Time of Setting of Hydraulic Cement by Vicat Needle: Standard Test Methods For
Time of Setting of Hydraulic Cement by Vicat Needle: Standard Test Methods For
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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C 191 – 04a
5.2 The measured time of setting is affected by the percent- 9. Conditioning
age and temperature of the water used, the amount of kneading 9.1 Maintain the temperature of the air in the vicinity of the
the paste received, and by the temperature and humidity of the mixing slab, the dry cement, molds, and base plates at 23.0 6
mixing room air and the moist cabinet or moist room air. 3.0°C.
5.3 The measured time of setting of hydraulic cement is 9.2 Maintain the temperature of the mixing water at 23.0 6
test-method specific. Time of setting as measured by this 2.0°C.
method will not necessarily be similar to other methods used 9.3 The relative humidity of the mixing room shall be not
for determining the time of setting of hydraulic cements. less than 50 %.
9.4 The moist cabinet or moist room shall be in accordance
6. Apparatus with Specification C 511.
6.1 Vicat Apparatus—See Annex A1.1 and Fig. A1.1. The 10. Preparation of Cement Paste4
Vicat apparatus for this test method shall have a movable rod,
10.1 The cement paste used for the determination of the
B, of mass 300 6 0.5g. The end of the rod used for measuring
time of setting is obtained from one of the following methods:
penetration shall have a removable needle, D, with a diameter
10.1.1 Prepare a new batch of paste by mixing 650 g of
of 1.00 6 0.05 mm and length no less than 50 mm.
cement with the percentage of mixing water required for
6.2 Reference Masses and Devices for Determining Mass, normal consistency (Test Method C 187), following the proce-
conforming to the requirements of Specification C 1005. The dure described in Practice C 305.
devices for determining mass shall be evaluated for precision 10.1.2 For method A, at the option of the tester, use the test
and bias at a total load of 1 kg. specimen used for determining normal consistency (see Note
6.3 Glass Graduates, 200 or 250-mL capacity, and conform- 2).
ing to the requirements of Specification C 1005. 10.1.3 At the option of the tester, use the paste remaining
6.4 Plane non-adsorptive plate, 100 6 5 mm square of from the batch used for the autoclave specimen (Test Method
similar planeness, corrosivity, and absorptivity to that of glass C 151) or from the normal consistency determination (Test
(see Annex A1.1, Fig. A1.1, H). Method C 187).
6.5 Flat trowel, having a sharpened straight-edged steel NOTE 2—The specimen used for the determination of the normal
blade 100 to 150 mm in length. consistency will have an irregular surface, making it unsuitable for
method B.
6.6 Conical ring, made of a rigid, non-corroding, non-
absorbent material and shall have a height of 40 6 1 mm, an 11. Calculation
inside diameter at the bottom of 70 6 3 mm, and an inside
11.1 Calculate the Vicat time of setting to the nearest 1 min
diameter at the top of 60 6 3 mm (see Annex A1.1, Fig. A1.1, as follows:
G).
6.7 Mixer, bowl, and paddle, conforming to Practice C 305. SS ~H – E!
~C – D! D D
3 ~C – 25! 1 E (1)
6.8 Automatic Vicat Needle Apparatus for Method B—The
apparatus shall be equipped essentially with a standard Vicat where:
needle. The needle shall have a 1.0 6 0.05 mm diameter and E = time in minutes of last penetration greater than 25 mm,
have a length of at least 50 mm. The total mass supported by H = time in minutes of first penetration less than 25 mm,
the needle tip at the time of measurement shall be 300 6 0.5 g. C = penetration reading at time E, and
The instrument shall be capable of automatically completing D = penetration reading at time H.
and recording penetration measurements of a test specimen at 11.2 Calculate the Vicat final time of setting by determining
predetermined time intervals not exceeding 10 min and make the elapsed time between the time of the initial contact between
cement and water and the time when the needle does not sink
each penetration test at least 5 mm away from any previous
visibly into the paste, rounded to the nearest 5 min.
penetration and at least 10 mm away from the inner side of the
mold. 12. Report
6.9 Specimen Mold for Method B—The cement paste is held 12.1 Report the time of setting and the method used as
in a conical ring as described in 6.6. follows:
Vicat time of setting (A or B) ______ min
7. Reagents and Materials Vical final time of setting (A or B) ______ min
7.1 Mixing Water—Potable water is satisfactory for routine Method A—Manual Vicat Needle Apparatus
tests. Use water conforming to the requirements of Specifica-
tion D 1193 for Type III or Type IV grade reagent water for all 13. Manual Vicat Apparatus
referee and cooperative tests. 13.1 The Vicat apparatus shall consist of a frame, A, Fig.
A1.1, bearing a movable rod, B, weighing 300 g, one end, C,
8. Sampling
8.1 When the test is required for acceptance testing, sample
cement in accordance with Practice C 183. 4
See Test Method C 187.
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the plunger end, being 10 mm in diameter for a distance of at actual penetration measurements to determine the time of
least 50 mm and the other end having a removable steel needle, setting are made, release the rod only by the setscrew. Make
D, 1 mm in diameter and 50 mm in length. The rod B is each penetration test at least 5 mm away from any previous
reversible, and can be held in any desired position by a set penetration and at least 10 mm away from the inner side of the
screw, E, and has an adjustable indicator, F, which moves over mold. Record the results of all penetration tests and, by
a scale (graduated in millimetres) attached to the frame, A. The interpolation, determine the time when a penetration of 25 mm
paste is held in a conical ring, G, resting on a plate of similar is obtained. The elapsed time between the initial contact of
planeness, corrosivity, and absorptivity to that of glass, H, cement and water and the penetration of 25 mm is the Vicat
about 100 mm square. The ring shall be made of a noncorrod- time of setting or Vicat initial time of setting.
ing, nonabsorbing material, and shall have an inside diameter 14.3 Determine the Vicat final time of setting end point to
of 70 mm at the base and 60 mm at the top and a height of 40 be the first penetration measurement that does not mark the
mm. In addition to the above, the Vicat apparatus shall conform specimen surface with a complete circular impression, verified
to the following requirements: by two additional penetration measurements performed on
Weight of plunger 300 6 0.5 g (0.661 lb 6 8 grains) different areas of the specimen surface. The elapsed time
Diameter of larger end of 10 6 0.05 mm (0.394 6 0.002 in.) between the initial contact of cement and water and the end
plunger
Diameter of needle 1 6 0.05 mm (0.039 6 0.002 in.) point determination above is the Vicat final time of setting.
Inside diameter of ring at 70 6 3 mm (2.75 6 0.12 in.) 14.4 Precautions—Keep all the apparatus free from vibra-
bottom tion during the penetration test. Keep the 1-mm needle straight
Inside diameter of ring at 60 6 3 mm (2.36 6 0.12 in.)
top and clean. The needle must be kept clean to prevent cement
Height of ring 40 6 1 mm (1.57 6 0.04 in.) from adhering to the sides of the needle and decreasing
Graduated scale The graduated scale, when compared with a penetration, and to prevent cement from adhering to the point
scale accurate to within 0.1 mm
at all points, shall not show any point greater and increasing penetration.
than 0.25 mm
15. Precision and Bias
14. Procedure A
15.1 Precision:
14.1 Molding Test Specimen—Quickly form the cement
15.1.1 The single-operator (within-laboratory) standard de-
paste, prepared as described in the section on preparation of
viation has been found to be 12 min for the initial time of
cement paste, into a ball with gloved hands and toss six times
setting, throughout the range of 49 to 202 min, and 20 min for
from one hand to the other, maintaining the hands about 150
the final time of settings throughout the range of 185 to 312
mm (6 in.) apart. Press the ball, resting in the palm of the hand,
min. Therefore, results of two properly conducted tests by the
into the larger end of the conical ring, G, Fig. A1.1, held in the
same operator on Vicat initial time of setting of similar paste
other hand, completely filling the ring with paste. Remove the
should not differ from each other by more than 34 min and on
excess at the larger end by a single movement of the palm of
Vicat final time of setting of similar pastes should not differ
the hand. Place the ring on its larger end onto the non-
from each other by more than 56 min.
absorptive plate, H, and slice off the excess paste at the smaller
end at the top of the ring by a single oblique stroke of the 15.1.2 The multilaboratory (between-laboratory) standard
trowel held at a slight angle with the top of the ring. Smooth deviation has been found to be 16 min for the initial time of
the top of the specimen, if necessary, with one or two light setting throughout the range of 49 to 207 min, and 43 min for
touches of the pointed end of the trowel. During the operation the final time of setting throughout the range of 185 to 312 min.
of cutting and smoothing, take care not to compress the paste. Therefore, results of two properly conducted tests from two
Immediately after molding, place the test specimen in the moist different laboratories on Vicat initial time of setting of similar
cabinet or moist room and allow it to remain there except when pastes should not differ from each other by more than 45 min,
penetration measurements are being made. The specimen shall and on Vicat final time of setting of similar pastes should not
remain in the conical mold, supported by the non-absorptive differ from each other by more than 122 min.
plate throughout the test period. 15.2 Bias—Since there are no accepted reference materials
14.2 Time of Setting Determination—Allow the time of suitable for determining the bias for the procedure in this test
setting specimen to remain in the moist cabinet or moist room method, no statement on bias is presented.
for 30 min after molding without being disturbed. Determine
the penetration of the 1-mm needle at this time and every 15 Method B—Automatic Vicat
min thereafter (every 10 min for Type III cements) until a
penetration of 25 mm or less is obtained. Perform the penetra- 16. Automatic Vicat Apparatus
tion test by lowering the needle D of the rod B until it rests on 16.1 Automatic Vicat Needle Apparatus—The apparatus
the surface of the cement paste. Tighten the setscrew, E, and set shall be equipped essentially with a standard Vicat needle. The
the indicator, F, at the upper end of the scale, or take an initial needle shall have a 1.0 6 0.05 mm diameter and have a length
reading. Release the rod quickly by releasing the set screw, E, of at least 50 mm. The total mass supported by the needle tip
and allow the needle to settle for 30 s; then take the reading to at the time of measurement shall be 300 6 0.5 g. The
determine the penetration. At the option of the tester, if the instrument shall be capable of automatically completing and
paste is obviously quite soft on the early readings, retard the recording penetration measurements of a test specimen at
fall of the rod to avoid bending the 1-mm needle, but when predetermined time intervals not exceeding 10 min and make
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each penetration test at least 5 mm away from any previous 18. Performance Requirement (Qualification) for
penetration and at least 10 mm away from the inner side of the Automatic Vicat Instrument
mold. 18.1 Scope—When time of setting results from the auto-
16.2 Specimen Mold—The cement paste is held in a conical matic Vicat apparatus are to be used for acceptance or rejection
ring with the height of 40 6 1 mm and a removable base plate. of cement, the method used shall comply with the qualification
The test surface shall have a minimum diameter of 60 6 3 mm. requirements of this section. A method is considered to consist
of the specific instrument and the molding procedure meeting
17. Procedure the requirements of this standard, and used in a consistent
17.1 Molding the Specimen—Quickly form the cement manner by a given laboratory.
paste, prepared as described in the section on preparation of 18.2 Hydraulic Cement Samples Required—Select three
cement paste, into a ball with gloved hands and toss six times cements that comply with requirements of Specifications
from one hand to the other, maintaining the hands about 150 C 150, C 595, or C 1157, and that when tested in accordance
mm apart. Press the ball, resting in the palm of the hand, into with Method A, shall include the following:
the larger end of the conical ring, held in the other hand, 18.2.1 One cement that has an initial time of setting of less
completely filling the ring with paste. Remove the excess at the than 110 min,
larger end by a single movement of the palm of the hand. Place 18.2.2 One cement with an initial time of setting of greater
the ring on its larger end on the base plate. Use a trowel to than 150 min,
remove the excess paste at the top of the mold. Holding the 18.2.3 One cement with a final time of setting of less than
trowel at about a 30° incline with the leading edge raised and 180 min, and
starting near the center of the mold, level the paste by drawing 18.2.4 One cement with a final time of setting of greater
the trowel across the top of the mold using a sawing motion; than 210 min (see Note 5).
repeat the procedure for the other half of the surface. Then NOTE 5—Laboratories are advised to reserve sufficient cement for
smooth the surface level to the top of the mold making steady future qualification and standardization.
and complete strokes across the entire surface with the trailing 18.3 Tests—Using the method to be qualified and including
edge of the trowel. Repeat the cutting and smoothing steps but the standardization formula described in the section on stan-
at 90° from the previous cut. Repeat the steps as required to dardization, make single determinations of the times of initial
produce a surface level with the top of the mold. Usually the and final setting on each of the three cements. On the same day,
paste is level within two cycles, but occasionally three will be conduct companion time of setting determinations according to
required. Avoid excessive strokes and compaction. Since the Method A. Make single determinations of the normal consis-
automatic Vicat device references to the top edge of the mold, tency on each cement, and use that amount of water for all
it is imperative that the top surface of the paste be uniform and replicate batches. Complete three rounds of tests on different
level with the top of the mold. days, repeating all the steps of the methods. Conduct the
17.2 Time of Setting Determinations—Follow the manufac- qualification tests on specimens prepared separately from the
turer’s instructions and complete the required instrument standardization testing.
calibration and zero procedures. Set the instrument to measure 18.4 Calculations—Calculate the three–round averages for
no less frequently than every 10 min (see Note 3). Position the initial and final time of setting for each cement and method. A
molded specimen in the automatic Vicat apparatus and initiate method complies with the initial time of setting qualification
the measurements (see Note 4). requirements if the difference between the initial time of setting
NOTE 3—Automatic devices are usually capable of measurement more average values for Method A and the corresponding average
frequently than once every 10 min and more frequent measurement values of Method B is not greater than 25 min for any sample,
minimizes interpolation. and the range for any three replicate tests by Method B does
NOTE 4—The initial time of setting according to Method A is deter- not exceed 30 min. Likewise, a method complies with the final
mined as the elapsed time required to achieve a penetration of 25 mm and time of setting qualification requirements if the difference
the final time of setting as the total time elapsed until the needle does not between the final time of setting average values for Method A
sink visibly into the paste. The end points established by a qualified
and corresponding average values for Method B is not greater
automatic Vicat test method may deviate significantly from end points
specified in Method A, and require standardization to correct bias. than 45 min for any sample, and the range for any three
replicate tests by Method B does not exceed 30 min. Example
17.3 Determine the range of applicability of the method qualification data are given in Appendix X1.
from the range of the average time of setting of the cements 18.5 Standardization—When standardization is required in
used for qualification and standardization, and limit that range order to achieve agreement between Method A and Method B,
to 30 min greater than the maximum, and 30 min less than the it can be applied to either the initial time of setting, final time
minimum. of setting, or both. A standardization formula shall be based on
17.4 Performance Requirement (Qualification) for Auto- a comparison of test results obtained using Method A and the
matic Vicat Instrument: chosen method using the automatic instrument (Method B).
17.4.1 When time of setting results from the automatic Vicat Results of tests from at least five different hydraulic cements
apparatus are to be used for acceptance or rejection of cement, shall be required for standardization. The cements shall have a
the method used shall comply with the qualification require- minimum range of 60 min initial time of setting, and a
ments covered in Annex A2. minimum range of 90 min final time of setting when tested in
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accordance with Method A. If desired, the three cements used 19.1.4 The average of a Cement and Concrete Reference
for instrument qualification may be used, but make new Laboratory (CCRL) sample differs from the value obtained by
determinations. Use the same method as used for instrument the method by more than 45 min for either the initial or final
qualification, including all the same steps. Valid standardiza- time of setting.
tion formulas shall be mathematically derived and applied to
20. Precision and Bias
all samples (see Note 6).
20.1 Precision—No precision data are available at this time.
NOTE 6—Generally, the automatic instruments are computer operated A laboratory is advised to develop its own precision data for
and easily adapted to standardization calculations. the method and instrument used. Based on qualification re-
quirements, the precision of the method should not be greater
19. Requalification of a Method than that of Method A.
19.1 Requalify the method at least once per year and when 20.2 Bias—Since there are no accepted reference materials
any of the following conditions occur: suitable for determining the bias for the procedure in this test
19.1.1 The instrument has been significantly modified. method, no statement on bias is presented.
19.1.2 The instrument has been substantially repaired. 21. Keywords
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
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 Method A. Make single determinations of the normal consis-
apparatus are to be used for acceptance or rejection of cement, tency on each cement, and use that amount of water for all
the method used shall comply with the qualification require- replicate batches. Complete three rounds of tests on different
ments covered in this section. A method is considered to days, repeating all the steps of the methods. Conduct the
consist of the specific instrument and the molding procedure qualification tests on specimens prepared separately from the
meeting the requirements of this test method, and used in a standardization testing.
consistent manner by a given laboratory.
A2.4 Calculations—Calculate the three-round averages for
A2.2 Hydraulic Cement Samples Required—Select three initial and final time of setting for each cement and method. A
cements that comply with requirements of Specifications C method complies with the initial time of setting qualification
150, C 595, or C 1157, and that when tested in accordance with requirements if the difference between the initial time of setting
Method A, shall include the following: average values for Method A and the corresponding average
A2.2.1 One cement that has an initial time of setting of less values of Method B is not greater than 25 min for any sample,
than 110 min, and the range for any three replicate tests by Method B does
A2.2.2 One cement with an initial time of setting of greater not exceed 30 min. Likewise, a method complies with the final
than 150 min, time of setting qualification requirements if the difference
A2.2.3 One cement with a final time of setting of less than between the final time of setting average values for Method A
180 min, and and corresponding average values for Method B is not greater
A2.2.4 One cement with a final time of setting of greater than 45 min for any sample, and the range for any three
than 210 min (see Note A2.1). replicate tests by Method B does not exceed 30 min. Example
NOTE A2.1—Laboratories are advised to reserve sufficient cement for
qualification data are given in Appendix X1.
future qualification and standardization.
A2.5 Standardization—When standardization is required in
A2.3 Tests—Using the method to be qualified and including order to achieve agreement between Method A and Method B,
the standardization formula described in the section on stan- it can be applied to either the initial time of setting, final time
dardization, make single determinations of the times of initial of setting, or both. A standardization formula shall be based on
and final setting on each of the three cements. On the same day, a comparison of test results obtained using Method A and the
conduct companion time of setting determinations according to chosen method using the automatic instrument (Method B).
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Results of tests from at least five different hydraulic cements qualification, including all the same steps. Valid standardiza-
shall be required for standardization. The cements shall have a tion formulas shall be mathematically derived and applied to
minimum range of 60 min initial time of setting, and a all samples (see Note A2.2).
minimum range of 90 min final time of setting when tested in
accordance with Method A. If desired, the three cements used NOTE A2.2—Generally, the automatic instruments are computer oper-
for instrument qualification may be used, but make new ated and easily adapted to standardization calculations.
determinations. Use the same method as used for instrument
A3.1 Requalify the method at least once per year and when providing data meeting the performance requirements.
any of the following conditions occur:
A3.5 The average of a Cement and Concrete Reference
A3.2 The instrument has been significantly modified.
Laboratory (CCRL) sample differs from the value obtained by
A3.3 The instrument has been substantially repaired. the method by more than 45 min for either the initial or final
A3.4 Substantial evidence indicates that the method is not time of setting.
APPENDIX
(Nonmandatory Information)
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TABLE X1.2 Time of Final Setting, min
Diff. Avg.
Round Final C 191 Final Auto (Spec. 45
Cement No. Method A Method 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
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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