Astm 2017-D6278 PDF
Astm 2017-D6278 PDF
Astm 2017-D6278 PDF
for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
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This test method is under the jurisdiction of ASTM Committee D02 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
Subcommittee D02.07 on Flow Properties. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Jan. 1, 2017. Published February 2017. Originally the ASTM website.
approved in 1998. Last previous edition approved in 2012 as D6278 – 12ɛ1. DOI: 3
Available from CEC Secretariat, Interlynk Administrative Services, Ltd., Lynk
10.1520/D6278-17E01. House, 17 Peckleton Lane, Desford, Leicestershire, LE9 9JU, United Kingdom.
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cooling vessel is through a three-way stopcock of the same nozzle orifice (1). Vres does not include the atomization
design used on the discharge of the fluid reservoir. If using a chamber volume. When the residual undrained volume is
rate-dependent chiller, the exterior cooling jacket shall be known, go to 10.4.
supplied with an adjustable volume of cold water. 10.2.2 To determine residual undrained volume, first re-
move as much fluid as possible by briefly running the pump.
7. Materials
10.2.3 Remove the high-pressure lines (16) in Fig. A1.1,
7.1 Diesel Fuel (No. 2), initially required to adjust the diesel and drain. Remove the plug at the end of the pump gallery to
injector nozzle valve opening pressure. drain the remaining oil in the pump. Drain atomization
7.2 Calibration Fluid RL233, used to ensure that when the chamber (2).
apparatus is adjusted to within a prescribed pressure range, the 10.2.4 Reassemble the system and close all drains. The
correct viscosity loss is obtained. upper three-way stopcock (6) shall be open to the lower
reservoir (7) and the lower three-way cock (8) shall be open to
NOTE 8—RL233 meets the requirements of this test method and is
acceptable during a transition period between suppliers. See research the pump suction (10).
report for details.6 10.2.5 Add 170 mL of RL233 calibration oil to the lower
reservoir (7) and observe the level. Start the pump and run for
8. Hazards several minutes until the oil is transparent and free of sus-
8.1 Warning—Use a safety shield between the high-pressure pended air.
components and the operator during use of equipment. 10.2.6 Stop the pump. Drain the fluid in the atomization
8.2 Precaution—During operation, the line between the chamber into a beaker and then pour the fluid back into the
pump and nozzle, ((16) in Fig. A1.1), is under a pressure of at lower reservoir; draining to waste will result in an error in the
least 13.0 MPa (130 bar, or 1885 psi). Pressures above the measurement of Vres. Allow the system to drain for 20 min and
upper limit of 18.0 MPa (180 bar or 2611 psi) are possible if free air trapped in the transparent connecting tube between the
filter plugging occurs. Shut off the pump prior to tightening any lower reservoir and pump.
fitting that is not properly sealed. 10.2.7 Observe the difference in oil level in the lower
reservoir compared to that noted in 10.2.5. Record this differ-
9. Sampling ence as the residual volume, Vres.
9.1 Approximately 600 mL of fluid is needed per test. NOTE 9—Undrained residual volumes of 15 mL to 30 mL have been
9.2 The test fluid shall be at room temperature, uniform in reported by various users of this test. Vres measurements in excess of this
may occur when fluid in the atomization chamber is not poured back into
appearance, and free of any visible insoluble material prior to the lower reservoir as in 10.2.6, or if the length of line (10) is excessive.
placing in the test equipment.
10.2.8 Calculate the run volume, Vrun, which is the subtrac-
9.3 Water and insolubles shall be removed before testing, or
tive difference between 170 mL and Vres.
filter blocking and nozzle wear may occur. Filter blocking can
be detected by a sudden change in gauge pressure. The 10.3 Warm-up—A half-hour warm up period is required
transport of insolubles to the shear zone will shorten nozzle before proceeding to calibrate with RL233. Set the stroke
life. counter shut-off to 30 times n strokes, and start the pump.
10. Calibration and Standardization NOTE 10—This warm-up period is only required for the first within-day
calibration.
10.1 Nozzle Adjustments—If the nozzle to be used is new or
has not been pre-calibrated, adjust the diesel injector nozzle 10.4 Cleaning the Apparatus, Setting the Stroke Counter,
holder with the nozzle in place. Adjust the nozzle using diesel and Adjusting the Pump Stroke:
fuel and a nozzle tester so that the valve opening pressure is 10.4.1 Drain residual oil by way of drain line (19) from the
13.0 MPa (1885 psi) under static conditions. If the nozzle has atomization chamber into a waste container. Drain fluid in the
been pre-calibrated with RL233 calibration oil, adjust the valve cooling jacket by means of stopcock (6) (Fig. A1.1) and the
opening pressure to the calibration pressure prescribed, which fluid reservoir by means of stopcock (8), into suitable waste
must be between 13.0 MPa and 18.0 MPa (2611 psi). containers.
10.1.1 Install the nozzle and the nozzle holder in the test 10.4.2 After fluid has drained, leave the stopcock on the
apparatus. The pintle/spray nozzle shall be tightly fitted in the drain line to the atomization chamber open and the three-way
chamber to avoid leakage of oil around the external surface of stopcock (6) positioned so that fluid in the cooling jacket drains
the spray nozzle. to a waste container. Position stopcock (8) so that the drain is
10.2 Measurement of Residual Undrained Volume, Vres: closed but the fluid reservoir is open to pump suction through
10.2.1 The residual undrained oil volume of the system is line (10). Add a minimum of 50 mL of RL233 to the fluid
the volume of the system between the three-way stopcock reservoir.
below the fluid reservoir (8) in Fig. A1.1, and the injector NOTE 11—Steps 10.4.2 – 10.4.7 are representative of the first and
second purges with 50 mL fluid that are needed to remove used oil from
the apparatus prior to calibration and testing. For these steps, the stopcock
6
Supporting data have been filed at ASTM International Headquarters and may below the atomization chamber and cooling jackets are set so that oil will
be obtained by requesting Research Report RR:D02-1629. flow into waste containers.
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10.4.3 Free the apparatus of air in the line by use of the 10.4.21 When the volume in the fluid reservoir is not within
venting screw (14) and by manual compression of the trans- 62.5 mL of Vtot, drain the fluid from the cooling jacket back
parent flexible tube that connects the pump to the fluid into the fluid reservoir, adjust the pump stroke by means of the
reservoir. pump adjustment screw (12), and repeat steps beginning with
10.4.4 Set the stroke counter so that the pump will run a 10.4.16.
sufficient length of time to evacuate the fluid out of the fluid 10.5 Removal of Fluid—Open the stopcock below the at-
reservoir. omization chamber and drain to waste. Drain the fluid from the
10.4.5 Start the pump. Observe the fluid level in the cooling jacket into a waste container. Position stopcock (8) so
reservoir and stop the pump when all the fluid is out of the base that all fluid in the fluid reservoir is removed to a waste
of the reservoir but is still fully-retained in line (10). container. When drainage is complete, position stopcock (8) so
10.4.6 Add a minimum of 50 mL of RL233 fluid to the fluid that the drain is closed and the pump inlet line (10) is open.
reservoir a second time and operate the pump until the fluid
10.6 Calibration with RL233:
reservoir is empty but line (10) is still filled with fluid.
10.6.1 Ensure that the ambient (room) temperature is be-
10.4.7 After all oil has drained, close the stopcock on the tween 20 °C to 25 °C.
atomization chamber drain line (19), position stopcock (6) so 10.6.2 Add a minimum of 50 mL of RL233 to the fluid
that fluid will flow from the cooling jacket into the fluid reservoir. Position the three-way stopcock (6) in Fig. A1.1,
reservoir. below the cooling vessel to discharge fluid into a suitable waste
10.4.8 Remove the thermometer or temperature probe from container and leave the stopcock open below the atomization
the fluid reservoir. chamber. Operate the pump until the fluid reservoir is empty
NOTE 12—The thermometer and assembly can interfere with the but line (10) is still filled with fluid.
obtainment of accurate volume measurements in the fluid reservoir, hence 10.6.3 Free the apparatus of air in the line by manual
its removal is called for when the accurate determination of fluid volume compression of the flexible tube that connects the pump to the
is needed. A thermocouple or thermistor probe is a suitable alternative to fluid reservoir. When necessary, venting screw (14) is also used
a thermometer.
for this purpose.
10.4.9 Add a minimum amount of fluid equal to the sum of 10.6.4 Add a minimum of 50 mL of test fluid to the fluid
30 mL plus Vrun, determined in 10.2.8, to the fluid reservoir. reservoir a second time and operate the pump until the fluid
10.4.10 Close the stopcock below the atomization chamber reservoir is empty again but line (10) is full.
drain line (19) and position stopcock (6) so that the fluid will 10.6.5 Close the stopcock below the atomization chamber,
drain from the cooling jacket into the fluid reservoir. position the stopcock below the fluid reservoir so that the line
NOTE 13—The atomization chamber drain line is always closed for the
to the pump is open, and retain the position of the stopcock
third cleaning run and all test runs. below the cooling jacket so that the first 50 mL of RL233 can
be drained into a waste container.
10.4.11 Free the apparatus of air in the line by manual
10.6.6 Place a volume of RL233 in the fluid reservoir equal
compression of the flexible tube (10) that connects the pump to
to Vrun plus 30 mL.
the fluid reservoir. The venting screw (14) is also used for this
10.6.7 Start the pump, and stop the pump when there is a
purpose.
50 mL drop of fluid in the fluid reservoir. After draining is
10.4.12 Record the number on the stroke counter. complete, re-position the stopcock below the cooling jacket so
10.4.13 Use a stopwatch or other timing device and run the subsequent fluid flows directly into the fluid reservoir.
pump for 1 min 6 1 s. Record new counter value, n. 10.6.8 Set the stroke counter for automatic shutoff at the
10.4.14 Determine n, the difference in the stroke count from required number of impulses (30 multiplied by n impulses per
10.4.12 and 10.4.13 as follows: minute). The flow rate will be 170 mL ⁄min as set in 10.4.
n 5 n2 2 n1 (1) 10.6.9 Adjust, if necessary, the volume of fluid in the fluid
reservoir to Vrun.
10.4.15 Set the stroke counter shutoff to the product of three 10.6.10 Place the temperature measuring device in the fluid
times n. The pump shall run for 3 min. Obtain a timing device reservoir, and start the pump.
to observe the time the stroke counter is on to ensure n is 10.6.11 After about 10 min of operation, adjust the water
correct. Start the pump and allow oil to circulate until the flow to control the fluid temperature at 30 °C to 35 °C, as
impulse counter shuts down the instrument. measured at the discharge point of the fluid reservoir. Approxi-
10.4.16 When all fluid has drained, adjust the volume of oil mately 10 min of operation will be required before the tem-
in the fluid reservoir so that the volume is equal to Vrun. perature can be stabilized.
10.4.17 Set the impulse counter to 0.5 (n). 10.6.12 At approximately ten cycles of operation, record the
10.4.18 Close stopcock (6) so that fluid will be stored in the gauge pressure reading to the nearest 0.1 MPa, when a
cooling jacket after the pump is started. glycerol-filled pressure gauge is being used, or to 0.01 MPa,
10.4.19 Start the pump. When the pump stops and draining when an electronic pressure device is employed.
is complete, subtract the volume now in the fluid reservoir 10.6.13 After 30 cycles has elapsed and the pump has
from Vrun. stopped, open the stopcock below the atomization chamber and
10.4.20 If the difference is within 62.5 mL of one-half of drain fluid into a waste container. Open the three-way stopcock
the total volume (Vtot = Vrun + Vres), proceed to 10.6. below the fluid reservoir and discharge the first 10 mL to
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15 mL as waste in order to flush out the drain line. Discharge 10.7.1 Calibration with RL233 Fluid—Frequent testing of
the remaining fluid into a clean sample container. After the the apparatus with the calibration oil is recommended. The
fluid has drained, close the three-way stopcock. apparatus must be recalibrated after 540 test cycles.
10.6.14 Remove the thermometer or temperature probe. 10.7.2 Calibration with RL233 and Monitoring System Sta-
10.6.15 Using Test Method D445, determine the kinematic bility and Precision with a Quality Control Oil per Practice
viscosity at 100 °C of unsheared (untested) RL233, as well as D6299—A quality control oil can be used to monitor calibra-
the sheared fluid from 10.6.13. Use the same viscometer tube tion once the nozzle has been calibrated with RL233 fluid. This
for the measurement of each oil. Quality Control fluid shall have a new oil kinematic viscosity
10.6.16 Calculate viscosity loss (VL) as follows: at 100 °C of between 14.0 mm2/s to 17.0 mm2/s and after test
kinematic viscosity decrease at 100 °C of between 2.0 mm2/s
VL 5 Vu 2 Vs (2)
and 3.0 mm2/s. The base oil for this fluid shall have a kinematic
where: viscosity of between 4.0 mm2/s to 8.0 mm2/s at 100 °C. The
Vu = kinematic viscosity of unsheared oil at 100 °C, mm2/s, calibration procedure is as follows:
and 10.7.2.1 Calibrate with RL233.
Vs = kinematic viscosity of sheared oil at 100 °C, mm2/s. 10.7.2.2 Monitor stability and precision of the system
through QC sample testing per Practice D6299, paragraph 7.1.
10.6.17 VL for RL233 shall be within the range of
This will initially require 15 in control samples to develop a
2.70 mm2/s to 2.90 mm2/s at 100 °C at a gauge pressure
control chart.
reading between 13.0 MPa and 18.0 MPa, as recorded after
10.7.2.3 The quality control oil shall be run on the same day
10 min of test time. If this is achieved, the gauge pressure
that a test fluid is evaluated.
recorded in 10.6.12 will subsequently be referred to as the
10.7.2.4 Any deviation or trend indicated in the control
calibration pressure.
chart shall call for a recheck with RL233 fluid. A recheck with
10.6.18 If VL is less than 2.7 mm2/s, increase the gauge
RL233 must be done after 7 days even if no recheck has been
pressure. If VL is greater than 2.9 mm2/s, reduce the gauge
called.
pressure, provided that the gauge pressure recorded in 10.6.12
is greater than 13.0 MPa and less than 18.0 MPa. To alter the NOTE 17—The reproducibility and repeatability reported in the test
pressure, remove the dust cover of the spray nozzle holder (see method is based on data obtained when the test instruments were
calibrated on a daily basis with RL233.
Fig. A1.4), loosen the locking nut, and turn the adjustment
screw that regulates valve opening pressure. Then, tighten the
11. Procedure
locking nut and replace the dust cover. The nozzle and nozzle
holder need not be removed from the apparatus. Upon retesting 11.1 Flow Rate Adjustment for Test Oil—Open the stopcock
RL233, the values shall be within the tighter range of on the atomization chamber and drain any previous fluid out of
2.75 mm2/s to 2.85 mm2/s at 100 °C at a gauge pressure the chamber. Position the three-way stopcock ((6) in Fig. A1.1)
reading between 13.0 MPa and 18.0 MPa, as recorded after below the cooling jacket to discharge fluid into a suitable waste
10 min of test time. container. Then, position stopcock (8) so that the drain line is
closed but line (10) is open from the fluid reservoir to the
NOTE 14—It is extremely important that the locking nut be completely
pump.
tightened. When it is not, some leakage of fluid around the outside of the
nozzle assembly may occur. This may result in a reduction of mechanical 11.1.1 Add a minimum of 50 mL of test fluid to the fluid
shearing for some oils, which can adversely influence precision. This reservoir.
condition can be monitored by use of a recorder and an electronic pressure 11.1.2 Free the apparatus of air in the line by manual
measurement device. Leakage results in a sudden drop in pressure when compression of the flexible tube that connects the pump to the
fluid bypasses the nozzle orifice.
fluid reservoir. When necessary, the venting screw (14) is also
10.6.19 When VL is greater than 2.85 mm2/s at a gauge used for this purpose.
pressure of only 13.0 MPa, pre-condition the nozzle by substi- 11.1.3 Operate the pump until the fluid reservoir is empty,
tution of a fully-formulated engine lubricant as the test fluid. but line (10) is full.
The stroke counter shut-off shall be adjusted so that the test 11.1.4 Add a minimum of 50 mL of test fluid to the fluid
time is at least 8 h, instead of 30 min. Upon retesting RL233 reservoir a second time and operate the pump until the fluid
the values shall be within the tighter range of 2.75 mm2/s to reservoir is empty again but line (10) is still full.
2.85 mm2/s at 100 °C at a gauge pressure reading between 11.1.5 After draining is complete, close the stopcock on the
13.0 MPa and 18.0 MPa, as recorded after 10 min of test time. atomization chamber and position stopcock (6) so that fluid
NOTE 15—Suitable break-in oils include fully-formulated SAE 15W-40 will flow from the cooling jacket into the fluid reservoir.
heavy-duty engine lubricants. 11.1.6 Add an amount of test fluid to the fluid reservoir
10.6.20 When viscosity decrease is below 2.75 mm2/s at a equal to the sum of 30 mL plus Vrun.
gauge pressure of 18.0 MPa, another nozzle shall be installed 11.1.7 Free the apparatus of air in the line by use of the
and the calibration procedure shall be repeated. venting screw (14) and by manual compression of the flexible
tube that connects the pump to the fluid reservoir.
NOTE 16—Before calibration with a new nozzle, it is advisable to 11.1.8 Set the stroke counter to the product of three times n.
subject the nozzle to at least a 4 h run-in with break-in oil. The pump shall run for 3 min. Obtain a timing device to
10.7 Calibration Period: observe the time the stroke counter is on to ensure n is correct.
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Start the pump and allow oil to circulate until the impulse 15 mL as waste in order to flush out the drain line. Discharge
counter shuts down the instrument. the remaining fluid into a clean sample container. Remove the
11.1.9 Adjust the oil level in the fluid reservoir to Vrun by thermometer assembly or probe.
draining any excess oil to a waste container, or adding oil when 11.2.11 Using Test Method D445, determine the kinematic
needed. viscosity at 100 °C of unsheared (untested) test fluid, as well as
11.1.10 Set the impulse counter to the product of 0.5 times the sheared fluid from 11.2.10. Use the same viscometer tube
n. for the measurement of each oil.
11.1.11 Close stopcock (6) so that fluid will be stored in the
cooling jacket after the pump is started. 12. Calculation
11.1.12 Start the pump. When the pump stops, subtract the 12.1 Calculate the percent viscosity loss (PVL) of the
volume now in the fluid reservoir (7) from Vrun. sheared oil as follows:
11.1.13 When the difference is within 6 2.5 mL of half of PVL 5 100 3 ~ V u 2 V s ! /V u (3)
Vtot , proceed to 11.2.
11.1.14 If the volume in the fluid reservoir is not within6 where:
2.5 mL of Vtot, adjust the pump stroke slightly by means of the Vu = kinematic viscosity of unsheared oil at 100 °C, mm2/s,
pump adjustment screw (12) drain the fluid from the cooling and
jacket into the fluid reservoir, and repeat steps beginning with Vs = kinematic viscosity of sheared oil at 100 °C, mm2/s.
11.1.9.
13. Report
11.2 Removal of Fluid—Leave stopcock below atomization
13.1 Report the following information:
chamber closed. Drain the fluid from the cooling jacket into a
13.1.1 The calibration pressure, in MPa.
waste container then re-position the stopcock so that the fluid
13.1.2 Kinematic viscosity of the unsheared oil at 100 °C.
will flow into the fluid reservoir. Then open the three-way
13.1.3 Kinematic viscosity of the sheared oil at 100 °C.
stopcock below the fluid reservoir to discharge fluid into a
13.1.4 Percent viscosity loss (PVL) as calculated in 12.1.
waste container.
11.2.1 Test Oil Evaluation—Re-position stopcock (8) so that 14. Precision and Bias
line (10) is open. Leave the stopcock below the atomization
chamber closed. Re-position stopcock (6) below the cooling 14.1 The precision of this test method as determined by the
jacket so that the first 50 mL of test oil is sent to a waste statistical examination of interlaboratory test results is as
container. follows:7
14.1.1 Repeatability—The difference between successive
11.2.2 Place a volume of test oil in the fluid reservoir equal
test results, obtained by the same operator with the same
to Vrun plus 30 mL.
apparatus under constant operating conditions on identical test
11.2.3 Free the apparatus of air in the line by manual
material would, in the long run, and in the normal and correct
compression of the flexible tube that connects the pump to the
operation of the test method, exceed the following values only
fluid reservoir. When necessary, the venting screw (14) is also
in one case in twenty:
used for this purpose.
1.05 %
11.2.4 Start the pump, and stop the pump when there is a 50
14.1.2 Reproducibility—The difference between two single
mL drop of fluid in the fluid reservoir. When draining is
and independent results, obtained by different operators work-
complete, re-position the stopcock below the cooling jacket so
ing in different laboratories on identical test material would, in
subsequent fluid flows directly into the fluid reservoir.
the long run, and in the normal and correct operation of the test
11.2.5 Set the stroke counter for automatic shutoff at the
method, exceed the following values only in one case in
required number of impulses (30 multiplied by n impulses per
twenty:
minute).
2.68 %
11.2.6 When necessary, adjust the volume in the fluid
reservoir to Vrun. NOTE 19—The indicated repeatability and reproducibility values for
11.2.7 Insert the thermometer assembly or temperature PVL represent the subtractive difference between the reported percent
kinematic viscosity loss values for the two determinations being com-
probe in the fluid reservoir. pared.
11.2.8 Start the pump.
11.2.9 Within the first 10 min, adjust the water flow to 14.2 Bias—All test results are relative to those of the
control the fluid temperature at 30 °C to 35 °C, as measured at calibration fluid. Therefore, no estimate of bias can be justified.
the discharge point of the fluid reservoir. 15. Keywords
NOTE 18—It is not necessary to record the gauge pressure reading here, 15.1 diesel injector apparatus; mechanical shear stability;
which may differ from the previously recorded calibration pressure.
polymer containing fluid; viscosity loss
11.2.10 After 30 cycles has elapsed and the pump had
stopped, open the stopcock below the atomization chamber and 7
Supporting data have been filed at ASTM International Headquarters and may
drain fluid into a waste container. Open the three-way stopcock be obtained by requesting Research Report RR:D02-1426. Contact ASTM Customer
below the fluid reservoir and discharge the first 10 mL to Service at [email protected].
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D6278 − 17´1
ANNEX
(Mandatory Information)
A1. EQUIPMENT
NOTE 1—Legend
(1) Spray Nozzle
(2) Atomization chamber
(3) Outlet of the atomization chamber
(4) Distributor plate
(5) Fluid cooling vessel
(6) Three-way cock downstream of glass
(7) Fluid reservoir
(8) Three-way cock downstream of glass container
(9) Support column
(10) Connection with pump-suction opening
(11) Double-plunger injection pump
(12) Pump setting screw
(13) Electric motor
(14) Venting screw/pump
(15) Stroke counter
(16) Pressure tubing from pump to injector
(17) Return line for overflowing liquid
(18) Pressure sensing device
(19) Drain line of atomization chamber
FIG. A1.1 Apparatus for Shear Stability Testing
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FIG. A1.3 Atomization Chamber with Spray Nozzle and Nozzle Holder
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SUMMARY OF CHANGES
Subcommittee D02.07 has identified the location of selected changes to this standard since the last issue
(D6278 – 12ɛ1) that may impact the use of this standard. (Approved Jan. 1, 2017.)
(1) Editorial revisions to meet Form and Style requirements. (8) Revised 11.1.8 to read like 10.4.15.
(2) Updates to Section 10, Calibration and Standardization. (9) Revised 11.1.13 and 11.1.14 to Vtot.
(3) Moved 10.4 and Note 10 to 10.3. (10) Revised 11.1.14 to repeat back to 11.1.9 to match calibra-
(4) Revised 10.4.20 to define Vtot. tion steps.
(5) Deleted former 10.6.12.1 (redundant statement). (11) Revised Fig. A1.1 with corresponding edits to the legend
(6) Revised 10.7.1 to clarify 540 test cycles. and text.
(7) Updated Section 11, Procedure.
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