C191 Setting Time
C191 Setting Time
C191 Setting Time
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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Periodic penetration tests are performed on this paste by time intervals not exceeding 10 min and make each penetration
allowing a 1 mm Vicat needle to settle into this paste. The Vicat test at least 5 mm away from any previous penetration and at
initial time of setting is the time elapsed between the initial least 10 mm away from the inner side of the mold.
contact of cement and water and the time when the penetration 6.9 Specimen Mold for Method B—The cement paste is held
is measured or calculated to be 25 mm. The Vicat final time of in a conical ring with the height of 40 6 1 mm and a removable
setting is the time elapsed between initial contact of cement base plate. The test surface shall have a minimum diameter of
and water and the time when the needle does not leave a 60 6 3 mm.
complete circular impression in the paste surface.
6.10 Inspect and document Section 6 apparatus for confor-
5. Significance and Use mance to the requirements of this test method at least every
5.1 This test method provides a means of determining 21⁄2 years (see Note 2).
compliance with a specification limit for Vicat time of setting. NOTE 2—Specification C1005 requires annual compliance checks for
Refer to the appropriate specification for the cement to the reference masses and for the devices for determining mass.
determine if this test method is used for specification compli-
ance. 7. Reagents and Materials
5.2 Time of setting measured by this method will not 7.1 Mixing Water—Potable water is satisfactory for routine
necessarily provide the same results as the time of setting of tests. Use reagent water for all referee and cooperative tests.
hydraulic cement paste measured by other methods, or the time
of setting of mortar or concrete. 8. Sampling
6. Apparatus 8.1 When the test is required for acceptance testing, sample
cement in accordance with Practice C183/C183M.
6.1 Vicat Apparatus—See Annex A1.1 and Fig. A1.1. The
Vicat apparatus for this test method shall have a movable rod, 9. Conditioning
B, of mass 300 6 0.5 g.
6.1.1 The end of the rod used for measuring penetration 9.1 Maintain the temperature and the humidity of the
shall have a straight steel removable needle with a diameter of mixing room and the temperature of the mixing water in
1.00 6 0.05 mm and length no less than 50 mm. accordance with Specification C511 (see section titled “Re-
6.1.2 The needle end that contacts the specimen shall be flat, quirements for Cement Mixing Rooms”).
plane, and at right angles to the axis of the rod. 9.2 The moist cabinet or moist room shall be in accordance
6.2 Reference Masses and Devices for Determining Mass, with Specification C511.
conforming to the requirements of Specification C1005. The 9.3 The dry materials shall be within the temperature range
devices for determining mass shall be evaluated for continuing of the mixing room prior to testing.
precise performance utilizing the procedure in Specification
C1005, Appendix X1 using a verification check mass of 10. Preparation of Cement Paste
approximately 1000 g. NOTE 3—See Test Method C187.
6.3 Glass Graduates, 200 or 250 mL capacity, and conform- 10.1 The cement paste used for the determination of the
ing to the requirements of Specification C1005. time of setting is obtained from one of the following methods:
6.4 Plane Non-Adsorptive Plate, 100 6 5 mm square of 10.1.1 Prepare a new batch of paste by mixing 650 g of
similar planeness, corrosivity, and absorptivity to that of glass cement with the percentage of mixing water required for
(see Annex A1.1, Fig. A1.1, H). normal consistency (Test Method C187), following the proce-
dure described in Practice C305.
6.5 Flat Trowel, having a sharpened straight-edged steel 10.1.2 For method A, at the option of the tester, use the test
blade 100 to 150 mm in length. The edges when placed on a specimen used for determining normal consistency (see Note
plane surface shall not depart from straightness by more than 4).
1 mm. 10.1.3 At the option of the tester, use the paste remaining
6.6 Conical Ring, made of a rigid, non-corroding, non- from the batch used for the autoclave specimen (Test Method
absorbent material and having a height of 40 6 1 mm, an C151/C151M) or from the normal consistency determination
inside diameter at the bottom of 70 6 3 mm, and an inside (Test Method C187).
diameter at the top of 60 6 3 mm (see Annex A1.1, Fig. A1.1, NOTE 4—The specimen used for the determination of the normal
G). consistency will have an irregular surface, making it unsuitable for
6.7 Mixer, Bowl, and Paddle, conforming to Practice C305. method B.
6.8 Automatic Vicat Needle Apparatus for Method B—The 11. Calculation
apparatus shall be equipped with a Vicat needle as described in
6.1.1 and 6.1.2. The total mass supported by the needle tip at 11.1 Calculate the Vicat time of setting to the nearest 1 min
the time of measurement shall be 300 6 0.5 g. The instrument as follows:
shall be capable of automatically completing and recording
penetration measurements of a test specimen at predetermined SS ~~ H 2 E!
C 2 D!D D
3 ~ C 2 25! 1E (1)
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where: fall of the rod to avoid bending the 1 mm needle, but when
E = time in minutes of last penetration greater than 25 mm, actual penetration measurements to determine the time of
H = time in minutes of first penetration less than 25 mm, setting are made, release the rod only by the setscrew. Make
C = penetration reading at time E, and each penetration test at least 5 mm away from any previous
D = penetration reading at time H. penetration and at least 10 mm away from the inner side of the
11.2 Calculate the Vicat final time of setting by determining mold. Record the results of all penetration tests and, by
the elapsed time between the time of the initial contact between interpolation, determine the time when a penetration of 25 mm
cement and water and the time when the Vicat final time of is obtained. The elapsed time between the initial contact of
setting end-point described in 14.3 is determined, rounded to cement and water and the penetration of 25 mm is the Vicat
the nearest 5 min. time of setting or Vicat initial time of setting.
14.3 Determine the Vicat final time of setting end point to
12. Report be the first penetration measurement that does not mark the
12.1 Report the time of setting and the method used as specimen surface with a complete circular impression. Verify
follows: final set by performing two additional penetration measure-
Vicat time of setting (A or B) ______ min
ments on different areas of the specimen surface. Obtain
Vicat final time of setting (A or B) ______ min verification measurements within 90 s of the first “final set”
measurement. The elapsed time between the initial contact of
cement and water and the end point determination above is the
Method A—Manual Vicat Needle Apparatus
Vicat final time of setting.
13. Manual Vicat Apparatus 14.4 Precautions—Keep all the apparatus free from vibra-
13.1 Refer to the Apparatus section, 6.1, 6.4, and 6.6, and tion during the penetration test. Keep the 1 mm needle straight
Annex A1 for a description of the Vicat apparatus. and clean. The needle must be kept clean to prevent cement
from adhering to the sides of the needle and decreasing
14. Procedure A penetration, and to prevent cement from adhering to the point
and increasing penetration.
14.1 Molding Test Specimen—Quickly form the cement
paste, prepared as described in the section on preparation of 15. Precision and Bias
cement paste, into a ball with gloved hands and toss six times
from one hand to the other, maintaining the hands about 15.1 Precision:
150 mm (6 in.) apart. Press the ball, resting in the palm of the 15.1.1 The single-operator (within-laboratory) standard de-
hand, into the larger end of the conical ring, G, Fig. A1.1, held viation has been found to be 12 min for the initial time of
in the other hand, completely filling the ring with paste. setting, throughout the range of 49 to 202 min, and 20 min for
Remove the excess at the larger end by a single movement of the final time of settings throughout the range of 185 to
the palm of the hand. Place the ring on its larger end onto the 312 min. Therefore, results of two properly conducted tests by
non-absorptive plate, H, and slice off the excess paste at the the same operator on Vicat initial time of setting of similar
smaller end at the top of the ring by a single oblique stroke of paste should not differ from each other by more than 34 min
the trowel held at a slight angle with the top of the ring. and on Vicat final time of setting of similar pastes should not
Smooth the top of the specimen, if necessary, with one or two differ from each other by more than 56 min.
light touches of the pointed end of the trowel. During the 15.1.2 The multilaboratory (between-laboratory) standard
operation of cutting and smoothing, take care not to compress deviation has been found to be 16 min for the initial time of
the paste. Immediately after molding, place the test specimen setting throughout the range of 49 to 207 min, and 43 min for
in the moist cabinet or moist room and allow it to remain there the final time of setting throughout the range of 185 to 312 min.
except when penetration measurements are being made. The Therefore, results of two properly conducted tests from two
specimen shall remain in the conical mold, supported by the different laboratories on Vicat initial time of setting of similar
non-absorptive plate throughout the test period. pastes should not differ from each other by more than 45 min,
and on Vicat final time of setting of similar pastes should not
14.2 Time of Setting Determination—Allow the time of
differ from each other by more than 122 min.
setting specimen to remain in the moist cabinet or moist room
for 30 min after molding without being disturbed. Determine 15.2 Bias—Since there are no accepted reference materials
the penetration of the 1 mm needle at this time and every suitable for determining the bias for the procedure in this test
15 min thereafter (every 10 min for Type III cements) until a method, no statement on bias is presented.
penetration of 25 mm or less is obtained. Perform the penetra-
tion test by lowering the needle D of the rod B until it rests on
Method B—Automatic Vicat
the surface of the cement paste. Tighten the setscrew, E, and set
the indicator, F, at the upper end of the scale, or take an initial
reading. Release the rod quickly by releasing the set screw, E, 16. Automatic Vicat Apparatus
and allow the needle to settle for 30 s; then take the reading to 16.1 Automatic Vicat Needle Apparatus—Refer to the Ap-
determine the penetration. At the option of the tester, if the paratus section, 6.8 and 6.9, for a description of the Automatic
paste is obviously quite soft on the early readings, retard the Vicat needle apparatus.
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17. Procedure requirements of this section. A method is considered to consist
17.1 Molding the Specimen—Quickly form the cement of the specific instrument and the molding procedure meeting
paste, prepared as described in the section on preparation of the requirements of this standard, and used in a consistent
cement paste, into a ball with gloved hands and toss six times manner by a given laboratory.
from one hand to the other, maintaining the hands about 18.2 Hydraulic Cement Samples Required—Select three
150 mm apart. Press the ball, resting in the palm of the hand, cements that comply with requirements of Specifications
into the larger end of the conical ring, held in the other hand, C150/C150M, C595/C595M, or C1157/C1157M, and that
completely filling the ring with paste. Remove the excess at the when tested in accordance with Method A, shall include the
larger end by a single movement of the palm of the hand. Place following:
the ring on its larger end on the base plate. Use a trowel to 18.2.1 One cement that has an initial time of setting of less
remove the excess paste at the top of the mold. Holding the than 110 min,
trowel at about a 30° incline with the leading edge raised and 18.2.2 One cement with an initial time of setting of greater
starting near the center of the mold, level the paste by drawing than 150 min,
the trowel across the top of the mold using a sawing motion; 18.2.3 One cement with a final time of setting of less than
repeat the procedure for the other half of the surface. Then 180 min, and
smooth the surface level to the top of the mold making steady 18.2.4 One cement with a final time of setting of greater
and complete strokes across the entire surface with the trailing than 210 min (see Note 7).
edge of the trowel. Repeat the cutting and smoothing steps but
NOTE 7—Laboratories are advised to reserve sufficient cement for
at 90° from the previous cut. Repeat the steps as required to future qualification and standardization.
produce a surface level with the top of the mold. Usually the
paste is level within two cycles, but occasionally three will be 18.3 Tests—Using the method to be qualified and including
required. Avoid excessive strokes and compaction. Since the the standardization formula described in the section on
automatic Vicat device references to the top edge of the mold, standardization, make single determinations of the times of
it is imperative that the top surface of the paste be uniform and initial and final setting on each of the three cements. On the
level with the top of the mold. same day, conduct companion time of setting determinations
according to Method A. Make single determinations of the
17.2 Time of Setting Determinations—Follow the manufac- normal consistency on each cement, and use that amount of
turer’s instructions and complete the required instrument water for all replicate batches. Complete three rounds of tests
calibration and zero procedures. Set the instrument to measure on different days, repeating all the steps of the methods.
no less frequently than every 10 min (see Note 5). Position the Conduct the qualification tests on specimens prepared sepa-
molded specimen in the automatic Vicat apparatus and initiate rately from the standardization testing.
the measurements (see Note 6).
18.4 Calculations—Calculate the three–round averages for
NOTE 5—Automatic devices are usually capable of measurement more initial and final time of setting for each cement and method. A
frequently than once every 10 min and more frequent measurement
minimizes interpolation.
method complies with the initial time of setting qualification
NOTE 6—The initial time of setting according to Method A is deter- requirements if the difference between the initial time of setting
mined as the elapsed time required to achieve a penetration of 25 mm and average values for Method A and the corresponding average
the final time of setting as the total time elapsed until the needle does not values of Method B is not greater than 25 min for any sample,
leave a complete circular impression in the paste surface. The end points and the range for any three replicate tests by Method B does
established by a qualified automatic Vicat test method may deviate
significantly from end points specified in Method A, and require standard-
not exceed 30 min. Likewise, a method complies with the final
ization to correct bias. time of setting qualification requirements if the difference
between the final time of setting average values for Method A
17.3 Determine the range of applicability of the method
and corresponding average values for Method B is not greater
from the range of the average time of setting of the cements
than 45 min for any sample, and the range for any three
used for qualification and standardization, and limit that range
replicate tests by Method B does not exceed 30 min. Example
to 30 min greater than the maximum, and 30 min less than the
qualification data are given in Appendix X1.
minimum.
18.5 Standardization—When standardization is required in
17.4 Performance Requirement (Qualification) for Auto-
order to achieve agreement between Method A and Method B,
matic Vicat Instrument:
it can be applied to either the initial time of setting, final time
17.4.1 When time of setting results from the automatic Vicat of setting, or both. A standardization formula shall be based on
apparatus are to be used for acceptance or rejection of cement, a comparison of test results obtained using Method A and the
the method used shall comply with the qualification require- chosen method using the automatic instrument (Method B).
ments covered in Annex A2. Results of tests from at least five different hydraulic cements
shall be required for standardization. The cements shall have a
18. Performance Requirement (Qualification) for minimum range of 60 min initial time of setting, and a
Automatic Vicat Instrument minimum range of 90 min final time of setting when tested in
18.1 Scope—When time of setting results from the auto- accordance with Method A. If desired, the three cements used
matic Vicat apparatus are to be used for acceptance or rejection for instrument qualification may be used, but make new
of cement, the method used shall comply with the qualification determinations. Use the same method as used for instrument
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qualification, including all the same steps. Valid standardiza- 20. Precision and Bias
tion formulas shall be mathematically derived and applied to
20.1 Precision—Since Method B represents procedures spe-
all samples (see Note 8).
cific to a laboratory that have been qualified in comparison to
NOTE 8—Generally, the automatic instruments are computer operated Method A, no statement on precision is being made.
and easily adapted to standardization calculations.
19. Requalification of a Method 20.2 Bias—Since there are no accepted reference materials
suitable for determining the bias for the procedure in this test
19.1 Requalify the method at least once per year and when method, no statement on bias is presented.
any of the following conditions occur:
19.1.1 The instrument has been significantly modified.
21. Keywords
19.1.2 The instrument has been substantially repaired.
19.1.3 Substantial evidence indicates that the method is not 21.1 automatic vicat; hydraulic-cement paste; time of set-
providing data meeting the performance requirements. ting; vicat; vicat needle
19.1.4 The average of a Cement and Concrete Reference
Laboratory (CCRL) sample differs from the value obtained by
the method by more than 45 min for either the initial or final
time of setting.
ANNEXES
(Mandatory Information)
A1.1 The Vicat apparatus shall consist of a frame, A, Fig. position by a setscrew, E, and has an adjustable indicator, F,
A1.1, bearing a movable rod, B, with a mass as specified by the which moves over a scale graduated in millimetres and
method referencing this apparatus, one end, C, the plunger end, attached to the frame, A. The gradations on the graduated scale,
with a diameter as specified by the method referencing this when compared to a scale accurate to within 0.1 mm at all
apparatus, and the other end having a mass or a removable steel points, shall not show a variance from the reference scale
needle, D, as specified by the method referencing this appara- greater than 0.25 mm.
tus. The rod, B, is reversible, and can be held in any desired
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A2.1 When time of setting results from the automatic Vicat future qualification and standardization.
apparatus are to be used for acceptance or rejection of cement,
A2.3 Tests—Using the method to be qualified and including
the method used shall comply with the qualification require-
the standardization formula described in the section on
ments covered in this section. A method is considered to
consist of the specific instrument and the molding procedure standardization, make single determinations of the times of
meeting the requirements of this test method, and used in a initial and final setting on each of the three cements. On the
consistent manner by a given laboratory. same day, conduct companion time of setting determinations
according to Method A. Make single determinations of the
A2.2 Hydraulic Cement Samples Required—Select three normal consistency on each cement, and use that amount of
cements that comply with requirements of Specifications water for all replicate batches. Complete three rounds of tests
C150/C150M, C595/C595M, or C1157/C1157M, and that on different days, repeating all the steps of the methods.
when tested in accordance with Method A, shall include the Conduct the qualification tests on specimens prepared sepa-
following: rately from the standardization testing.
A2.2.1 One cement that has an initial time of setting of less A2.4 Calculations—Calculate the three-round averages for
than 110 min, initial and final time of setting for each cement and method. A
A2.2.2 One cement with an initial time of setting of greater method complies with the initial time of setting qualification
than 150 min, requirements if the difference between the initial time of setting
A2.2.3 One cement with a final time of setting of less than average values for Method A and the corresponding average
180 min, and values of Method B is not greater than 25 min for any sample,
and the range for any three replicate tests by Method B does
A2.2.4 One cement with a final time of setting of greater not exceed 30 min. Likewise, a method complies with the final
than 210 min (see Note A2.1). time of setting qualification requirements if the difference
NOTE A2.1—Laboratories are advised to reserve sufficient cement for between the final time of setting average values for Method A
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and corresponding average values for Method B is not greater shall be required for standardization. The cements shall have a
than 45 min for any sample, and the range for any three minimum range of 60 min initial time of setting, and a
replicate tests by Method B does not exceed 30 min. Example minimum range of 90 min final time of setting when tested in
qualification data are given in Appendix X1. accordance with Method A. If desired, the three cements used
for instrument qualification may be used, but make new
A2.5 Standardization—When standardization is required in
determinations. Use the same method as used for instrument
order to achieve agreement between Method A and Method B,
qualification, including all the same steps. Valid standardiza-
it can be applied to either the initial time of setting, final time
of setting, or both. A standardization formula shall be based on tion formulas shall be mathematically derived and applied to
a comparison of test results obtained using Method A and the all samples (see Note A2.2).
chosen method using the automatic instrument (Method B). NOTE A2.2—Generally, the automatic instruments are computer oper-
Results of tests from at least five different hydraulic cements ated and easily adapted to standardization calculations.
A3.1 Requalify the method at least once per year and when A3.5 The average of a Cement and Concrete Reference
any of the following conditions occur: Laboratory (CCRL) sample differs from the value obtained by
the method by more than 45 min for either the initial or final
A3.2 The instrument has been significantly modified. time of setting.
A3.3 The instrument has been substantially repaired.
A3.4 Substantial evidence indicates that the method is not
providing data meeting the performance requirements.
APPENDIX
(Nonmandatory Information)
For additional useful information on details of cement test methods, reference may be made to the “Manual of Cement
Testing,” which appears in the Annual Book of ASTM Standards, Vol 04.01.
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TABLE X1.2 Time of Final Setting, min
Final C191 Final Auto Diff. Avg.
Round
Cement Test Test Method (Spec. 45
No.
Method A B Max.)
A 1 150 150 ...
A 2 145 150 ...
A 3 170 125 ...
Range (Spec. 30 max) 25 25 ...
Average 155.0 141.7 13.3
B 1 185 180 ...
B 2 200 180 ...
B 3 185 155 ...
Range (Spec. 30 max) 15 25 ...
Average 190.0 171.7 18.3
C 1 235 225 ...
C 2 240 220 ...
C 3 240 215 ...
Range (Spec. 30 max) 5 10 ...
Average 238.3 220.0 18.3
SUMMARY OF CHANGES
Committee C01 has identified the location of selected changes to this standard since the last issue (C191 – 19)
that may impact the use of this standard. (Approved Oct. 1, 2021.)
(1) Removed Specification D1193 from Referenced Docu- (2) Revised 3.1.1 and 7.1.
ments.
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