abl friction round-robin procedure: gas analysis (ga)

ABL Friction Round-Robin Procedure: Gas Analysis (GA)

Title: ABL Friction Round-Robin Procedure: Gas Analysis (GA)

No.: ETUG-152-GA Page: 1 of 13

Reference: UN Test 3 (b) (iv) Rev: 3 Date: 22 APR 2016

Operator/ Test Individual: Test Date:

THIS PROCEDURE CAN BE USED AS A COMPANION TO THE ABL FRICTION TRAINING MODULE AND TEST METHOD MATRIX

1.0 SCOPE

1.1 This document describes the basic safety requirements and procedures for conducting the ABL Friction Test for the Round Robin. Sample preparation, test configuration, and test operations are reviewed. The procedure for analyzing, evaluating and interpreting the data is also described. The explosive sample may be solid, slurry, powder, or granulated in form.

1.2 Material used for the 2015 Round Robin is 4 micron HMX from the same lot at the Orbital-ATK Bacchus site.

2.0 REQUIREMENTS

2.1 Copies of this procedure shall be made available in the testing area control room.

2.2 Persons conducting this test must be trained in this procedure and the applicable support procedures. The record of this training must be properly documented.

2.3 The qualification of personnel to perform this procedure shall be determined by the Testing Supervisor.

2.4 The general operating procedure for the testing area shall be the overall governing procedure and shall be followed in conjunction with the safety rules and techniques in this procedure.

3.0 APPLICABLE DOCUMENTS

3.1 General Operating Procedure for the test site (e.g. “Tooele Army Depot Standard Operating Procedure for Explosives Testing”, Rev 2 (2/26/13) or current revision)

3.1.1 Emergency/Disaster Plan for the test site.

3.1.2 Waste Disposal Procedure for the test site.

3.2 Explosives Spill Handling Procedure (e.g. SMS-144-TM, current revision)

3.3 Definition of Terms for Explosives (e.g. SMS-100-DEF, current revision)

3.4 Safety Data Sheet (SDS) for each material to be tested.

3.5 Approved test plans are applicable when used in conjunction with this procedure.

3.6 ETUG Procedure for ABL Friction Test Rev 2, October 2, 2014.

3.7 ABL Friction Machine Manual

3.8 Statistical Relative Comparison Method.

4.0 PERSONAL PROTECTIVE EQUIPMENT (PPE)

4.1 Equipment Description Use* Application

4.1.1 Conductive safety shoes X All steps

4.1.2 Safety glasses X All steps

4.1.3 Flame retardant lab coat or coveralls X All steps




4.1.4 Latex, Nitrile gloves, or similar gloves X Sample handling

4.1.5 *Legend: X–Required; O–Optional

5.0 SAFETY & HEALTH CONSIDERATIONS DATE COMPLETED

5.1 Review SDSs for safety and health considerations. ☐:_____________

5.2 Read, understand, and follow the safety requirements and the use of safety equipment as established in the general operating procedure for the area. ☐:_____________

5.3 Operators shall have read this procedure, accompanying test plan, if any, and the SDSs provided and know the hazards associated with the materials being handled. ☐:_____________

5.4 The test samples and flammable solvents should be kept in the sample prep area until needed for testing.

5.5 Safety Systems Function

5.5.1 Ground mats and wires Allow electrostatic charge to dissipate, preventing a dangerous accumulation and discharge of electrostatic energy that could ignite energetic materials.

6.0 MATERIALS AND EQUIPMENT LIST

6.1 Material Quantity / Description

6.1.1 Test material (HMX) 5 grams

6.1.2 Test material (other standard material) 5 grams

6.1.3 Sensitivity data sheet For recording results

6.1.4 Solvent Commercial grade acetone, methanol or equivalent.

6.1.5 Wiping tissues Kimwipes, Kleenex, or cheesecloth

6.1.6 Sample Applicator Template (included with sample shipment)

24 gauge thick (0.20”) with a rectangular hole (0.23” x 0.38”) to apply the sample in a uniform way; see video here: www.etusersgroup.org/round-robin-current

6.1.7 Normal 20# paper Paper to use to zero the pressure

6.1.8 Marker Black felt tip

6.1.9 Gloves Compatible with test sample and cleaning solvent

6.1.10 Respirator Personal air filter system for potentially contaminated air, as required

6.1.11 Ear plugs or similar Hearing protection, as required

6.1.12 Velostat container Conductive Velostat container with securable lid

6.2 Equipment Quantity / Description

6.2.1 ABL Friction Test Machine See UN Test 3 (b (iv) for more details

6.2.2 ABL Friction wheels Wheels are 2” diameter and 0.125” thick with Rockwell C 58-62 hardness and 1.27 – 1.78 µm (50 – 70 µin) surface roughness

6.2.3 ABL Friction anvils Anvils are 7” long and 2 ¼” wide with Rockwell C 55-62 hardness and 1.27 – 1.78 µm (50 – 70 µin) surface roughness

6.2.4 Hydraulic ram Up to 1000 psi pressure on the 1” diameter ram




6.2.5 Applicator spatula/ spoon Able to apply the sample as shown in the example video here: www.etusersgroup.org/round-robin-current

6.2.6 Reaction detection device Gas analyzer capable of detection of the CO concentration (in parts per million) with a sensitivity of at least 0.5 ppm CO.

6.2.7 Gas analyzer chamber Chamber drawings found on the website: www.etusersgroup.org/round-robin-current. Chambers can also be ordered online when ordering the HMX sample.

6.2.8 Temperature/Humidity probe Data record

6.2.9 Natural hair brush For cleaning of residual dust

7.0 MACHINE VERIFICATION

7.1 Complete the Operational Check Details Date Completed

7.1.1 Verify and document the proper surface finish on the anvil and insert

1.27 – 1.78 µm (50 – 70 µin) surface roughness ☐:_____________

7.1.2 Zero the pressure readout by completing the pressure calibration by placing a piece of paper between the wheel and anvil and just as the paper is barely contacted, the pressure gauge is reset to zero. Additional verification/documentation at other pressures can be completed using a load cell such as Interface Model LBMU coupled with the hand-held indicator (Model 9320). The force from the load cell would correspond to the pressure readout multiplied by the area of the ram (1” in dia).

Zero pressure is when the wheel just contacts the paper.

☐:_____________

7.1.3 Complete a Slide Contact Integrity Check:

Lower the wheel onto the plate at a position that is 9/16” from the edge of the anvil. The pressure at the ram should be 100 psi and the anvil dropped at 8 fps.

Record an image of the streak.

Check the wheel mark on the anvil for full, continuous, and smooth contact between the wheel and anvil. If check is unsuccessful make necessary adjustments including the checks detailed in 7.1.3.1 and 7.1.3.2 below.

An example satisfactory trace is shown in the picture below.

☐:_____________

7.1.3.1 If integrity check above (7.1.3) doesn’t yield a full, continuous, straight trace, check slider for tightness of fit in the guide bars to ensure minimal lateral movement. If tolerance is greater than 0.040” consult owner’s manual for adjustment guidelines.

☐:_____________




7.1.3.2 If integrity check above (7.1.3) doesn’t yield a full, continuous, straight trace, on the lateral and longitudinal traversing carriage use a feeler gauge and check the clearance of the dovetail components on the lower slide mechanism. The gap should be less than 0.010”.

☐:_____________

7.1.3.3 Care should be taken when loosening or tightening bolts as energetic material may be present in the threaded area. Water, acetone, or an equivalent solvent shall be used in the threaded areas to desensitize any energetic residue prior to loosening or tightening as necessary

7.2 Complete the Sliding Velocity Calibration Details Date Completed

7.2.1 If the sliding velocity calibration was performed more than 6 months ago, ensure that the pendulum speed is calibrated to 8 fps using the linear potentiometer.

Linear potentiometer and associated software provided with ABL Friction machine.

☐:_____________

8.0 GAS ANALYZER VERIFICATION

8.1 Verify Zero of the Gas Analyzer Details Date Completed

8.2 Attach a nitrogen bottle or other inert gas (no CO present) to the gas analyzer and allow gas to flow through it.

Follow the manufacturer’s instructions regarding operation and the inert gas flow rate and connection scheme.

☐:_____________

8.3 Once the inert gas is flowing, and any warm up time has been observed, ensure that the gas analyzer is reading zero for CO. If not follow the manufacturer’s instructions and zero the CO value.

For example: With the inert gas flowing, the above image shows a CO concentration of -0.2 ppm which is within the tolerance of zero. ☐:_____________




8.4 Verify Span of the Gas Analyzer Details Date Completed

8.5 Attach a span gas bottle with known concentration of CO to the gas analyzer and begin the flow.

Follow the manufacturer’s instructions regarding operation and the span gas flow rate and connection scheme.

☐:_____________

8.6 Verify that the concentration read by the gas analyzer is equal to the concentration on the calibration gas mixture (within the specified tolerance). If the value does not agree, follow the manufacturer’s instructions and set the CO value.

For example: With the gas composition of 1000 ppm CO (±2%) flowing, the monitor agrees with that value within the tolerance (1017). ☐:_____________

9.0 GAS ANALYZER REACTION THRESHOLD

9.1 Obtain Variation of CO Baseline Details Typical Variation

9.1.1 Run the gas analyzer for 3-5 minutes and note the fluctuation of the CO concentration reading. This fluctuation is the noise in the system. How much variation is in the CO reading, ±0.1, ±0.2 ppm or more? Record the variation in the reading in the column at right.

Typical variation of the CO reading in the CAI ZRE gas analyzer is 0.1 ppm.

9.2 Reaction Threshold Details

9.2.1 The threshold CO indicating a reaction or decomposition event has occurred is 1 ppm CO change over the CO variation

For example: if at a test level of 0.1 Joules the variation in the CO reading (as determined in Section 9.1) is 0.2 ppm, the reaction determination threshold is 1.2 ppm. If a CO ppm change of 1.2 ppm or greater is observed then the trial is labeled a reaction.




10.0 VERIFY SITE REPEATABILITY DETAILS DATE COMPLETED

Test a standard material such as PETN or RDX. Test the sample twice using the Bruceton Method and determine if the results are different (or not) using the SRC Method (see www.etusersgroup.org/round-robin-current for the details of the SRC Method)

10.1 Gas Analysis Detection Method Details Date Completed

10.1.1 Ensure that the gas analyzer has been zeroed and spanned for carbon monoxide (CO) according to Section 8 above.

Follow the manufacturer’s instructions to ensure proper function of the gas analyzer, including observance of a warm-up time. ☐:_____________

10.1.2 Ensure that the reaction threshold level for the concentration of CO has been determined as specified in Section 9 above.

☐:_____________

10.1.3 Ensure that the gas chamber is used. It should be the same configuration per the drawings on the website: www.etusersgroup.org/round-robin-current The chamber slides over the hydraulic ram and facilitates the collection of gases. The gas pickup line attaches in the back.

The chamber is used to ensure gases from any potential reaction reach the gas analyzer.

☐:_____________

10.1.4 Use the specified test levels at right (evenly spaced logarithmically) to complete the Bruceton testing. A trial is completed at one level and if a go occurs, the next test is completed at the next lowest level. If a no-go occurs, the test is completed at the next highest level. 30 trials are completed with a standard material such as PETN or RDX.

20, 25, 35, 45, 55, 70, 85, 110, 140, 180, 230, 295, 375, 480, 610, 780, 1000 psi. If the travel length is less than an inch at the higher pressures, note the actual travel length on the test data sheet. ☐:_____________

10.1.5 Apply the sample using a template that is 20 thousandths of an inch thick with a rectangular hole (0.23” x 0.38”). The sample is placed into the template and lightly tapped to distribute the sample uniformly without consolidation on the anvil. The edge of the template/ sample should be directly below the wheel so that as the wheel travels it contacts more of the sample.

The sample application template is shipped with the Round Robin sample.

☐:_____________

10.1.6 Review the example video of the sample being applied to the friction anvil.

The video can be found here: www.etusersgroup.org/round-robin-current ☐:_____________

10.1.7 A new surface at the wheel and anvil are used for each test. The wheel is indexed using the pins at the bulkhead and the anvil is indexed to a new location for each test.

☐:_____________




10.1.8 Perform 30 trials and record test pressures and test results. Use a gas analyzer to determine the CO concentration for each trial to determine if a reaction occurred using the above determined criteria (change of 1ppm plus the variation ppm level).

☐:_____________

10.1.9 Calculate the logarithmic Bruceton parameters (F50 and s-logistic) using the Statistical Relative Comparison (SRC) method as documented here: http://www.etusersgroup.org/wp-content/uploads/2011/05/StatisticalRelativeComparisonMethod.pdf.

Use 0.245 for , the impetus interval, which is the average spacing distance in natural log of psi units between the above test levels.

F50: __________

s(logistic): __________

10.1.10 An example 30 trial test using the negative or no-go results, the following table is obtained where the # indicates the number of no-go’s:

The F50 value is 3.807+0.245*(20/14+0.5) = 4.28 (or exp(4.20) = 72.2 psi) and slogistic is 1.62*0.245*((14*42-20*20)/(14*14)+0.029)*0.551 = 0.22 Here, ϵ is 3.807 [ln(45)] and δ is 0.245 (which is the interval in natural log units between the test pressures).

10.1.11 Wait at least 3 days after the first test of the repeatability verification before completing testing again with the same material under the same conditions.

The wait time is specified to ensure that the laboratory can repeat the test in a repeatable way.

Wait time: ___________

10.1.12 Repeat the testing completed in Sections 10.1.1 to 10.1.7 with the same material, conditions, and number of trials. Obtain the F50 and s-logistic parameters for the second test from the second set of test data.

F50: __________

s(logistic): __________

10.1.13 Determine if there are significant differences between the test results using the SRC method by determining the test statistic.

The test statistic:

𝑡 = |(𝐹501 − 𝐹502) √𝑠12+𝑠2

2

𝑛⁄ | ∙

0.551.

Where s is the logistic sigma (slogistic) mentioned in Section 10.1.7 and 10.1.8. n is the number of trials (30). t: _________

10.1.14 For example, if the F50 and sigma values are 4.28 and 0.22 respectively for the 1st test with the 2

nd test

yielding 4.0 and 0.3 from a Bruceton with 30 trials then the test statistic, t, is 2.27. The test statistic is a measure of the difference between the two sample’s test results.




10.1.15 If the test statistic is greater than 3.75 than the differences between the two trials are significant. Otherwise, the results do not indicate the results are significantly different and the site repeatability is verified.

The smaller the test statistic the more likely are the differences between results to be insignificant.

If the site repeatability is not verified, make necessary adjustments and repeat verification.

Verified?: Yes/No

Date: __________

11.0 ROUND ROBIN HMXSAMPLE RECEIPT AND PREPARATION

DETAILS DATE COMPLETED

11.1 Sample (4 micron HMX from the same lot at the Orbital-ATK Bacchus site) is received in a DOT-SP 8451 shipping container.

Laboratories must be party to DOT-SP 8451 to receive the 25 gram shipment. ☐:_____________

11.2 The sample is shipped wet and must be dried. Dry the sample in an oven for 20-24 hours at 50°C. ☐:_____________

11.3 Place 5-grams of sample material in a conductive Velostat container and secure the lid/cover. Label the container

☐:_____________

11.4 Prior to testing, condition the sample at 65-75°F and 10-45% relative humidity, if possible, for 2 hours prior to testing.

Annotate the conditions during the testing (rel. humidity and temperature) ☐:_____________

12.0 MACHINE VERIFICATION

12.1 Complete the Operational Check Details Date Completed

12.1.1 Verify and document the proper surface finish on the anvil and insert

1.27 – 1.78 µm (50 – 70 µin) surface roughness ☐:_____________

12.1.2 Zero the pressure readout by completing the pressure calibration by placing a piece of paper between the wheel and anvil and just as the paper is barely contacted, the pressure gauge is reset to zero.

Zero pressure is when the wheel just contacts the paper.

☐:_____________

12.1.3 Complete a Slide Contact Integrity Check:

Lower the wheel onto the plate at a position that is 9/16” from the edge of the anvil. The pressure at the ram should be 100 psi and the anvil dropped at 8 fps.

Record an image of the streak.

Check the wheel mark on the anvil for full, continuous, and smooth contact between the wheel and anvil. If check is unsuccessful make necessary adjustments including the checks detailed in 12.1.3.1 and 12.1.3.2 below.

An example satisfactory trace is shown in the picture below.

☐:_____________




12.1.3.1 If integrity check above (12.1.3) doesn’t yield a full, continuous, straight trace, check slider for tightness of fit in the guide bars to ensure minimal lateral movement. If tolerance is greater than 0.040” consult owner’s manual for adjustment guidelines.

☐:_____________

12.1.3.2 If integrity check above (12.1.3) doesn’t yield a full, continuous, straight trace, on the lateral and longitudinal traversing carriage use a feeler gauge and check the clearance of the dovetail components on the lower slide mechanism. The gap should be less than 0.010”.

☐:_____________

12.1.3.3 Care should be taken when loosening or tightening bolts as energetic material may be present in the threaded area. Water, acetone, or an equivalent solvent shall be used in the threaded areas to desensitize any energetic residue prior to loosening or tightening as necessary

12.2 Complete the Sliding Velocity Calibration Details Date Completed

12.2.1 If the sliding velocity calibration was performed more than 6 months ago, ensure that the pendulum speed is calibrated to 8 fps using the linear potentiometer.

Linear potentiometer and associated software provided with ABL Friction machine.

☐:_____________

13.0 COMPLETE BRUCETON TESTING WITH HMX





☐:_____________






☐:_____________

13.1.4 Use the specified test levels at right (evenly spaced logarithmically) to complete the Bruceton testing. A trial is completed at one level and if a go occurs, the next test is completed at the next lowest level. If a no-go occurs, the test is completed at the next highest level. 30 trials are completed with a standard material such as PETN or RDX.

20, 25, 35, 45, 55, 70, 85, 110, 140, 180, 230, 295, 375, 480, 610, 780, 1000 psi. If the travel length is less than an inch at the higher pressures, note the actual travel length on the test data sheet. ☐:_____________


The sample application template is shipped with the Round Robin sample. The sample is NOT consolidated or pressed in the template.

☐:_____________

13.1.6 Ensure that you have reviewed the example video of the sample being applied to the anvil.



☐:_____________

13.1.8 Perform 30 trials and record test pressures and test results. Use a gas analyzer to determine the CO concentration for each trial to determine if a reaction occurred using the above determined criteria (change of 1ppm plus the variation ppm level).

-

☐:_____________

13.1.9 Calculate the logarithmic Bruceton parameters (F50 and s-logistic) using the Statistical Relative Comparison (SRC) method as documented here: http://www.etusersgroup.org/wp-content/uploads/2011/05/StatisticalRelativeComparisonMethod.pdf.

Use 0.245 for , the impetus interval, which is the average spacing distance in natural log of psi units between the above test levels.

F50: __________

s(logistic): __________




13.1.10 An example 30 trial test using the negative or no-go results, the following table is obtained where the # indicates the number of no-go’s:

The F50 value is 3.807+0.245*(20/14+0.5) = 4.28 (or exp(4.20) = 72.2 psi) and slogistic is 1.62*0.245*((14*42-20*20)/(14*14)+0.029)*0.551 = 0.22 Here, ϵ is 3.807 [ln(45)] and δ is 0.245 (which is the interval in natural log units between the test pressures).

14.0 COMPLETE 60 TRIALS AT 180 PSI





☐:_____________



☐:_____________


The sample application template is shipped with the Round Robin sample. The sample is NOT consolidated or pressed in the template.

☐:_____________

14.1.5 Ensure that you have reviewed the example video of the sample being applied to the anvil.



☐:_____________




14.1.7 Perform 60 trials with the conditioned Round Robin sample at a pressure of 180 psi. Results are recorded. Use a gas analyzer to determine the CO concentration for each trial to determine if a reaction occurred using the above determined criteria (change of 1ppm plus the variation ppm level).

☐:_____________

14.2 Record the number of Go’s that occurred out of the 60 trials completed.

# of Go’s: _________

# of trials: _________

14.3 Submit this completed form/ procedure as well as results to the Round Robin coordinator, Clint Guymon, at [email protected].

The ETUG will compile the results and inform you of the results from the other laboratories. Agreement/ disagreement determined statistically with the SRC Method. ☐:_____________

15.0 CLEANUP PROCEDURE

15.1 Out-of-place, contaminated, or partially-reacted energetic materials shall be collected and addressed as soon as practical.

15.2 All energetic materials shall be placed in an appropriate day box for temporary (overnight) storage or returned to the magazine for long-term storage.

15.3 Tools and equipment are to be stored in the designated storage area when not in use.

15.4 Clean the floor using a broom and dust pan to sweep up any floor scrap in work areas and place into the designated collector.

15.5 Test areas shall be kept clean and orderly.

16.0 FORCED SHUTDOWN PROCEDURES

16.1 Condition Action

16.1.1 Lightning within 15 miles

Power failure and loss of backup diesel generator

Other site specific conditions

Follow the site specific instructions which may include:

1. SHUTDOWN: Bring operations to a safe stop, evacuate to a safe distance, and assess the situation.

2. Return energetic materials to appropriate designated storage locations if safe to do so.

3. Follow the area procedure for leaving energetic materials out overnight as appropriate.

RESUMING OPERATIONS: The test site director will direct the return to work once the forced shutdown condition is resolved.




17.0 GENERAL EMERGENCY PROCEDURES

17.1 Condition Action

17.1.1 Serious injury

Unplanned ignition/ initiation

Natural disaster

Follow the site specific instructions which may include:

1. SHUTDOWN: Bring operations to a safe stop, evacuate to a safe distance, and assess the situation.

a. The area SHALL be preserved until the investigation of the unplanned event is complete.

2. Render immediate aid as needed. 3. Contact emergency responders and seek for

medical attention as needed. 4. Contact supervision.

RESUMING OPERATIONS: The test site director will direct the return to work once operations are approved to resume.

18.0 REVISION CHANGES DATE

18.1 Revision 1 05 JUN 2015

18.1.1 Original document

18.2 Revision 2 10 SEP 2015

18.2.1 Changed testing from 230 psi to 180 psi in Section 14.

18.3 Revision 3 22 APR 2016

18.3.1 Added the following to Section 7.1.2:

“Additional verification/documentation at other pressures can be completed using a load cell such as Interface Model LBMU coupled with the hand-held indicator (Model 9320). The force from the load cell would correspond to the pressure readout multiplied by the area of the ram (1” in dia).”

18.3.2 Added the following to Section 8.3 “…and any warm up time has been observed….”

18.3.3 Added the following to the details of Section 10.1.1, 13.1.1, 14.1.1 “…including observance of a warm-up time”

abl friction round-robin procedure: gas analysis (ga)

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