UNIVERSITY OF NEGROS OCCIDENTAL – RECOLETOS

COLLEGE OF ENGINEERING
CIVIL ENGINEERING DEPARTMENT

LABORATORY TEST NO. 9:

TIME OF SETTING OF SETTING OF CEMENT BY VICAT APPARATUS
(ASTM C191)

I. INTRODUCTION

Definitions

Scope of Test
1. These methods determine the time of setting of hydraulic cement by means of
the Vicat needle. Two test methods are given; Method A is the Reference Test
Method using the manually operated standard Vicat apparatus, while Method
B permits the use of an automatic Vicat machine that has, in accordance with
the qualification requirements of this method, demonstrated acceptable
performance.
2. The values stated in SI units are to be regarded as the standard. Values in
parentheses are for information only.
3. This standard does not purport to address all of the safety concerns, if any,
associated with its use. It is the responsibility of the user of this standard to
establish appropriate safety and health practices and determine the
applicability of regulatory limitations prior to use. See 4 for a specific warning
statement.
4. Warning—Fresh hydraulic cementitious mixtures are caustic and may cause
chemical burns to skin and tissue upon prolonged exposure. The use of gloves,
protective clothing, and eye protection is recommended. Wash contact area
with copious amounts of water after contact. Wash eyes for a minimum of 15
min. Avoid exposure of the body to clothing saturated with the liquid phase of
the unhardened material. Remove contaminated clothing immediately after
exposure.

NOTE 1—For the method for determining the time of setting by Gillmore needles,
see Test Method C 266.

Object of Test
1. This test method provides a means of determining compliance with a
specification limit for Vicat time of setting. Refer to the appropriate
specification for the cement to determine if this test method is used for
specification compliance.
 2. The measured time of setting is affected by the percentage and temperature of
the water used, the amount of kneading the paste received, and by the
temperature and humidity of the mixing room air and the moist cabinet or
moist room air.
3. The measured time of setting of hydraulic cement is test-method specific. Time
of setting as measured by this method will not necessarily be similar to other
methods used for determining the time of setting of hydraulic cements.

II. APPARATUS AND SUPPLIES

1. Vicat Apparatus—See Annex A1.1 and Fig. A1.1. The Vicat apparatus for this test
method shall have a movable rod, B, of mass 300±0.5g. The end of the rod used for
measuring penetration shall have a removable needle, D, with a diameter of 1.00±0.05
mm and length no less than 50 mm.

2. Reference Masses and Devices for Determining Mass, conforming to the

requirements of Specification C 1005. The devices for determining mass shall be
evaluated for precision and bias at a total load of 1 kg.
3. Glass Graduates, 200 or 250-mL capacity, and conforming to the requirements of
Specification C 1005.
4. Plane non-adsorptive plate, 100±5 mm square of similar planeness, corrosively, and
absorptivity to that of glass (see Annex A1.1, Fig. A1.1, H).
5. Flat trowel, having a sharpened straight-edged steel blade 100 to 150 mm in length.
 6. Conical ring, made of a rigid, non-corroding, nonabsorbent material and shall have a
height of 40±1 mm, an inside diameter at the bottom of 70±3 mm, and an inside
diameter at the top of 60±3 mm (see Annex A1.1, Fig.A1.1,G).
7. Mixer, bowl, and paddle, conforming to Practice C 305.
8. Automatic Vicat Needle Apparatus for Method B—The apparatus shall be equipped
essentially with a standard Vicat needle. The needle shall have a 1.0±0.05 mm
diameter and have a length of at least 50 mm. The total mass supported by the needle
tip at the time of measurement shall be 300±0.5 g. The instrument shall be capable of
automatically completing and recording penetration measurements of a test specimen
at predetermined time intervals not exceeding 10 min and make each penetration test
at least 5 mm away from any previous penetration and at least 10 mm away from the
inner side of the mold.
9. Specimen Mold for Method B- The cement paste is held in a conical ring as
described in 6.
10. Reagents and Materials
1. Mixing Water—Potable water is satisfactory for routine tests. Use water
conforming to the requirements of Specification D 1193 for Type III or Type
IV grade reagent water for all referee and cooperative tests.

III. PREPARATION OF SAMPLES AND TEST SPECIMENS

Sampling
When the test is required for acceptance testing, sample cement in accordance with
Practice C 183.

Conditioning
1. Maintain the temperature of the air in the vicinity of the mixing slab, the dry cement,
molds, and base plates at 23.0±3.0°C.
2. Maintain the temperature of the mixing water at 23.0±2.0°C.
3. The relative humidity of the mixing room shall be not less than 50 %.
4. The moist cabinet or moist room shall be in accordance with Specification C 511.

Preparation of Cement Paste

1. The cement paste used for the determination of the time of setting is obtained from
one of the following methods:
1.1 Prepare a new batch of paste by mixing 650 g of cement with the percentage of
mixing water required for normal consistency (Test Method C 187), following the
procedure described in Practice C 305.
1.2 For method A, at the option of the tester, use the test specimen used for determining
normal consistency (see Note2).
1.3 At the option of the tester, use the paste remaining from the batch used for the
autoclave specimen (Test Method C 151) or from the normal consistency
determination (Test Method C 187).
 NOTE 2—The specimen used for the determination of the normal consistency will
have an irregular surface, making it unsuitable for method B.

PROCEDURE A

1. Molding Test Specimen—Quickly form the cement paste, prepared as described in the
section on preparation of cement paste, into a ball with the gloved hands and toss six
times from one hand to the other, maintaining the hands about 150 mm (6 in.) apart.
Press the ball, resting in the palm of the hand, into the larger end of the conical ring,
G, Fig. A1.1, held in the other hand, completely filling the ring with paste. Remove the
excess at the larger end by a single movement of the palm of the hand. Place the ring
on its larger end onto the non-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 trowel held at a slight
angle with the top of the ring. Smooth the top of the specimen, if necessary, with one
or two light touches of the pointed end of the trowel. During the operation of cutting
and smoothing, take care not to compress the paste. Immediately after molding, place
the test specimen in the moist cabinet or moist room and allow it to remain there except
when penetration measurements are being made. The specimen shall remain in the
conical mold, supported by the non-absorptive plate throughout the test period.

PROCEDURE B

1. Molding the Specimen—Quickly form the cement paste, prepared as described in the
section on preparation of cement paste, into a ball with the gloved hands and toss six
times from one hand to the other, maintaining the hands about 150 mm apart. Press the
ball, resting in the palm of the hand, into the larger end of the conical ring, held in the
other hand, completely filling the ring with paste. Remove the excess at the larger end
by a single movement of the palm of the hand. Place the ring on its larger end on the
base plate. Use a trowel to remove the excess paste at the top of the mold. Holding the
trowel at about a 30° incline with the leading edge raised and starting near the center
of the mold, level the paste by drawing the trowel across the top of the mold using a
sawing motion; repeat the procedure for the other half of the surface. Then smooth the
surface level to the top of the mold making steady and complete strokes across the
entire surface with the trailing edge of the trowel. Repeat the cutting and smoothing
steps but at 90° from the previous cut. Repeat the steps as required to produce a surface
level with the top of the mold. Usually the paste is level within two cycles, but
occasionally three will be required. Avoid excessive strokes and compaction. Since the
automatic Vicat device references to the top edge of the mold, it is imperative that the
top surface of the paste be uniform and level with the top of the mold.
IV. ADJUSTMENT AND CALIBRATION OF MECHANICAL DEVICE

METHOD A—MANUAL VICAT NEEDLE APPARATUS

Manual Vicat Apparatus

1. The Vicat apparatus shall consist of a frame, A, Fig. A1.1, bearing a movable rod, B,
weighing 300 g, one end, C, the plunger end, being 10 mm in diameter for a distance
of at least 50 mm and the other end having a removable steel needle, D, 1 mm in
diameter and 50 mm in length. The rod B is reversible, and can be held in any desired
position by a set screw, E, and has an adjustable indicator, F, which moves over a scale
(graduated in millimetres) attached to the frame, A. The paste is held in a conical ring,
G, resting on a plate of similar planeness, corrosivity, and absorptivity to that of glass,
H, about 100 mm square. The ring shall be made of a noncorroding, nonabsorbing
material, and shall have an inside diameter of 70 mm at the base and 60 mm at the top
and a height of 40 mm. In addition to the above, the Vicat apparatus shall conform to
the following requirements:

METHOD B—AUTOMATIC VICAT

Automatic Vicat Apparatus

1. Automatic Vicat Needle Apparatus—The apparatus shall be equipped essentially with
a standard Vicat needle. The needle shall have a 1.0±0.05 mm diameter and have a
length of at least 50 mm. The total mass supported by the needle tip at the time of
measurement shall be 300±0.5 g. The instrument shall be capable of automatically
completing and recording penetration measurements of a test specimen at
predetermined time intervals not exceeding 10 min and make each penetration test at
least 5 mm away from any previous penetration and at least 10 mm away from the
inner side of the mold.
2. Specimen Mold—The cement paste is held in a conical ring with the height of 40±1
mm and a removable base plate. The test surface shall have a minimum diameter of
60±3 mm.
V. PROCEDURE

PROCEDURE A

1. Time of Setting Determination— Allow the time of setting specimen to remain in the
moist cabinet or moist room for 30 min after molding without being disturbed.
Determine the penetration of the 1-mm needle at this time and every 15 min thereafter
(every 10 min for Type III cements) until a penetration of 25 mm or less is obtained.
Perform the penetration test by lowering the needle D of the rod B until it rests on the
surface of the cement paste. Tighten the set screw, 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, and allow the needle to settle for 30 s; then take the reading to
determine the penetration. At the option of the tester, if the paste is obviously quite soft
on the early readings, retard the fall of the rod to avoid bending the 1-mm needle, but
when actual penetration measurements to determine the time of setting are made,
release the rod only by the set screw. Make each penetration test at least 5 mm away
from any previous penetration and at least 10 mm away from the inner side of the mold.
Record the results of all penetration tests and, by interpolation, determine the time
when a penetration of 25 mm is obtained. The elapsed time between the initial contact
of cement and water and the penetration of 25 mm is the Vicat time of setting or Vicat
initial time of setting.

2. The Vicat final time of setting is the elapsed time between the time of initial contact of
cement and water and the time when the needle does not sink visibly into the paste.

3. Precautions—Keep all the apparatus free from vibration during the penetration test.
Keep the 1-mm needle straight and clean. The needle must be kept clean to prevent
cement from adhering to the sides of the needle and decreasing penetration, and to
prevent cement from adhering to the point and increasing penetration.

PROCEDURE B

1. Time of Setting Determinations—Follow the manufacturer’s instructions and complete

the required instrument calibration and zero procedures. Set the instrument to measure
no less frequently than every 10 min (see Note 3). Position the molded specimen in the
automatic Vicat apparatus and initiate the measurements (see Note 4).

NOTE 3—Automatic devices are usually capable of measurement more frequently than
once every 10 min and more frequent measurement minimizes interpolation.

NOTE 4—The initial time of setting according to Method A is determined as the

elapsed time required to achieve a penetration of 25 mm and the final time of setting
as the total time elapsed until the needle does not sink visibly into the paste. The end
 points established by a qualified automatic Vicat test method may deviate significantly
from end points specified in Method A, and require standardization to correct bias.

2. Determine the range of applicability of the method from the range of the average time
of setting of the cements used for qualification and standardization, and limit that range
to 30 min greater than the maximum, and 30 min less than the minimum.

3. Performance Requirement (Qualification) for Automatic Vicat Instrument:

3.1 When time of setting results from the automatic Vicat apparatus are to be used for
acceptance or rejection of cement, the method used shall comply with the
qualification requirements covered in Annex A2.

4. Performance Requirement (Qualification) for Automatic Vicat Instrument

4.1 Scope—When time of setting results from the automatic Vicat apparatus are to be
used for acceptance or rejection of cement, the method used shall comply with the
qualification requirements of this section. A method is considered to consist of the
specific instrument and the molding procedure meeting the requirements of this
standard, and used in a consistent manner by a given laboratory.
4.2 Hydraulic Cement Samples Required—Select three cements that comply with
requirements of Specifications C 150, C 595, or C 1157, and that when tested in
accordance with Method A, shall include the following:
1. One cement that has an initial time of setting of less than 110 min,
2. One cement with an initial time of setting of greater than 150 min,
3. One cement with a final time of setting of less than 180 min, and
4. One cement with a final time of setting of greater than 210 min
(see Note 5).

NOTE 5—Laboratories are advised to reserve sufficient cement for future

qualification and standardization.
4.3 Tests—Using the method to be qualified and including the standardization formula
described in the section on standardization, make single determinations of the
times of initial and final setting on each of the three cements. On the same day,
conduct companion time of setting determinations according to Method A. Make
single determinations of the normal consistency on each cement, and use that
amount of water for all replicate batches. Complete three rounds of tests on
different days, repeating all the steps of the methods. Conduct the qualification
tests on specimens prepared separately from the standardization testing.

4.4 Calculations—Calculate the three–round averages for initial and final time of
setting for each cement and method. A method complies with the initial time of
setting qualification requirements if the difference between the initial time of
setting average values for Method A and the corresponding average 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 not exceed 30 min. Likewise, a method complies
 with the final time of setting qualification requirements if the difference between
the final time of setting average values for Method A and corresponding average
values for Method B is not greater than 45 min for any sample, and the range for
any three replicate tests by Method B does not exceed 30 min. Example
qualification data are given in Appendix X1.

4.5 Standardization—When standardization is required in order to achieve agreement

between Method A and Method B, it can be applied to either the initial time of
setting, final time of setting, or both. A standardization formula shall be based on
a comparison of test results obtained using Method A and the chosen method using
the automatic instrument (Method B). Results of tests from at least five different
hydraulic cements shall be required for standardization. The cements shall have a
minimum range of 60 min initial time of setting, and a minimum range of 90 min
final time of setting when tested in accordance with Method A. If desired, the three
cements used for instrument qualification may be used, but make new
determinations. Use the same method as used for instrument qualification,
including all the same steps. Valid standardization formulas shall be
mathematically derived and applied to all samples (see Note 6).
NOTE 6—Generally, the automatic instruments are computer operated
and easily adapted to standardization calculations.
4.6 Requalification of a Method
1. Requalify the method at least once per year and when any of the following
conditions occur:
1.1 The instrument has been significantly modified.
1.2 The instrument has been substantially repaired.
1.3 Substantial evidence indicates that the method is not providing data
meeting the performance requirements.
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.
 UNIVERSITY OF NEGROS OCCIDENTAL – RECOLETOS
COLLEGE OF ENGINEERING
CIVIL ENGINEERING DEPARTMENT

CETEST44P Name: Date Performed: Date Submitted:

Section:

Laboratory Test No.: Group No.: Score: Grade:

A.Y. ___________
Title:
 1st
 2nd
 Summer Instructor:

VI. DATA AND TABULATION

Report the time of setting and the method used as follows:

Duration (min.) Penetration (mm) Duration (min.) Penetration (mm)

0 - 30 180
45 195
60 210
75 225
90 240
105 255
120 270
135 285
150 300
165 315

VII. CALCULATIONS
1. Calculate the Vicat time of setting to the nearest 1 min as follows:
 2. Calculate the Vicat final time of setting by determining the elapsed time between the
time of the initial contact between cement and water and the time when the needle
does not sink visibly into the paste, rounded to the nearest 5 min.

METHOD A
*Precision and Bias
Precision:
1. The single-operator (within-laboratory) standard deviation has been found to be 12 min for
the initial time of setting, throughout the range of 49 to 202 min, and 20 min for the final time
of settings throughout the range of 185 to 312 min. Therefore, results of two properly conducted
tests by the same operator on Vicat initial time of setting of similar paste should not differ from
each other by more than 34 min and on Vicat final time of setting of similar pastes should not
differ from each other by more than 56 min.
2. The multilaboratory (between-laboratory) standard deviation has been found to be 16 min
for the initial time of setting throughout the range of 49 to 207 min, and 43 min for the final
time of setting throughout the range of 185 to 312 min. Therefore, results of two properly
conducted tests from two different laboratories on Vicat initial time of setting of similar pastes
should not differ from each other by more than 45 min, and on Vicat final time of setting of
similar pastes should not differ from each other by more than 122 min.
Bias—Since there are no accepted reference materials suitable for determining the bias for the
procedure in this test method, no statement on bias is presented.

METHOD B

*Precision and Bias

1. Precision—No precision data are available at this time. A laboratory is advised to develop
its own precision data for the method and instrument used. Based on qualification requirements,
the precision of the method should not be greater
than that of Method A.
 3. Bias—Since there are no accepted reference materials Suitable for determining the bias
for the procedure in this test method, no statement on bias is presented.

VIII. RESULTS AND DISCUSSION

IX. CONCLUSION

X. REFERENCES
1. ASTM Standards:
C 150 Specification for Portland Cement
C 151 Test Method for Autoclave Expansion of Portland Cement
C 183 Practice for Sampling and the Amount of Testing of Hydraulic Cement
C 187 Test Method for Normal Consistency of Hydraulic Cement
C 219 Terminology Relating to Hydraulic Cement
C 266 Test Method for Time of Setting of Hydraulic Cement Paste by
Gillmore Needles
C 305 Practice for Mechanical Mixing of Hydraulic Cement Pastes and
Mortars of Plastic Consistency
C 490 Practice for Use of Apparatus for the Determination of Length Change
of Hardened Cement Paste, Mortar, and Concrete
C 511 Specification for Moist Cabinets, Moist Rooms, and Water Storage
Tanks Used in the Testing of Hydraulic Cements and Concretes
C 595 Specification for Blended Hydraulic Cements
C 1005 Specification for Reference Masses and Devices for Determining
Mass and Volume for Use in the Physical Testing of Hydraulic Cements
C 1157 Performance Specification for Blended Hydraulic Cement
D 1193 Specification for Reagent Water