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PS:

232-1983 (R)

PAKISTAN STANDARD

SPECIFICATION FOR
PORTLAND CEMENT
(ORDINARY, HIGH STRENGTH AND RAPID HARDENING)

____________________________________________________________________________
Pakistan Standards & Quality Control Authority (PSQCA)
Standards Development Centre (SDC/PSQCA)
39-Garden Road, Saddar, Karachi-74400, Pakistan.
PS:232 – 1983 (R)

PAKISTAN STANDARD SPECIFICATION


FOR
PORTLAND CEMENT

(ORDINARY, HIGH STRENGTH AND RAPID HARDENING)


0. FOREWORD

0.1 This Pakistan Standard has been revised by the authority of the General Council of
Pakistan Standards Institution after the draft prepared by the Sectional Committee for
Clay Bricks, Cements, Cement Blocks and Hollow Blocks had been approved and
endorsed by the Building Materials Divisional Council on 28th December, 1983 in order
to bring it into line with present practice followed in the production and testing of
Cement.

0.2 Detailed test methods described in the appendices to PS: 232 : 1962 have been revised
and also various details of the concrete cube strength test, introduced in PS:232-1962,
have been made more stringent in order to produce more consistent results.

0.3 Specified minima for compressive strength for ordinary High strength and rapid
hardening Portland Cement are now given at ages of 3,7 and 28 days. The 3 and 7 days
strengths represent substantial increases over the values in the previous edition. The
introduction of a 28 days strength requirement is considered to provide a better
indication of Cement quality than the 7 days strength.

0.4 The optional requirement for the 1-day tensile strength of rapid hardening Portland
Cement has been omitted since experience has shown that this test produces rather
variable results and is very invoked.

0.5 The clause 13 on delivery has been omitted as being a contractual arrangement but a
requirement for marking has been introduced.

0.6 The specific surface test is a better method of testing fineness of the cement. This
measures the surface area of the particles per unit mass. Sieve test for determining the
fineness has been omitted.

0.7 In preparing this Pakistan Standard the views and suggestions of all the interests have
been taken into full consideration in addition to the following Standard Specification,
the use of which is acknowledged with thanks.

0.8 This standard is Pakistan intended chiefly to cover the technical provision relating to
the testing etc. of the material and it does not include all the necessary provisions of a
contract.
PS:232 – 1983 (R)
(2)

1. BS:12:1978 Ordinary and rapid-hardening Portland Cement.


2. BS:4550-1978 Method of testing cement.
3. BS:4627-1970 Glossary of terms relating to types of cement, their
properties and components.
4. PS:746-1969 Definition and Terminology of Cement.
5. PS:747-1969 Chemical Analysis of Cement-Determination of Sulphur
as Sulphide.
6. PS:748-1969 Chemical Analysis of Cement-Main Constivents of
Portland Cement.
7. PS:749-1969 Chemical Analysis of Cements-Determination of
titanium, phosphorus, manganess and of free lime.
8. BS:812 Methods for sampling and testing of mineral aggregates,
sands and filters.

9. BS:1881/4/70 Methods of testing concrete for strength.


10. BS:1610-1964 Methods for the load verification of testing machines.
11. ISO/R-147- 1960 Load calibration of testing machine for tensile testing of
steel.

12. ISO/R-376-1964 Calibration of static proving devices.


13. ISO:1920-1976 Concrete tests-Dimension, tolerance and applicability of
test specimen.
14. PS:424-1964 Load calibration of testing machines for tensile Testing of
Steel.
1. SCOPE

1.1 This Pakistan Standard specifies requirements for the composition, the manufacture,
sampling, testing methods and the chemical and physical properties of ordinary and rapid-
hardening Portland Cement.

Note: The term ‘rapid-hardening’ has been adopted in this standard because its use has
been accepted in Pakistan. It is synonymous with the designation “high early strength” which
is used in other countries and should not be confused with ‘Quick-setting’ cements which are
not covered by this standard.

2. Composition and manufacture of Portland Cement

2.1 The cement, whether ordinary or rapid-hardening, shall be obtained by pulverizing


clinker, consisting mostly of calcium silicates, obtained by heating to partial fusion a
predetermined and homogeneous mixture of materials containing principally lime (CaO) and
silica (Sio2) with a smaller proportion of alumina (A12O3) and iron oxide (Fe2O3).
PS:232 – 1983 (R)
(3)

2.2 The cement shall contain no additions except as provided for below :

a) Water or gypsum or anhydrite, or other derivatives of calcium sulphate, or any


combination of these substances; the amount of addition to be such that the
limits shown for sulphuric anhydride and loss on ignition shall not be exceeded.

b) Metallic iron from the grinding process shall not be regarded as an addition.

2.3 However, coloured Portland Cements shall be deemed to comply with the requirements
of this Pakistan Standard provided that:

a) The pigments comply with the requirements of BS:1014: (Relevant Pakistan


standard is under preparation);

b) The chemical composition of the Portland Cement constituent complies with


clause 5 of this Pakistan Standard;

c) The cement as a whole complies with the requirements of this Pakistan Standard
with the exception of clause 5.

3. TESTS

3.1 The sample or samples, taken as described in clause 11, shall be tested in the manner
specified for:

a) fineness (clause 4)
b) chemical composition (clause 5)
c) compressive strength (clause 6)
d) setting time (clause 7)
e) soundness (clause 8)

4. FINENESS

4.1 The cement shall be tested for fineness by the method described in Appendix ‘A’ and
shall have a specific surface of not less than:

Ordinary Portland Cement 225m2/kg (2250 cm2/g) Rapid Hardening Portland Cement
325 m2/Kg (3250 cm2/g)

5. CHEMICAL COMPOSITION

5.1 The chemical composition of the cement shall comply with the following requirements.

5.1.1 Lime saturation factor (LSF). The lime saturation factor shall be not greater than 1.02
end not less than 0.66 when calculated by the formula:
(CaO) – 0.7 (SO )
3
L.S.F = 2.8 (Si02) + 1.2 (A1203) + 0.65 (Fe203)
PS:232 – 1983 (R)
(4)

Where each symbol in parentheses refers to the percentage (by mass of total cement) of
the oxide, as determined by the methods described in Appendix B-1 for Si03, B-2 for Ca0, B-3
for AI203, B-4 for Fe203 and B-5 for S03 of this Pakistan Standard, excluding any contained in
the insoluble residue referred to in 5.2.

5.2 Insoluble residue

The mass of insoluble residue, as determined by the method described in Appendix C


of this Standard, shall not exceed 1.5%.

5.3 Magnesia

The mass of magnesia, as determined by the method described in Appendix D, shall not
exceed 4.0%.

5.4 Sulphuric anhydride

The mass of total sulphur expressed as SO3 and determined by the method described in
Appendix E, shall not exceed the appropriate value in table 1.

TABLE 1, MAXIMUM TOTAL SULPHUR EXPRESSED AS SO3 (%)

When tricalcium aluminate is 5% or When tricalcium aluminate is


Cement
less more than 5%

OPC 2.5 3.0

HSPC 2.5 3.0

RHPC 3.0 3.5

The tricalcium aluminate content (C3A) is calculated by the formula : C3A = 2.65
(A1203) – 1.69 (Fe203)

Where

C = Ca0

A = A1203

Where each symbol in parentheses refers to the percentage (by mass of total cement) of
the oxide, as determined by the method described in Appendix B-3 for A1203 and B-4 for
Fe203, excluding any A1203 contained in the insoluble residue referred to in clause 5.2.
PS:232 – 1983 (R)
(5)
5.5 Loss on ignition

The loss on ignition, as determined by method described in Appendix F, shall not


exceed 3.0% for cement in temperate climates or 4.0% for cement in tropical climates.

6. COMPRESSIVE STRENGTH

6.1 General. The cement shall be tested for compressive strength by one of the
methods specified in 6.2 and 6.3. The method of test shall be agreed between the vendor* and
the purchaser at the time of placing the order. In the event of a dispute, a retest shall be carried
out in the presence of representatives of the two parties concerned.

6.2 Average compressive strength of three mortar cubes, prepared, stored and tested as
described in Appendix ‘H’ shall be:

i. Ordinary Portland Cement:

at 3 days (72 ±1 h) Not less than 15.0 N/mm2 (2200 PSI or 155.0 kg/cm2)

at 7 days (168±2 h) Higher than the compressive strength at 3 days and not less than
23.5 N/mm2 (3400 PSI or 239.0 kg/cm2)

at 28 days Higher than the compressive strength at 7 days and not less than
34.5 N/mm2(5000 PSI or 352.0 kg/cm2).

ii. High Strength Portland Cement :

at 3 days (72 ±1 h) Not less than 23.0 N/mm2 (3336 PSI or 234.0 kg/cm2)

at 7 days (168±2 h) Higher than the compressive strength at 3 days and not less than
32.5 N/mm2 (4690 PSI or 330.0 kg/cm2)

at 28 days Higher than the compressive strength at 7 days and not less than
41 N/mm2 (5950 PSI or 418.0 kg/cm2)

iii. Rapid Hardening Portland Cement:

at 3 days (72 ±1 h) Not less than 29 N/mm2 (4205 PSI or 296.0 kg/cm2)
at 7 days (168±2 h) Higher than the compressive strength at 3 days and not less than
36.0 N/mm2 (5220 PSI or 367 Kg/cm2)
at 28 days Higher than the compressive strength at 7 days and not less than
46 N/mm2 (6670 PSI or 469.0 kg/cm2)
6.3 Average compressive strength of three concrete cubes, prepared, stored and tested as
described in Appendix ‘G’ shall be:
PS:232 – 1983 (R)
(6)
i. Ordinary Portland Cement:
at 3 days (72 ±1 h) Not less than 8.5 N/mm2 (91200 PSI or 84.0 kg/cm2)
at 7 days (168±2 h) Higher than the compressive strength at 3 days and not less than
14.0 N/mm2 (2800 PSI or 197.0 kg/cm2)
at 28 days Higher than the compressive strength at 7 days and not less than
19.0 N/mm2 (2800 PSI or 197.0 kg/cm2)

ii. High Strength Portland Cement :

at 3 days (72± 1h) Not less than 13.0 N/mm2 (1885 PSI or 132.5 kg/cm2)
at 7 days (168±2 h) Higher than the compressive strength at 3 days and not less than
18.0 N/mm2 (2610 PSI or 184.0 kg/cm2)
at 28 days Higher than the compressive strength at 7 days and not less than
29.0 N/mm2 (4200 PSI or 296.0 kg/cm2)

iii. Rapid Hardening Portland Cement:

at 3 days (72± 1h) Not less than 18.0 N/mm2 (2610 PSI or 1830 kg/cm2)
at 7 days (168±2 h) Higher than the compressive strength at 3 days and not less than
22.0 N/mm2 (3190 PSI or 224.0 kg/cm2)
at 28 days Higher than the compressive strength at 7 days and not less than
33.0 N/mm2 (4785 PSI or 336.0 kg/cm2)

7. SETTING TIME

7.1 The setting times of cement paste of standard consistence as determined by the methods
described in Appendix ‘1’ and Appendix ‘J’ shall be :

initial setting time : not less than 45 min.

final setting time : not more than 10 h

8. SOUNDNESS

8.1 The cement shall not have a expansion of more than 10 mm when tested for soundness
by the method described at Appendix ‘K’

8.2 If the cement fails to comply with this requirement, a further test shall be made in the
manner described. For this test, another portion of the same sample shall be used after it has
been aerated by being spread out to a depth of 70 mm to 80 mm at a relative humidity of
50% to 80% for a total period of 7 days. The expansion of this aerated sub sample shall not
exceed 5 mm.
PS:232 – 1983 (R)

(7)
9. MANUFACTURER’S CERTIFICATE

The manufacturer shall be satisfied that the cement at the time of its delivery complies
with the requirements of this Pakistan Standard and, if requested, he shall forward a certificate
to this effect to the purchaser or his representative. The certificate shall include the results of
the tests on samples of cement relating to the material delivered. The following test
information shall be provided :

*The term ‘Vendor’ in this Standard means the seller of this cement, whether he be the
manufacturer of the cement or not, fineness, compressive strength at 3,7 and 28 days, initial
and Final setting times and soundness.

10. INDEPENDENT TESTS

10.1 If the purchase or his representative requires independent test, they shall be carried out
in accordance with this Pakistan Standard on the written instruction of the purchaser or his
representative.

11. SAMPLING

11.1 If a sample is required for independent tests, it shall be taken, at the option of the
purchaser or his representative, before delivery or within 1 week after delivery of the cement,
by the method described in Appendix L. The tests shall be commenced within 4 weeks of
delivery. If the vendor so desires, he or his representative shall be present at the sampling.

12. FACILITIES FOR SAMPLING AND IDENTIFYING

12.1 When a sample of cement for testing is to be taken on the premises of the vendor, he
shall afford every facility and provide all labour and materials for taking and packing the
sample and as far as possible for Subsequently Indentifying the cement sampled.

Note : It is recognized that there may sometimes be difficulty in complying with the last
requirement since it may not be possible to identify a particular consignment of cement after it
has been placed with other cement in a silo on the user’s site.

13. COMPLIANCE

13.1 Any consignment or part of a consignment which when sampled in accordance with
clause 11 fails to comply with any one or more of the requirements of this standard, shall be
delede deemed not to comply with this Pakistan Standard.
PS:232 – 1983 (R)
(8)

14. CEMENT IN TROPICAL CLIMATES

14.1 The temperatures specifically mentioned in clause 3 of appendix-1 are applicable to


temperate climates. Cement intended for use in tropical climates may be tested at temperatures
exceeding 21 oC. When so tested, cement complying with the requirements hereins specified
for temperate climates shall be deemed to comply with this Pakistan Standard.

15. MARKING

15.1 Ordinary or rapid-hardening Portland Cement manufactured in compliance with this


Pakistan Standard shall be marked in relation to the product (e.g. on the bag, the manufacture’s
certificate, the delivery note or the invoice, etc.) with the following particulars :

a) The name, trade mark or other means of identification of the vendor ;


b) The name of the material, i.e., ordinary or rapid-hardening Portland cement ;
c) The number and year of this Pakistan Standard, i.e., PS:232 : 1983 ;
d) PSI certification mark.

*When cement is tested at temperatures above 21oC the strength and setting time
requirements may be altered by agreement between purchaser and the vendor. It should be
noted that an increase in the testing temperature increases the early compressive strength and
reduces the setting time.

APPENDIX A

Methods of testing Cement (Fineness test)

1. TEST PRINCIPLE

The fineness of cement is determined by a procedure giving specific surface expressed


as total surface area in square metres per kilogram.

2. APPARATUS

The following apparatus are required.

2.1 Permeability cell. The permeability cell shall consist of a metal cylinder made in
two flanged parts which are bolted together, containing a perforated plate on which is
supported a medium filter-paper 32 mm in diameter. The joint between flangtes is rendered
airtight by means of rubber or other suitable gasket. The permeability cell is provided with a
plunger by means of which the cement sample is formed, as described below, into a cylindrical
bed supported by the filter paper.
PS:232 – 1983 (R)
(9)

The essential dimensions are given below :

Internal diameter of upper of cylinder D = 25.00±0.03 mm or


D = 25.40±0.03 mm
0.05
External diameter of plunger D= 0.08
mm

Depth of bed space when plunger is fully inserted 10.00±0.03


+ 0 mm

Depth of recess in lower part of cylinder 1.6 – 0.3 mm


-0

Thickness of perforated plate 1.6+0.03 mm


-0

The perforated plate is a push fit in the recess.

A typical cell is shown in figure 1

2.2 Manometers. The permeability cell shall be connected to a bed manometer and a
flowmeter manometer as shown in figure 2. The arms of the manometer and of the flowmeter
are about 600 mm long. The capillary tube of the flowmeter shall have a bore of not less than
0.5 mm and its dimensions shall be such that the flowmeter constant C (as defined in 3.2) is
between 20 X 10-12 and 40 X 10-12 metric units. The liquid in both U-tubes is kerosene
(paraffin oil).

The necessary airflow may be produced by any convenient means, but the air entering
the apparatus shall be dried by passing a through tower pecked with a suitable desiccant, e.g.
silica gel.

Note. – While the apparatus described above should be regarded as standard, alternative
forms of air permeability apparatus may also be used provided they have been calibrated
against the standard apparatus.

2.3 Balance capable of weighing up to at least 10 g. to an accuracy of ± 0.0005 g.

3. PREPARATION

3.1 Checking of the dimensions of the permeability cell.

Check the dimensions of the cell when the apparatus is received, and after every 50
determinations, by suitable means. The depth of the bed space may be conveniently measured
by using a test piece of hardened steel, of diameter D 0.2 mm and 10.10±0.03 mm deep to
simulate the cement bed. Place the test piece on the filter-paper in the cell, insert the plunger
and check with a feeler gauge that the gap between the shoulder of the plunger and the top of
the cell is 0.10±0.03 mm.
PS:232 – 1983 (R)

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3.2 Determination of the flowmeter constant. Check the flowmeter constant every three
months. Pass dryair through the flowmeter at a constant rate for a measured time interval.
Collect the issuing air over kerosene and measure its volume. Note the flowmeter reating.
Calcualte the flowmeter constant C as follows :
Vn
C= Th2PL

Where

V is the volume (in ml) of dry air passed

N is the viscosity (in Ns/m2) of air at the calibration temperature

T is the time (in s) during which air is collected

h2 is the flowmeter reading (in mm)

PL is the density (in Kg/m3) of the Kerosine at the calibration temperature.

The viscosity of air in N s/m2 at temperatures in the range of 15 oC to 25 oC is shown


below multiplied by 106.

Temp. oC 15 17 19 21 23 25
to 16 to18 to20 to22 to 24

Viscosity 17.8 17.9 18.0 18.1 18.2 18.3

Repeat this process for five flowmeter readings over the range of 250 mm to 550 mm.
Calculate the average value of C and express the result o to the nearest 0.1 X 10-12 metric units.

3.3 Calibration of the apparatus. – calculate the value of K for each apparatus as follows
and express the result to the
3–1
nearest 10m
1.40 A
K=
1–є CL
PS:232 – 1983 (R)

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Where

Є is the porosity, i.e., 0.475 (see clause 4).


A is the area (in mm2) of the cement bed.
L is the depth (in mm) of the cement bed.
C is the flowmeter constant.

For apparatus made tot the alternative dimensions specified in 2.1

D = 25.00 mm 25.40 mm
A = 490.9 mm2 506.7 mm2
L = 10.00 mm 10.00 mm
and K = 612 6.12

√ C √ C

3.4 Assembling and testing of the apparatus. - Change the filter-paper after every
determination. In reassembling the permeability cell ensure that the two parts are firmly bolted
together and test the cell and its connections for leakage.

Note. This is best done by disconnecting at the monometer the rubber tube leading
from the lower and of the cell, sealing the tube with a screw clip, applying air pressure until the
monometer shows a difference in level of at least 500 mm and then sealing off the air inlet.
The reading of the monometer should not change by more than 0.5 mm in a period of 1 min.

4. PROCEUDRE

Select a mass of cement from table 1 for a 25.00 mm cell or from table 2 for a 25.40
mm cell which, when compacted, will give a porosity of 0.475 at the measured density of the
cement. (The porosity is defined as the ratio of the volume of pore space to the total volume of
the bed). Weigh the cement to ± 0.0005 g and brush it into the permeability cell, which is
gently shaken from side to side to level off the surface. If the cement is lumpy it may first be
rubbed gently with a spatula on glazed paper
PS:232 – 1983 (R)
(12)

Table – 1. Mass of cement (in g) required to form a bed 25.00 mm in diameter and 10.00 mm deep having a porosity of 0.475 over
density range 2800 kg/m3 to 3290 kg/m3

Density Kg/m3 0 10 20 30 40 50 60 70 80 90
2800 7.216 7.247 7.267 7.293 7.319 7.345 7.370 7.396 7.422 7.448
2900 7.474 7.499 7.525 7.551 7.577 7.602 7.628 7.654 7.680 7.705
3000 7.731 7.757 7.783 7.809 7.834 7.860 7.886 7.912 7.937 7.963
3100 7.989 8.015 8.040 8.066 8.092 8.118 8.144 8.169 8.195 8.221
3200 8.242 8.272 8.298 8.324 8.350 8.376 8.401 8.427 8.453 8.479

Table 2.-Mass of cement (in g) required to form a bed 25.40 in diameter and 10.00 mm deep having a porosity of 0.475 over density range
2800 kg/m3 to kg/m3

Density Kg/m3 0 10 20 30 40 50 60 70 80 90
2800 7.449 7.475 7.502 7.528 7.555 7.582 7.608 7.635 7.661 7.688
2900 7.715 7.741 7.768 7.794 7.821 7.848 7.874 7.901 7.927 7.954
3000 7.981 8.007 8.034 8.060 8.087 8.114 8.140 8.167 8.193 8.220
3100 8.247 8.273 8.300 8.326 8.353 8.380 8.406 8.433 8.459 8.486
3200 8.513 8.539 8.566 8.592 8.619 8.646 8.672 8.699 8.725 8.752
PS:232 – 1983 (R)

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Compact the contents by allowing the cell to fall four time from a height of about 10
mm on the bench. Next, slowly insert the plunger and push it home so that the shoulder of
the plunger is in contact with the top of the permeability cell. Do not twist the plunger while
in contact with the cement surface but slowly withdraw it with a twisting motion.

If, on inspection, the cement bed is seen to be disturbed, knock the sample out and
repeat the operation with a fresh sample.

Insert the upper bung and slowly turn on the air ; - Next insert the lower bung slowly
and carefully in order to avoid forcing air through the cement in the wrong direction. Adjust
the rate of airflow until the flowmeter monometer shows a difference in level of 300 mm to
500 mm. When the levels are constant, indicating that steady conditions have been obtained,
take readings of the difference in level h1 of the bed monometer and of the difference in
level h2 of the flowmeter monometer. Repeat these observations at a different airflow \rate
within the above range.

5. CALCULATION

Calculate the average value of the ratio h1/h2. Calculate the specific surface, Sw, as
follows and express the result to the nearest 5 m2 / kg.

K h1
Sw =

Where

K is the constant of the apparatus determined in accordance with 3.3

e is the density (in Kg/m3) of the cement determined in accordance with


Section 2,2

h1 is the average ratio of the monometer readings determined in accordance


with
h2 clause 4.
PS:232 – 1983 (R)

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PS:232 – 1983 (R)

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PS:232 – 1983 (R)

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Appendix B-1

1. METHOD RECOMMENDED FOR DETERMINATION OF SILICA:

1.1 Procedure. Mix thoroughly 1.000 g of the sample and about 1.0 g of ammonium
chloride in a 100 ml beaker, cover the beaker with a watch glass and add catiously 10 ml of
hydrochloric acid, allowing the acid to run down the lip of the covered beaker. After the
chemical action has subsided lift the cover, add one or two drops of nigric acid, stir the
mixture with a glass road, replace the cover and set the beaker on a water bath for 30 min.
Filter through a 90 mm rapid filter paper, transferring the jelly like mess of silicic acid to the
filter as completely as possible without dilution and allowing the solution to drain through.
Scrub the beaker with a rubber policeman, rinse the beaker and policeman and wash the
filter two or three times with hot hydrochloric acid ( 1+99 ). Then was the filter with ten or
twelve small portions of hot water, allowing each portion to drain through completely.
Reserve the filtrate and washings.

Transfer the filter paper and residue to a weighed platinum crucible, dry and ignite,
at first slowly until the carbon of the paper is completely consumed without inflaming and
finally at 1200 0C for 30-45 min. Cool in a desiccator to room temperature (this will take
about 15 min.) and weigh the residue as impure silica.

Treat the silica thus obtained, which will contain small amounts of impurities, in the
crucible with 0.5 ml to 1 ml of the water, 2 drops of sulphuric acid and about 10 ml
hydrofluoric acid and avaporate cautiously to dryness. Heat the small residue finally at
1200oC for a minute or two, cool and weigh. The difference between this weight and the
weight previously obtained represents the amount of silica. To this amount of silica add the
amount of silica determined in the filtrate as described in clause 1.2. Fuse the residue with
not more than 0.5 g of potassium pyrosulphate. Dissolve the cold melt in 5 ml of
hydrochloric acid (1+4) and add the solution to the reserved filtrate. Dilute the solution in a
volumetric flask to 500 ml. Mix and reserve.

1.2 Determination of silica remaining in solution.

Note. – In an acid medium, silica forms a yellow silicomolybdate complex with


ammonium molybdate. The complex is quantitatively converted to molybdemnum blue by 1
amino-2-nephtol-4 sulphonic acid. The interference of phosphate is removed by ammonium
citrate.

1.2.1 Special reagents. – Prepare special reagents by the following methods.

(1) Ammonium molybdate. – Dissolve 10 g of ammonium polybdate in water,


make up to 100 ml and filter. Store in polythene bottle. Do not keep for more than one
week.

(2) Citric acid. – Dissolve 10 g of citricacid, monohydrate, in water and make up


to 100 ml.
PS:232 – 1983 (R)

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(3) Reducing Solution. – Weigh 0.15 g of 1-amino-2-naphthol-4-sulphonic acid,


1.4 g of sodium sulphite and 9.0 g of sodium metabisulphite, dissolve in water, make up to
100 ml and filter if necessary. Prepare a fresh solution each week unless refrigerator storage
is available.

Note. 0.7 g of sodium sulphite, anhydrous, may be substituted for 1.4 g of sodium
sulphite, hydrated.

(4) Standard silica solutions

Stock solution. Weigh 0.2000 g of freshly ignited ‘Specpure’ silica or purest quartz
ground in agate into a platinum crucible containing 2.0 g of sodium carbonate, anhydrous.
Mix, cover the crucible and fuse for 15 min. Dissolve the cooled melt in water in apolythene
beaker and make up to 200 ml.

Store in a polythene bottle.

1 ml contains 1 mg Sio2.

Working solution. Pipette 5 ml to stock solution and dilute with water to 250 ml.
Mix and store in a polythene bottle. The solution should be made up fresh each week.

1 ml contains 0.02 mg Sio.2

(5) Copmpensating solution. – Dissolve 0.8 g of ammonium chloride and 8 ml of


hydrochloric acid in water and dilute to 100 ml.

1.2.2 Procedure. To prepare a calibration graph, pipette 10 ml of working standard


solution, in 2 ml inerements, into a series of 100 ml volumetric flasks. Add 5.0 ml of
compensating solution to each and dilute to approximately 20 ml. Add 5 ml ammonium
molybdate solution, rinse the necks of the flask, swirl to mix and allow to stand for 5 – 10
min Add 5 ml of citric acid solution to each flask, rinse, mix and wait 5 min. Add 2 ml of
rducing solution, make up to 100 ml with water and mix. Allow to stand for at least 30 min
before measuring the colour. The colour is stable for at least 24 h.

Prepare a sample solution by diluting the filtrate from the silica separation (1.00 go
of cement, see 1.1) to 500 ml. Pipette 20 ml of this olution into a 100 ml volumetric lfask.
Add 5 ml of ammonium molybdate solution and contain as in preceding paragraph.

1.2.3 Measurement. – The colour can be measured by visual comparision or


instrumentally, using an absorptiometer or a spectrophotomer (as 650 mm). The size
of absorption cell will depend on the instrument available.
PS:232 – 1983 (R)

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Appendix B-2

1. METHOD RECOMMENDED FOR DETERMINATION OF CALCIUM


OXIDE

1.1 Reagents. Prepare reagents by the following methods:

(1) Potassium hydroxide solution. – Dissolve 200 g of potassium hydroxide in


one litre of water.

(2) Glycerol solution. – Dilute 200 ml of glycerol to one litre with water.

(3) Triethamolamine. Solution. – Dilute 200 ml of pure triethanolamine to one


litre with water.

(4) Murexide indicator. Grind together 0.5 g of murexide (ammonium


purpurate colour Inxex 56083) and 100 g of sodium chloride to form a homogeneous
mixture.

(5) Diamino-ethane-tetra-acetate solution (EDTA). Dissolve 6.67 g of


disodium-diamino-ethane-tetra-acetate (EDTA disodium salt) in distilled water, adjust to PH
10 with potassium hydroxide solution and dilute to one litre. Store in a polythene bottle.

1.1.2 Standardization.- To standardize, dissolve about 0.1 g, accurately weighted, of pure


calcium carbonate in dilute hydrochloric acid, taking care that no loss of liquid occurs.
Warm to remove carbon dioxide, cool and dilute to about 200 ml with water. Adjust the pH
to 12.2-12.5 with potassium hydroxide solution. Add approximately 0.06 g of murexide
indicator and titrate with EDTA solution in a photometric end-point detector*. An increase
in optical density occurs as the end-point is approached.

As the end-point is approached make successive, small, equal increments of the


EDTA and note the steady galvanometer reading after each increment. Continue until the
galvanometer is not, or is only slightly, affected by the addition of ε-DTA.

Plot the galvanometer readings against the volume of EDTA and find the end-point
by the intersection of the line of steepest slope and the line of constant optical density. Use
only those points in the immediate vicinity of the end-point. See example in Fig 1.

If W = weight of CaCO3

And t = ml of RDTA for equivalence,

then 1 ml EDTA = 56.08 X 1000 W mg CaO.


100.09 X t
PS:232 – 1983 (R)

( 19 )

1.3 Procedure. – Commence with a portion of the filtrate and washings obtained by the
procedure specified for total silica in clause 1.1 Appendix B-1.

Take 50 ml aliquots, add 20 ml of glycerol solution and 20 ml of triethanolamine and


adjust to pH 12.2-12.5 with potassium hydroxide, using a pH meter. Add approximately
0.06 g of murexide indicator.

Titrate with EDTA (1 ml = 1.0 mg of CaO, i.e. about 6.67g of disodium salt/litre) in
the photo-electric end-point detector.

Record the volume of EDTA added and the galvanometer readings obtained Plot
Volume of EDTA against galvanometer-readings, using only those results in the immediate
vicinity at the endpoint, and find the exect end –point as in the example.

1.4 Calculation

CaO%=VE

Where V ml = EDTA required for equivalence per 1 g of Cement and


E=Standardization factor of the EDTA solution.

Appendix = B-3
1. METHOD RECOMMENDED FOR DETERMINATION OF ALUMINA:

1.1 Reagents. – Prepare reagents by the following methods:

(1) Aluminium Stock solution. – 1 mg of A12O3 per ml. Weight 0.2647 g of aluminium
metal (99.99% pure) into a ploy-propylene beaker. Add 30 ml of water and 1 g of sodium
hydroxide. When solution is complete, cool and wash into a 500 ml volumetric flask, add 10
ml of hydrochloric acid, cool, makeup to the mark with water and mix.

(2) Aluminium standard solution. – 0.2 mg of A12O3 per ml. Pipette 50 ml of the 1
mg/ml solution into a 250 ml volumetric flask, make up to the mark and mix.

(3) Ammonia (1+1). – Add 500 ml of ammonia solution to 500 ml of water and mix.

(4) Ammonium acetate. – (40%) Dissolve 200g of ammonium acetate in water and
makeup to 500 ml. Mix and filter.

(5) Ammonium chloride, Solid.

(6) Chloroform. – Containing as stabilizer not more than 2% ethanol.


PS:232 – 1983 (R)

( 20 )
(7) Cupferron. (6%). – Dissolve 3 g solid, which must be pale in colour and as nearly
white as is available, in 50 ml of water. Add about 1 g of activated charcoal, stir well and
filter. The solution shall be discarded at the first sign of deterioration; the rate of
deterioration can be reduced by storing in a refrigerator. It is also recommended that the
solid reagent should be stored in the cold.

(8) Hydrochloric acid

(9) Hydroxyammonium chloride. – Dissolve the required quantity in a little water and
filter, if necessary, before use.

(10) 8-Ihydroxyquinonlium (5%). – Dissolve 50 g of 8-quinolinol in 120 ml of glacial


acetic acid, dilute to 1 litre with water and filter.

(11) Methyl red indicator. Dissolve 0.2 g of methyl red in 100 ml of ethanol (95%).

(12) Nitric acid

(13) 1 : 10-Phenanthroline (1%).-Dissolve 0.1 g of 1:10-Phenanthroline hydrate in a


mixture of 5 ml of glaciaf acetic acid and 5 ml of water. A larger quantity may be prepared
if required for immediate use.

1.2 Procedure

1.2.1 Comence by using a portion of the filtrate and washings obtained by the procedure
specified for total silica in clause 1.1 of Appendix B-1.

1.2.2 Pipette out exactly 100 ml into a 250 ml borosilicate glass beaker, of any shape
preferred by analyst. Pipette out a further 100 ml similarly. Treat each aliquote as follows.

Bring the solution to the boil. Add ammonia, from a dispensing buretto or other
suitable vessel, until the liquid is just alkaline to methyl red. Do not add any bromine.

Either : Pour through a 90 mm or 110 mm rapid, hardened, ashless filter paper


and allow to drain completely. Do not wash. Discard the filtrate, place the original beaker
under the funnel and sissolve the R2O3 precipitate on the paper, using hydrochloric acid ( a
total of just 20 ml) and boiling water alternately. The total volume should not exceed about
80 ml, but it is imperative to ensure that the R2O3 is completely redissolved.

or. Preferably : Pour into a centrifuge-tube, without rinsing and spint at about
3000 rev/min for 10 min. Pour off the liquid as completely as possible into a clean beaker; it
is very unlikely that any R2O3 will thus be lost but if it is, recover it by filtering the poured
off liquid. Dissolve the R2O3 in the centrifuge tube using 20 ml of hydrochloric acid and
warm water and rinse all back into the original 250 ml beaker ; the total volume should not
exceed about 80 ml.
PS:232 – 1983 (R)

( 21 )

1.2.3 Cool the solution (of the R2O3 from 0.2 g of cement) to 10oC or lower. Similarly
cool the water, cupferron solution and chloroform to be used.

Transfer the solution to a 250 ml conical seporatingf Funned (with glass stopper and
preferably with polytetrafluorethylene stopcockey) which has been marked at 100 ml. Wash
out the beaker with cool water into the funnel until this mark has been reached. Add 5 ml of
cooled cupferron solution. Add also 10 ml, chloroform Stopper, shake vigorously and
release excess pressure by carefully loosening the glass stopper (not by opening the
stopcock). Rinse the stopper into the funnel. Stand long enough to allow the layers to
separate. Without delay run off the lower (chloroform) layer into a beaker, as completely as
possible without rising loss of the equeous layer.

Add a few drops of cupferron solution to the aqueous layer. Only a white precipitate,
re-dissolving, should be produced. (If a coloured precipitate appears, ad 2.5 ml of cupferron
solution plus 10 ml of chloroform and repeat from above. Add further 10 ml portions of
chloroform and rpeat from above (without adding cupferron) till the chloroform layer is
colourless and the aqueous layer is clear. Discard the chloroform extracts.

1.2.4 Rund and wash the aqueous layer, filtered if necessary, into a 500 ml conical or tall-
shape beaker carrying a mark at 200 ml. Heat on the water-bath until any small amount of
chloroform present seems to have been removed, then boil carefully to ensure complete
removal. (To ensure a final precipitate of adequate size in the blank add 50.0 ml of standard
aluminium solution, equivalent to 10.0mg of A12O3. to the blank at this point.)

1.2.5 Adjust volume to about 200 ml. – Add the required quantity of 8-hydroxyquinoline
solution : for samples with up to 7.5% A12O3 this will be 10 ml; increase proportionately for
higher percentages. Add slowly, while stirring with a thermo meter, 40 ml of ammonium
ecetate solution. Continue to stir as the liquid is heated to 60-65o Co and maintain this
temperature for 10 min. stirring occasionally. If 65oC is exceeded, break down of the iron-
phenanthroline complex any lead to high results for alumina. Allow to cool for 30 min.

1.2.6 Filter through a sintered glass crucible of a porosity approximately equivalent to


Grade No.4 and about 40 ml capacity, which has been weighed after washing with cid and
drying at 140oC. (It is advisable to check that further acid washing does not alter the weight
of the crucibles used (with a rubber policeman complete the transfer of the precipitate from
the beaker (and from the thermometer). Wash with water at 40-50o C, suck dry, transfer the
crucible to an oven, maintain at 140o C for 2 h, cool for 30 min. in a desiccator and weigh.
Check constancy of weight after a further 30 min. of heating. The precipitate should be
close to mimosa yellow, a greenish precipitate indicates that iron has escaped separation and
complexing.
PS:232 – 1983 (R)

( 22 )

1.2.7 A12O3 = weight of precipitate X 0.1110. Adjust the result according to the difference
between the ‘blank’ and the A12 O3 that it is known to contain. Calculate the volues
obtained from the aliquots to percentages and report the average percentage of the two, to
the nearest 0.01% as the alumina content of the sample.
11.10 (s-b)
Thus : A12O3% =
0.2
Where : s = weight of precipitate from 0.2 g of cement and

b-weight of precipitate from ‘blank’ – 0.090 (0.090 being the weight


in grammes of aluminium oxinate equivalent to 0:010 g of A12O3.

1.2.8 Alternative routine method for tropical elimates for routine work in tropical climates
the following method of determination of alumina may be used as an alternative, though the
method described above remains the reference method.

Prfoceed as in 1.2.1 and 1.2.2, but instead of ’20 ml’ hydrochloric acid, as in 1.2.2,
substitute ‘the smallest effective quantity then, nearly neutrelize the hot solution (of the R2
O3 from 0.2 g of cement) with sodium hydroxide solution. Bhoil 100 ml of sodium
hydroxide. 10% solution and pour the hot R2O3 solution into it while stirring. Filter off the
precipitated iron and titanium on a hardened repid paper and wash well with warm
sodiumhydroxide 5% solution.

Acidify the filtrate with hydrochloric acid, using a very little methyl red as indicator.
Nearly neutralize with ammonia, add exactly 2 ml of hydrochloric acid and boil off any
CO2. Cool to 50oC, add 1 g of hydroxyammonium chloride (dissolved in a little water) and 5
ml of 1 : 10-phenanthroline solution, stir and maintain near 50oC for 5 min.

Continue as in 1.2.5, 1.2.6 and 1.2.7.

APPENDIX B – 4

1. METHOD RECOMMENDED FOR DETERMINATION OF IRON OXIDE

1.1 Reagents

Prepare reagents by the following methods :

(1) Stannous chloride solution. Dissolve 5 g of SnC12.2H2O in 10 ml of hydrochloric


acid and dilute to 100 ml. Add2 pieces of iron-free tin and boil until the solution is clear.
Keep the solution in a dropping bottle containing some metallic tin.
PS:232 – 1983 (R)
( 23 )

(2) Barium diphenylamine sulphonate indicator. Dissolve 0.3 g of barium diphe


nyalmine sulphonate in 100 ml of water.

(3) Standard potassium dichromate solution. (1ml=0.004 g Fe2O3). Dissolve 2.457 g of


dried K2Cr2O7 in water and dilute to 1 litre.

(4) Mercuric chloride safurated solution.

1.2 Procedure :

To 1.000 g of sample in a 250 ml conical flask add 40 ml of cold water and while
stirring the mixture vigorously add 10 ml of hydrochloric acid. If necessary, heat the
solution and break up the cement with the flattened tip of a glass rod until it is certain that
all the cement is completely decomposed.

Head the solution to boiling and treat with SnC12 solution, adding this drop by drop
with swirling until the solution becomes colourless. Add one drop in excess and cool the
solution to room temperature. Rinse down the interior of the beaker with water and add, all
at one time, 10 ml of saturated HgC12 solution, Mix vigorously for 1 min and add 10 ml of
H3 PO4 (1+1) and two drops of barium diphenylamine sulphonate indicator, Add sufficient
weter so that the volume after titration is between 75 mland 100 ml. Titrate with the
standard K2Cr207 solution. The end-point is taken where one drop causes an intense purple
colour which remains unchanged by further addition of standard K2Cr2 solution.

1.3 CALCULATION

Calculate percentage of Fe203 as fallows:

Fe2O3% = 0.004 V X 100

Where V = ml of K2Cr2O7 solution required by 1 g of cement sample.

APPENDIX-B-5

1. METHOD RECOMMENDED FOR DETERMINATION OF SULPHURIC


ANHYDRIDE

1.1 To 1.000,g of cement in a 250 ml beaker add 25 ml of cold water and while stirring
vigorously add 5 ml of hydrochloric acid. If necessary, heat the solution and break-up the
cement with the flattened end of a glass rod until decomposition is complete. Dilute the
solution to 150 ml and heat it just below boiling point for 15 min. Filter on a medium filter
paper and wash the residue thoroughly with hot water. Dilute the solution to 250 ml and
boil. Add 10 ml lot hot barium chloride solution (100 g 01) dropwise from a pipette, boil
until the precipitate is properly formed, let the solution stand at Just below boiling point for
at least 30 min and leave to cool for 12-24 h.
PS:232 – 1983 (R)

( 24 )

Ensure that the volume of the solution remains between 225 ml and 260 ml adding
water if necessary. Filter the precipitate on a slow filter paper, wash free from chlorides and
place the filter paper and its contents in a weighed platinum or porcelain crucible. Heat
slowly and burn of the filter paper without flaming Ignite at 800oC for 15 min, cool in a
desiccator and weigh the barium sulphate.

Verify that the obtained weight remains constant after a second ignition of 5 min.

1.2 Calculate SO3 content as follows:

SO3% = W X 34.3

Where W = weight of BaSO4 in grammes.

APPENDIX C

1. METHOD RECOMMENDED FOR DETERMINATION OF INSOLUBLE


RESIDUE

1.1 Procedure:

To 1.000 g of sample add 10 ml of cold water and whilst vigorously swirling the
mixture add 5 ml of hydrochloric acid.

If necessary, warm the solution gently and disperse the sample until decomposition
of the cement is complete.

Dilute the solution to 50 ml and digest for 15 min at a temperature just below
boiling. Filter the residue on a medium filter paper, wash six times with hot water and then
transfer the filter paper and its contents back to the reaction beaker.

Add 100 ml (10g/1) of sodium hydroxide, and maintain the solution at a temperature
just below boiling point for 15 min. In the presence of methyl red as indicator acidify the
solution with hydrochloric acid and add an excess amount equivalent to 4 or 5 drops of
hydrochloric acid. Filter on a medium filter paper and wash the residue 12 to 15 times with a
hot solution of ammonium nitrate (20g/1).

Ignite the residue to constant weight in a weighed crucible at 900oC to 1000oC.


PS:232 – 1983 (R)

( 25 )

1.2 Analysis of Insoluble Residue.

If the insoluble residue does not exceed 0.36% assume that it contains 2/3 Sio2 and
1/3 A12O3.

If the insoluble residue exceeds 0.36% fuse it with sodium carbonate plus borax,
take up in water plus hydrochloric acid and datermine Si, A1, Fe and Ti by colorimetric
procedures as required.

If barium sulphate or other abnormal insolubles are present the analyst should design
a method appropriate for them and indicate it in his report.

APPENDIX-D

1. METHOD RECOMMENDED FOR DETERMINATION OF MAGNESIA

1.1 Reagents, Paper reagents by the following methods.

(1) Triethanclamine solution. As in clause 1.1 Appendix B-2.

(2) Methyl thymol blue complexone indicator. Grind together 0.5 g of methyl thymol
blue complexone and 100 g of potassium nitrate to form a homogeneous mixture.

(3) Diamino-ethane-tetra-acetate solution (EDTA). The solution used in clause 1.1.


Appendix B-2 is suitable.

1 ml = E mg CaO = 0.719E mg Mg0.

(4) Ammonium chloride/ammonia buffer (pH 10.0). Dissolve 70g of ammonium


chloride in water, add 570 ml of ammonium hydroxide solution and dilute to 1 litre with
water.

1.2 Procedure : Commence by using a portion of the filtrate and washings obtained
by the procedure specified for total silica in clause 1.1. Appendix B-1.

To a 50 ml aliquot add 20 ml of triethanolamine solution and adjust the pH to 10.0


with ammonium chloride/ammonia buffer. Titrate for the sum of magnesia and calcium with
EDTA solution, using methyl thymolblue complexone indicator and a photometric end-
point detector. Find the endpoint in the same way as given in Appendix B-2. Note that as the
end-point is approached the optical density decreases.
PS:232 – 1983 (R)
( 26 )

1.3 Calculation

Mgo % = (X-V) + 0.719 E

Where V and E have the values obtained under clause 1.4 Appendix B-2 and X is the
volume of EDTA required in the titration for the sun of magnesium and calcium.

APPENDIX – E.

1.1 Method Recommended ror Determination of Total SULPHUR.

1.2 Procedure

To 1.000 of cement add 25 ml of saturated bromine water and while stirring


vigorously and add 5 ml of hydrochloric acid saturated with bromine. If necessary, heat the
solution and break up the cement with the flattened end of a glass rod until decomposition is
complete. Dilute the solution to 150 ml and heat it to boiling point until all the promino has
been driven off. Then proceed as in clause 1.1 Appendix B-5.

1.3 Calculation

S% = WX 13.73

where W-weight of barium sulphate in grammes.

APPENDIX – F

1. METHOD RECOMMENDED FOR DETERMINATION OF LOSS-ON-


IGNITION

1.2 Procedure. In a weighed covered platinum crucible (20 ml to 25 ml) head 1.000 g
of the sample to constant weight in a muffle furnace at 925 ± 25 oC. The initial heating takes
15 min, subsequent period last 5 min.

1.2.1 Expression of results. The percentage loss-on-ignition is calculated to the nearest 0.1
%.

Note. If heating is carried out at a different temperature, this fact should be


mentioned in the analysis report.

1.3 Procedure. Weigh approximately 1 g of the cement sample into a shallow


platinum or silica dish of diameter 25 – 40 mm and heat for 30±5 min at a temperature of
925 + 25 oC. Allow to cool, covered in a desicator cover magnesium perchlorate. Weigh and
calculate the percentage loss-on-ignition.
PS:232 – 1983 (R)
( 27 )

APPENDIX – G

METHODS OF TESTING CEMENT

1. COMPRESSIVE STRENGTH OF CONCRETE CUBES

1.1 Test Principle. The strength of cement is determined by compressive strength tests
on 11 mm concrete cubes, made with specified coarse and fine aggregates, mixed by
machine and compacted manufally with a compacting bar.

Note. – The water/cement ratio is 0.60 (C1, table2) for all cements except
supersualphated and high alumina, for which values of 0.55 (C2, table2) and 0.45 (C3, table
2) respectively are used.

1.2 Refererence. The titles of the standards publications referred to in this clause of
this Section are listed on the back cover.

1.3 Apparatus. The following apparatus is required.

1.3.1 Moulds

1.3.1.1 Size. The moulds shall be 100 mm cubes.

1.3.1.2 Constructil. The mould shall be of ferrous metal (preferably cast iron or cast steel)
and rigid enough to prevent distortion. The surface hardness of each internal face shall be at
least 95 Rockwell (Scale B) hardness value. It shall be constructed in such a manner that it
facilitates the removal of the moulded, specimen without damage, the parts of the mould,
when assembled, shall be positively and rigidly held together by suitable means, both
during the filling and on subsequent handling of the filled mould.

Each mould shall be provided with a steel base plate which shall be rigidly attached
to the mould and shall support it without leakage or distortion.

1.3.1.3 Tolerances. The mould shall be such that, when assembled ready for use, the
dimensions and internal faces are accurate within the following limits.

(a) Dimensions. The depth of the mould and the distance between either pair of
opposite internal faces, each based on the average of four symmetrically
placed measurements, shall be 100.00 ± 0.15 mm.

(b) Flatness. The surface of each internal face shall lie between two perallel
planes 0.03 mm apart. The joints between the sections of the mould and
between the bottom surface of the mould and the top surface of the base plate
shall lie between two parellel planes 0.06 mm apart.
PS:232 – 1983 (R)
( 28 )

(c ) Squareness. The surface of each internal face shall lie between two parallel
planes 0.5 mm apart which are perpendicular to the bottom surface of the
mould and also to the adjacent internal faces.

(d) Parallelism. The top surface of the mould shall lie between two parallel
planes 1.0 mm apart, parallel to the bottom surface.

(e) Surface texture. The surface textural of each internal face shall be 3.2
m CLA.

1.3.1.4 Assembly. In assembling the cleaned mould ready for use, the joints between
the sections of the mould and between the bottom of the mould and the base plate shall be
sealed by a thin film of gresse or other suitable method to prevent escape of water. Any
excess grease shall be carefully removed. – The internal faces of the assembled mould shall
be thinly couted with mould oil to prevent adhesion of the concrete.

1.3.3 Trowel. The trowel shall have a cast steel blade, a suitable type is shown in
figure 2.

1.3.4 Compacting bar. The compacting bar shall be a steel bar weighting 1.8 Kg and
having a ramming face 25 mm square.

1.3.5 Tank. The tenk shall contain clean tap water, which shell be renewed at least avery
saven days with water at the specified temperature.

Specimens made with high alumina, supersulphated or Portland-tube cements shalkl


not be placed in the same tank.

1.3.6 Compression testing machine. The compression testing machine shall be of


suitable capacity for the test and shall comply with the requirements described in Appendix-
M.

1.4 Temperature and humidity conditions. The temperature throughout the entire
test procedure shall be controlled about a madpoint of 20oC with permitted variations as
shown in table 1. The minimum relative humidity shall be as given in table 1.

TABLE 1. Temperature and humidity conditions

Situation Permitted Minimum


temperature relative humidity
variation
o
C %
Mixing room ±2 65
Moist curing chamber ±1 90
Water curing tank … ±1 ---
Compression testing room … ±2 50
PS:232 – 1983 (R)
( 29 )

Note. – A record should be kept for reference purposes of the actual temperature and
relative humidity conditions.

Before use, all materials, moulds and other appliances shall be brought to the same
temperature as the air in the mixing room, by storing them in the room for a sufficient time.

1.5 Preparation of speumen. – The specimens shall be prepared as follows.

1.5.1 Number of cubes. Make batches of six or nine cubes, three for testing at each of the
specified ages.

1.5.2 Aggregates. The coarse aggregate and the sand shall comply with the requirements
described in Appendix- ‘O’ and ‘P’

If the moisture content of the coarse aggregate, when tested by the standard (oven
drying) method specified in Appendix ‘M’, exceeds 0.1% it shall be dried at a temperature
not exceeding 110 oC. Sieve the coarse aggregate on 10 mm and 5 mm sieves with square
holes so that it is substantially free from oversized and undersized particles.

1.5.3 Proportioning. – The masses of the individual materials for batches of six or nine
cubes are given in table 2 and 3.

1.5.4 Mixing. – Place the weighed materials in the mixer pan in the following order :

Sand, Cement, Coarse aggregate.

Hold the mixing water ready and start the mixer. After 15 s and the water uniformly
during the next 15 s; then continue mixing for a total time of 180 ± 5 s. After the machine
mixing turn the concrete over in the pan a few times with a trowel to remove any slight
segregation. If this is not possible, transfer the concrete to another suitable vessel and turn it
over similarly therein.

1.5.5 Compacting. – Half fill the cube moulds as quickly as possible. Compact each with
exactly 35 strokes of the compacting bar, uniformly distributed over the cross section of the
mould. Place a further quantity of concrete in each mould to form the top layer and compact
similarly. The strike off the top of each cube and smooth with the trowel so that the surface
of the concrete is level with the top of the mould. Complete the entire operation within 15
min from the completion of the mixing.

Mix type (see Material Proportions by Mass


note to 1.1) mass 6 cubes 9 cubes
g g
C1 Cement 1.0 2200±5 3200±5
Sand 2.5 5500 8000
Coarse aggregate 3.5 7700±10 11200±10
Water 0.60 1320±5 1920±5
PS:232 – 1983 (R)

( 30 )

C2 Cement 1.0 2200±5 3200±5


Sand 2.5 5500 8000
Coarse 3.5 7700±10 11200±10
aggregate 0.55 1210±5 1760±5
Water

C3 Cement 1.0 2940±5 4270±5


Sand 1.875 5500 8000
Coarse 2.625 7700±10 11200±10
aggregate 0.45 1320±5 1920±5
Water

TABLE 3. Mass of individual fractions of sand:

Mass

6 cubes 9 cubes

Fraction A(2.36 mm to 1.18 mm) g g


B(1.18 mm to 600 m) 550±5 800±5
C(600 m to 150 m) 1650±5 2400±5
D(300 m to 150 m) 1400±5 2000±5
E(150 m to 90 m) 800±5 1200±5

1.6 Storage of specimens.-Immediately after preparation place the moulds in a single


layer on a level surface in the moist curing chamber. In order to reduce evaporation, cover
the exposed top of the cubes with a flat impervious sheet (e.g. of clean thin rubber for
plastics, or lightly oiled steel) making contact with the upper edge of the mould. After
24±0.5h mark the cubes for later identification and remove from the moulds. Immediately
submerge all specimens, except those to be tested at 24 h, in the tank and arrange them in
such a way that the temperature variation specified in table 1 is not exceeded. Leave the
cubes in the tank until just prior to the test.

Specimens to be tested at 24 h are marked and demoulded 15 min to 20 min before


the test and are covered with a damp cloth so that they remain in the moist condition. If the
concrete has not achieved sufficient strength after 24 h to be handled without fear of
damage, delay the demoulding for a further period of 24 h but state this fact in the test
report.
PS:232 – 1983 (R)
( 31 )

1.7 Testing of specimens.- Determine the compressive strength of the cubes, under the
temperature and relative humidity conditions specified in table 1 for the compression testing
room: at the specified age, calculated from the time of adding the water to the other
materials, by the procedure specified in Appendix-M, the auxiliary platens. Test the
specimens within the following limits :

24 ± 0.5 h
3 days (72 ± 1 h)
7 days (168 ± 4 h)
and 28 days (28 days ± 4 h)

1.8 Calculation. – Calculate the average of the individual results of the set of three
specimens tested at the same age, end express the result to the nearest 0.5 N/mm2. If one
result within the set varies by more than ±5% from the everage of the set, discard the result
and recalculate the average of the remaining results. If more than one result varies by more
than ±5% from the average, discard the set of results.

1.9 Report. – Report the individual results and the average compressive strength to the
nearest 0.5 N/mm2 indicating if any result has been discarded.

APPENDIX – H

1. COMPRESSIVE STRENGTH OF MORTAR CUBES

1.1 Test principle. – The strength of cement is determined by compressive strength tests
on 70.7 mm mortar cubes, made with a specified sand, mixed by hand and compacted by
means of standard vibration machine.

1.2 Reference. The titles of the standards publications referred to in this clause of
this Section are listed on the back cover.

1.3 Apparatus. The following apparatus is required.

1.3.1 Moulds.

1.3.1.1 Size. The moulds shall be 70.7 mm cubes, the area of each face being 5000 mm2.

1.3.1.2 Construction. – The mould shall be of metal that is not attached by cement mortar
and rigid enough to prevent distortion. It shall be constructed in such a manner as to
facilitate the removal of the moulded specimen without damage. The parts of the mould,
when assembled, shall be positively and rigidly held together, by suitable means, both
during the filling and on subsequent handling of the filled mould. Each mould shall be
provided with a steel base plate to support it without leakage. The weight of the mould and
base plate shall be such as to comply with the requirements given in 1.3.3, for the mass of
the machine.
PS:232 – 1983 (R)

( 32 )
1.3.1.3 Tolerances. The mould shall be such that, when assembled ready for use, the
dimensions and internal faces are accurate within the following limits :

(a) Dimensions. The depth of the mould and the distance between either pair of
opposite internal faces, each based on the average of four symmetrically
placed measurements, is 70.7 ± 0.1 mm.

(b) Flatness. The surface of each internal face shall lie between two parallel
planes 0.03 mm apart. The Joints between the sections of the mould and
between the bottom surface of the mould and the top surface of the base shall
lie between two parallel planes 0.06 mm apart.

(c) Squareness. – The surface of each internal face shall lie between two parallel
planes 0.5 mm apart which are perpendicular to the bottom surface of the
mould and also to the adjacent internal faces.

1.3.2 Trowels. – The trowels shall have a cast steel blade, a suitable type is shown in
figure 1.

1.3.3 Vibration machine. The vibration machine shall consist of a table mounted on coil
springs to carry the cube mould, and a revolving shaft provided with an accentric. By means
of a balance weight beneath the base plate attached rigidly to the table, the centre of gravity
of the whole machine, including the cube and mould, shall be rought either to the centre of
the eccentric shaft or within a distance of 25 mm below it. In consequence of this, the
revoling eccentric imparts an equal circular motion to all parts of the machine and mould,
this motion being equivalent to equal vartical and horizontal simple harmonic vibration 90o
out of phase. The minimum running speed of the mechine shall be well above its natural
frequency on its supporting springs, so that the amplitude of vibration is supporting springs,
so that the amplitude of vibration is independent of the speed. The motor shall be preferably
of the synchronous type and the drive is by means of an endless belt running on a crowed
pulley on the motor and a crowned pully on the vibrator. The machine shall be provided
with a suitable clamp to bold the assembled mould firmly on the table, and with a suitable
hopper to facilitate filling of the mould.

The machine shall be constructed to comply with the following essential


requirements.

Mass of machine on its supporting springs (excluding mass of solid eccentric but
excluding mass of mould, mould clamp, hopper and cube) 29 Kg approx.

Out-of-balance moment of
eccentric shaft 0.016 N m

Normal running speed of eccentric shaft 12000 ± 400 r/min

A typical vibration machine of the type described above is shown in figure 3.


PS:232 – 1983 (R)

( 33 )

1.3.4 Tank. The tank shall contain clean top water which shall be renewed at least every
seven days with water at the specified temperature.

1.3.5 Compression testing machine. – The compression testing machine shall be of


suitable capacity for the test and shall be comply generally with the requirements described
in Appendix ‘M’. It shall be capable of applying load at the rate specified in 1.7 of this
Appendix. The auxiliary platens shall comply with the requirements of Appendix ‘M’.

1.4 Temperature and humidity conditions. – The temperature throughout the entire test
procedure shall be controlled about a midpoint of 20oC with permitted variations as shown
in table 1. The minimum relative humidity shall be as given in table 1.

TABLE 1. TEMPERATURE AND HUMIDITY CONDITIONS

Situation Permitted Minimum


temperature relative humidity
variation
o
C %
Mixing room ±2 65
Moist curing chamber … ±1 90
Water curing tank ±1 ---
Compression testing room … ±2 50

Note. – A record should be kept, for reference purposes of the actual temperature and
relative humidity conditions.

Before use, all materials, moulds and other appliances shall be brought to the same
temperature as the air in the mixing room, by storing them in the room for a sufficient time.

1.5 Preparation of specimens. – The specimens shall be prepared as follows.

1.5.1 Number of cubes. Make three cubes for testing at each of the specified ages.

1.5.2 Aggregate. The sand shall comply with the requirements of Appendix ‘Q’ of this
Pakistan Standard.

1.5.3 Proportioning. The mass (es) of cement, sand and water for each cube are
given in table 2.
PS:232 – 1983 (R)
( 34 )

TABLE 2. MIXES FOR MORTAR CUBES

Mix Proportions by All cements other than high alumina


Material
type mass cement : mass
g

VI Cement 1.0 185 ± 1

Sand 3.0 555 ± 1


Water 0.4 74 ± 1
High alumina cement:
mass
g

V2 Cement 1.0 190 ± 1


Sand 3.0 570 ± 1
Water 0.4 76 ± 1

1.5.4 Mixing. Before mixing, clamp the assembled mould on the table of the
vibration machine and attach the hopper to the top of the mould. Mix the mortar for each
cube separately on a non-porous surface that has been wiped over with a damp cloth. Mix
the cement and the sand dry, for 1 min, by means of the two trowels. Then add the water and
mix the whole for 4 min with the two trowels.

1.5.5 Compacting. Place the whole of the mortar in the hopper of the mould by the use of
suitable scoop as quickly as possible and compact by vibration for a period of 120 ± 5 s.

1.6 Storage of specimens. Immediately after vibration, remove the hopper and place the
moulds in a single layer on a level surface in the moist curing chamber. In order to reduce
evaporation, cover the exposed top of the cubes with a flat impervious sheet (e.g. clean thin
rubber or plastics, or lightly oiled steel) making contact with the upper edge of the mould.
After 24±0.5 h mark the cubes for later identification and remove from the moulds.
Immediately submerge all specimens, except those to be tested at 24 h, in the tank and
arrange them in such a way that the temperature variation specified in table 1 is not
exceeded. Leave the cubes in the tank until just prior to the test.

Specimens to be tested at 24 h are marked and demoulded 15 min to 20 min before


the test and are covered with a damp cloth so that they remain in the moist condition. If the
mortar has not achieved sufficient strength after 24 h to be handled without fear of demage,
delay the demoulding for 2 further period of 24 h but state this fact in the test report.

1.7 Testing of specimens. Determine the compressive strength of the cubes, under the
temperature and relative humidity conditions specified in table 1 for the compression testing
room, at the specified age, calculated from the time of adding the water to the other
materials, by the procedure specified in Appendix ‘M’ and using the auxiliary platens,
except that the load is applied at a rate of approximately 35 N/mm2 per minute.
PS:232 – 1983 (R)
(35)

Test the specimens within the following limits :

24 ± 0.5 h
3 days (72 ± 1 h)
7 days (168 ± 2 h)
and 28 days (28 days ± 4 h)

1.8 Calculation. Calculate the average of the individual results of the set of three
specimens tested at the same age and express the result to the nearest 0.5 N/mm2. If one
result within the set varies by more than ± 5% from the everage of the set, discard the result
and recalculate the everage of the remaining results. If more than one result varies by more
than ± 5% from the average, discard the whole set of results.

1.9 Report. Report the individual results and the average compressive strength to
2
the nearest 0.5 N/mm , indicating if any result has been discarded.
PS:232 – 1983 (R)
(36)
PS:232 – 1983 (R)
(37)
PS:232 – 1983 (R)
(37)

APPENDIX – I

METHOD OF TESTING CEMENT DETERMINATION OF STANDARD


CONSISTANCE.

1. TEST PRINCIPALE

The quantity of water required to give a cement paste of standard consistence is


determined by using the Vicat apparatus.

This quantity of water gives the water content of the pastes for the determination of
settings times (Appendix ‘J’ and of soundness Appendix ‘K’).

Note. For high alumina cement this test is not carried out and a value of 22% is
assumed.

2. APPARATUS

2.1 Mould. The mould (figure 1) consists of a split ring (E). It shall have an
internal diameter 80.0 ± 0.1 mm and a height of 40.0 ± 0.5 mm. The mould rests on a non-
porous plate which is lightly greased. A metal plate 3 mm thick is suitable.

To ensure interchangeability of the clamping rings, the external diameter at the base
of the mould shall be 89.0 ± 0.1 mm with a taper of 2o on the side. Total taper shall be 4o
inwards from base to top. The outer clamping ring is similarly tapered. When assembled,
this ring shall be clear above the base of the mould, by a distance of 15 mm to 18 mm.

2.2 Frame. The frame D (figure 1) bears a movable rod B supporting a cap A and
carrying an indicator which moves over a graduated scale attached to the frame. The other
end of the movable rod has a cylindrical hole and knurled screw the suitable for the insertion
of various attachments. There shall be a clearance of about 6 mm between the lower end of
the attachments, when they are raised, and the top edge of the mould to enable the mould to
be located in position without damage to the attachments. The total mass of the moving unit,
when in use, complete with attachments, shall be 300 ± 1 g.

2.3 Plunger. The plunger G (figure 1) is of polished brass 10.00 ± 0.05 mm in


diameter with a projection at the fitting and for insertion into the movable rod B. Its length
shall be 50 V 1 mm and the lower face is flat. Its mass shall be 9.0 ± 0.5 g.

2.4 Trowels. The trowels shall have a cast steel blade; a suitable type is shown in
figure 2.

3. Temperature and humidity conditions keep the temperature of the mixing room at 20
o
V 2 C and the relative humidity at not less than 65%. Before use, ensure that all materials,
moulds and other appliances are at the same temperature as the air in the mixing room by
storing them in the room for a sufficient time.
PS:232 – 1983 (R)
(38)
4. PROCEDURE

4.1 General. Weigh, to ± 1 g, about 400 g of cement and a measured quantity of


water. Mix these materials vigorously for 240 ± 5s on a non-porous surface, by means of the
two trowels. Fill the mould with the cement paste within the next 15 s in one layer and
smooth off the surface of the paste level with the top of the mould as quickly as possible. In
filling the mould use gloved hands and the blade of the trowel only. Complete the operation
within 255 s from the addition of the water to the cement. Immediately after filling the
mould, place it centrally under the movable rod B bearing the plunger G. Lower the plunger
gently into contact with the surface of the cement paste, then quickly release it and allow it
to sink into the surface. Note the amount of settlement.

4.2 Determination of standard consistence. Make up trial pastes of varying quantities of


water and carry out the procedure specified in 4.1 unit that quantity is found giving a paste
which permits the settlement of the plunger G to a point 5 V 1 mm from the bottom of the
mould. Record the quantity of water used.

5. CALCULATION

Calculate the weight of water required to vive a paste of standard consistence as a


percentage of the mass of the dry cement to the nearest 0.5.

6. REPORT
Report the standard consistence to the nearest 0.5 %.
PS:232 – 1983 (R)
(39)
PS:232 – 1983 (R)
(40)

APPENDIX – J

METHODS OF TESTING CEMENT (SETTING TIMES)

1. TEST PRINCIPLE

The initial and final setting times of cement are determined by using the Vicat
apparatus.

2. APPARATUS

The following apparatus is required.

2.1 Mould. The mould shall comply with the requirements of 2.1 Appendix ‘I’
(see figure 1).

2.2 Frame. The Frame shall comply with the requirements of 2.2 of Appendix ‘I’ (see
figure 1).

2.3 Initial setting time needle. The initial setting time needle, C, which is round, is made
of hardened or tempered steel and shall be of diameter 1.13 ± 0.05 mm. Its effective length,
excluding the hilt (fitting end) is 50 ± 1mm and the lower face is falt. Its mass shall be 9.0 ±
0.5 g.

2.4 Final setting time needle. The final setting time needle, F, is made of the same
material and shall have the same mass, shape and section as the needle (C) but it shall be 30
± 2 mm in length, and be fitted with a metal attachment hollowed out so as to leave a
circular cutting edge 5.0 ± 0.1 mm in diameter.

The depth hollowed out shall be 0.5 ± 0.1 mm. A vent hole 0.76 mm diameter is
provided as shown in figure 1. The length of projection of the needle beyond the cutting
edge shall be 0.5 ± 0.1 mm.

2.5 Trowels. Trowels shall comply with the requirements of 2.4 of Appendix ‘I’.

3. TEMPERATURE AND HUMIDITY CONDITIONS

The temperature throughout the entire test procedure shall be controlled about a mid
point of 20o with permitted variations as shown in table 1. The minimum relatives humidity
shall be as given in table 1.
PS:232 – 1983 (R)
(41)

TABLE 1. TEMPERATURE AND HUMIDITY CONDITIONS


SITUATION PERMITTED MINIMUM
TEMPERATURE RELATIVE
VERIATION HUMIDITY
o
C %
...
Mixing room ± 2 65
...
Moist curing chamber ± 1 90

Note. A record should be kept, for reference purposes, of the actual temperature and
relative humidity conditions.

Before use, all materials, moulds and other appliances shall be brought to the same
temperature as the air in the mixing room, by storing them in the room for a sufficient time.

4. PROCEDURE

4.1 General. Using the procedure described in 4.1 of Appendix ‘I’, mix about 400
g of cement with the quantity of water required to give a paste of standard consistence, fill
the mould within the prescribed time and place immediately in the moist curing chamber.

4.2 Determination of initial setting time. Place the mould under the moveable rod B
bearing the needle C. Lower the needle gently into contact with the surface of the cement
paste, at least 10 mm from the edge of the mould, then quickly release it and allow it to sink
into the surface. Repeat this process until the needle, when brought into contact with on
undisturbed part of the surface of the cement paste, at least 10 mm from previous
penetrations, and released as described, penetrates to appoint 5 ± 1 mm from the bottom of
the mould. Record the period elapsing between the time when this condition is reached and
the time of adding the water to the cement.

4.3 Determination of final setting time. Replace the needle C by the needle F. Lower the
needle gently into contact with the surface of the cement pasts, then quickly release it and
allow it to sink into the surface. Repeat this process until only the needle madkes an
impression on an undisturbed part of the surface of the cement paste, but the attachment
fails to do so. Record the period elapsing between the time when this condition is reached
and the time of adding the water to the cement.

Note. If a scum forms on the surface of the cement paste, the undersite of the specimen
may be used for the determination of final setting time.
PS:232 – 1983 (R)
(42)

5. REPORT

REPORT THE INITIAL SETTING TIMES TO THE NEAREST 5 MIN.


PS:232 – 1983 (R)
(43)

APPENDIX – K

METHODS OF TEDSTING CEMENT SOUNDNESS TEST

1. TESTING PRINCIPLE

The soundness of cement is determined by the ‘Le Chatelier’ method of measuring


its expansion, either after immersion in cold and in boiling water or, for supersulphated
cement, after immersion in cold water.

2. APPERATUS

The following apparatus is required.

2.1 Small split cylinder (figure 1) of spring brass or other suitable metal of 0.5 mm
thickness, forming a mould 30mm internal diemeter and 30 mm high. The inside surface of
the mould shall be thinly coated with mould oil. On either side of the split are attached two
pointers (AA). The distance from these ends to the centre of the cylinder shall be 165 mm.
The split shall be not more than 0.5 mm wide.

2.2 Two glass plates to cover the mould.

3. PROCEDURE

3.1 Immersion in cold and boiling water. Using the procedure described in 4.1 of
Appendix ‘I’ mix about 100 g of cement with the quantity of water required to give a paste
of standard consistence. Place the mould on one glass plate and fill it with the cement paste,
taking care to keep the split of the mould gently closed whilst this operation is being
performed. Next, cover the mould with the other glass plate, upon which a small weight is
placed. Immerse the whole immediately in water at a temperature of 20 ± 1 oC and leave
there for 24 ± 0.5h.

Then remove the mould from the water. Measure the distance separating the
indicator points to the nearest 0.5 mm and again immerse in water at a temperature of 20 ± 1
o
C. Bring the water the boiling point in 25 min to 30 min and keep boiling for 1 h. Next
remove the mould from the water and allow to cool. Again measure the distance separating
the indicator points to the nearest 0.5 mm : the difference between the two measurements
represents the expansion of the cement.

3.2 Immersion in cold water. Using the procedure described in 4.1 of Appendix ‘I’, mix
about 100 g of cement with the quantity of water required to give a paste of standard
consistence. Place the mould on one glass plate and fill it with the cement paste, taking care
to keep the split of the mould gently closed whilst this operation is being performed. Then
cover the mould with the other glass plate, upon which a small weight is placed. Measure
the distance separating the indicator points to the nearest 0.5 mm. Immerse the whole
immediately in water at a temperature of 20 ± 1oC and leave there for 24 ± 0.5 b.
PS:232 – 1983 (R)
(44)

The remove the mould from the water. Measure the distance separating the indicator
points to the nearest 0.5 mm. The difference between the two measurements represents the
expansion of the cement.

4. REPORT

Report the expansion to the nearest 1 mm.

APPENDIX – L

METHOD OF TESTING CEMENT SAMPLING

1. SCOPE

of the Pakistan Standard describes methods for obtaining samples of cement


for test purpose from deliveries.

The sampling situations covered by this standard are :

Cement in bags, drums or other packages:

Cement in bulk – delivery vehicles:

Cement on discharge from a storage silo.

2. GENERAL

Samples shall be taken using clean, dry equipment and shall be stored in clean, dry,
airtight sample containers.

3. SIZE OF SAMPLES

Samples shall be of 7 kg minimum mass taken in accordance with clause 5.


PS:232 – 1983 (R)
(45)

4. REPRESENTATION

The quantity of cement represented by a sample shall not normally exceed 21 t.

When the mass of cement in any container exceeds 21 t, special arrangements, based
on the general principles of the sampling methods described in this standard, shall be agreed
between the parties concerned.

5. SAMPLING METHODS

5.1 Cement in bags, drums or other packages. Samples shall consist of at least five sub-
samples obtained, if possible, from different containers. The containers to be sampled shall
be selected by :

(a) allocating, in a systematic order, a number to each container in the delivery :

(b) dividing the total number of containers by the number of sub-samples


required to identify different parts of the delivery.

(c) Selecting at random from each part, a container to be sampled.

When there are fewer than five containers, each container shall be sampled and
approximately the same quantity of cement shall be taken from each container.

The use of a sampling tube is preferred.

5.1.1 Sampling by sampling tube. A suitable form of tube is shown in figure 1. Marks on
the collars of both tubes correspond to the center line of the slots so that, then the mark on
the inner tube is lined up with the mark on the outer tube, the slots are open.

The closed sampling tube shall be inserted into an opened container and driven into
the cement. The tube shall then be opened and rotated until it takes a full core of cement
from substantially the entire length of the container.

5.1.2 Sampling by other methods. When no sampling tube is available, the container shall
be opened and a sub-sample taken by means of a scoop or other appropriate tool.
PS:232 – 1983 (R)

(46)

5.2 Cement in a bulk-delivery vehicle. A sample shall be obtained by use of sampling


ladle. A suitable form of ladle shown in figure 2. Before any cement is discharged, the
inspection cover on the top of the delivery vehicle shall be removed.

The top 150 mm (approximately) of the cement shall be) scraped aside. The exposed
surface shall be sampled by lading from it a sufficient number of sub-samples. The ladle
shall not be overfilled and care shall be exercised to avoid loss of any part of a sub-sample
when transferring it from the ladle to the sample container.

5.3 Cement from the discharge of a storage silo.

A sub-sample shall be obtained from the silo discharge by use of a scoop or other
appropriate tool. At least three sub-samples shall be taken evenly spaced through the
discharge from the silo. The sub-samples shall be combined to form the sample.

A sample of cement taken from a silo shall be taken as representing only the quantity
of the cement discharged at the time of sampling. It shall not be taken as representing a
particular batch or delivery of cement to the silo unless the silo is known to contain no other
cement.

6. STORAGE AND DELIVERY OF SAMPLES

Immediately after being taken, the sample shall be stored in a clean, dry, airtight
container made of metal or glass. The volume of air remaining in the filled container shall
be the minimum practicable.

7. CERTIFICATE OF SAMPLING

The sample shall be accompanied by a certificate of sampling on which shall be


recorded information identifying the material and the method of sampling.

The general form of certification is shown in figure 3.


PS:232 – 1983 (R)

(47)
PS:232 – 1983 (R)

(48)

(a) Side view (b) Front view

Approximate dimensions of sampling ladle

Diameter 225 mm.


Depth of ladle 175 mm.
Handle Length 1800 mm

Figure 2. Typical sampling ladle


PS:232 – 1983 (R)

(49)

PS: 232:1982 (Revised) Appendix ‘L’

Certificate of sampling
In accordance with PS : 232 : 1983 (Revised) Appendix ‘L’

Material

Type of cement

Source of supply

Nature and size of consignment sampled

Identification of consignment sampled

SAMPLING

Date of sampling

Method of sampling

Name and signature of sampler

Figure 3. Certificate of sampling

APPENDIX – M

TESTING MACHINE TEST FOR CEMENT

Compression Testing Machine, ehe Testing Machine may be of any reliable type of
suitable Capacity for the test and capable, of applying the load at the Rate Specified in 2.1.3.

The testing machine shall be equipped with two rigid bearing platens made of a
material which will not deform irreversible or wear excessively in normal size. They shall
be at least as large as the nominal size of the specimen to which the load is applied.

The upper machine platen shall be able to align freely as contact is made with the
specimen, but the platens shall be restrained (by friction or other means) from tilting with
respect to each other during loading.

The flatness tolerance (flatness 1) for the area to be in compact with the specimen
shall be 0.03 mm wide and the surface texture shall be 3.2 mm CLA.
PS:232 – 1983 (R)

(50)

1.1 Auxiliary platens. An auxiliary platen 25.0 ± 0.4 mm thick may be interposed
between the specimen and each machine platen. The upper auxiliary platen shall rest on the
specimen and not be attached to the upper machine platen.

1.1.1 Material. The platens shall be made of a material which will not deform irreversibly
or wear excessively in normal use.

1.1.2 Tolerances. The platens shall be such that they are accurate within the following
limits :

(1) Dimensions. The distance between either pair of opposite edges, based on
the average of four symmetrically placed measurements, shall be the nominal
size of the specimen + 0.2 mm. – O.Omm

(2) Flatness. The flatness tolerance (flatness 1) for each contact face shall be
0.03 mm wide.

(3) Square ness. The square ness tolerance (‘square ness 1’) for each edge with
respect to the adjacent edge as datum edge shall be 0.5 mm wide.

(4) Parallelism. The parallelism tolerance (‘parallelism’) for one contact face
with respect to the other contact face as datum face shall be 0.06 mm wide.

(5) Surface texture. The surface texture of each contact face shall be 3.2 mm
CLA.

2. PROCEDURE

2.1 General. Cubes stored in water shall be tested immediately on removal from
the water, whilst they are still wet, Cubes for testing at 24 h shall be tested in the moist
condition and no-fined cubes shall be tested in the air-dry condition. Surface water and grit
shall be wiped off the cube and any projecting fins removed.

2.1.2 Placing the cube in the testing machine. The bearing surfaces of the testing machine
and of any auxiliary platens shall be wiped clean and any loose grit or other material
removed from the surfaces of the cube which are to be in contact with the compression
platens. The test cube shall be placed in the machine in such a manner that the load shall be
applied to opposite sides of the cube as cast, i.e. not to the top and bottom. The cube shall be
placed on the lower machine platen and carefully centred.
PS:232 – 1983 (R)

(51)

A block or blocks may be interposed between the cube or the auxiliary platen and
the lower machine platen providing that the system is stable throughout the test and means
are available for the cube to be correctly centred. Not more than two blocks plus on
auxiliary platen may be used. Each block shall be solid, shall support the cube or the
auxiliary platen over the whole of its area and have a rectangular vertical section. The
properties of the material, and the surface flatness, surface texture and parallelism of the
contact faces of each block shall comply with the requirements specified for auxiliary
platens in clause 1.1. Each block shall be not less than 24.6 mm thick.

No other packing shall be used at any of the interfaces between the cube, auxiliary
platens, blocks and machine platens.

2.1.3 Loading. The load shall be applied without shock and increased continuously at a
rate of approximately 15 MN/m2 min until no greater load can be sustained. The maximum
load applied to the cube shall be recorded. The appearance of the concrete and any unusual
features in the type of failure shall be noted.

Note. An unusual failure is one where the four vertical faces of the cube are not
equally damaged and the cause should be investigated.

3. Calculation. The compressive strength of each cube shall be calculated by


dividing to the maximum load by the nominal cross-sectional area and shall be expressed to
the nearest 0.5 MN/m2.

4. Report. The following information shall be included in the report on


each cube :

(1) date of test,

(2) identification mark and nominal size of specimen.

(3) age of cube.

(4) compressive strength.

(5) appearance of concrete and type of fracture, if these are unusual.


PS:232 – 1983 (R)

(52)

Appendix – N

1. DETERMINATION OF MOISTURE CONTENT OF AGGREGATE


(STANDARD OVEN DRY METHOD).

1.1 General. The oven-drying method provides a measure of the total water present in a
sample of aggregate and is the standard procedure. This method is particularly appropriate
when a single sample of aggregate is received at a laboratory for test.

1.2 Apparatus. The following apparatus is required.

1.2.1 A balance of adequate capacity (normally a balance of 3 Kg capacity would be


appropriate) accurate to 0.5 g and of such a type as to permit the weighing of the container
specified below .

1.2.2 An airtight non-corrodible container of about 3 Kg capacity.

1.2.3 A scoop (a convenient size is about 200 mm long and 120 mm wide).

1.2.4 A well ventilated oven thermostatically controlled to maintain a temperature of


105 ± 5oC.

1.3 Sample for test. The mass of the sample of aggregate to be tested shall be between
1.8 Kg and 2.2 Kg. It shall be prepared taking the precautions given in clause 1.2.

Note. The size of sample of fine aggregates may be reduced to not less than 500 g
provided weighing are made using a balance of adequate a capacity and accurate to 0.1 g.
The size of sample of coarse aggregate with a nominal size exceeding 40 mm may need to
be greater than the mass specified to permit accurate sampling; the balance used for the
weighing should be accurate to 0.05% of the mass of the sample.

1.4 Test procedure. Clean the container with its lid, dry it and then weight it (mass A).
Then place the sample in the container by means of the Scoop, replace the lid and re-weigh
the whole (mass B). Remove the lid, place the container and sample in the oven and dry it at
a temperature of 105 ± 5 oC for a period of 16 h to 24 h. The remove the container and
sample from the oven, replace the lid and allow the whole to cool for 0.5 h to 1 h, after
which weigh again (mass C.)
PS:232 – 1983 (R)

(53)

1.5 Calculations, - The moisture content shall be calculated as follows :

Moisture content (% by dry mass)

B–C
= X 100
C–A
or

Moisture content (% by wet mass)

B–C
= X 100
B–A

1.6 Reporting of result. - The moisture content shall be reported to the nearest 0.1%
stating whether by dry mass of by wet mass. The percentage by dry mass shall be reported
unless the percentage by wet mass is specifically requested.

Appendix – O

Method of testing cement Standard coarse Aggregate


for concrete cubes

1. SCOPE:

This part of this Pakistan Standard specifies the source and properties of a standard
coarse aggregate to be used with a standard sand for making concrete cubes.

2. SOURCE :

The coarse aggregate shall consist of clean, substantially free from dust and dry
crushed granite, in one fraction, 10 mm to 5 mm nominal size.

3. SAMPLING:

A sample for the purpose of the test specified in clause 5 shall be obtained generally
by the method of sampling coarse and fine aggregates specified in BS:812 : Part 1. A main
sample of about 30 Kg shall be taken from a consignment and shall be reduced to about 500
g by a total of six passes through a sample divider.
PS:232 – 1983 (R)

(54)

4. GRADING:

The grading of the sample obtained as in clause 4 shall be within the following limits
when determined by the normal test procedure for sieve analysis using square hole
perforated plate test sieves of nominal aperture size of 10.0 mm and 5.00 mm within the
tolerances.

Test sieve Percentage by mass


passing BS sieve

10.0 mm 90 to 100
5.00 mm 0 to 10

Appendix – P

Methods of testing cement Standard sand for concrete cubes

1. SCOPE:

This part of this Pakistan Standard specifies the source, preparation and properties of
a standard sand to be used with a standard coarse aggregate for making concrete cubes.

2. SOURCE:

Natural (uncrushed) silica sand in five fractions shall be obtained by extracting them
from sands derived from the sources listed in table 1. Where alternative sources are given,
either sand, or a mixture of both, may be used.

3. SAMPLING :

Using a suitable scoop or similar device, a main sample of about 8 Kg shall be taken
from a single bag selected at random from each of the fractions of sand comprising a
delivery not exceeding 500 Kg of each fraction. For either of the tests specified in clauses 4
and 5 the main sample of each fraction shall be reduced to about 250 g by five passes
through a sample divider. For the purpose of the test specified in clause 6 the main sample
of each fraction shall be split into eight 1 kg samples by three passes through a sample
divider. Six of these samples shall be passed again through a sample divider to produce six
pairs of nominally identical sub samples of about 500 g of each of the five fractions. The
remaining two 1 Kg samples may be used for the tests specified in clauses 4 and 5.
PS:232 – 1983 (R)

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4. MOISTURE CONTENT :

The moisture content of the sample of each sand fraction obtained as specified in
clause 3 shall not exceed 0.1% by dry mass when tested by the standard (oven drying)
method specified in Appendix ‘N’.

TABLE 1. Locations of the sources of testing sand

Fraction Sources
A (2.36 mm to 1.18 mm) Joseph Arnold and Sons Ltd.,
Leighton Buzzard, Bedfordshire.
George Garside (Sand) Ltd.,
Leighton Buzzard, Bedfordshire.
B (1.18 mm to 600 mm) Joseph Arnold and Sons Ltd.,
Leighton Buzzard, Bedfordshire.
George Garside (Sand) Ltd.,
Leighton Buzzard, Bedfordshire.
C (600 mm to 300 mm) Joseph Arnold and Sons Ltd.,
Leighton Buzzard, Bedfordshire.
George Garside (Sand) Ltd.,
Leighton Buzzard, Bedfordshire.
D (300 m to 150 m) Joseph Arnold and Sons Ltd.,
Leighton Buzzard, Bedfordshire.
E (150 m to 90 m) The Nene Barge and Lighter Co. Ltd., Elton
Sand Pit, High Holborn Farm, Wansford
Road, Elton, nr. Peterborough,
Combridgeshire.

5. GRADING :

The grading of the sample of each sand fraction weighing not less than 200 g,
obtained as specified in clause 3 shall be within the limits given in figure 1 when determined
by the normal test procedure for sieve analysis, using the appropriate woven wire test sieves.

6. AIR-ENTRAINING CHARACTERISTICS

6.1 Test Principle. – The sand shall show limited air-entrainment propensity when tested
using the materials, apparatus and procedure specified in 6.2 to 6.6 to compare the air
contents, calculated from determined densities, of fresh mortar mixes without and with the
addition of an air-detraining agent. The difference between the air content of a fresh mortar
mixes without and with the addition of an air-detraining agent. The difference between the
air content of a fresh mortar mix using the sand as received and that of a similar mortar mix
containing an air-detraining agent, shall be evaluated from a pair of mortar mixes prepared
and tested as closely together as possible under the same conditions. The average difference
in air content obtained from six such pairs of mortar mixes shall not exceed 1.5 %.
PS:232 – 1983 (R)

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6.2 Materials. - The following materials are required.

6.2.1 Reference Portland cement. – The reference Portland cement shall be an ordinary
Portland cement that has been specially selected for the purpose of checking the
airentraining characteristics of sand. It can be obtained from the UK Port land cement
manufacturers who will supply data on its compliance with the requirements of PS:232:1983
(Revised). It shall be identified as Appendix ‘O’ Reference Portland Cement, and shall be
stored in a sealed container.

6.2.2 Sand. – Each fraction of sand shall be sampled in accordance with clause 3.

6.2.3 Water. – Distilled water shall be used.

6.2.4 Air-detraining agent. – The air-detraining agent shall be tri-n-butyl orthophosphate,


laboratory reagent grade.

6.3 Apparatus. – The following apparatus is required.

6.3.1 Mixer. – The mixer shall be electrically driven and shall consist essentially of :

stainless steel mixing bowl of about 5 litre capacity and of the shape and dimensions
shown in figure 2, provided with means by which it can be securely fixed to the
mixer frame during mixing and by which the height of the bowl in relation to the
mixer blade and, to some extent, the gap between the blade and the bowl can be
finely adjusted and fixed.

A stainless steel mixer blade of the shape and dimensions shown in figure 2,
revolving about its axis as it is driven in a planetary movement around the bowl by
an electric motor at controlled speeds; the two directions of rotation shall be
opposite.

Where several mixers are in use, blades and bowls shall form sets which shall
always used together.

The tolerances shown in figure 2 shall be checked every month.

The following speeds shall be maintained during mixing.

Mixer blade Planetary movement

R/min r/min

Low speed 140±5 62±5


High speed 285±10 125±10

6.3.2 Scraper. – A flexible scraper of rubber or plastics material, suitable for removing
mortar adhering to the mixer blade and to the inside surface of the mixing bowl.
PS:232 – 1983 (R)

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6.3.3 Balance, of sufficient capacity and an accuracy of ± 0.1 g.

6.3.4 Container. – A rigid, Thick walled, cylindrical brass container, of about 0.5 litre
capacity, with an internal diameter of about 75 mm. The internal surfaces shall be smooth;
the joint between the bottom and the walls should preferably have a slight radius.

6.3.5 Glass plate, of sufficient size to cover the container.

6.3.6 Tamper, cylindrical, 37.5±0.5 mm in diameter weighing about 250g and made of
nylon or similar hard plastics.

The tamping face shall be flat and at right angles to the length of the temper.

6.3.7 Straight-edge, metal, of suitable length to strike off the surface of the mortar in the
container.

6.4 Calibration of container. – Weigh , to ±0.1 g, the brass container and the glass plate
cover in a clean and dry condition. Fill the container with distilled water at the mixing room
temperature. Slide the glass plate cover over the top of the container, making certain that no
air bubbles are trapped under the glass plate, wipe dry the exposed surfaces of the container
and the glass plate, and weigh to ±0.1 g. By removing the glass plate and topping up the
container with more distilled water and proceeding as before, make two additional
weighings of the container filled with water. Calculate the average mass of water in the full
container and determine the capacity of the container to the nearest 0.1 cm3 taking the
relative density of water as 1.00.

6.5.1 Composition of mortar. – The amounts of the individual materials for each mortar
mix are given in table 2. When required, 1.0 ml of the air-detraining agent is added.

TABLE 2. Masses of individual materials

Material Proportions Mass


by mass
g
Reference Portland cement 1.0 450±1

}
Sand fraction A 3.0 350±1
B 500±1
C 200±1
D
E
200±1

100±1
Total 1350

Distilled water 0.5 225±1


PS:232 – 1983 (R)

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6.5.2 Preparation of mortar

6.5.2.1 Temperature and relative humidity. For the preparation of each mortar mix,
the mixing room apparatus and all the materials shall be at a temperature of 20±2oC. The
relative humidity of the air in the mixing room shall be not less than 65%.

6.5.2.2 Mixing of mortar using the sand received. Mixing shall be done mechanically
by means of the mixer specified in 6.3.1.

6.5.2.2.1 Pour 225 g of distilled water into the dry mixing bowl and add the cement.

6.5.2.2.2 Immediately start the mixer at the low speed and after 30 s, add the sand
steadily during the next 30 s. Switch the mixer to the higher speed and continue the mixing
for on additional 30 s.

6.5.2.2.3 Stop the mixer for 90 s. During the first 15s, remove by means of the scraper
all the mortar adhering to the wall and bottom part of the bowl and place ion the middle of
the bowl. Cover the bowl during the remaining 75s.

6.5.2.2.4 Continue the mixing at the higher speed for 60s.

6.5.2.2.5 The timing of the various mixing stages shall be adhered to within ±1s.

6.5.2.2.6 Immediately test the mortar in accordance with 6.5.3.

6.5.2.3 Mixing for mortar with addition of air-detraining agent. This mortar mix
shall be prepared and tested immediately after completion of the preparation and testing of
the mortar mix using the sand as received. It shall be prepared by the procedure specified in
6.5.2.2. except that 1.0 ml of the air-detraining agent shall be added from a burette, syringe
or suitable pipette directly to the water in the mixing bowl before the cement is added. All
apparatus coming into contact with this mortar shall be thoroughly washed and cleaned after
use.

6.5.3 Determination of density of fresh mortar. Weigh, to ±0.1 g. the clean and dry
container. Immediately after completion of mixing of the mortar in accordance with 6.5.2.2
or 6.5.2.3, fill the container with mortar in four layers each about 25 mm deep. After the
addition of the first increment, tamp the surface gently 20 times with the tamper. Distribute
the strokes evenly, over the surface only, to give an essentially flat surface. Then place
further layers and tamp each in turn in the same way. Adjust the final layer so that the
excess to be struck off is small. With the straight-edge held almost vertical, strike off the
surface plane and level with the top of the container with a sawing action making one pass
in each of two directions at right angles. Clean and dry the outside of the filled container and
weigh to ± 0.1 g.
PS:232 – 1983 (R)
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6.6 Calculation and expression of results.

6.6.1 Calculate the density D of the batch of mortar in the first pair using the sand as
received, to the nearest Kg/m from the mass of mortar in the container determined in
accordance with 7.5.3 and the capacity of the container determined in accordance with 6.4.

6.6.2 Calculate to the nearest 0.1% the air content Aa as a percentage of the volume of the
mortar, using the formula:

Aa = 100 – 0.04336 Da

6.6.3 Calculate, using the same formula, the air content Ab of the batch of mortar in the
first pair using the air-detraining agent.

6.6.4 Evaluate Aa – Ab for the first pair of batches.

6.6.5 Repeat these calculation for the six pairs of batches and calculate the average value.

6.6.6 The sand shall be deemed to comply with the specified requirement if does not
exceed 1.5%.

7. MARKING

Each of the prepared sand fractions processed in accordance with this part of this
standard shall be supplied in suitable containers marked with the following particulars:

(a) the name, trade mark or other means of identification of the processor;

(b) the designation of the sand fraction;

(c) the number of this Pakistan Standard, PS:232:1982 (Revised), Appendix ‘P’.
PS:232 – 1983 (R)
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PS:232 – 1983 (R)
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APPENDIX – Q

Methods of testing cement Standard sand for mortar cubes

1. SCOPE:

This part of this Pakistan Standard specified the course, preparation and properties of
sand to be used for making mortar cubes.

2. SOURCE

Natural (uncrushed) thoroughly washed and dried silica sand of the white variety
shall be obtained from Leighton Buzzard, Bedfordshire.

3. SAMPLING

Using a suitable scoop or similar device, a main sample of about 8 Kg. Shall be
taken from a single bag selected at random from a delivery not exceeding 500 Kg. For the
purposes of either of thew tests specified in clause

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