Designation: D7891 − 15

Standard Test Method for

Shear Testing of Powders Using the Freeman Technology
FT4 Powder Rheometer Shear Cell1
This standard is issued under the fixed designation D7891; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope 1.5 Units—The values stated in SI units are to be regarded

1.1 This method covers the apparatus and procedures for as standard. No other units of measurement are included in this
measuring the incipient failure properties of a powder as a standard.
function of the normal stress for a given level of consolidation. 1.6 This standard does not purport to address all of the
The method also allows the further determination of the safety concerns, if any, associated with its use. It is the
unconfined yield strength, internal friction angles, cohesion, responsibility of the user of this standard to establish appro-
flow function, major principal stress and wall friction angle priate safety and health practices and determine the applica-
(with the appropriate wall coupon fitted to the correct acces- bility of regulatory limitations prior to use.
sory).
2. Referenced Documents
1.2 These parameters are most commonly used for the
design of storage hoppers and bins using industry standard 2.1 ASTM Standards:
calculations and procedures. They can also provide relative D653 Terminology Relating to Soil, Rock, and Contained
classification or comparison of the flow behavior of different Fluids
powders or different batches of the same powder if similar D2216 Test Methods for Laboratory Determination of Water
stress and shear regimes are encountered within the processing (Moisture) Content of Soil and Rock by Mass
equipment. D3740 Practice for Minimum Requirements for Agencies
Engaged in Testing and/or Inspection of Soil and Rock as
1.3 The apparatus is suitable for measuring the properties of Used in Engineering Design and Construction
powders with a maximum particle size of 1 mm. It is possible D6026 Practice for Using Significant Digits in Geotechnical
to test powders which have a small proportion of particles of 1 Data
mm or greater, but they should be present in the bulk sample as D6128 Test Method for Shear Testing of Bulk Solids Using
no more than 5 % of the total mass in samples with a normal the Jenike Shear Cell
(Gaussian) size distribution. D6682 Test Method for Measuring Shear Stresses of Pow-
1.4 All observed and calculated values shall conform to the ders Using Peschl Rotational Split Level Shear Tester
guidelines for significant digits and rounding established in D6773 Test Method for Bulk Solids Using Schulze Ring
Practice D6026. Shear Tester
1.4.1 The procedures used to specify how data are collected/
recorded or calculated, in this standard are regarded as the 3. Terminology
industry standard. In addition, they are representative of the 3.1 Definitions—For definitions of common technical terms
significant digits that generally should be retained. The proce- in this standard, refer to Terminology D653.
dures used do not consider material variation, purpose for 3.2 Definitions of Terms Specific to This Standard:
obtaining the data, special purpose studies, or any consider- 3.2.1 conditioning, v—in powders, the process of homog-
ations for the user’s objectives; and it is common practice to enizing the stress of a powder specimen by use of a specialized
increase or reduce significant digits of reported data to be blade attachment.
commensurate with these considerations. It is beyond the scope
3.2.2 wall friction coupon, n—in powders, a test piece used
of this standard to consider significant digits used in analysis
in the wall friction test that is manufactured from a material
methods for engineering design.
that represents the material of construction of the silo/bin/
hopper that stores the powder.
1
This test method is under the jurisdiction of ASTM Committee D18 on Soil and
Rock and is the direct responsibility of Subcommittee D18.24 on Characterization 4. Summary of Test Method
and Handling of Powders and Bulk Solids.
Current edition approved March 1, 2015. Published March 2015. DOI: 10.1520/ 4.1 Selection of the Appropriate Testing Regime—The par-
D7891-15. ticular consolidating stress level or levels used to evaluate the

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

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 D7891 − 15
flow properties of the powder will depend on the reason for dependent on the competence of the personnel performing it, and the
generating the data, as outlined in Section 5, and should suitability of the equipment and facilities used. Agencies that meet the
criteria of Practice D3740 are generally considered capable of competent
broadly reflect the stresses that the powder will be subjected to and objective testing/sampling/inspection/etc. Users of this test method
in its processing environment. are cautioned that compliance with Practice D3740 does not in itself
4.2 Preparation of the specimen—The specimen is added to assure reliable results. Reliable results depend on many factors; Practice
D3740 provides a means of evaluating some of those factors (4).
the test vessel and its mass determined using the instrument’s Practice D3740 was developed for agencies engaged in the testing
built-in balance. The selected test program is then initiated and and/or inspection of soil and rock. As such it is not totally applicable to
runs independently of the operator other than the interchange agencies performing this test method. However, users of this test method
of the spindle-mounted attachments for different sections of the should recognize that the framework of Practice D3740 is appropriate for
test. The powder first undergoes a conditioning cycle using the evaluating the quality of an agency performing this practice. Currently
there is no known qualifying national authority that inspects agencies that
blade attachment which removes any variability introduced perform this test method.
during filling or from the material’s previous history. The
piston attachment is then fitted and is used to compress the 6. Apparatus
powder to the required consolidating stress as determined in 6.1 The FT4 Powder Rheometer is shown in Fig. 1. It is a
the selected test program. Excess powder is then removed from computer-controlled instrument which simultaneously mea-
the test cell by means of a leveling assembly to leave a sures the force and torque required to mobilize a powder
specimen of compressed powder with a level surface that is contained in a range of vessel types using a series of spindle-
ready for shear testing. The shear head is then fitted to the mounted attachments driven by an electric motor located on a
instrument. carriage, driven by another electric motor, which moves the
4.3 Measurement of Shear Stress—The instantaneous shear attachments in the vertical direction.
stress is then measured by re-establishing the consolidating 6.1.1 The force is measured by a force transducer located
stress with the shear head and then pre-shearing the specimen beneath and fixed to the table that supports the test vessel
until a steady state condition is reached. The powder is then during the measurement process.
subjected to a reduced normal load and then sheared until the 6.1.2 The torque (shear resistance) is evaluated by measur-
shear force reaches a maximum and then decreases. ing the moment on the attachment using a torque transducer.
4.4 Measurement of Wall Friction as a Function of Normal 6.2 The shear cell vessel is shown in Fig. 2. It consists of a
Stress—The same specimen preparation method is used for this serrated base, made from a suitable engineering plastic such as
test, but a wall friction attachment, fitted with a coupon polyoxymethylene (POM), onto which are mounted two boro-
representing the material against which the powder is required silicate glass cylinders (50-mm × 85-mL vessel) connected by
to flow, is used instead of a shear head. a POM leveling assembly.
6.2.1 The shear cell vessel is located on the powder rheom-
5. Significance and Use eter using a POM clamp ring.
5.1 The test can be used to evaluate the following: 6.2.2 A POM funnel is also fitted to assist with the filling of
5.1.1 Classification or Comparison of Powders—There are the vessel.
several parameters that can be used to classify powders relative 6.3 Attachments are fitted to the powder rheometer to
to each other, the most useful being the measured shear facilitate various test procedures.
stresses, cohesion, flow function and angle of internal friction. 6.3.1 The first is a twisted blade (shown in Fig. 3(A)) that is
5.1.2 Sensitivity Analysis—The shear cell can be used to used to condition the test specimen thus generating a repeatable
evaluate the relative effects of a range of powder properties stress condition within the powder.
and/or environmental parameters such as (but not limited to)
NOTE 2—This conditioning process eliminates the effects of the
humidity, particle size and size distribution, particle shape and powder’s history and also any operator-induced effects generated during
shape distribution, moisture content and temperature. the filling process.
5.1.3 Quality Control—The test can, in some circumstances, 6.3.2 The second (Fig. 3(B)) is a compaction piston that
be used to assess the flow properties of a raw material, compresses the specimen to achieve the desired consolidating
intermediate or product against pre-determined acceptance normal stress.
criteria. 6.3.3 The third (Fig. 3(C)) is a shear head consisting of 18
5.1.4 Storage Vessel Design—Mathematical models exist blades that are used to generate shearing within the powder.
for the determination of storage vessel design parameters 6.3.4 The fourth (Fig. 3(D)) is a wall friction head and an
which are based on the flow properties of powders as generated interchangeable coupon representing the material of construc-
by shear cell testing, requiring shear testing at a range of tion against which the powder will be required to flow.
consolidating stresses as well as the measurement of the wall 6.3.5 All of the attachments (Fig. 3) are made from stainless
friction angle with respect to the material of construction of the steel and stainless steel+anodized aluminum.
storage vessel. The methods are detailed in Refs. (1-3).2
NOTE 3—The blades located in the shear head are thin and thus
NOTE 1—The quality of the result produced by this test method is relatively sharp. Care must be taken when handling the shear head to
prevent skin abrasions and cuts.
2
The boldface numbers in parentheses refer to a list of references at the end of 6.4 Additionally, it is possible to employ shear cells with 10
this standard. mL and 1 mL capacity in conjunction with the FT4 Powder

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 D7891 − 15

FIG. 1 FT4 Powder Rheometer (The left hand image shows the instrument with the shear head fitted; the right hand image shows the
shear head and shear cell vessel.)

operation of the 10-mL shear cell is identical to that described

herein for the 85-mL shear cell but using a smaller shear cell
and range of attachments. The limit on the maximum particle
size is commensurately reduced to a maximum particle size of
0.5 mm. The 1-mL shear cell uses a significantly different cell
design and attachments, which is beyond the scope of this
standard.

7. Preparation of Apparatus
7.1 Since the integrity of the blades within the shear cell
head is critical to generating accurate and reliable data, handle
the shear head with care, store it in the case provided and
inspect it for damage at regular intervals.
7.2 Make sure that the shear cell vessel components and the
spindle-mounted attachments are clean and free from grease
and other contaminants (5).
7.3 The following items are required to assemble the shear
cell vessel: two 50-mm × 85-mL glass cylinders, a 50-mm
serrated base; a 50-mm clamp ring; a 50-mm leveling assem-
bly; and a 50-mm funnel. These items are shown in Fig. 4. A
fully detailed assembly procedure is also available (6).
7.4 To assemble the shear cell vessel, position the clamp
ring approximately 1 mm from the end of one of the glass
cylinders and loosely fit the clamp ring onto the glass cylinder
FIG. 2 Shear Cell Vessel (Fig. 5). The clamp ring must not project past the end of the
glass cylinder, otherwise misalignment may occur. Make sure
that the gap in the clamp ring is approximately centralized with
Rheometer if the quantity of available test specimen is less than the printing on the glass cylinder. Secure the clamp ring using
85 mL (at the chosen consolidation stress). The mode of the hex driver ensuring that the screw is not over tightened.

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 D7891 − 15

FIG. 3 Spindle-Mounted Attachments Used in Shear and Wall Friction Tests: Blade (A); Vented Piston (B); Shear Head (C); Wall Friction
Head (D)

FIG. 4 Components Required to Assemble the 50-mm × 85-mL Shear Cell Vessel

7.5 Locate the serrated base into the glass cylinder adjacent 7.6 Open the leveling assembly and place it on top of the
to the clamp ring. Carefully rotate the serrated base to make glass cylinder at the opposite end to the clamp ring and serrated
sure that the entire circumference is in contact with the glass base. Make sure that the gap in leveling assembly is approxi-
cylinder (Fig. 6). mately in line with the gap in the clamp ring.

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 D7891 − 15
9. Procedure
9.1 With the assembled shear cell vessel (Section 7) located
on the instrument table, tare (zero) the mass of the empty shear
cell vessel using the built-in balance prior to filling with the test
specimen.
9.2 Once tared, remove the shear cell vessel for filling.
9.3 Fill the tared shear cell vessel with sufficient powder
such that, following the compression stage, the specimen is not
compressed below the split level of the leveling assembly.
NOTE 6—The amount of specimen required depends on the compress-
ibility of the particular powder and the consolidating stress level chosen
for the test. If the powder’s compressibility with respect to the consoli-
dating stress is known from a previously completed compressibility test
(8), the required mass of uncompressed powder can be determined based
FIG. 5 Fitting the Clamp Ring on the chosen consolidating stress of the shear test.
NOTE 7—If the level of the powder is below the level of the leveling
assembly following the compression phase, the test should be classified as
a failure and re-run with a greater starting volume.
9.4 Return the filled shear cell vessel and securely fasten it
7.7 Carefully invert the glass cylinder, clamp ring, serrated
to the instrument table using the clamping assembly. The mass
base and leveling assembly and place on the edge of a flat
of the powder specimen is then registered within the data file
surface (Fig. 7) so that the glass cylinder can be fitted flush
associated with the test.
with the inner face of the leveling assembly without impedi-
ment from the upper part of the leveling assembly. 9.5 Measurement of Shear Stress:
7.8 Push down gently on both the glass cylinder and the 9.5.1 Select the appropriate test program from the program
leveling assembly so that they are both flush with the flat library. There are four standard test programs available which
surface. are based on consolidating stresses of 3, 6, 9 and 15 kPa. These
programs can be modified if other consolidating stresses are
7.9 Tighten the leveling assembly with the hex driver such required.
that the leveling assembly and the glass cylinder are securely
located. NOTE 8—For advanced users the test method can be modified in detail
with respect to shear rate, number and length of pre-shear cycles. These
7.10 Confirm that the glass cylinder and leveling assembly options are detailed in Annex A1 and Ref. (9).
are flush, and check that the leveling assembly operates 9.5.2 Once selected, the test program will display images of
smoothly. the correct test vessel and attachment that are required to
7.11 Close the leveling assembly. commence the test. For a shear test, the shear cell vessel and
blade are used for initiating the preparation of the sample.
7.12 Place the other 50-mm × 85-mL glass cylinder into the 9.5.3 Push the start button on the computer screen to
top half of the leveling assembly and gently rotate the upper commence the test program which will cause the blade to be
glass cylinder to make sure that it is in contact with the glass slowly lowered into the shear cell vessel after which it will
cylinder below. perform a conditioning cycle by traversing through the powder
7.13 Tighten the leveling assembly with the hex driver such along a prescribed helical path.
that the leveling assembly and the upper glass cylinder are 9.5.4 Once the conditioning cycle is complete and the test
securely located (Fig. 8). has been automatically paused, exchange the blade attachment
for the vented piston attachment following the on-screen
7.14 Place the funnel on top of assembled shear cell vessel instructions.
(Fig. 9) and locate on the FT4 Powder Rheometer.
9.5.4.1 After the exchange has been confirmed, the program
NOTE 4—The assembled shear cell vessel is described as a 50-mm will continue by moving the vented piston attachment into the
× 85-mL split vessel assembly, which indicates the glass cylinders’ shear cell vessel to compress the powder until the target
internal diameter and the precise volume of the lower section of vessel consolidating stress has been achieved and held for 60 seconds.
with the base fitted.
9.5.5 Once the compression cycle is complete and the test
has been automatically paused, remove the funnel.
8. Calibration and Standardization
9.5.6 After confirming this step, use the leveling assembly
8.1 Calibrate the instrument in accordance with the manu- to separate and remove the excess powder left in the upper
facturer’s instructions. section of the shear cell vessel, and collect it in a suitable
container.
NOTE 5—The force and torque transducers located within the instru-
ment are calibrated using proprietary fixtures in conjunction with calibra- 9.5.7 Leaving the leveling assembly in the open position,
tion masses that are supplied with the instrument. (7) replace the vented piston with the shear head.

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FIG. 6 Fitting the Serrated Base

FIG. 7 Fitting the Leveling Assembly

9.5.8 Move the shear head to the surface of the powder at a 9.5.11 Repeat 9.5.9 and 9.5.11 a maximum of ten times or
speed of 0.5 mm/s and then slowly move it down at a until two consecutive steady state shear stress values are within
maximum speed of 0.08 mm/second until the target consoli- 1 % of each other.
dating stress is re-established and held for 60 seconds.
9.5.9 Perform a pre-shearing cycle by rotating the shear NOTE 9—If convergence does not occur in ten cycles, the powder is
unstable, possibly due to degradation within the shear zone and may mean
head within the powder at a fixed rate of 18 degrees/min while
that the powder is not suitable for shear testing.
maintaining the target consolidating stress until steady state
NOTE 10—The operator may modify the test programs to utilize
shear stress has been achieved. alternative pre-shearing schemes if required (Annex A1).
9.5.10 Stop rotating the shear head in the direction of shear
and establish a zero torque level by rotating in the opposite 9.5.12 Once the pre-shear requirements are met, initiate the
direction. shear testing cycle.

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 D7891 − 15

FIG. 8 Fitting the Upper Glass Cylinder

an integer value which is ~70-80 % of the consolidating stress)

and hold for 20 seconds while maintaining zero torque.
9.5.12.2 Re-initiate shear until a maximum shear stress is
achieved and the shear stress has subsequently reduced.
NOTE 11—The maximum shear stress recorded is the peak shear point
for the selected normal stress.
9.5.13 Re-establish the consolidating stress and then re-
initiate a single pre-shearing cycle.
9.5.14 Once steady state pre-shear has been re-established at
the consolidating stress, use the program to select another
lower normal test stress and repeat 9.5.13 and 9.5.14.
9.5.15 Repeat 9.5.12 to 9.5.15 until the program has com-
pleted all the test conditions that have been specified.
9.5.16 The standard test routines contain five measurement
points between ~20-80 % of the consolidating stress, but the
operator can modify the program to utilize additional or
alternative measurement points if required.
9.6 Measurement of Wall Friction:
9.6.1 The measurement of wall friction follows a similar
protocol to the measurement of the powders’ shear stress
except that, instead of using the shear head, an attachment is
used, which has been fitted with a 48-mm diameter coupon of
the material of construction to be evaluated.
NOTE 12—This material represents the wall of a storage vessel (or other
FIG. 9 Shear Cell Vessel Located on Instrument Table Prior to powder processing equipment) against which the powder will be required
Taring (Zeroing) of the Empty Shear Cell Vessel Mass to interact.
9.6.2 Make sure that the selected wall material coupon is
9.5.12.1 Reduce the normal stress on the specimen to a clean, dry and free of any surface contaminants.
pre-selected value lower than the consolidating stress (typically 9.6.3 Repeat 9.1 to 9.5.6.

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 D7891 − 15
9.6.4 Once the compression cycle is complete and the 3·T
τ5 (2)
instrument has paused the test program, remove the funnel. 2·π·r 3
9.6.5 Use the leveling assembly to separate and remove the
where:
excess powder left in the upper section of the shear cell vessel,
which is collected in a suitable container. τ = shear stress (kPa)
T = measured torque (Nm)
9.6.6 Leaving the leveling assembly in the open position,
r = radius of the shear head (m)
replace the vented piston with the wall friction attachment.
9.6.7 Move the wall friction attachment to the surface of the 10.4 Use pro-rating, if necessary, to compensate for slight
powder, then move the head further down at a maximum speed changes in pre-shear stress during a series of shear measure-
of 0.08 mm/second until the target consolidating stress is ments. Pro-rating involves recalculating the shear stress for
re-established and held for 60 seconds. each test point using the following formula:
9.6.8 Perform a pre-shearing cycle by rotating the wall τ p average
friction attachment against the powder at a fixed rate of 18 τ s,pro2rated 5 τ s 3 (3)
τp
degrees/min while maintaining the target consolidating stress
until a steady state shear stress has been achieved. where:
9.6.9 Stop rotating the wall friction attachment in the τs,pro-rated = pro-rated shear stress (kPa)
direction of shear and establish a zero torque level by rotating τs = measured shear stress (kPa)
in the opposite direction. τp average = average of all pre-shear shear stresses (kPa)
τp = measured pre-shear shear stress preceding shear
NOTE 13—The standard wall friction programs have a single pre-shear step (kPa)
as a default setting.
10.5 Plot the pre-shear point and all the valid shear test
9.6.10 Reduce the normal stress on the specimen to a
points as normal stress/shear stress data pairs (Fig. 10). Draw
pre-selected value lower than the consolidating stress and hold
a least mean squares, linear regression line through the test
for 20 seconds while maintaining zero torque.
points, and extrapolate this line to the normal stress level of the
9.6.11 Re-initiate shear until a maximum shear stress is
pre-shear point and, in the opposite direction, to meet the
achieved and the shear stress has subsequently reduced.
y-axis (where the normal stress is zero). This line is known as
9.6.12 Maintain shear for 45 seconds such that the kine-
the yield locus. The angle that the yield locus makes with the
matic shear stress can be calculated.
horizontal axis in known as the angle of internal friction and is
9.6.13 Stop rotating the wall friction attachment in the
designated as φ. The point at which the yield locus crosses the
direction of shear and establish a zero torque level by rotating
y-axis is known as the cohesion, C.
in the opposite direction.
9.6.14 Establish the next normal stress level and re-initiate 10.6 Check to make sure that the yield locus passes above or
rotation of the wall friction attachment. through the pre-shear point. If it passes below the pre-shear
9.6.15 Repeat 9.6.13 and 9.6.14 until all the test conditions point, scrutinize the individual test points to make sure that
have been completed. they are valid or re-run the test.
9.6.16 The standard test routines contain five measurement 10.7 Draw a Mohr stress circle such that its center is located
points between ~20-80 % of the consolidating stress, but the on the x-axis, it is tangential to the yield locus, and the origin
operator can modify the program to utilize additional or is a point on the circle. The non-zero intersection of this circle
alternative measurement points if required. with the x-axis defines the unconfined yield strength, fc.

10. Calculation or Interpretation of Results 10.8 Draw a second Mohr stress circle such that its center is
located on the x-axis, it passes through the pre-shear point, and
10.1 Record the force, torque and position values generated it is tangent to the yield locus. This circle intersects the x-axis
during the test program. at two positions—the greater of which defines the major
NOTE 14—This data, which is stored in a computer file, can be principal stress, σ1, seen in the powder at this level of
evaluated using the software program Data Analysis, which is provided consolidation during steady state flow, as shown in Fig. 10.
with the Freeman Technology FT4 Powder Rheometer.
10.9 Draw a line from the origin that is tangential to the
10.2 Calculate the normal stress by dividing the normal major Mohr circle. This line is the effective yield locus, and the
force measured by the instrument load cell by the cross- angle that this line subtends to the x-axis is the effective angle
sectional area of the shear head. of friction, δ.
N
σ5 (1) 10.10 Construct a flow function, FF, by drawing a smooth
A
curve through a series of data points, each of which represents
where: a pair of values of major principal stress and unconfined yield
σ = normal stress (kPa) strength.
N = measured force (N) 10.11 Calculation of Wall Friction Angle:
A = area of the shear head (m2) 10.11.1 Plot the pre-shear point and all valid shear test
10.3 Calculate the shear stress from the measured torque points as normal stress/shear stress data pairs (Fig. 11). Draw
using the following equation: a least mean squares regression line through all the data points.

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FIG. 10 Graphical Representation of the Shear Points, Mohr Circle Constructions and the Derived Parameters

FIG. 11 Graphical Representation of the Wall Yield Locus

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 D7891 − 15
This is known as the wall yield locus (WYL), and the angle 11.3.5 Humidity of environment where the powder was
that is subtends to the x-axis is known as the angle of wall tested to two significant digits.
friction, φ'. 11.4 Provide in plot form the following properties as a
Calculate the wall friction angle by: function of major principal stress, σ1. Record all stresses to
φ ' 5 tan21 S D
τw
σw
(4)
three significant digits and all angles to nearest 1°:
11.4.1 Unconfined yield strength, σc
where: 11.4.2 Angle of internal friction, φ.
11.4.3 Effective angle of friction, δ.
φ' = angle of wall friction (degrees) 11.4.4 Cohesion, C.
σw = normal stress at steady state flow (kPa)
τw = shear stress at steady state flow (kPa) 11.4.5 Wall friction angle, φ'.

10.11.2 In some cases the WYL is not linear and/or may not 12. Precision and Bias
pass through (or close to) the origin. In these less common
instances, then the alternative analysis presented in Test 12.1 Precision—Test data on precision is not presented due
Method D6128 may be employed. to the nature of the powder tested by this standard. It is either
not feasible or too costly at this time to have ten or more
11. Report: Test Data Sheet(s)/Form(s) laboratories participate in a round-robin testing program. In
11.1 The methodology used to specify how data are re- addition, it is either not feasible or too costly to produce
corded on the test data sheet(s)/form(s), as given below, is multiple specimens that have uniform physical properties. Any
covered in 1.4. variation observed in the data is just as likely to be due to
specimen variation as to operator or laboratory testing varia-
11.2 Record as a minimum the following general informa- tion.
tion (data):
11.2.1 Requesting agency or client and/or identifying num- 12.2 Subcommittee D18.24 is seeking any data from the
ber for job or project. users of this standard that might be used to make a limited
11.2.2 Technician name or initials. statement on precision.
11.2.3 Date test was run. 12.3 Bias—There is no accepted reference value for this
11.3 Record the following test specific information (data): standard; therefore bias cannot be determined.
11.3.1 Generic name of powder tested.
11.3.2 Chemical name of sample, if known. 13. Keywords
11.3.3 Specimen moisture (water) content, if determined. 13.1 effective angle of friction; effective yield locus;
Record value to nearest 0.1 %. Indicate method used to flowability; flow function; Freeman Technology, FT4 Powder
determine moisture if not Test Method D2216. Rheometer; internal friction angle; powder; rotational shear
11.3.4 Temperature of specimen to the nearest 1°C. cell; unconfined yield strength; wall friction; wall friction angle

ANNEX

(Mandatory Information)

A1. PRE-SHEAR PROTOCOLS AND SHEAR PEAKS

A1.1 Adjusting Pre-Shear Protocols specifiable limit) is also available. Thus it is possible to
A1.1.1 There is still some debate as to the appropriate replicate the methodologies specified in Test Methods D6682
degree of pre-shearing required to achieve critical consolida- and D6773.
tion prior to undertaking a shear test. Within any FT4 shear test
A1.2 Identifying Shear Peaks
program it is possible to select and adjust the pre-shearing
protocols such that the length and number of pre-shears is A1.2.1 The recommended procedure for the FT4 Powder
completely flexible. An automated routine is included as Rheometer is to undertake multiple pre-shears such that the
standard to identify a pre-shear peak and move the program peak stress of the last two pre-shears are within 1 % of each
onto the next step. This can be disabled and a defined time other or a maximum of ten pre-shear steps have been com-
period/shear distance can be specified. The number of pre- pleted before shear testing is initiated. The shear peaks are
shears can also be specified from a minimum of one, to automatically identified, and the program steps forward to the
between two and 100. A criterion to exit a multiple pre- next part of the program 20 seconds after a peak has been
shearing routine based on the convergence of the observed detected.
peak shear stresses of the last two pre-shear steps (to a

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REFERENCES

(1) Jenike, A. W. 1964, Storage and Flow of Solids, University of Utah, (6) W7020, 50 mm Vessel Assemblies, Issue D, Freeman Technology
Bulletin 123. Support Document, August 2010.
(2) Schulze, D. 2007, Powders and bulk solids. Behavior, (7) W6010, FT4 Calibration Manual, Issue B, Freeman Technology
Characterization, Storage and Flow, 2nd edn, Springer Verlag. Support Document, October 2012.
(3) Roberts, A. W. 1993, Basic Principles of Bulk Solids Storage, Flow & (8) W7008, Compressibility, Issue B, Freeman Technology Support
Handling TUNRA Bulk Solids Research Associates. Document, April 2013.
(4) INF122, Sampling, Freeman Technology Support Document, 2007. (9) W7107, Pre-Shearing Protocols for Shear Cell Testing, Freeman
(5) W7004, Cleaning, Issue A, Freeman Technology Support Document, Technology Support Document, Issue A, February 2011.
April 2007.

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