated based on weight loss. The pit depths were measured using an anvil micrometer and the pitting corrosion rate was calculated based on the pit depth.
Figures 17 and 18 show the test bottles at the beginning of the test while Figures 19 and 20 show the test bottles at the end of the test. It was noted that the Gly-Flo bottle containing the C-1045 coupon had become discolored during the test. There was a slight gray tint to the pink liquid.
Figures 21 and 22 show the C-4140 coupons at the beginning and at the end of the test. Coupon #11 was in the HW-525 and coupon #12 was in the Gly-Flo. The corrosion rate of the coupon in HW-525 (1.74 mpy) was slightly higher than the corrosion rate of the coupon that was in the Gly-Flo (1.17 mpy). Neither of the coupons had any signs of pitting; therefore, the pitting rates were zero.
Figures 23 and 24 show the C-1045 coupons at the beginning and at the end of the test. Coupon #1 was in the HW-525 and coupon #2 was in the Gly-Flo. The corrosion rate of the coupon in HW-525 (0.84 mpy) was slightly less than the corrosion rate of the coupon that was in the Gly-Flo (1.38 mpy). The coupon that was in the Gly-Flo was tarnished.
This surface discoloration is clearly seen in Figure 24. Neither coupon was pitted however and the pitting rate was zero.
Figures 25 and 26 show the 316L stainless steel coupons at the beginning and at the end of the test. Coupon #31 was in the HW-525 and coupon #32 was in the Gly-Flo. The corrosion rate of the coupon in HW-525 (0.54 mpy) was slightly higher than the corrosion rate of the coupon that was in the Gly-Flo (0.24 mpy). Both of these corrosion rates are extremely low. Neither of the coupons had any signs of pitting.
Figures 27 and 28 show the 15-5 ph stainless steel coupons at the beginning and at the end of the test. Coupon #1 was in the HW-525 and coupon #2 was in the Gly-Flo. The corrosion rate of the coupon in HW-525 was only 0.18 mpy and the corrosion rate of the coupon that was in the Gly-Flo was 0.0mpy. There was no pitting on these coupons. The results of the corrosion tests indicate that neither the HW-525 nor the Gly-Flo are very corrosive to the metals which were tested.
The corrosion test report is included in Attachment H.
I. Bio-degradation Test
A sample of the catalyzed Gly-Flo sealant was weighed and immersed in sea water at a temperature of 66 °C (150°F) for seventy-two (72) hours. At the end of the test the material was visually inspected for changes and re-weighted. The sample had lost a slight amount of weight. The original weight was 1.0384 grams. The final weight was 1.0131 grams. This represents a weight loss of 2.4 %. The sample, which had a slight pink color at the start of the test, appeared to have been bleached by the seawater. The material appeared to be chemically inert. The seawater, which had been clear at the start of the test, had a slight haze at the end of the test. The sample at the end of the test is shown in Figure 29.
The results of the bio-degradation test are included in Attachment I.
J. Falex, Pin-on-Vee Testing
The Falex Pin-on-Vee tests were conducted at The Lubrizol Corporation laboratories in Cleveland, Ohio. The testing was under the direction of Thomas Derevjanik, research engineer and group leader of the mechanical production bench testing department. All tests were observed by Cedric D. Adams.
The test results include the initial and final temperature of the liquid, the true fail load in pounds and the type of failure. The report shows that the HW-525 had a torque type failure at 2300 pounds of load. The Gly-Flo had a wear type failure at 2700 pounds of load. The Falex test apparatus is shown in Figure 30.
A close-up of the pin and vee block is shown in Figure 31. Figure 32 shows the technician conducting the test. A close-up of a new vee block, pin, and shear pin are shown in Figure 33. The vee block and pin after the test with Gly-Flo are shown in Figure 34. The wear on the pin is obvious. The pin from the HW-525 test is shown in Figure 35. The shear pin had sheared in the test due to torque failure. The test procedure and test results are included in Attachment J. Also included is a technical paper "Falex Procedures for Evaluating Lubricants" by F. A. Faville and W. A. Faville published in the Journal of the American Society of Lubrication Engineers, August, 1968, which describes the test in detail and describes the interpretations of the test results.
K. Filter Test
The filter test, which has been developed by Seal-Tite®, was performed to determine if the sealant would plug restrictions in a system. The test apparatus is shown in Figure 36. The Gly-Flo sealant was pumped from a reservoir through a 40-micron filter at low flow rates for 3 minutes. The filter and filter housing are shown in Figures 37 and 38. A differential pressure of approximately 50 psi was noted across the filter but no plugging took place. When the flow rate was increased using an electric pump the differential pressure increased to greater than 100 psi. This high differential pressure shut down the pump but did not plug the 40-micron filter. if you have any questions or if I may be of further assistance, please do not hesitate to call.
Cedric D. Adams
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Specialized Test-Gly-Flo
C.D.A. and Associates, Inc.
April 14, 1999
Re: Report Number 990367, Filter Test
Addendum to Report Number 990029, Specialized testing of Seal-Tite® sealant and HW-525
The filter test was conducted to certify the capabilities of the Seal-Tite® Gly-Flo sealant. This test completes the series of tests performed with the Gly-Flo sealant. The sealant was received by c.d.a. and associates, inc. as a field strength compound. The compound, which is referred to as Gly-Flo, was reported to be 50 percent Seal-Tite® sealant and 50 percent HW-525.
Filter Test
The filter test, which was developed by Seal-Tite®, was performed to determine if the Gly-Flo sealant would plug restrictions or mesh filters in a system. The apparatus used for this test consisted of a reservoir for the Gly-Flo sealant, a liquid transfer pump, a filter housing, and a downstream reservoir to collect the Gly-Flo, which had been pumped through the filter. The sealant was pumped through a 10-micron filter at a flow rate of 3 to 4 gallons per minute for 1 hour. It was noted that, during this period the upstream pressure varied slightly as the flow rate varied, however, the maximum pressure noted was slightly less than 50 psi. At the end of the test, the filter housing was opened and the filter was removed. Figure 1 shows the filter in the filter housing at the end of the test. Figure 2 shows the filter as compared to a new filter. There was some liquid on the filter surface; however, no solid material or plugging was noted.
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