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SNI 2049:2015

National Standardization
Agency
Portland
cement
Indonesian National

ICS 91.100.10
Standard
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All rights reserved. No part of this document may be published or reproduced by any means or in
any form, and no part of this document may be distributed electronically or in print without written
permission from BSN.

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Published in Jakarta
SNI 2049:2015

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Register Contents

Table of Contents ....................................................................................................................... i


Table List ................................................................................................................................. iii
List of Images .......................................................................................................................... iv
Preface...................................................................................................................................... v
1 Scope ................................................................................................................................. 1
2 Normative references ......................................................................................................... 1
3 Terms and definitions ......................................................................................................... 1
4 Types and uses.................................................................................................................. 2
5 Quality requirements .......................................................................................................... 2
6 Sampling method ............................................................................................................... 5
7 Test method ..................................................................................................................... 10
7.1 Chemical test method ....................................................................................................10
7.1.1 Cement test method and permissible variations ................................................... 10
7.1.2 General ................................................................................................................. 12
7.1.3 Referee method .................................................................................................... 14
7.1.3.1 Insoluble part ................................................................................................... 14
7.1.3.2 Silicon dioxide (SiO )2 ...................................................................................... 15
7.1.3.3 Ammonium hydroxide group (R O )23...............................................................18
7.1.3.4 Iron(III) oxide (Fe O )23 ..................................................................................... 20
7.1.3.5 Phosphorus pentaoxide (P O )25 ......................................................................22
7.1.3.6 Titanium dioxide (TiO )2 ................................................................................... 24
7.1.3.7 Zinc oxide ........................................................................................................ 26
7.1.3.8 Aluminum oxide ............................................................................................... 26
7.1.3.9 Calcium oxide (CaO) ....................................................................................... 26
7.1.3.10 Magnesium oxide (MgO) ................................................................................. 29
7.1.3.11 Sulfur ...............................................................................................................30
7.1.3.12 Missing incandescence .................................................................................... 34
7.1.3.13 Sodium and potassium oxides .........................................................................35
7.1.3.14 Manganese oxide ............................................................................................ 39
7.1.3.15 Chloride ...........................................................................................................41
7.1.3.16 Organic compounds soluble in chloroform.......................................................45

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7.1.4 Alternative test method (Optional) ....................................................................... 48
7.1.4.1 Calcium oxide................................................................................................... 48
7.1.4.2 Magnesium oxide volumetric method ............................................................... 49
7.1.4.3 Titanium dioxide ............................................................................................... 52
7.1.4.4 Phosphorus pentaoxide.................................................................................... 57
7.1.4.5 Manganese oxide ............................................................................................. 60
7.1.4.6 Free calcium oxide ........................................................................................... 61
7.2 Physics test method ...................................................................................................... 64
7.2.1 Auxiliary materials and equipment ....................................................................... 64
7.2.2 Smoothness testing with blaine tool and turbidimeter .......................................... 65
7.2.2.1 With blaine tool ................................................................................................. 65
7.2.2.2 With turbidimeter .............................................................................................. 75
7.2.3 Normal consistency testing .................................................................................. 89
7.2.4 Binding time testing .............................................................................................. 92
7.2.5 Expansion testing with autoclave ......................................................................... 98
7.2.6 Determination of compressive strength of hydraulic cement mortar .................. 103
7.2.7 Rapid rigid testing of portland cement (paste method)....................................... 114
7.2.8 Determination of heat of hydration ..................................................................... 118
7.2.9 Sulfate-induced expansion testing...................................................................... 126
7.2.10 Mortar air content testing.................................................................................... 129
8 Test pass requirement ....................................................................................................132
9 Packaging.......................................................................................................................132
10 Marking requirements.....................................................................................................132
11 Storage and transportation .............................................................................................132
Appendix A ............................................................................................................................ 133
Appendix B ............................................................................................................................ 134
Appendix C............................................................................................................................136
Bibliography...........................................................................................................................139

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Register Table

Table 1 ̶ Main chemical requirements ....................................................................................... 2


Table 2 ̶ Additional chemical requirements ............................................................................... 3
Table 3 ̶ Main physics requirements ......................................................................................... 4
Table 4 ̶ Additional physics requirements ................................................................................. 4
Table 5 ̶ Testing time interval after sampling............................................................................. 6
Table 6 ̶ Permissible difference in test results ......................................................................... 11
Table 7 ̶ Comparison of MgO content with the amount of reagents required .......................... 51
Table 8 ̶ Comparison of MgO content with the amount of standard solution ........................... 52

Table 9 ̶ Specific gravity of mercury, air viscosity (η) andη at a given temperature .... 73

Table 10 ̶ Porosity values of cementitious coatings ................................................................ 73


Table 11 ̶ Air flow time range .................................................................................................. 74
Table 12 ̶ Turbidimeter equipment dimensions ....................................................................... 78
Table 13 ̶ Values of h, d and h/d2 used in calibration of turbidimeter equipment .................... 82
Table 14 ̶ Burette dimensions .................................................................................................. 82
Table 15̶Example of
turbidimeter test data recording and specific surface calculation........................88
Table 16 ̶ Allowable variation of molding dies (mm) ..............................................................104
Table 17 ̶ Standard sand requirements .................................................................................106
Table 18 ̶ Composition of mortar ...........................................................................................108
Table 19 ̶ Testing time tolerance ...........................................................................................110
Table 20 ̶ Rigor ......................................................................................................................113
Table 21 ̶ Deviation ...............................................................................................................129
Table 22 ̶ Ottawa sand grain gradation .................................................................................130

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Register Image

Figure 1 ̶ Cement sampling pipe................................................................................................8


Figure 2 ̶ Packaged cement take-up pipe ..................................................................................8
Figure 3 ̶ Blaine tool................................................................................................................. 67
Figure 4a ̶ Front view of turbidimeter with door open ..............................................................75
Figure 4b ̶ Front view of turbidimeter with door open ..............................................................76
Figure 5 - Turbidimeter rear view ............................................................................................76
Figure 6 - Time burette............................................................................................................77
Figure 7 - Turbidimeter electrical system ................................................................................ 77
Figure 8 - Vicat tool ................................................................................................................ 89
Figure 9 - Gilmore tool ........................................................................................................... 97
Figure 10 - Cement paste slab shape .....................................................................................98
Figure 11 - Prism mold ............................................................................................................ 99
Figure 12 - Comparator ......................................................................................................... 100
Figure 13 - Mixer machine .................................................................................................... 104
Figure 14 - Stirrer ..................................................................................................................104
Figure 15 - Bowl ....................................................................................................................105
Figure 16 - Flow table ...........................................................................................................105
Figure 17 - Collision sequence .............................................................................................. 110
Figure 18 - Calorimeter apparatus ........................................................................................ 119
Figure 19 - Calorimeter stirrer ............................................................................................... 119

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Preface

SNI 2049:2015, Portland cement is a revision of SNI 15-2049-2004, Portland cement. This
standard was revised with the intention of increasing the national capacity of the cement
industry and increasing exports of cement commodities. The main technical change in this
standard is the increase in compressive strength requirements for the age of 3 days, 7 days
and 28 days for type I. In addition, there is also a change in packaging, namely an increase
in the compressive strength requirements for type I cement. In addition, there is also a
change in packaging, namely the addition of 25 kg and 40 kg packaging.

This standard was prepared and formulated by Technical Committee 91-02, Chemistry and
Construction Materials. This standard is the result of a consensus held in Jakarta on April 29,
2013, which was attended by representatives of stakeholders such as producers, consumers,
testing centers and other relevant technical agencies. This standard has also gone through
the stages of national consensus, namely opinion polls on November 27, 2013 - January 25,
2014, and
voting from May 12 - July 10, 2014.

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SNI 2049:2015

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Portland cement

1 scope

This standard specifies the quality requirements, sampling system and test methods of
Portland cement. The standard is applicable to 5 types of Portland cement, with a packaging
limit of up to 50 kg and excluding cement used for ready mix.

2 Reference normative

ASTM C 430-08, Standard Test Method for Fineness of Hydraulic Cement by the 45-µm (No
325) Sieve

ASTM C 670-13, Standard Practice for Preparing Precision and Bias Statements for Test
Methods for Construction Materials

3 Terms and

definitions 3.1
portland cement
hydraulic cement produced by grinding portland cement slag consisting mainly of calcium
silicates of a hydraulic nature and ground together with additives in the form of one or more
crystalline forms of calcium sulfate compounds and may be added with other additives

3.2
air content of hydraulic cement
hydraulic cement containing an additional amount of air which causes the air contained in the
mortar to be within the limits specified when measured by a method.

3.3
cement paste
cement and water mixture either hardened or unhardened

3.4
false set
rapid loss of plastic properties of cement paste, mortar or concrete

3.5
damp room
an enclosed space for the storage and hardening of samples of paste, mortar and concrete
that has a high temperature and relative humidity that can be adjusted

3.6
mortar
a mixture consisting of cement, fine aggregate and water in either a hardened or unhardened
state.

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4 Types and uses

4.1 Type I is portland cement for general use that does not require special requirements as
required by other types.

4.2 Type II is portland cement which in use requires resistance to sulfates or medium
hydration heat.

4.3 Type III Portland cement which requires high strength at the initial stage after bonding
occurs.

4.4 Type IV is portland cement which requires a low hydration heat.

4.5 Type V is portland cement which in use requires high resistance to sulfate.

5 Terms quality

5.1 The chemical requirements of Portland cement should meet the following requirements:

Table 1 ̶ Main chemical requirements


unit in %
Types of portland cement
No. Descri
I II III IV V
ption
b,c)
1 SiO2 , minimum - 20.0 - - -
2 Al O23 , maximum - 6,0 - - -
3 Fe O23 , maximum - 6.0 b,c) - 6,5 -
4 MgO, maximum 6,0 6,0 6,0 6,0 6,0
5 SO3 , maximum
If C3 A 8.0 If 3,0 3,0 3,5 2,3 2,3
d) d) d)
C3   8.0 3,5 4,5
6 Missing incandescence, maximum 5,0 3,0 3,0 2,5 3,0
7 Insoluble part, maximum 3,0 1,5 1,5 1,5 1,5
8 C3 S, maximum a) - - - 35 b) -
9 C2 S, minimum a) - - - 40 b) -
10 C3 A, maximum a) - 8,0 15 7 b) 5 b)
11 C4 AF + 2C3 A or a)
C4 AF + C2 F, maximum - - - - 25 c)
NOTE
a)
Chemical restriction requirements based on calculations for a particular potential compound do
not necessarily imply that the oxide of that potential compound is in a pure state.
C = CaO, S = SiO2 , A = Al O23 , F = Fe O23 , Example C3 A = 3CaO.Al O23
Titanium dioxide (TiO2 ) and phosphorus pentaoxide (P O25 ) belong to Al O23.
The value commonly used for Al O23 in calculating potential compounds (e.g. C3 A) for
specification purposes is the amount of precipitate obtained by addition of NH4 OH minus the
amount of Fe O23 (R O23 - Fe O23 ) obtained in wet chemical analysis.

If: % Al O23 0.64, then the percentages of C3 S, C2 S, C3 A and C4 AF are calculated as


follows..:
% Fe O23

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Table 1 - Key chemical requirements (continued)
Types of portland cement
No. Descri
I II III IV V
ption

C3 S = (4.071 x %CaO) - (7.600 x %SiO2 ) - (6.718 x %Al O23 ) - (1.430 x %Fe O23 ) - (2.852 x
% SO )3

C2 S = (2.867 x %SiO2 ) - (0.7544 x % C3 S)

C3 A = (2.650 x % Al O23 ) - (1.692 x % Fe O23

) C4 AF = (3.043 x % Fe O )23

When: % Al O 23  0.64, a solid solution is formed (C4 AF + C2 F) = 4CaO. Al O23 .Fe O23
% Fe O23

Cement with this composition does not contain C3 A. Then (C4 AF


+ C2 F) and C3 S are calculated as follows:
(C4 AF + C2 F) = (2.100 x %Al O23 ) + (1.702 x %Fe O )23
C3 S = (4.071 x %CaO) - (7.600 x %SiO2 ) - (4.479 x %Al O23 ) - (2.859 x %Fe O23 ) - (2.852 x
% SO )3

C2 S is still calculated using the above formula: Calculations for all potential compounds are
based on their oxide determination results calculated to as close to 0.1% as possible. All
calculation results are reported to the nearest possible 1.0%.
b)
If the heat of hydration as listed in the table of additional physical requirements (Table 4) is
required, then this chemical requirement does not apply.
c)
If the expansion due to sulfate listed in the table of additional physical requirements (Table 4) is
required, then this chemical requirement does not apply.

d)
Unusable.

Table 2 ̶ Additional chemical


requirements a) unit in %
Types of portland cement
No. Descri
I II III IV V
ption
1 C3 A, maximum - - 8 - -
2 C3 A, minimum - - 5 - -
3 (C3 S + 2 C3 A), maximum - 58 b) - - -
4 Alkali, as
(Na2 O + 0.658 K2 O), maximum of 0,60 c) 0,60 c) 0,60 c) 0,60 c) 0,60 c)

NOTE
a)
These additional chemical conditions apply only if specifically required.
b)
Same as the description forb) in the main chemistry requirement.
c)
Only applicable when cement is used in concrete whose aggregates are reactive to alkali.

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5.2 The physical requirements of Portland cement should meet the following requirements:

Table 3 ̶ Main physics requirements


Types of portland cement
No. Descri I II III IV V
ption
1 Smoothness:
Air permeability test, m2 /kg with
apparatus:
- Turbidimeter, min 160 160 160 160 160
- Blaine, min 280 280 280 280 280

2 Immutability:
Expansion by autoclave, max % 0,80 0,80 0,80 0,80 0,80
3 Compressive strength:
- 1-day old, kg/cm2 , minimum - - 120 - -
- Age 3 days, kg/cm2 , minimum 135 100 240 - 80
70 a)
- 7 days old, kg/cm2 , minimum 215 175 - 70 150
120 a)
- Age 28 days, kg/cm2 , minimum 300 - - 170 210
4 Bonding time (alternative method) with
tools:
a) Gillmore
- Start, minutes, minimum 60 60 60 60 60
- End, minute, maximum 600 600 600 600 600
b) Vicat
- Start, minutes, minimum 45 45 45 45 45
- End, minute, maximum 375 375 375 375 375
NOTE
a)
This compressive strength requirement applies if the heat of hydration requirements as listed in
the table of requirements
(Table 4) or if the conditions C3 S + C3 A as listed in the table of additional chemical conditions
are required (Table 2).

Table 4 ̶ Additional physics requirementsa)


Types of Portland cement
No. Descri I II III IV V
ption
1 Binding pseudo final 50 50 50 50 50
penetration, % minimum
2 Calor of hydration
- 7 days old, cal/gram, - 70 b) - 60 -
max
- 28 days old, cal/gram, - - - 70 -
max
3 Compressive
strength: kg/cm2 , - 280 - - -
Age 28
days,
minimum
4 Expansion due to sulfate 14 - 220 b) - - 0,040
days, %, maximum

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5 Air content of mortar, 12 12 12 12 12


% volume, maximum

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Table 4 - Additional physics requirements (continued)
Types of portland cement
No. Descri I II III IV V
ption
NOTE
a)
These additional physics requirements apply only if specifically requested.
b)
When this heat of hydration condition is required, the C3 S + C3 A condition as listed in the
supplementary chemical table (Table 2) is not necessary.
This compressive strength requirement applies when the heat of hydration requirements as
listed in the table of additional physical requirements (Table 4) or when the C3 S + C3 A
requirements as listed in the table of additional chemical requirements (Table 2) are
required.

6 How to take examples

6.1 Description of specific terms for standardized methods

6.1.1 Cement lot

A cement lot is a specific quantity of cement submitted for inspection at any given time. A lot
may represent one or more bins that have been consecutively filled with cement. A lot may
also represent the contents of one or more transport units removed from the same bin.

6.1.2 Customized sampling frequency

This is a test program prepared for testing of only two samples of cement obtained from each
lot, and prepared for testing at the usual stages as described below.

The program uses a likelihood factor and is designed so that if the test results of both
samples meet the requirements of the program, it can be interpreted with 95% confidence
and less than 5% of the samples will fall outside the specification limits.

6.2 Purpose and use

6.2.1 The sampling procedures outlined are intended for use in the provision of sampling
of hydraulic cement, once it has been manufactured and is ready for market.

This procedure is not intended as a sampling procedure for quality control during the
production process.

The outlined test procedures include the number of samples for the tests to be performed
and provide guidance on the preparation of reports.

6.2.2 Most of the requirements and specifications required by building construction are
that the hydraulic cement to be used in the work must meet the requirements as stated in the
purchase specifications, such as the specifications according to Article 5.

Where such regulations or specifications require sampling of the cement produced, the
provisions given in 6.4.1 shall be implemented.

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6.3 Implementation procedure

6.3.1 This implementation procedure covers the process of sampling and testing with a
view to establishing whether the cement sample meets the requirements of the acceptance
specification. Testing of cement samples is carried out using certain methods to determine
whether the test results obtained from the cement samples meet the specifications and the
test results are stated as the basis for acceptance or rejection of the cement lot represented
by the samples.

6.3.2 It is neither intended nor required that cement should be tested using all the chemical
and physical test methods listed in this standard.

6.4 Type and size of cement sample; sampling

6.4.1 Grab samples are cement obtained from conveyor belts, from bulk cement
warehouses or from bulk cement vessels.

Samples can also be taken from a continuous flow of cement at 10-minute intervals using an
automatic sampling device, also called a sample citation.

The quoted samples taken at each such interval, over a period of time should be combined
into a composite sample, representing the cement produced over a period of time.

6.4.2 All cement samples, whether quoted samples or composite samples weigh at least 5
kg.

6.4.3 The cement samples shall be packed in air and water vapor tight packages that have
been numbered regularly and consecutively.

6.5 Time required to complete the test

6.5.1 The cement producer shall make arrangements so that the cement can be sampled,
the tests being carried out as early as possible before the time when the test results are
required. So that at least the applicable time interval in 6.5.2 can be followed.

6.5.2 Where this has been done, the testing laboratory shall prepare the test results no
later than the number of days listed after the sampling time.

Table 5 ̶ Testing time interval after sampling


No Testing Time interval
. (days)
1 Compressive strength (1 day old test result) 8
Chemical analysis, autoclave, normal consistency with
vicat tool, smoothness with blaine tool, fast stiffening
pasta method.
2 Compressive strength (3-day old test results) 10
3 Compressive strength and heat of hydration (7-day old 14
test results)
4 Expansion due to sulfate (14-day old test result) 21
5 Compressive strength and heat of hydration (28-day 35
test results)

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6.6 Sampling

6.6.1 From a conveyor belt being conveyed to a bulk cement warehouse

Take a sample of cement quotations weighing at least 5 kg at an interval of approximately 6


hours.

6.6.2 Cement sampling at the time of transfer

Sampling of cement from the warehouse when the cement is being transferred from one bin
to another. Take one cement sample from the cement stream being moved, for every 400
tons of cement or multiples thereof, but sampling should not be less than the cement
samples and combined to obtain a composite sample.

6.6.3 Other methods of sampling

If the two sampling methods above cannot be used, cement samples can be obtained using
one of the methods below:

6.6.3.1 From the bulk cement warehouse at the dispensing pit

Take a sample of cement from the discharge pit at a time of constant cement flow, until
sampling is complete. Estimate the amount of cement to be sampled in tons using the
formula:

0,001 73 x d³ x 0.2
35,314
Description:
dada is the depth of cement in meters, which is above the discharge pit.

Where cement samples are taken from a cylindrical bulk cement warehouse, samples shall
be taken from one of the dispensing holes only. If the quantity of bulk cement in the
warehouse exceeds 1 200 tons, and also if the warehouse is rectangular, the cement
samples taken but not from the dispensing holes, shall be of such quantity that they shall
represent more than half of the quantity of cement stored in the warehouse.

While the cement is flowing through the dispensing hole take a sample of the cement at each
interval, so that it should represent more than half of the cement stored in the warehouse.

While the cement is flowing through the discharge hole take samples of cement at each
interval, so that at every flow of 400 tons of cement at least 2 samples are taken from the bin
or silo.

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6.6.3.2 From bulk cement warehouses and bulk cement vessels using sampling
equipment

When the depth of bulk cement to be taken For not exceeding 2.1 meters,
example
Cement samples can be obtained using the bulk cement sampling device shown in Figure 1.
It is between 1.5 m and 1.8 m long and has an outer diameter of approximately 35 mm,
consisting of two brass-coated pipes with a series of holes that can be inserted into them.
opens and closes with a detour inner pipe. Pipe end outer shape
Pointed, making it easier to penetrate.

Take cement for of points that spread out with an with depth which is
example average
different so that the entire cement taken will be represented.

6.6.3.3 From bag cement with using tools taker example in


bag

Insert the sampling device in the bag as shown in Figure 2, in a way that
crosswise through the hole of the cement bag. Then close the air hole with your thumb, then
pull tool The. Take one For of cement bags for every 5 tons or
examp
le
multiples.

Figure 1 ̶ Cement sampling pipe

Figure 2Packaged cement take-up pipe

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6.6.3.4 From bulk cement delivery by train or truck

6.6.3.4.1 Single delivery

If the delivery is made using only one train car or one cement truck, which is continuously
loaded and which comes from a single source, take a sample of cement weighing 5 kg.

If it is not continuously loaded and the source is unknown, combine 5 or more portions of
cement samples from different points to serve as test samples.

6.6.3.4.2 Plural delivery

If the shipment consists of multiple rail cars or multiple cement trucks loaded from the same
source and on the same day, take cement samples for every 100 tons or multiples thereof,
but not less than 2 samples. Treat such cement samples as sample lots of cement. And test
the samples in accordance with the procedure described in the section "Weight of samples
for testing".

6.7 Storage of cement samples

After the cement sample is taken, immediately place it in an air and water vapor tight place to
prevent water absorption or aeration of the cement sample. If the cement sample is placed in
a can, close it tightly and seal it immediately. Use bags consisting of several layers of water
vapor tight paper, or plastic bags, which are strong enough not to break, try to seal them
immediately after filling in such a way that the air in the bag escapes and water vapor
absorption and aeration are prevented.

Cement samples should be treated as described in the section "Preparation of test samples".

6.8 Test sample preparation

Before testing, sift the cement through an 850 µm sieve (sieve no. 200 or other sieve having
approximately the same opening size).

In order to mix the sample well, break up the lumps, and pick up the impurities. Discard
hardened dirt and lumps that cannot be broken during sieving. Store the cement in an airtight
place to prevent moisture absorption before testing.

6.9 Failure to meet requirements and retesting

6.9.1 If any of the test results fail to meet the requirements, the cement lot is not reported
as cement that does not meet the specification requirements until the failure is confirmed by
the number of retests.

6.9.2 A retest may consist of one type of test or all tests in full.

6.9.3 Re-testing shall be carried out in accordance with the provisions of the specification
used. If this provision is not given, the procedure below should be used.

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6.9.4 Re-test some of the cement samples used in the initial test. Use other methods for the
determination of the cement properties required in the retest and in this case only the test
results obtained by other methods shall be used.

Retesting shall consist of the required number of determinations as for the initial test. The
number of repetitions used is the basis for the precision requirement. Where two or more
determinations are required, the reported price shall be the average price of all test results
that fall within the limits of precision of the method at 95% confidence level, as stated in the
specification used or generally recognized.

7 How to test

7.1 Test method chemistry

Any test method that demonstrates acceptable accuracy and drift can be used for hydraulic
cement analysis, including referee test methods, as described in 7.1.1.

Specific chemical test methods are given for the convenience of those who wish to use them.
The test methods are grouped as referee test methods and alternative test methods. The
referee test method is an accepted wet chemistry test method, which provides an integrated
basic scheme of hydraulic cement analysis.

Alternative test methods generally provide individual determinations of specific components


and can be used alone or as an alternative and integrated determination when desired by the
analyst as indicated for individual methods. Each analyst must be able to demonstrate high
skills as described in 7.1.1, if this method is used.

7.1.1 Cement test methods and permitted variations

7.1.1.1 Referee test method

Referee test methods such as those listed in 7.1.3.1 through 7.1.3.16 or other test methods
specified in accordance with 7.1.4, are used when the results of analysis by referee test
methods are doubtful to meet the chemical requirements.

In such cases, the cement cannot be rejected as not meeting the chemical requirements
unless all determinations of the elements and all necessary preliminary separations have
been made by the referee test method.

In case of doubt, the analysis should be done twice on different days.

If the results do not comply with the permissible variations in Table 1, the determination is
repeated until 2 or 3 results comply with the permissible variations for the purpose of
comparative analysis and calculation of acceptable average results, the percentages should
be calculated to as close as possible to 0.01 (or 0.0001 for chloroform-soluble organic
compounds), although some average results are reported to an accuracy of 0.1.

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Table 6 ̶ Permissible difference in test results
Maximum difference from
Maximum
the average of two
No. Component difference of
determinations according
two tests
to SRM Certificate
(units in %)
1 SiO2 (Silicon dioxide) 0,16  0,2
2 Al O23 (Aluminum oxide) 0,20  0,2
3 Fe O23 (Iron(III) oxide) 0,10  0,10
4 CaO (Calcium oxide) 0,20  0,30
5 MgO (Magnesium oxide) 0,16  0,2
6 SO3 (Sulfur trioxide) 0,10  0,1
7 HP (Missing 0,10  0,10
incandescent)
8 Na2O (Sodium oxide) 0,03  0,05
9 K2O (Potassium oxide) 0,03  0,05
10 TiO2 (Titanium dioxide) 0,02  0,03
11 P2O5 (Phosphorus 0,03  0,03
pentaoxide)
12 ZnO (Zinc oxide) 0,03  0,03
13 Mn2O3 (Manganese oxide) 0,03  0,03
14 S (Sulfide) 0,01 -
15 Cl (Chloride) 0,003 -
16 IR (Insoluble part) 0,10 -
17 FL (Free calcium oxide) 0,20 -
Alk sol (Water-soluble alkali
18 0,75/w -
Chl sol (Organic compound
19 which is soluble in 0,004 -
chloroform)

7.1.1.2 Alternative test method

In some cases alternative methods provide shorter procedures or are more suitable for
routine determination of certain components than the referee test method (see NOTE).
In some cases, more complex and lengthy procedures may still be used as alternative test
methods to compare results with different procedures or to be used when special materials
are being tested with foreseeable disturbances, or when special preparation for analysis is
required. Test results from alternative test methods may be used as a basis for acceptance
or rejection when the results clearly indicate that the cement does or does not meet the
requirements of the specification.
NOTE It is not intended to limit the use of referee test methods for reference analysis. A referee test
method should be used rather than an alternative test method when absolutely necessary. A reference
test method should be used if an alternative test method is not provided.

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Dual analysis and blanket determination are not required when using an alternative test
method. But if a blanket determination is desired for an alternative test, this one may be used
and it need not be done if it has been obtained together with the analysis.
The final result, if corrected against the blank value, must be shown in each case.

7.1.2 General

a) Reagents whose weight is expressed as "approximately 5 grams" are simply weighed to


the rough value.
b) The content of the solution stated as "approximately 300 mL is sufficient to be observed
by eye, the content of "10 mL" is sufficient with a measuring cup and the content stated as
"exactly 25 mL" must be measured with a burette or pipette.
c) "Cold" should mean room temperature, "warm" a temperature between (30-40)o C, and
"hot" should mean a temperature close to that of boiling water (90-95)o C.
d) Burette readings should be up to 0.01 mL and if used is a solution with a low titer, a micro
burette should be used.
e) If water is used in the test, then water means distilled water.

7.1.2.1 Equipment and materials

7.1.2.1.1 Equipment
(1) Weighing equipment: Analytical scales with a capacity of not more than 200 grams.
Scales must be capable of producing repeat readings with a difference of no more than
0.000 2 grams with an accuracy of 0.000 2 grams.
(2) Laboratory equipment made of glass and polyethylene materials:
a) Measuring flasks, burettes and pipettes must be in a high degree of precision.
b) Special types of glassware such as colored glass, high-silica glass and alkali-
resistant glass.
c) Containers made of polyethylene for all alkaline solutions and standard solutions.
d) The desiccator is equipped with a desiccant such as magnesium perchlorate,
activated alumina, or sulfuric acid. Anhydrous calcium sulfate may also be used,
but calcium chloride is not appropriate in this analysis.
e) Filter paper: coarse-pored, fine-pored, and medium-pored.
f) Crucibles: A crucible made of platinum with a capacity of (15-30) mL.
g) Heating furnace: A furnace equipped with a pyrometer with an accuracy of  25o C.

7.1.2.1.2 Material
For all tests "chemical grade" reagents should be used, unless otherwise recommended.
Other reagents used should be of sufficiently high purity without compromising the accuracy
of the determination.
(1) Reagent concentration
a) Ready-to-use reagents
Standard solutions of ready-to-use reagents or in diluted concentrations can be used
if the purity specifications are provided.

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b) Concentrated acid and ammonium hydroxide
When acids and ammonium hydroxide are only provided with requirements by name
and chemical formula, it should be interpreted that the reagents should be in a
concentrated state according to specific gravity (b.j) or concentration by weight as
follows:
Acetic acid (CH3 COOH) 99,95%
Hydrochloric acid (HCl) b.j 1.19
Hydrofluoric acid (HF) 48%
Nitric acid (HNO )3 b.j 1.42
Phosphoric acid (H3 PO )4 85%
Sulfuric acid (H2 SO )4 b.j 1.84
Ammonium hydroxide (NH4 OH) b.j 0.90
c) Acid and dilute ammonium hydroxide
Specified as a ratio of the volume of concentrated reagent to the volume of water
added, for example HCl (1+99), meaning 1 volume of concentrated HCl (b.j 1.19) is
added to 99 volumes of water.
d) Standard solution
The concentration of the standard solution is expressed in normality (N) or as an
equivalence in grams per milliLiter of the component being determined. At least three
determinations must be made to obtain the average result of the standardization.

e). Concentration of non standard solution is prepared by dissolving solid reagent in a


certain weight unit dissolved in water solvent, unless the solvent is specified
otherwise.
(2) Indicator solution
a) Methyl red: 2 grams of methyl red/L in 95% ethanol.
b) Phenolphtalein: 1 gram phenolphthalein/L in 95% ethanol.

7.1.2.2 Suggested report sequence of portland cement chemical analysis


components
(1) Major component
a) SiO2 (Silicon dioxide)
b) Al O23 (Aluminum oxide)
c) Fe O23 (Iron(III) oxide)
d) CaO (Calcium oxide)
e) MgO (Magnesium oxide)
f) SO3 (Sulfur trioxide)
g) Missing incandescence

(2) Minor components


a) Na2 O (Sodium oxide)
b) K2 O (Potassium oxide)
c) TiO2 (Titanium dioxide)
d) P O25 (Phosphorus pentaoxide)
e) ZnO (Zinc oxide)
f) Sulfide of sulphur
g) Mn O23 (Manganese oxide)

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(3) Split determination
a) Insoluble part
b) Organic compounds soluble in chloroform
c) Free calcium oxide
d) Water-soluble alkali

7.1.3 Referee method

7.1.3.1 Insoluble parts

7.1.3.1.1 Test method summary

In this method the insoluble portion of cement is determined by digesting the sample in HCl.
After filtration, it is further digested with sodium hydroxide. The residue obtained is
incinerated and weighed.

When this test method is used on blended cement, decomposition in acid is considered
complete if the Portland cement slag is completely decomposed.

Ammonium nitrate solution is used in the final wash to prevent fine insoluble materials from
escaping the filter paper.

7.1.3.1.2 Reagents

a) Ammonium nitrate solution (NH4 NO3 20 grams/L).


b) Sodium hydroxide solution (NaOH 10 g/L).

7.1.3.1.3 Procedure

a) Weigh 1 gram of sample, put it into a 250 mL beaker, add 25 mL of water and 5 mL of
HCl.
b) If necessary, heat the solution and press the sample with the tip of a glass stirring rod
until it is completely decomposed.
c) Dilute the solution to 50 mL with hot water and heat it on a hot plate to near boiling point.
d) Filter through medium porous filter paper into a 400 mL beaker, wash the beaker, filter
paper and precipitate 10 times with hot water and the filtrate is used for the
determination of SO3 .
e) Transfer the filter paper and sediment to the original beaker, add 100 mL of hot NaOH
solution (10 g/L) and digest for 15 min at almost boiling temperature.
f) During digestion occasionally stir the mixture and break the filter paper with a stir bar.
Acidify the solution with HCl and using methyl red as an indicator, add excess HCl (4-5)
drops.
g) Filter with medium-porous filter paper and wash the precipitate at least 14 times with hot
NH4 NO3 solution (20 g/L) to ensure that the filter paper and contents are completely
washed. Place the filter paper and its contents into a crucible of known weight. Burn and
incandesce at a temperature of (900 - 1 000)o C for at least 30 minutes. Cool in a
desiccator and weigh.

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h) Blangko
Perform a blanket determination using the same reagent and method. Take into account
the results as a correction in the calculation.

7.1.3.1.4 Calculations
Calculate the insoluble portion with accuracy to 0.01%.

Sludge weight X 100


% insoluble part = Sample
weight

7.1.3.2 Silicon dioxide (SiO )2

For portland cement where the insoluble part is not yet known, first determine it in
accordance with 7.1.3.1.

For portland cement where the percentage of insoluble parts is less than 1%, go to 7.1.3.2.1,
for cement where the insoluble parts are greater than 1%, go to 7.1.3.2.2.

7.1.3.2.1 Silicon dioxide with insoluble part smaller than 1%

7.1.3.2.1.1Summary of test method

In this test method silicon dioxide (SiO2 ) is determined gravimetrically.

Add ammonium chloride and the solution should not be evaporated to dryness. This method
was developed primarily for hydraulic cements that are almost completely biodegradable with
hydrochloric acid and should not be used for hydraulic cements that contain a large
proportion of acid-insoluble ingredients and require the prior dissolution of sodium carbonate.
For such cements, or if a standard specification for the cement being analyzed is required,
the procedure in 7.1.3.2.2 should be used.

7.1.3.2.1.2 Reagents

a) Ammonium chloride (NH4 Cl).


b) Hydrochloric acid (HCl).
c) Hydrochloric acid (HCl) (1+99).
d) Nitric acid (HNO3 ).
e) Sulfuric acid (H2 SO4 )(1+1).
f) Hydrofluoric acid (HF).

7.1.3.2.1.3 Procedure

a) Mix evenly 0.5 grams of cement sample with approximately 0.5 grams of NH4 Cl in a 50
mL beaker, cover the beaker with a watch glass and carefully add 5 mL of HCl by
pouring through the inner edge of the beaker. After the chemical reaction is complete,
remove the watch glass, add 1 or 2 drops of HNO3 , stir the mixture with a glass stirring
rod, cover again and place the beaker on a steam bath for 30 minutes.

During this digest time stir the contents of the glass frequently and break up any
remaining lumps to facilitate complete decomposition of the cement.

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Attach a medium-porous filter paper to the funnel, transfer the silicic acid clot onto the
filter as much as possible without dilution, and allow the solution to drip off.
Rub the inner wall of the beaker with a stir bar fitted with a rubber buffer, and rinse the
beaker and stir bar with hot HCl (1+99).
Wash the filter paper with hot HCl (1+99) and then wash with hot water in small amounts
for 10 or 12 times, save the filtrate and wash water for determination of the ammonium
hydroxide group.
b) Transfer the filter paper and precipitate to a crucible of known weight, dry and slowly
incandesce at low temperature until the carbon from the filter paper disappears without
any flame from the filter paper, then continue incandescence at (1 100 - 1 200)o C for 1
hour.
Then re-massage until the weight remains (w1 ). Treat the SiO2 obtained which still
contains a small amount of impurities in a crucible with 1 mL or 2 mL of water, 2 drops of
H2 SO4 (1+1) and approximately 10 mL of HF, and evaporate carefully until dry.
Finally incandesce the scanty residue at (1 050 - 1 100)o C for 5 minutes, cool in a
desiccator and weigh (w2 ). The weight difference between this (w2 ) and before HF
treatment (w1 ) is the weight of SiO2 . Keep in mind that the weight of the residue
remaining after evaporation of SiO2 is a combination of aluminum oxide and iron (III)
oxide, and include it in the solution obtained for the determination of the ammonium
hydroxide group.
c) If the result of evaporation with HF exceeds 0.002 0 gram, the determination of silica
shall be repeated, steps shall be taken to ensure the decomposition of the sample before
the separation of silica is carried out and the subsequent determination of (Al O 23 + Fe
O23 , CaO and MgO) shall be determined with a new filtrate and the residue obtained
after adding HF shall weigh 0.002 0 gram or less, except as specified in 7.1.3.2.1.3 item
d) and 7.1.3.2.1.3 item e).
d) If after two or three determinations are repeated and it is found that the residue obtained
after adding HF remains greater than 0.002 0 grams, it can be stated that there was
impurity at the time of sampling or during the cement manufacturing process the
combustion was not complete. In such cases the precipitate obtained should not be
melted and added to the filtrate for the determination of the ammonium hydroxide group,
but report the result as the precipitate obtained.
e) In this state, add 0.5 grams of sodium or potassium pyrosulfate (Na S O 227 or K S O227 )
to the crucible and heat almost incandescent until the impurity precipitate melts, cool and
dissolve with water and unite with the filtrate, and unite with the washing stored for the
determination of the ammonium hydroxide group.
f) Perform a blanket determination using the same reagents and test method and calculate
the results as a correction in the calculation.

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7.1.3.2.1.4 Calculations
Calculate the SiO content2 with accuracy to 0.1%.

(w -w12 )
% SiO2 = X 100
w

Description:
w1 is the weight of the precipitate before adding HF,
grams; w2 is the weight of the precipitate after
adding HF, grams; w is the weight of the sample,
grams.

7.1.3.2.2 Silicon dioxide with insoluble part greater than 1%

7.1.3.2.2.1 Summary of test method

This test method is based on the melting of sodium carbonate followed by repeated
evaporation of hydrochloric acid solution until dry to deform the silica into an insoluble form.

The solution was filtered and the insoluble silica precipitate was emitted and weighed. SiO 2
was evaporated with HF, then emitted and weighed.

7.1.3.2.2.2 Reagents

a) Sodium carbonate (Na2 CO3 ).


b) Hydrochloric acid (HCl).
c) Hydrochloric acid (HCl) (1+3).
d) Hydrochloric acid (HCl) (1+99).
e) Hydrochloric acid (HCl) (1+1).

7.1.3.2.2.3 Procedure

a) Weigh a quantity of sample that has been incinerated equivalent to 0.5 gram of sample
as calculated according to the following formula:

{0.5 (100.00-
W=
HP)}
Description:
100

W is the weight of the sample that is


incandescent, grams; HP is the
loss of incandescence, %.
Materials that have been incinerated at loss determination can be used as examples.
Mix evenly the sample with (4-6) grams of Na2 CO3 by grinding in an agate mortar.
Coat the bottom of the crucible with a thin layer of Na2 CO3 , add the cement- Na2 CO3
mixture on top then cover the mixture with a thin layer of Na2 CO3 .
Place the closed crucible over a medium flame and slowly raise the flame to maximum
( 1 100o C) and maintain this temperature until the mixture is quiescent ( 45 minutes).
Remove the burner, remove the cover and place it elsewhere, clamp the crucible with
tongs and rotate the crucible slowly so that the contents of the melt spread and solidify
as a thin layer on the inside of the cup wall.

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Cool the crucible and lid. Rinse the outer wall of the crucible and place the crucible in a
300 mL casserole that is one-third water.
Warm the casserole and stir so that the crust in the crucible is cracked and can be
removed easily.
Using a glass stirring rod, remove the crucible from the casserole, rinse with water until
clean. Rinse the crucible and lid with HCl (1+3), the rinse water is added to the
casserole.
Carefully and slowly add 20 mL of HCl (b.j 1.19) to the covered casserole. Remove and
rinse the lid. If granular particles are present, the melting was incomplete and the test
should be repeated using a new sample.
Attention:
The sequence of test steps must be followed correctly to produce precise and thorough
results.

b) Evaporate the solution to dryness on a steam bath (until no lumps are visible) without
further heating the residue, add (5-10) mL HCl, let stand for at least 2 min, add an equal
amount of water (5 mL-10 mL).
Cover the crucible and digest for 10 minutes on a steam bath or hot plate. Dilute the
solution with equal amounts of hot water, filter with medium-porous filter paper and wash
the separated SiO2 with hot HCl (1+99), then with hot water, reserving the precipitate.

c) Evaporate the filtrate again to dryness and bake the precipitate in an oven at (105- 110)o
C for 1 hour, cool, add (10-15) mL HCl (1+1) and digest on a steam bath or hot plate for
10 minutes. Dilute with an equal amount of water, immediately filter with new filter paper,
and wash the SiO precipitate2 as in 7.1.3.2.2.3 item b), mix the filtrate and wash water
and save for determination of ammonium hydroxide group according to 7.1.3.3
determination of ammonium hydroxide group. Continue the determination of SiO2 in
accordance with 7.1.3.2.1.3 item b).

7.1.3.3 Ammonium hydroxide group (R O )23

7.1.3.3.1 Test method summary


In this method aluminum oxide, iron (III) oxide, titanium dioxide, and phosphorus pentaoxide
are precipitated from the filtrate, after SiO2 is separated by adding ammonium hydroxide. If
done more carefully the manganese dioxide precipitate will precipitate. The precipitate is
incinerated and weighed as oxide.

7.1.3.3.2 Reagents
a) Hydrochloric acid (HCl b.j 1.19).
b) Hydrochloric acid (HCl) (1+2).
c) Ammonium hydroxide (NH4 OH)(1+1).
d) Ammonium nitrate (NH4 NO3 ).

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7.1.3.3.3 Procedure
a) The filtrate deposited in 7.1.3.2.1.3 item a) (see procedure item) which is 200 mL in
volume, if necessary add HCl to confirm the total amount of acid in the filtrate (10-15)
mL.
Add a few drops of methyl red indicator and heat to boiling.
Then drop NH4 OH (1+1) until the solution is yellow, and add one drop of excess.
Heat the solution containing the precipitate to boiling and boil for (50-60) seconds.
To avoid bumping during the boiling of the solution, it can be done in another way,
namely:
Digest on a hot plate that has the same temperature as the steam bath for 10 minutes.
Allow the precipitate to drop (no more than five minutes) and filter using medium-porous
filter paper. Wash with hot ammonium nitrate solution (NH4 NO3 20 grams/L), for a small
precipitate wash twice, while for a large precipitate wash four times.

b) Collect the filtrate and transfer the sediment along with the filter paper into the beaker
originally used for settling.
Dissolve the precipitate with hot HCl (1+2). Stir until the filter paper disintegrates and
then dilute the solution with 100 mL boiling water. Re-precipitate the hydroxide according
to 7.1.3.3.3 item a). Filter the solution and wash the precipitate with (4-10) mL of hot
ammonium nitrate solution (NH4 NO3 20 grams/L).
Combine the filtrate and its washing solution with the original phratate and save for CaO
determination according to 7.1.3.9.3 item a).

c) Place the precipitate in a crucible of known weight, heat gently until the carbon from the
filter paper is removed, and finally to prevent reduction, carefully incandesce at (1 050 -
1 100)o C until the weight remains and weigh as ammonium hydroxide group.

d) Perform a blanket determination using the same reagents and methods and calculate
the results as a correction in the calculation.

7.1.3.3.4 Calculations
Calculate the content of R O23 with an accuracy of 0.1%.

Sludge weight x 100


% R O23 =
Sample weight

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7.1.3.4 Iron(III) oxide (Fe O )23

7.1.3.4.1 Test method summary


The Fe O23 content of cement is determined from individual samples by reducing iron(III) to
iron(II) with tin(II) chloride (SnCl2 ) and titrating with potassium bichromate standard solution
(K2 Cr O27 ).
This determination is not affected by titanium and vanadium that may be present in the
cement.

7.1.3.4.2 Reagents
a) Barium diphenylamine sulfonate indicator solution.
Dissolve 0.3 grams of barium diphenylamine sulfonate in 100 mL of water.
b) Potassium dichromate standard solution (1 mL = 0.004 grams Fe O )23
- Blend and dry the potassium dichromate primary standard reagent (K 2 Cr O27 ) NBS
136 at (180-200)o C until the weight remains.
- Weigh carefully 2.457 00 grams for 1 Liter of prepared solution.
- Dissolve in water and dilute to the desired volume in an appropriately sized flask. This
standard solution is the primary standard solution and need not be further determined.

c) Tin(II) chloride solution


- Dissolve 5 grams of tin(II) chloride (SnCl2 .2H2 O) in 10 mL of HCl and dilute to 100 mL.
- Add iron-free tin granules and simmer until the solution is in a sealed drop bottle
containing the tin granules.

7.1.3.4.3 Procedure
For portland cement where the insoluble part is not known, first determine the insoluble part
in accordance with the test described in this procedure. If the insoluble portion is known,
perform according to 7.1.3.4.3 item a) or 7.1.3.4.3 item b).
a) For portland cement with insoluble part content smaller than 1%
- Weigh 1 gram of sample into a 500 mL beaker or other suitable container.
- Add 40 mL of cold water, while shaking the container add 10 mL of HCl. If necessary
heat the solution and crush the cement with a flat-tipped glass stir bar until all the
cement is completely broken down. Continue analysis according to
7.1.3.4.3 item b) i).
b) For cement with insoluble part content greater than 1%
- Weigh 0.500 grams of sample, mix with 1 g of LiBO2 using a mortar and pestle.
Transfer into a crucible that before heating contains 0.1 gram of LiBO 2 scattered at
the bottom.

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- Cover with 0.1 gram of LiBO2 that was first used to clean the mortar and pestle. Place
the uncovered crucible in a furnace that has been set at 1 100o C for 15 minutes.
Remove the crucible from the furnace and check the melting for perfection. If the
melting is not complete, return the crucible to the furnace for 30 minutes. Check the
melting perfection again. If the melting remains incomplete, discard the sample and
repeat the melting procedure using 0.250 grams of sample or a lesser amount of
sample with the same amount of LiBO .2
- When the fusion is complete, immediately shake, carefully remove the melt and pour
it into a 150 mL beaker containing 10 mL HCl and 50 mL water. Stir continuously until
the melt dissolves, usually 10 minutes or less.
- If a magnetic stirrer is used, remove and rinse the stir bar and continue the analysis
as per 7.1.3.4.3 item b) i).
i) Heat the solution to boiling and add SnCl2 solution drop by drop while stirring
and boiling until the solution is colorless.
Add one drop of excess and cool the solution to room temperature by placing
the beaker in a pan of cold water.
After cooling and without delay rinse the inside walls of the beaker with water,
and add at once 10 mL of cold saturated mercuric chloride (HgCl2 ) solution.
Stir the solution rapidly for one minute by shaking the beaker and add 10 mL
of H3 PO4 (1+1) and two drops of barium diphenylamine sulfonate indicator
solution. Add enough water until the volume after titration ranges between (75-
100) mL.
Titration with potassium dichromate standard solution. An end point will be
indicated where one drop causes a steady mauve-red color on addition of
excess K2 Cr O27 solution.

7.1.3.4.4 Blangko
Make a blank determination using the same procedure with the same reagents. Record the
volume of K2 Cr O27 solution required to establish the end point as described in 7.1.3.4.3 item
b) i).

A certain amount of iron is required to reach the end point, if there is no obvious mauve color
after adding four drops of K2 Cr O27 standard solution, then there is no iron in the blank.

7.1.3.4.5 Calculations

Calculate the Fe content of O23 with an accuracy of 0.01% (reported with an accuracy of
0.1%) as follows:

% Fe O23 = E x (V-B) 100


x W
Description:
E is the equivalence of Fe O23 to K2 Cr O27 solution, grams/mL;
V is the milliliters of K2 Cr O27 required in the sample determination;
Bad is the milliliters of K2 Cr O27 required in the blank
determination; W is the weight of the sample with an accuracy of 0.1
milligram.

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7.1.3.5 Phosphorus pentaoxide (P O )25
7.1.3.5.1 Test method summary

This colorimetric test method is used to determine P O25 in Portland cement. Under these
test conditions there are usually no other interfering elements in Portland cement.

7.1.3.5.2 Equipment

Spectrophotometer, the instrument shall be equipped to measure the absorbance of the


solution at a wavelength of 725 nm. Wavelength measurements should be repeatable within
a tolerance of  1 nm or smaller. In the absorbance region from 0.1 - 1.0, absorbance
measurements should be repeatable within a tolerance of 1% or smaller. To ensure that the
spectrophotometer can be used with a satisfactory degree of accuracy, qualify the instrument
according to the specifications using procedure 7.1.3.5.4.

7.1.3.5.3 Reagents

a) Ammonium molybdate solution


- Place 500.0 mL of H2 SO4 10.6 N in a 1 liter volumetric flask.
- Dissolve 25.0 grams of ammonium molybdate (NH )46 Mo O724 .4H2 O) in 250 mL of
warm water and transfer to a volumetric flask containing H2 SO4 , while shaking the
flask.
- Cool, dilute to 1 Liter with water, and store in a plastic bottle.
b) Ascorbic acid powder
To facilitate its dissolution, use the finest one.
c) Raw hydrochloric acid (6.5  0.1N)
- Dilute 540 mL HCl (b.j 1.19) to 1 Liter with water.
- Treat the standard NaOH solution 7.1.3.5.3 item f) using phenolphthalein indicator.
- Determine the normality precisely and set it at 6.5 N  0.1 N by water dilution.
- Re-stand to ensure that proper normality is achieved.
d) Phosphate standard solution A
Dissolve 0.191 7 grams of dried potassium dihydrogen phosphate (KH2 PO4 ) in water
and dilute to 1 Liter in a measuring flask.
e) Phosphate standard solution B
Dilute 50 mL of phosphate solution A to 500 mL with water.

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f) Standard sodium hydroxide solution (1 N)
- Dissolve 40.0 grams of sodium hydroxide (NaOH) in water, add 10 mL of freshly
filtered barium hydroxide (Ba(OH)2 ) saturated solution, and dilute to 1 liter with
freshly boiled and cooled water.
- Shake the solution from time to time for several hours, and filter it into a plastic bottle.
Keep the bottle tightly closed to protect the solution from CO2 present in the air.
- Treat acidimetrically potassium phthalic acid or benzoic acid issued by NBS (standard
samples 84 f and 350), using the test method given in the certificate accompanying
the samples.
- Establish the normality of the solution appropriately.
g) Raw sulfuric acid (10.6 N  0.1 N)
To a 1-L volumetric flask cooled in water, add approximately 600 mL of water, then add
300 mL of H2 SO4 (b.j 1.840) slowly and carefully. After cooling to room temperature,
dilute to 1 Liter with water.
Treat against standard NaOH solution 7.1.3.5.3 item f) using phenolphthalein as
indicator.
Establish normality and set to 10.6 N ± 0.1 N by water dilution. Re-treat to
ensure that proper normality is achieved.

7.1.3.5.4 Procedure

a) Prepare a series of phosphate solutions from (0-0.5)% P O25 .


Prepare each by adding an appropriate volume of phosphate standard solution B and
25.0 mL of 6.5 N hydrochloric acid to a 250 mL volumetric flask. Dilute to the limit mark
with water.
NOTE One milliLiter of standard phosphate solution B in 250 mL of solution is equivalent to
0.004% P O25 gram of cement sample. A series of concentrated solutions (mother liquor) of
standard phosphate B whose volumes are: 0; 12.5; 25; 50; 74; 100 and 125 mL are equivalent to
the level of P O25 in the cement sample.
0; 0.05; 0.10; 0.20; 0.30; 0.40; and 0.50%.
b) Prepare a blank by adding 25.0 mL of standard HCl to a 250 mL measuring flask and
diluting to 250 mL with water. Perform staining on a series of phosphate solutions and
blanks according to 7.1.3.5.4 items e) to 7.1.3.5.4 items g) until color occurs.
c) Plot the absorbance value (standard absorbance minus the blank absorbance) obtained
as ordinate and the concentration of P O25 as abscissa. Construct a curve showing the
relationship between absorbance and concentration of P O25 .
d) Transfer 0.25 grams of sample into a 250 mL beaker and moisten with 10 mL of cold
water to prevent clumping. Add 25.0 mL of standard HCL and digest with moderate
heating and stirring until the solution is complete. Filter into a 250 mL volumetric flask
and wash the filter paper and the separated silica precipitate with hot water. Allow the
solution to cool and dilute with water to 250 mL.

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e) Transfer 50.0 mL aliquot of the sample into a 250 mL beaker, add 5.0 mL ammonium
molybdate solution and 0.1 gram ascorbic acid powder. Stir the contents of the beaker
by shaking until ascorbic acid dissolves completely. Heat the solution to boiling, remove
the cover and continue boiling for (1.5 ± 0.5) minutes. Cool to room temperature and
transfer into a 50 mL measuring flask. Rinse the beaker with a little water and add the
rinse water to the flask. Dilute to 50 mL with water.
f) Perform a blank measurement at a wavelength of 725.0 nm.
g) Prepare 50.0 mL aliquot of the blank solution prepared as for the sample solution.
Measure the absorbance in accordance with 7.1.3.5.4 item f) and subtract the
absorbance value obtained for the sample solution in 7.1.3.5.4 item e). To obtain the
final absorbance of the sample solution.
h) Using the pure absorbance value obtained, record the percentage of P O 25 in the cement
sample as shown on the calibration curve. Report %P O25 with an accuracy of 0.01.

7.1.3.6 Titanium dioxide (TiO )2

7.1.3.6.1 Test method summary

In this test method, titanium dioxide (TiO2 ) in Portland cement is determined colorimetrically
using the tiron reagent. Under these test conditions, only iron, which is an element in
Portland cement, causes very little disturbance, equivalent to 0.01% for every 1% Fe O23 .

7.1.3.6.2 Equipment

Spectrophotometer, the instrument should be equipped to measure the absorbance of the


solution at a wavelength of 410 nm. The wavelength measurement should be repeatable if ±1
nm is obtained. In the absorbance region from 0.1 - 1.0, absorbance measurements should
be repeatable within a tolerance of 1% or smaller.

7.1.3.6.3 Reagents

a) Buffer pH 4.7
68 g NaC H O232 .3H2 O plus 380 mL water and 100 mL CH3 COOH 5 N
b) Ethylendinitrilo tetra acetate dihydrate dinatrium salt (EDTA 0.2 M)
- Dissolve 37.5 grams of EDTA in 350 mL of warm water and filter.
- Add 0.25 grams of FeCl3 .6H2 O and dilute to 500 mL.
c) Hydrochloric acid (1+6)
d) Raw hydrochloric acid (6.5 N)
Dilute 540 mL HCl (b.j 1.19) to 1 Liter with water.
e) Ammonium hydroxide (NH4 OH)( 1+1)
f) Potassium pyrosulfate

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g) Titanium dioxide, mother liquor A
- Slowly melt 0.031 4 grams of TiO2 99.74% (NBS SRM 154b) in a crucible over a small
flame or another titan compound as a substitute and add approximately 2 grams or 3
grams of K S O227 .
- Allow to cool, and crucible in a beaker containing 125 mL of H2 SO4 (1+1).
- Heat and stir until the melt is completely dissolved.
- Cool, transfer into a 250 mL volumetric flask, and dilute the solution to the limit mark.
h) Titanium dioxide, aqueous standard solution B (1 mL = 0.012 5 mgram TiO )2
Pipette 50 mL of mother liquor A TiO2 into a 500 mL volumetric flask, and dilute to the
limit. One mL of this solution is equal to 0.0125 mg TiO2 which is equivalent to 0.05%
TiO2 if the procedure in 7.1.3.6.4 items e) through to
7.1.3.6.4 item f).
i) Sulfuric acid (1+1)
j) Tiron (dinatrium-1,2-dihydroxydabenzen-3,5 disulfonate)

7.1.3.6.4 Procedure
a) Prepare a series of aqueous standard solutions B TiO2 covering concentrations from
0%-1.0% TiO2 . Prepare each solution in a 50 mL measuring flask.

NOTE One mL of dilute standard solution B of TiO2 in 50 mL is equivalent to 0.05% TiO2 for
0 .250 0 grams of cement sample. 0, 5, 10, 15 and 20 mL solutions of standard solution TiO2 are
equivalent
with TiO content2 in the sample of 0; 0.25; 0.50; 0.75; and 1%. Dilute each to 25 mL with water.
b) Add chemical reagents according to the procedure in 7.1.3.6.4 item e) until color
appears.
c) Measure absorbance in accordance with 7.1.3.6.4 item f).
d) Plot the absorbance value as ordinate and the concentration of TiO2 as abscissa.
Construct a curve showing the relationship between absorbance and concentration.
e) Transfer 25.0 mL aliquot of the sample prepared in 7.1.3.5.4 item d) (see determination
of P O25 ) into a 50 mL volumetric flask. Add 5 mL tiron and 5 mL EDTA, mix and then
add dropwise NH4 OH (1+1).
Stir carefully after each drop until a color change from yellow to green, blue, or ruby red
occurs. Then return to a yellow color by adding dropwise HCl (1+6) and stirring after
each drop.
Add 5 mL of buffer, dilute to the limit and shake.
f) Measure the absorbance of the blank solution at a wavelength of 410 nm.
g) Using the absorbance price determined in 7.1.3.6.4 item f), record the TiO content 2 of
the cement sample as shown in the calibration curve with an accuracy of 0.01.
Correct for the presence of iron in the sample to determine the actual TiO2 with the
following formula:
Actual TiO2 = % TiO2 measurement - (0.01 x % Fe O23 ).
Report % TiO2 with an accuracy of 0.01.

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7.1.3.7 Zinc oxide

Any test method can be used in zinc oxide testing, provided that it is able to meet the
requirements listed in the table of allowable differences in test results (Table 6).

7.1.3.8 Aluminum oxide

Calculation:
Calculate the percentage of Al O23 by subtracting the sum of Fe O23 , TiO2 and P O25 from the
percentage of the ammonium hydroxide group. All determinations shall be by the referee
method as described in the items concerned. All percentages should be calculated to an
accuracy of 0.01%. Report Al O23 to an accuracy of 0.1% for non-referee analysis, the
percentages of Fe O23 , TiO2 and P O25 may be established by some procedures for which
qualifications have been indicated.

7.1.3.9 Calcium oxide (CaO)

7.1.3.9.1 Test method summary


In this test method, manganese is removed from the filtrate after the determination of SiO 2
and ammonium hydroxide group. Then calcium oxide is precipitated as oxalate. After
filtration, the oxalate is dissolved again and titrated with potassium permanganate (KMnO4 ).

NOTE For the referee test method or for high accuracy determination, the separation of manganese
according to 7.1.3.9.3 point b). For low accuracy determination, and if only the amount of manganese
oxide is insignificant, 7.1.3.9.3 item b) may be ignored.

Strontium is usually present in portland cement as a minor element, and is precipitated


together with calcium as oxalate and then titrated and calculated as CaO.
If the SrO content is known and correction of CaO to SrO is desired, for example, for
research purposes or to compare results with SRM certification values, CaO determined by
this method may be corrected to SrO.

In the determination to meet cement specifications, CaO to SrO correction is not necessary.

7.1.3.9.2 Reagents

a) Ammonium acetate solution (50 g/L)


b) Potassium permanganate standard solution (0.18 N).
- prepare a potassium permanganate solution (KMnO4 ) containing 5.69 grams/L.
- Leave this solution at room temperature for at least one week, or bring to a boil and
cool to room temperature.
- Remove the clear solution without disturbing the sediment at the bottom of the bottle;
then filter the separated solution through a glass wool funnel or through a glass filter.
- Do not filter through materials containing organic substances.
- Store in a dark-colored bottle, preferably one that has been painted black on the
outside.

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- Standardize to (0.700 0 - 0.800 0) grams of sodium oxalate primary standard, in
accordance with the sodium oxalate standardization instructions, and record the
temperature at which the standardization is performed (see NOTE).
- Calculate the CaO equivalence of the solution as follows:
1 mL of 1N KMnO4 solution is equivalent to 0.067 01 grams of pure sodium oxalate.

Weight of Na oxalate x purity fraction


KMnO normality4 =
mL of KMnO solution4 x 0.067 01

1 mL of 1N KMnO4 solution is equivalent to 0.028 04 grams of CaO.

F= Normality of KMnO solution4 x 0.028 04 x 100


0,5
Description:
F is the equivalence of CaO to KMnO solution4 in % CaO/mL based on 0.5 grams
of cement sample.

NOTE Because the KMnO4 solution is not stable, it is re-standardized at least every two
months.

7.1.3.9.3 Procedure

a) Acidify the combined filtrate determined on deposition of ammonium hydroxide group


7.1.3.3.3 item b).
Neutralize with HCl until the color of the methyl red endpoint is reached, add 6 drops
more HCl to make it completely acidic.
b) Manganese separation
- Evaporate to a volume of 100 mL.
- Add 40 mL of saturated bromine water to the hot solution and add NH4 OH
immediately until the solution is alkaline.
- The addition of 10 mL of NH4 OH is generally sufficient.
- A piece of filter paper approximately 1 cm wide2 , place it into the beaker and press
it down with the help of the stir bar tip to prevent bumping and early precipitation of
manganese oxide hydrate (MnO).
- Simmer the solution for 5 minutes or so, making sure it is completely alkalized at
all times.
- Allow the precipitate to drop, filter using medium-porous filter paper, and wash with
hot water.
- If the sediment does not appear immediately, allow up to one hour of settling time
before filtering.
- Separate any manganese dioxide that has precipitated. Acidify the filtrate with HCl
using litmus paper as an indicator and boil until the bromine evaporates (NOTE 1).
NOTE 1Potassium iodide starch paper can be used to show the perfection
of evaporation from excess bromine. Apply the moist paper to the vapor of the boiling
solution. The paper should not change color, and if the paper turns blue, bromine is still
present.

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c) Add 5 mL of HCl, dilute to 200 mL and add a few drops of methyl red indicator and 30
mL of warm ammonium oxalate solution (50 g/L) (NOTE 2). Heat the solution to (70-
80)o C and add NH4 OH (1+1) dropwise, while stirring until a color change from red to
yellow occurs (NOTE 3). hLeave the solution without further heating for (60  5) minutes
(not more), with occasional stirring during the first 30 minutes.

NOTE 2 If the ammonium oxalate solution is not clear, it should be filtered before use.

NOTE 3 This neutralization should be carried out slowly, otherwise the calcium oxalate
precipitate tends to escape through the filter paper. If a number of these determinations are
made simultaneously the following technique may help to ensure slow neutralization. Add 2 or 3
drops of NH4 OH to the first beaker while stirring, then 2 or 3 drops to the second beaker, and
so on, returning to the first beaker with the addition of 2 or 3 more drops until the color of the
indicator in each beaker changes.

d) Filter using fine filter paper, and wash the sediment 8 to 10 times with hot water, the
total amount of water used in beaker rinsing and washing should not exceed 75 mL.
During this washing, the water from the washing bottle should be directly toward the
inside of the filter paper, until the sediment drops, then spray with water slowly directly
toward the center of the filter paper so that the sediment is stirred and washed
completely. Acidify the filtrate with HCl and store for MgO determination.
e) Place the beaker under the funnel containing the sediment, pierce the conical top of the
filter paper with the stirring rod, place the stirring rod in the beaker, and wash the
sediment into the beaker and wash the sediment into the beaker using hot water. Drip
10 drops of H2 SO4 (1+1) around the top edge of the filter paper. Wash the filter paper
5 times with hot water.
Dilute to 200 mL, and add 10 mL of H2 SO4 (1+1). Heat the solution at a temperature
near boiling point, and immediately titrate with 0.18 N KMnO4 solution (NOTE 4).

NOTE 4 Since the KMnO4 solution is not stable, it is re-standardized at least every two months.

Continue titrating slowly until the correct pink color persists for at least 10 seconds.
Add the filter paper containing the precipitate and immerse it. If the pink color does not
appear, continue the titration until the color is not less than 10 seconds.

NOTE 5 The temperature of the solution of KMnO4 0.18 N as penetration should not vary from
the standardization temperature by more than 5.5o C. Larger deviations may cause serious
errors in the determination of CaO.

7.1.3.9.4 Blangko

Make a blank determination with the same procedure and using the same amount of reagent and
record the milliliters of KMnO4 required for the determination of the end point.

NOTE When the amount of calcium oxalate is very small, oxidation by KMnO4 proceeds
slowly. Before titration add a small amount of MnSO4 to the solution as a catalyst.

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7.1.3.9.5 Calculations
Calculate the percentage of CaO with an accuracy of 0.1 as follows:

% CaO = E(V-B)

Description:
E is the equivalence of CaO to KMnO solution4 in % CaO/mL based on 0.5 grams of sample;
V is the KMnO4 solution required by the sample, mL; B is
the KMnO4 solution required by the blank, mL.

If necessary, correct the percentage of CaO to SrO as follows:

%CaOc = %CaOi - 0.54 %SrO

Description:
CaOc = corrected CaO;
CaOi = CaO obtained from 7.1.3.9.5
0.54 = molecular weight ratio of CaO to SrO (56,08 )
103,62

7.1.3.10 Magnesium oxide (MgO)

7.1.3.10.1 Test method summary

In this test method, magnesium is precipitated as magnesium ammonium phosphate from the
filtrate after separation of calcium. The precipitate is incinerated and weighed as ammonium
pyrophosphate (Mg P O227 ). The MgO equivalence was then calculated.

7.1.3.10.2 Reagents
Biased ammonium phosphate (100 g/L) (NH )42 HPO4 .

7.1.3.10.3 Procedure
- Acidify the filtrate from the determination of CaO 7.1.3.9.3 item d) with HCl and
evaporate with boiling to approximately 250 mL.
- Refrigerate solution to temperature room temperature, add 10
mL ammonium phosphate ((NH )42 HPO4 ) bialkaline (100 g/L) and 30 mL
NH4 OH.
- Stir the solution vigorously during the addition of NH4 OH and then extend the stirring
time by 10 min -15 min.
- Leave the solution for at least 8 hours at air temperature.
- Wash the residue 5 or 6 times with NH4 OH (1+20) and incandesce it in a crucible or
porcelain cup of known weight, first heated slowly until the filter paper is filtered into
charcoal and then burn it, and finally incandesce it at 1 100o C for 30 min - 45 min.

NOTE Care must be taken during this refinishing. Phosphate deposits may be reduced by contact
with carbon at high temperatures. There is a dangerous possibility of carbon trapping by the
precipitate during too rapid annealing.
- Weigh the residue as magnesium pyrophosphate (Mg P O227 ).

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7.1.3.10.4 Blangko
Make a blank determination with the same procedure and using the same amount of reagent,
and correct the results obtained in the analysis.

7.1.3.10.5 Calculations
Calculate the percentage of MgO with an accuracy of 0.1 as follows:

% MgO = W x 72.4

Description:
W is grams Mg P O227 ;
72.4 is the ratio of 2 MgO molecules to Mg P O227 (0.362) divided by the weight of the
sample used (0.5 grams) multiplied by 100.

NOTE Care must be taken during this refinishing. Phosphate deposits may be reduced by contact with
carbon at high temperatures. There is a dangerous possibility of carbon trapping by the precipitate
during too rapid annealing.

7.1.3.11 Sulfur

7.1.3.11.1 Sulfur trioxide

7.1.3.11.1.1 Test method

summary

In this test method sulfate is precipitated from an acidic solution of cement with barium chloride
(BaCl2 ).
The precipitate was incinerated and weighed as barium sulfate (BaSO4 ) and the SO
equivalence calculated3 .

7.1.3.11.1.2 Procedure

a) To 1 gram of sample, add 25 mL of cold water, while mixing stir vigorously and add 5 mL
of HCl.

NOTE 1 The acid filtrate produced in the determination of the insoluble residue 7.1.3.1.3 may be
used for the determination of SO3 unless another sample is used.

b) If necessary, heat the solution and crush the sample with the stem end of a flat-tipped
glass stirrer until the cement is completely broken down.

NOTE 2 The brown residue of the manganese component is negligible.

c) Dilute the solution to 50 mL and digest for 15 min at near boiling temperature. Filter
through medium-porous filter paper and wash the residue with hot water.
d) Dilute the filtrate to 250 mL and heat to boiling.
e) Add slowly dropwise 10 mL of hot BaCl2 (100 g/L) and continue boiling until the
precipitate is completely formed. Digest the solution for (12-24) hours at near boiling
temperature.

NOTE 3 If rapid determination is desired, the digest time may be accelerated to a maximum of 3
hours. However cement may be rejected as meeting the specification requirements, based solely
on the results obtained when using a digest time of (12-24) hours.

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f) Keep the volume of solution between (225-260) mL and add water if necessary. Filter
through fine-pored filter paper, wash the precipitate with hot water, place the filter paper
and contents in a weighed crucible. Incinerate at (800-900)o C, cool in a desiccator and
weigh.

NOTE 4 When an instrument test method for sulphur is used or when comparing the results of the
wet analysis and the instrument test method is less than 0.05%.

7.1.3.11.1.3 Blangko

Make a blanket determination with the same procedure and use the same amount of reagent,
and correct the results obtained in the analysis.

7.1.3.11.1.4 Calculations

Calculate the percentage of SO3 with an accuracy of 0.01 as follows:

% SO3 = W x 34.3

Description:
Wis the gram of BaSO4 against the sample;
34.3 is the ratio of SO3 molecules to BaSO4 (0.343) multiplied by 100.

7.1.3.11.2 Sulfide

7.1.3.11.2.1 Test method summary


In this test method, sulphur sulfide is determined by slowly converting as hydrogen sulfide
(H2 S) from an acidic solution of cement in ammoniacal zinc sulfate (ZnSO4 ) or ammoniacal
cadmium chloride (CdCl2 ) solution.
Sulfide of sulfur was titrated with potassium iodate standard solution (KIO3 ). Sulfite,
thiosulfate and other intermediate compounds of sulfide and sulfate were considered absent.
If such compounds are present, they may cause errors in the determination.

7.1.3.11.2.2 Equipme

nt Gas generator flask.


Connect a 500 mL dry boiling flask with a long-stemmed separatory funnel through a rubber
bulb cap. The bent stem of the separatory funnel is adjusted so that it does not interfere with
the connecting bulb, the tip of the separatory funnel stem is dipped to the bottom of the
boiling flask, connect the separatory funnel with an air compressor.
Connect the bulb with an L-shaped glass pipe and a straight glass pipe that is 200 mm long.
Put the straight glass into a 400 mL tall beaker. A three-necked distillation flask with a long
gas tube is placed between the compressor and the separatory funnel and is an appropriate
aid in regulating the air flow.
The rubber used in this equipment should be of high purity, with low sulfur content and
should be washed with warm HCl.

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7.1.3.11.2.3 Reagents

a) Ammoniacal cadmium chloride solution


Dissolve 15 g of cadmium chloride (CdCl2 .2H2 O) in 150 mL of water and 350 mL of NH4 OH.
b) Ammoniacal zinc sulfate solution
Dissolve 50 grams of zinc sulfate (ZnSO4 .7H2 O) in 150 mL of waterand 350mL of NH4
OH. Filter the solution after allowing it to stand for at least 24 hours.
c) Potassium iodate standard solution (0.03 N)
- Prepare potassium iodate (KIO3 ) and Potassium iodide (KI) solutions as follows:
- Heat KIO3 at 180o C to constant weight. Weigh 1.070 1 gram of KIO3 and 12 grams of
KI.
- Dissolve and dilute to 1 Liter in a volumetric flask.
- This primary standard solution does not need to be standardized.
- One milliLiter of this solution is equivalent to 0.000 480 9 grams of sulfur.

NOTE This solution is very stable, but must be re-stabilized each time it is used. One year old
solution should be discarded or the concentration re-standardized.
d) Tin(II) chloride solution
To a small flask containing 10 grams of tin(II) chloride (SnCl2 .2H2 O), add 7 mL of HCl
(1+1), warm the mixture carefully until this salt dissolves, cool the solution, and add 95 mL
of water.
This solution should be prepared when needed, as these salts tend to hydrolyze.
e) Starch solution
To 100 mL of boiling water, add a cold suspension of 1 gram of starch solution in 5 mL of
water and cool. Add a cold solution of 1 gram of sodium hydroxide (NaOH) in 10 mL of
water, then 3 grams of potassium iodide (KI), and stir vigorously.

7.1.3.11.2.4 Procedure
a) Place 15 mL of ammoniacal ZnSO4 solution or ammoniacal CdCl2 solution (NOTE 2) and
10 mL of water into the flask and shake well to disperse the cement completely.
b) This step and the addition of SnCl2 must be done quickly to prevent cement binding.
c) Connect the flask with the funnel and bulb. Add 25 mL of SnCl2 solution through the
funnel and shake the flask. During shaking, keep the funnel closed and the bulb in the
ammoniacal ZnSO4 or ammoniacal CdCl2 solution.
d) Connect the funnel to a pressurized air source, open the funnel, and start flowing air
slowly until it boils.
e) Continue simmering carefully for 5 or 6 minutes.

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f) Stop heating and continue airflow for 3 or 4 minutes.
g) Remove the delivery tube and leave it in solution for use as a stirrer.
h) Cool the solution to (20-30)o C (NOTE 3), add 2 mL of starch solution and 40 mL of HCl
(1+1) and immediately titrate with 0.03 N KIO3 solution until a blue color is obtained that
does not disappear anymore (NOTE 4).

NOTE 1 In general ZnSO4 is better than CdCl2 because ZnSO4 is more soluble in NH4 OH than
CdCl2 . CdCl2 solution can be used when there is doubt about the presence of trace amounts of
sulphur sulphide, as the yellow color of cadmium sulphide (CdS) can detect trace amounts.

NOTE 2 If the sulfur content exceeds 0.2 or 0.25%, a small sample should be used so that the
titration with KIO solution3 does not exceed 25 mL.

NOTE 3 Cooling is essential as the endpoints are different in warm solutions.

NOTE 4 This solution is very stable, but should be re-stabilized every time it is used. One year old
solution should be discarded or the concentration re-stabilized.

NOTE 5 If the sulphur content is sufficient but cannot be estimated in advance, the result
obtained may be lower than it should be due to loss of H2 S during the slow titration. In this case
such determination should be repeated with the titration carried out more rapidly. Perform the
blank determination with the same procedure and using the same reagents, recording the volume
of KIO3 solution required to determine the end point as described in 7.1.3.11.2.4.

7.1.3.11.2.5 Calculations

Calculate the sulphide sulphur percentage (see 7.1.3.11.2) as follows:

% sulfide = E(V-B) x 20

Description:
E is the equivalence of sulfide to KIO solution 3;
V is the KIO3 solution required by the sample, mL;
Bad is the KIO3 solution required by the blank, mL
20 = 100 divided by the weight of the sample used (5 grams).

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7.1.3.12 Missing incandescent

7.1.3.12.1 Portland cement

7.1.3.12.1.1 Summary of test

method

In this test method the cement is incinerated in a heating furnace at a preset temperature.
The part lost is assumed to indicate the amount of water and CO2 in the cement. This
procedure is not suitable for determining the incandescent loss of portland blast-furnace slag
cement and slag cement.

7.1.3.12.1.2 Procedure

Weigh 1 gram of sample in a crucible of known weight. Cover and incandesce the crucible
and its contents to constant weight in a furnace at (950  50)o C. Allow at least 15 minutes for
the initial heating time and at least 5 minutes for each subsequent time period.

7.1.3.12.1.3 Calculations

Calculate the percentage loss of incandescence to an accuracy of 0.1 by multiplying the


weight lost in grams by 100.

W1 -W 2
% HP= x 100
W1

Description:
W1 is the initial sample weight;
W2 is the weight of the residual incandescent sample.

7.1.3.12.2 Blast-furnace slag portland cement and slag

cement 7.1.3.12.2.1 Summary of test methods

This test method provides a correction for the weight gain due to oxidation to sulfides that
typically occurs in blast-furnace slag portland cement and slag cement by determining the
increase in SO content3 during spinning.

7.1.3.12.2.2 Procedure

a) Weigh 1 gram of sample in a fixed platinum crucible and incandesce in an electric


furnace at (950 ± 50)o C for 15 minutes. Cool in a desiccator at room temperature and
weigh. Without being constant, carefully transfer the material into a 400 mL beaker.
Break up the lumps in the cement with a flat-tipped stir bar.
b) Determine the SO content of3 by methods 7.1.3.11.1.1 to 7.1.3.11.1.4. Also determine
the SO content3 of the same ungasified cement, using the same procedure.

7.1.3.12.2.3 Calculations

Calculate the percentage weight loss that occurs during heating and add 0.8 x the difference
in SO3 percentage of the heated sample and the original cement. Report the corrected
percentage as incandescent loss.

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7.1.3.13 Sodium and potassium oxides

7.1.3.13.1 Total alkali

7.1.3.13.1.1 Test method summary

This test method includes the determination of sodium oxide (Na2 O) and potassium oxide
(K2 O) by the flame photometry method or by the atomic absorption spectrophotometry
method.

NOTE This test method is suitable for hydraulic cements completely decomposed by HCl and should
not be used for the determination of total alkali in hydraulic cements containing high acid insoluble
materials, such as pozolanic cements. But it can be used for the determination of acid soluble alkali
only for such cements.

7.1.3.13.1.2 Equipment

Any type of flame photometer or atomic absorption spectrophotometer can be used as long
as the level of accuracy and precision is in accordance with the specifications.

NOTE For routine laboratory testing, it is recommended that instrument accuracy checks be carried
out routinely, either using NBS (National Bureau of Standards) standard cement or cement of known
alkali content.

7.1.3.13.1.3 Reagents and materials

a) Laboratory container
All containers shall be made of boron silicate glass and polyethylene containers shall
meet the requirements in accordance with 7.1.2.1.1 item (2).
b) Calcium carbonate
Calcium carbonate used in the preparation of calcium chloride standard solution should
not have a total alkali as sulfate greater than 0.020%.

NOTE Materials sold as primary raw materials or "low alkali" ACS usually meet this requirement.
However, the purchaser must be sure that the materials used are exactly what is required.
c) Calcium chloride (KCl)
d) Sodium chloride (NaCl)
e) Marketed solutions can be used instead of the solutions mentioned below.

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7.1.3.13.1.4 Solution preparation

a) Calcium chloride mother liquor


Add 300 mL of water to 112.5 grams of CaCO3 in a 1 500 mL beaker. While stirring,
slowly add 500 mL of HCl. Cool the solution to room temperature, strain into a 1 liter
volumetric flask, dilute to 1 liter and shake well. This mother liquor is equivalent to 63
000 ppm (6.3%) CaO.
b) Sodium-potassium chloride mother liquor
Dissolve 1.885 8 grams of sodium chloride (NaCl) and 1.583 grams of potassium
chloride (KCl) in water (both dried at (105-110)O C for several hours before weighing).
Dilute to 1 Liter in a volumetric flask and shake well. This mother liquor is equivalent to 1
000 ppm (0.10%) each for Na2 O and K2 O. Solutions separated from Na2 O and K2 O
can be used as long as they are of the same concentration for both calibration and
cement analysis.
c) Standard solution
Prepare the standard solution required for the instrument method used. Measure the
required volume of NaCl - KCl mother liquor using a calibrated pipette or pipette.
Calcium chloride mother liquor, if required, can be measured with an adequate
measuring cup. If the instrument used requires an inner standard, measure the standard
solution with a pipette or burette. Place each solution in a measuring flask, dilute to the
limit, and shake well.
If a more dilute solution is required in this method, pipette the required diluted solution
into an appropriately sized volumetric flask, add standard solution if necessary, dilute to
the limit mark, and shake well.

7.1.3.13.1.5 Tool calibration

In accordance with the manufacturer's operating instructions.

7.1.3.13.1.6 Procedure

(1) Cement solution


Prepare the cement solution according to the manufacturer's special procedure. If there is no
special procedure, or if required, perform according to the steps in 7.1.3.13.1.6 item (1) a) or
7.1.3.13.1.6 item (1) b).

NOTE The presence of SiO2 in the solution affects the accuracy of some flame photometers. In case
the instrument fails to give results with the desired degree of accuracy, the test should use a solution
from which SiO2 is separated. The separation method is in accordance with the method below.
a) Place (1.000 ± 0.001) gram of cement into a 150 mL beaker and disperse with 20 mL of water
by shaking the beaker, while shaking add 5.0 mL of HCl at a time. Dilute immediately up to 50
mL with water. Break up undispersed lumps of cement with a flat-tip stir bar. Digest on a
steam bath or hot plate for 15 minutes, then filter with medium-porous filter paper into a 100-
mL measuring flask. Wash the beaker and paper with hot water, cool this flask to room
temperature, dilute to 100 mL, shake the solution thoroughly.

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b) Place (1.000 ± 0.001) gram of cement into a platinum vaporizer cup and disperse with 10 mL
of water by shaking. While shaking, add 5.0 mL of HCl at a time. Break up the lumps with a
flat-tip stir bar and heat on a steam bath, until dry. Make sure that gelatin does not form
anymore. Treat the residue with 2.5 mL HCl and approximately 20 mL water. Digest on a
steam bath for 5 min - 10 min and immediately filter through 9 cm diameter filter paper into a
100 mL volumetric flask. Wash completely by backwashing with a quantity of hot water until
the total volume of solution is 80 mL - 95 mL. Cool to room temperature, dilute to the limit
mark, and shake well. If it has been found that separation of SiO2 is necessary to obtain the
desired accuracy for a particular flame photometer, SiO2 should always be separated if the
analysis is to be used as a basis for rejection because it does not meet the requirements, or it
is doubtful that it meets the specifications. When meeting the specifications, analyses are
performed with this instrument without separation of SiO2, provided that the deviation from the
certificate price obtained from the test performed, shall not be twice as great as the limit
indicated.
c) If the test method in use requires more dilute solutions, internal standards or both, make the
same dilutions as in 7.1.3.13.1.4 item c). The standard solution and sample solution to be
analyzed shall be prepared in the same manner and at the same dilution as the cementitious
standard solution analyzed for instrument qualification.

(2) Procedure for Na2 O (NOTE 1)

Heat and set up the instrument for the determination of Na2 O as described in 7.1.3.13.1.5.
Immediately set up the instrument, atomize the cementitious solution and record the scale
reading (NOTE 2). Select a number of standard solutions whose distribution of Na 2 O levels
is close to that of Na2 O in the cement solution and take the transmittance reading for each
solution.

The value should be the same as that previously set at the time of equipment calibration.

If not, the equipment is recalibrated for that element. Finally, take the unknown solution until
the reading is within one transmission or meter scale of that of the standard solution, or
within 0.01 weight percent for instruments equipped with digital readout devices, and the
reading for the standard in the same manner corresponds to the calibration price. Record the
average price of the two final readings obtained for the unknown solution.

NOTE 1 The determination of water-soluble alkali shall not be considered as a substitute for the
determination of total alkali in accordance with 7.1.3.13.1.2 to 7.1.3.13.1.7. Moreover, in this method it
is not assumed that all alkalis present in the cement are soluble. It is important that this procedure is
followed carefully when there are limitations for the water-soluble alkali content or when comparing a
batch of cement with a batch of cement based on the water-soluble alkali content.

NOTE 2 The sequence in determining Na2 O or K2 O is optimal. However, the determination should be
made immediately after the apparatus is set up and ready to be used for the purpose. If the reading
exceeds the maximum scale, do either transfer 50 mL of the diluted solution as prepared in
7.1.3.13.1.6 item (1) into a 100 mL beaker or if desired prepare a new solution using 0.500 grams of
cement and 2.5 mL of HCl in the initial addition of acid. In case silica has been separated from the 0.5
gram cement sample, treat this dehydrated cement with 1.25 mL of HCl and approximately 20 mL of
water, then digest, filter, and wash. For both of the above, add 5.0 mL of calcium chloride mother
liquor before diluting to the limit mark with water. If necessary, dilute further as specified in 7.1.3.13.1.4
item c) of this test method. Determine the alkali content of this solution according to 7.1.3.13.1.6 item
(2). and multiply by a factor of 2 to calculate the percentage of alkaline oxide.

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(3) Procedure for K O2

For the determination of K2 O repeat the procedure as described in 7.1.3.13.1.6 item (2). For
instruments that can read both Na2 O and K2 O simultaneously, the determination of K2 O is
performed at the same time as the determination of Na O.2

7.1.3.13.1.7 Calculations and reports

From the average records of Na2 O and K2 O on an unknown sample, report each oxide to an
accuracy of 0.01%.

7.1.3.13.2 Water-soluble alkali

NOTE The determination of water-soluble alkali shall not be considered as a substitute for the
determination of total alkali in accordance with 7.1.3.13.1.2 to 7.1.3.13.1.7. Moreover, in this method it
is not assumed that all alkalis present in the cement are soluble. It is important that this procedure is
followed carefully when there are limitations for the water-soluble alkali content or when comparing a
batch of cement with a batch of cement based on the water-soluble alkali content.

7.1.3.13.2.1 Procedure

a) Weigh 25.0 grams of sample into a 500 mL Erlenmeyer flask and add 250 mL of water.
Cover the flask with a rubber lid and shake well for 10 minutes at room temperature.
Filter through a buchner funnel fitted with a holder for dry filter paper, into a 500 mL
filter flask, using a weak vacuum. Do not wash.
b) Transfer 50 mL of the diluted solution from the filtrate to a 100 mL volumetric flask and
acidify with 0.5 mL of HCl (specific gravity 1.19). Add 9.0 mL of CaCl 2 (63 000 ppm
CaO) mother liquor, as described in 7.1.3.13.1.4 item a), to the 100 mL flask, diluting
the solution to 100 mL. If this test method requires a more dilute solution, a deep
standard or both, perform the same dilution as in 7.1.3.13.1.4 item c).

NOTE The diluted solution of the filtrate taken for analysis shall be based on the estimated
level of water-soluble alkali. If the estimated content of K2 O or Na2 O is more than 0.08% by
weight of cement, or if the level of water-soluble alkali is unknown, to 50 mL of the diluted
solution given in 7.1.3.13.2.1 item .b) add 1 mL of HCl and evaporate on a hot plate in a 250 mL
beaker to approximately 70 mL. Add 8 mL of CaCl2 mother liquor and transfer the sample to a
100 mL measuring flask, rinse the beaker with a little distilled water. Cool the solution to room
temperature and dilute to 100 mL.

c) Determine the Na2 O and K2 O content of this solution as described in 7.1.3.13.1.6 item
(2) and 7.1.3.13.1.6 item (3). Record the ppm of each alkali in the solution contained in
the 100 mL flask.

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7.1.3.13.2.2 Calculations

Calculate the percentage of total water-soluble alkali, expressed as Na2 O, to an accuracy of


0.01. Total water-soluble alkali, expressed as follows:

Na2 O = A + E

A = B (V x 10)
C = D/(V x 10)
E = C x 0.658

Description:
A is the sodium oxide content of the solution in water (Na2 O), %;
V is the volume of the original filtrate in the 100, mL flask;
B is the concentration of Na2 O in the solution contained in the 100 mL flask, ppm;
C is the content of water-soluble potassium oxide (K2 O), %;
D is the concentration of K2 O in the solution contained in the 100 mL flask, ppm;
E is the Na2 O equivalent content of the flask.

7.1.3.14 Manganese oxide

7.1.3.14.1 Test method summary

In this test procedure manganese oxide is determined volumetrically by titration of sodium


arsenite solution after Manganese in cement is oxidized with sodium metabismutate (NaBiO3
).

7.1.3.14.2 Reagents

a) Sodium arsenite standard solution (1 mL = 0.000 3 grams Mn O )23


Dissolve into 100 mL of water 3.0 grams of sodium carbonate (Na2 CO3 ) and then add
0.90 grams of arsenic trioxide (AS O23 ) heat the mixture until it dissolves as completely
as possible. If the solution is not clear or contains residue, filter the solution. Cool to
room temperature, transfer into a volumetric flask and dilute to a volume of 1 Liter.
Dissolve 0.58 grams of potassium permanganate (KMnO4 ) in 1 Liter of water and
standardize against 0.03 grams of sodium oxalate (Na C O224 ) an oxidimetric standard
issued by the National Bureau of Standard (Sample Standard No. 40 or its successor) in
accordance with the provisions on the sodium oxalate label.
Place 30.0 mL of KMnO4 solution into a 250 mL Erlenmeyer flask, then add 60 mL of
HNO3 (1+4) and 10 mL of sodium nitrite (NaNO2 , 50 g/L).
Bring the solution to a boil until all of the HNO2 has evaporated. Cool the solution, add
NaBiO3 and finally titrate with sodium arsenite standard solution (NaAsO2 ) as described
in 7.1.3.14.3 item b).

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Calculate the manganese oxide (Mn O23 ) equivalent of NaAsO2 solution, in grams/mL,
as follows:

E = (A x 7.08)/ BC

Description:
E is the equivalence of Mn O23 to NaAsO2 solution, grams/mL;
A is the gram of Na C O224 used;
B is the milliLiter of KMnO4 solution required by Na C O224 ;
C is the milliliters of NaAsO solution2 required by 30.0 mL of KMnO solution4 ;
7.08 is the ratio of Mn O23 molecules to 5Na C O224 (0.236) multiplied by 30.0 mL of
KMnO4 solution.

b) Sodium metabismutate (NaBiO )3


c) Sodium nitrite solution (NaNO2 50 g/L)

7.1.3.14.3 Procedure

a) Weigh (1.0-3.0) grams of sample (NOTE 1) into a 250 mL beaker and add (5-10) mL of
water, then with (60-75) mL of HNO3 (1+4). Bring the mixture to a boil until a perfect
solution is formed.

Add 10 mL of NaNO2 (50 g/L) solution to the above solution and boil until the nitrous acid
has all evaporated (NOTE 2), being careful not to let the volume of the solution become
so low as to cause the gelatinized SiO2 to precipitate. If some of the SiO2 separates, it
may be ignored, but if there is a red or brown residue, use more NaNO2 solution (50
grams/L) to complete the decomposition, and then boil again to remove the nitrous acid.
Filter the solution through medium-porous filter paper into a 250 mL erlenmeyer flask
and wash the filter paper with water.

NOTE 1 The amount of cement used for analysis depends on the Manganese content, varying
from 1 gram for ± 1% Mn O23 to 3 grams for 0.25% Mn O23 or less.

NOTE 2 When NaNO2 is added the evaporation of HNO2 with boiling should be complete. If
manganese is present in the cement, a small amount of NaBiO3 will give a mauve red color.

b) The solution should have a volume of (100-125) mL. Cool to room temperature.
Into the solution add a little at a time NaBiO3 until the total amount is 0.5 grams, while
shaking occasionally.
After the addition is complete, shake the solution once for 5 min and then add 50 mL of
pre-boiled cold HNO3 (1±33) to remove the nitrous acid.
Filter the solution through a Gooch cup lined with asbestos or carbon or a glass filter with
the aid of a sucker. Wash the residue 4 times with cold HNO3 (1+33).
Immediately titrate the filtrate with NaAsO standard solution2 .
The end point is reached when a yellow color is formed that is free from brown or red-
violet color and does not change with the addition of excess NaAsO2 solution.

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7.1.3.14.4 Blangko

Make a blanket determination, following the same procedure and reagent amounts,
correcting the results obtained in the analysis.

7.1.3.14.5 Calculations

Calculate the percentage of Mn O23 with an accuracy of 0.01 as follows:

% Mn O23 = (EV/S) x 100

Description:
E is the equivalence of Mn O23 to NaAsO2 gram/mL solution;
Vis the millimiter of NaAsO solution2 that the sample
requires; Sadis the gram of sample used.

7.1.3.15 Chloride

7.1.3.15.1 Test method summary

In this test method, the total chloride content in Portland cement is determined by
potentiometric titration with silver nitrate. This procedure can also be used for hardened
concrete, slag, and portland cement raw mix. Under these test conditions, no interfering
elements are present.

NOTE Insoluble silver salts or silver complexes that are stable in acidic solutions will interfere with
potentiometric measurements, the presence of iodide and bromide can interfere while fluoride does
not, sulfide salts at concentration levels commonly found in the material will not interfere because they
will be decomposed by acid treatment.

7.1.3.15.2 Equipment

a) Ion selective/chloride electrodes, silver/sulfide selective ion electrodes, or electrode rods


coated with silver chloride, using appropriate comparison electrodes.

NOTE Suitable electrodes can be obtained from Orion Beckman Instruments, Leeds and Northup.
After careful study of the manufacturer's instructions fill in the electrode filling solution. Silver
electrode rods should be electrolytically coated with a thin layer of AgCl. To coat the electrode,
dip a clean silver electrode rod into a saturated solution of potassium chloride (± 40 g/L) in water
and run an electric current from the dry cell through the electrode at a voltage of 1.5 V-6 V. A
carbon rod from the dry cell or other suitable electrode is connected to the negative pole end and
dipped in the solution to complete the electrical circuit. If the silver chloride electrode coating is
worn, renew the electrode by repeating the above procedure. All old silver chloride should be
removed from the silver electrode rod by gently rubbing with fine sandpaper followed by rinsing
the electrode rod with water.

b) Potentiometers with a millivolt scale that can be read to 1 mV or more accurately


potentiometers equipped with digital readout equipment, but not required.
c) Class A burette, 10 mL capacity with a scale division of 0.05 mL. A potentiometric
burette, equipped with a drip regulator, is preferable, but not required.

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7.1.3.15.3 Reagents

a) Sodium chloride (NaCl), primary raw grade. (check numbering (number) first or letter)
first)
b) Silver nitrate (AgNO3 ), reagent grade.
c) Potassium chloride (KCl), reagent grade (required specifically for silver electrode rods).
d) Solution preparation
(1) Sodium chloride standard solution (NaCl 0.05 N)
- Dry the sodium chloride (NaCl) at 105o C -110o C until the weight remains.
- Weigh 2.922 2 grams of dry NaCl.
- Dissolve in water and dilute to exactly 1 Liter in a volumetric flask and shake
well. This solution is standard and need not be further standardized.

(2) Silver nitrate standard solution (AgNO3 0.05 N)


- Dissolve 8.493 8 grams of silver nitrate (AgNO3 ) in water.
- Dilute to 1 Liter in a volumetric flask and shake well.
- Treat 5.00 mL of 0.05 N sodium chloride standard solution that has been
diluted to 150 mL with water followed by the titration test method given in
7.1.3.15.4 item d) starting with the sentence "Place the beaker on a magnetic
stirrer and so on".
- Exact normality should be calculated from the average of three assignments
as follows:
0,25
N=
V

Description:
The normality of the AgNO setting3 ;
0.25 is the milli equivalent of NaCl (5.0 mL x 0.05 N);
V is the volume of AgNO solution3 , mL.

Commercially available standard solutions may be used provided that their normality
is checked in accordance with the standardization procedure.

(3) Methyl orange indicator


Prepare a solution containing 2 grams of methyl orange in 1 Liter of 95% ethyl
alcohol.

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7.1.3.15.4 Procedure

a) Weigh 5.0 grams of cement or 10.0 grams of concrete sample into a 250 mL beaker
(NOTE 1).

Disperse the sample with 75 mL of water. Without delay add slowly 25 mL of HNO3 (1 +
1), breaking up lumps with a stir bar. If the smell of hydrogen sulfide is too strong, add 3
mL of 30% hydrogen peroxide (NOTE 2). Add 3 drops of methyl orange indicator and
stir. Cover the beaker with a watch glass and leave for (1-2) minutes. If a yellow to
orange-yellow color appears on the top of the precipitate, the solution is not acidic
enough.

Add diluted HNO3 (1+1) drop by drop while stirring so that the pink color or red color
does not disappear, then add 10 drops of excess. Heat the sealed beaker quickly until it
boils. Do not let it boil for more than a few seconds.
Remove from the hot plate (NOTE 3).

NOTE 1 Use 5 grams for cement samples, and 10 grams for samples of concrete and other
materials having a chloride content less than 0.15% Cl. For materials with higher chloride content,
the sample amount is reduced proportionally. Powdered materials do not need to be ground.
Coarse samples should be ground to pass a 20 mesh sieve. If the sample is too fine it will cause
excessive Silica gel to form during digest with nitric acid, resulting in longer filtration.

NOTE 2 Slag and slag cement containing high sulphur sulphide may interfere with the
determination.

NOTE 3 It is very important to keep the beaker closed during heating and degassing to prevent
loss of chloride on evaporation. The use of excessive acid should be avoided as it will accelerate
the detachment of the silver chloride layer from the Silver electrode rod. A slightly acidic slurry is
sufficient.

b) Wash the 9 cm diameter coarse-pored filter paper four times with 35 mL of water using a
suction device fitted with a 250 mL or 500 mL Buchner funnel mounted above the
suction flask. Discard the wash and rinse the flask once more with a little water. Replace
the suction equipment and filter the sample solution. Rinse the beaker and filter paper
twice with a little water. Transfer the filtrate from the flask into the beaker originally used
(NOTE 4).
NOTE 4 There is no need to clean the slurry residue from the rim of the beaker. Likewise, it is not
necessary to filter out all fine material. Titrations can be carried out in solutions containing small
amounts of solids.
Cool the filtrate to room temperature. The volume should not exceed 175 mL.
c) For instruments equipped with digital readouts it is necessary to establish an
approximate "equivalence point" by dipping the electrode into a beaker of water and
adjusting the instrument so that the reading is approximately 20 mv lower than the center
scale. Record the reading on the millivolt meter. Remove the beaker and wipe the
electrode with suction paper.

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d) In the cooled sample (NOTE 5) beaker from 7.1.3.15.4 item b) carefully pipet 2.00 mL of
0.05 N NaCl standard solution. Place the beaker on a magnetic stirrer and insert into it a
TFE - fluorocarbon coated magnetic stirring rod. Dip the electrode into the solution,
taking care that the stirrer does not hit the electrode, start the initial stirring at low speed.
Place the 10 mL burette dropper section, which has been filled to the limit mark with 0.05
N silver nitrate standard solution on the beaker (NOTE 6).

NOTE 5 It is advisable to maintain a fixed temperature during the measurement as the solubility
of silver chloride varies considerably with temperature at low concentrations.

NOTE 6 If the burette from which the solution is dispensed has droplets attached, it should be
rinsed into the beaker using a few milliliters of water each time after adding the diluent.
e) Titrate gradually, recording the amount of 0.05 N nitrate standard solution required to
obtain a millivoltmeter reading to 60.0 mV of the set equivalence point in water.
f) Continue titration, each time adding 0.20 mL painter volume. Record burette readings
and millivoltmeter readings in columns 1 and 2 on a 4-column recording form as shown
in Appendix A. Each addition of painter allows the electrodes to reach equilibrium with
the sample solution. Experience shows that adequate readings are obtained when the
minimum scale reading does not change within 5 seconds (usually within 2 minutes).
The closer to the equivalence point, the addition of the same amount of AgNO3 solution
will cause a greater change in the millivoltmeter reading. Past the equivalence point the
change will decrease again. Continue the titration for up to three more additions after the
predicted equivalence point that has been recorded.
g) Calculate the difference in millivolt readings from one painter addition to another and
enter the value in column 3 of the recording form.
h) Calculate the difference in the prices in column 3 from one addition to the next and enter
the result in column 4. The titration equivalence point will be within the maximum interval
of 4 MV recorded in column 3. The equivalence point can be interpolated from the data
listed in column 4 as shown in Appendix A.

7.1.3.15.5 Blangko

Make a blank determination using 75 mL of water as a substitute for the sample, follow the
same procedure as in 7.1.3.15.4 item a) starting with the sentence "Without delay add slowly
etc". Correction of the analytical results obtained by subtraction of the blank

NOTE For non-referee analysis, blanket assignment may not be done.

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7.1.3.15.6 Calculations

Calculate the percent chloride with an accuracy of 0.001% as follows:

3.545 x (V -V12 ) N
% Cl =
W

Description:
V1 is the milliLiter of AgNO3 0.05 N solution used for the sample titration (equivalent point);
V2 is the milliLiter of AgNO3 0.05 N solution used for the blank titration;
N is the exact normality of 0.05 N AgNO3 solution; W is the
weight of the sample, grams.

7.1.3.16 Organic compounds soluble in chloroform

7.1.3.16.1 Test method summary

This test method is specifically designed for the determination of vinsol and tallow resins in
Portland cement, although mineral oils, resins, calcium stearate, and other fatty acid
compounds and some organic compounds are included in this determination.
Care must be taken throughout this procedure. This test method can be used for cements
other than Portland cement.
Even if the cement contains a high proportion of insoluble parts, the emulsion will separate
slowly, and shaking should not be too vigorous, resulting in more chloroform and more
frequent washing.

7.1.3.16.2 Reagents

a) Chloroform
If the blank determination as described in 7.1.3.16.4 exceeds 0.001 5 grams of
chloroform should be distilled before use. The chloroform recovered may be slightly
acidic but can be reused on shaking with an acidic solution of the sample in a 1 Liter
separatory funnel.
The chloroform used to wash the filters and separators should be fresh or distilled.

b) Tin(II) chloride (SnCl2 ).

7.1.3.16.3 Procedure

a) Place 40 grams of cement in a 1 Liter Squibb separatory funnel (NOTE 1) and mix
thoroughly with 250 mL of water added in 2 equal parts.

Shake vigorously immediately to produce complete decomposition. Then add the second
part and shake again.
At the same time quickly add 185 mL into which 10 grams of SnCl has been dissolved2
(NOTE 2) immediately close the funnel, invert the funnel and shake it in a circular motion
for a few seconds to loosen and disperse the cement, be careful to avoid large internal
pressure because too strong shaking is not needed.

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Release the internal pressure immediately by opening and closing the shut-off tap. Repeat
shaking and releasing pressure until the cement is completely broken down.
If necessary, break up any remaining lumps of cement with a glass stirring rod.
Cool to room temperature immediately by placing the funnel under a stream of tap
water.

NOTE 1 The use of grease to lubricate the shut-off tap and shut-off cup on the separation funnel
should be avoided. Wetting the cover cup with water before use will make the job easier.

NOTE 2 The purpose of adding SnCl2 is to avoid oxidation of sulphur sulphide to elemental
sulphur, which is soluble in chloroform.

b) Add 75 mL of chloroform to the solution, cover the separatory funnel, shake vigorously
for 5 minutes, and leave for 15 minutes to allow the water and chloroform to separate.
The chloroform layer at the bottom is removed and collected into a 125 mL Squibb
separatory funnel, including the foam (NOTE 3) and a few milliliters of water layer,
making sure all the foam layer is removed.

Try to keep the amount of water layer carried over as little as possible, as too much
excess water in the 125 mL separatory funnel can cause incomplete extraction of the
foam and possibly lead to an emulsion that is difficult to separate. Shake another 250 mL
separatory funnel containing 50 mL of water and a few drops of HCl.
Shake the separatory funnel the same as in the first 250 mL separatory funnel situation.
When the chloroform separates, pour it into a flat bottom boiling flask (NOTE 4), being
careful not to allow water to enter the boiling flask.

NOTE 3 It is usually foamy in appearance. It may contain organic compounds that dissolve in
chloroform after shaking in a separatory funnel, where the ratio of water to chloroform is large.
The foam may be concentrated and remain in a small volume by slowly rotating the separatory
funnel after the foam has flowed into the narrow part of the separatory funnel.

NOTE 4 Then the liquid is distilled, the cork or rubber cover should not be heated, a 250 mL or
300 mL soil analysis flask, equipped with a condenser tube can be used. The condenser tube has
a notch near the neck and a cooling water jacket. Chloroform obtained back can be used again as
in
7.1.3.16.2 item a).

c) Add 25 mL of chloroform to the solution in the original 1 liter separatory funnel, and
perform as in 7.1.3.16.3 item b) store the original wash water in a 250 mL separatory
funnel.
Repeat using 25 mL of chloroform. Distill the combined chloroform extracts in a boiling
flask until the volume is reduced to (10-15) mL. Filter the separated solution into a 100
mL beaker or platinum crucible (NOTE 5) of known weight through medium-porous filter
paper and then rinse with fresh chloroform.

NOTE 5 A platinum vaporizer cup is preferable as it is quicker to reach temperature equilibrium. If


a beaker is used, it should be allowed to reach equilibrium temperature for at least 20 minutes
before weighing.

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Rinse the flask and wash the filter paper with a little fresh chloroform several times.
Evaporate the extract at low temperature not more than 63o C to dryness (NOTE 6) and
heat in an oven at (57-63)o C for 3 min.

NOTE 6 Care should be taken during filtration of the extract as many organic compounds soluble
in chloroform evaporate when heated for too long even at moderate temperatures. If protected
from dust accumulation, the solution can be evaporated at room temperature if left overnight. If
rapid evaporation is desired, the solution can be evaporated on a hot plate at low temperature
while a stream of dry air is applied through a glass tube with an inner diameter of 10 mm and a
thickness of approximately 3 mm. Then remove the beaker from the hot plate and continue to flow
dry air slowly until the residue looks dry then continue with a faster flow of dry air for 5 minutes at
room temperature before the beaker is placed in the oven at (57 - 63)o C. Every 3 minute heating
period in the oven, pass hot air into the container for  15 seconds before weighing. Dry air can
be passed after going through a desiccant, such as calcium chloride or sulfuric acid, followed by a
high-efficiency desiccant, such as magnesium perchlorate or anhydrous calcium sulfate, taking
care to avoid dust from the desiccant being carried away by the air. In addition to using
compressed air, which is often contaminated with oil, dirt and water vapor, it is also possible to
place a chloroform solution under a glass lid and flow air through the drying material using an
aspirator or vacuum pump. If only insol resin is known to be present, the residue is more stable
and can be heated at (100-150)o C, but not at (57-63)o C when other unstable organic elements
are also present to remove all traces of chloroform that may remain.

Flow dry air into the container for 15 seconds, cool and weigh.
Repeat heating and weighing until 2 consecutive weighings the difference is not more
than 0.001 0 grams. The last two higher weighing results are taken as the actual weight.

7.1.3.16.4 Blangko

Make a blanket determination. Incinerate 40 grams of cement sample at a temperature of


(950 - 1 000)o C for 1 hour and grind again. Treat the sample that has been incinerated using
the same procedure and amount of reagent in the analysis, correct the results obtained.

NOTE Be careful to work so that organic compounds burn completely. Spread the sample in a 100 mL
platinum vaporizer cup and it is recommended that a muflle furnace is not available, a high
temperature Maker type burner can be used. Complete stirring of the sample must be done
periodically every 5 minutes if using a burner.

7.1.3.16.5 Calculations

Calculate the percentage of organic compounds soluble in chloroform to an accuracy of


0.001 by multiplying the sample weight in grams of the residue by 2.5 (100 divided by the
sample weight used of 40 grams).

NOTE If the organic compound present in the cement is tallow, the residue is fatty acids derived from
hydroxide of the tallow in hot acid solution and the weight should be multiplied by 1.05 to obtain the
actual weight of glycerides in the tallow. If the preganic compound is calcium stearate, the residue is
stearic acid, and the weight is multiplied by 1.07 to obtain the actual weight of the calcium stearate.

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7.1.4 Alternative test method (Optional)

7.1.4.1 Calcium oxide

7.1.4.1.1 Test method summary


The test method includes gravimetric determination of CaO is SiO2 and ammonium hydroxide
groups are separated, followed by precipitation of calcium as oxalate.
The precipitate was converted to CaO by emission and weighed.
Strontium, usually present in Portland cement as a minor element, precipitates with calcium
as Oxalate and is thereafter calculated as CaO. If the SrO content is known and correction of
CaO for SrO is desired for example, for research purposes or to compare results with SRM
certificate values, CaO obtained by this test method can be corrected by subtraction of the
SrO percentage.
In the determination to meet cement specifications SrO correction for CaO is not necessary.

7.1.4.1.2 Procedure

NOTE 1 Where analysis is carried out to meet the specification it is likely that manganese is present in
sufficient quantities to cause the percentage determination of magnesium by the alternative test
method to exceed the specification requirements, Manganese shall be separated as described in
7.1.3.9.3 item b) prior to the determination of CaO by the alternative method.

Acidify the combined filtrates from the ammonium hydroxide group determinations in
7.1.3.3.1 to 7.1.3.3.4 as necessary, condensing to a volume of approximately 200 mL.
Add 5 mL of HCl, a few drops of methyl red indicator solution and 30 mL of warm Ammonium
oxalate solution (50 g/L) (NOTE 2). Heat the solution at (70-80)0 C and add NH4 OH (1+1)
dropwise with stirring until the color changes from red to yellow (NOTE 3).

NOTE 2 If the ammonium oxalate solution is not clear, it should be filtered before use.

NOTE 3 This neutralization should be carried out slowly, otherwise the calcium oxalate precipitate
tends to escape through the filter paper. If a number of these determinations are made simultaneously
the following technique may help to ensure slow neutralization. Add 2 or 3 drops of NH 4 OH to the first
beaker while stirring, then 2 or 3 drops to the second beaker, and so on, returning to the first beaker
with the addition of 2 or 3 more drops until the color of the indicator in each beaker changes.

Leave the solution without further heating for 1 hour (no more), with occasional stirring during
the first 30 minutes. Filter using fine filter paper and wash moderately with cold ammonium
oxalate solution (1 gram/L). Save the filtrate and washing water.

Transfer the precipitate and filter paper to the original beaker. Dissolve the oxalate precipitate
in 50 mL of hot HCl (1+4) and destroy the filter paper. Dilute to 200 mL with water, add a few
drops of methyl red indicator and 20 mL of ammonium oxalate solution, heat the solution to
almost boiling, and precipitate the calcium oxalate again by means of the acid solution
equipment with NH4 OH solution as described in 7.1.3.9.3 item a).
Leave the solution 1-2 hours, filter and wash as before.

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Combine the filtrates obtained and save for the determination of MgO according to
7.1.3.10.3, dry the precipitate in a lidded crucible of known weight.
Char the paper without flame, burn the carbon at the lowest possible temperature, finally
incandesce it with a tightly closed crucible in an electric furnace at a temperature of (1 100 - 1
200)o C.
Cool in a desiccator and weigh as CaO. Repeat
emulsification until the weight remains.

7.1.4.1.3 Blangko

Make a blanket determination, using the same procedure and amount of reagents in the
analysis and correct the results obtained.

7.1.4.1.4 Calculations

Calculate the percentage of CaO to an accuracy of 0.1 by multiplying the weight in grams of
CaO by 200 (100 divided by the weight of the sample used 0.5).
Correct with % CaO to SrO, if desired, by subtracting percent SrO.

7.1.4.2 Magnesium oxide volumetric method

7.1.4.2.1 Test method summary

This test method is a volumetric procedure suitable for use when the determination of silicon
dioxide (SiO2 ), aluminum oxide (Al O23 ), iron(III) oxide (Fe O23 ), and calcium oxide (CaO) is
neglected.

7.1.4.2.2 Reagents
a) Ammonium nitrate solution (20 grams NH4 NO3 /L)
b) Ammonium oxalate solution (50 g/L)
c) Hydroxyquinoline solution
- Dissolve 25 grams of 8-hydroxyquinoline in 60 mL of acetic acid.
- When the solution has dissolved completely, dilute to 2 Liters with cold water.
- A milliLiter of this solution is equivalent to 0.001 6 grams of MgO.
d) Potassium bromate-potassium bromide standard solution (0.2 N)
- Dissolve 20 grams of potassium bromide (KBr) and 5.57 grams of Potassium bromate
(KBrO3 ) in 200 mL of water and dilute to 1 Liter.
- Determine the concentration ratio of this solution to the 0.1 N Na S O223 solution in
7.1.4.2.2 item e) as follows:
• To 200 mL of water in a 500 mL Erlenmeyer flask add 25.0 mL of 0.2 N KBrO3 -
KBr solution.
• Add 20 mL HCl, shake, and immediately add 10 mL Potassium iodide (KI) (250
g/L).
• Shake and titrate immediately with Na S O223 solution until the solution is almost
colorless. Add 2 mL of starch solution and titrate until the blue color disappears.

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- Calculate the concentration ratio of KBrO3 -KBr solution to Na S O223 solution by
dividing the volume of Na S O223 solution by the volume of KBrO3 -KBr used in the
titration.
e) Potassium iodide standard solution (0.1 N)
- Dissolve 25 grams of sodium thiosulfate (Na S O223 .5H2 O) in 200 mL of water, add
0.1 gram of sodium carbonate (Na2 CO3 ), and dilute to 1 liter.
- Leave for at least 1 week. Immediately standardize this solution against the primary
standard Potassium bichromate (K2 Cr O27 ). One milliLiter of 0.10 N Na S O223
solution is equivalent to 0.000 504 grams of MgO.
f) Starch solution
To 500 mL of boiling water add a cold suspension of 5 grams of soluble starch in 25 mL
of water, cool the solution to room temperature, add all the cold solution made from 5
grams of sodium hydroxide (NaOH) in 50 mL of water, add 15 grams of KI, and mix
thoroughly.

7.1.4.2.3 Procedure

a) Disperse 0.5 grams (NOTE 1) of cement sample in a 400 mL beaker with 10 mL of


water, while shaking, at the same time add 10 mL of HCl.

Dilute immediately to 100 mL.

Heat slowly and crush any coarse particles with a flat-tipped stir bar until completely
decomposed, add 2 or 3 drops of HNO3 and heat to boiling (NOTE 2).

NOTE 1 If SiO2 ammonium hydroxide group, and CaO are separated and determined in
accordance with the appropriate method, both the reference method and the alternative test
method, the filtrate that remains can be used for the determination of MgO as described in
7.1.4.2.3 item a) starting from the last sentence in 7.1.4.2.3 item c), i.e. "Add 5 mL HCl etc.". .

NOTE 2 In the case of cement containing blast-furnace slag or appreciable amounts of sulphur
sulphide, add 12 drops of HNO3 and boil for 20 minutes to oxidize the iron and remove the
sulphide.

b) Add 3 drops of methyl red indicator to the solution and then add NH4 OH until the
solution is yellow.
Heat the solution to boiling and continue boiling for (50-60) seconds. If difficulties arise
due to bumping in the boiling of the Ammonia solution, a period of 10 minutes on a
steam bath, or on a heating plate of the same temperature can be used instead of further
boiling for 50 seconds-60 seconds on a burner.
Remove from the burner, steam bath, or heating plate and allow it to settle.
Use medium-porous filter paper, immediately filter the solution, wash the precipitate
twice with hot NH4 NO3 (20 grams/L), and keep the filtrate.
Transfer the precipitate with filter paper to a beaker and dissolve with 10 mL HCl (1+1).
Crush the filter paper. Dilute to  100 mL and heat to boiling.
The precipitate is filtered again and wash the hydroxide as above.

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Combine filtrate and first settling wash water, keeping the volume not exceeding
300 mL (NOTE 3). Add 5 mL of HCl, a few drops of methyl red indicator solution and 30
mL of warm ammonium oxalate solution (50 g/L).
Heat the solution at (70-80)o C and add dropwise NH4 OH (1+1), while stirring, until the
color changes from red to yellow (NOTE 4).
Leave the solution without further heating for 15 minutes on a steam bath.

Add 10 mL - 25 mL of 8-hydroxyquinoline reagent (NOTE 4) and 4 mL of NH4 OH/100


mL solution. Stir the solution on a mechanical stirrer for 15 minutes, remove from the
heat and allow the precipitate to settle (NOTE 5).
Filter the solution using medium porous filter paper and wash the precipitate with NH 4
OH (1+40). Dissolve the precipitate with (50-75) mL of hot HCl (1+9) in a 500 mL
Erlenmeyer flask.
Dilute the resulting solution to 200 mL and add 15 mL of HCl.
Cool the solution to 25o C and add by pipette or burette (10-35) mL of 0.2 N KBrO3 - KBr
solution (NOTE 6).
Stir the solution and leave for about 30 seconds to ensure complete bromination.
Add 10 mL of KI (250 g/L). Stir the solution obtained well and titrate with 0.1 N Na S O223
solution until the iodine color becomes pale yellow. At this stage add 2 mL of starch
solution and titrate the solution until the blue color disappears.

NOTE 3 In case the cement contains blast furnace, or is considered to contain appreciable
Manganese, acidify with HCl, dilute to 100 mL, and separate the manganese, as described in
7.1.3.9.3 item a).

NOTE 4 An excess of 8-hydroxyquinoline reagent is necessary to avoid low MgO yields, but too
much will give higher yields.

The instructions below should be used to establish the amount of reagent added.

Table 7 ̶ Comparison of MgO content with the amount of reagents required


Estimated MgO Approximate amount of
content, reagent required, mL
%
0 - 1,5 10
1,5 - 3,0 15
3,0 - 4,5 20
4,5 - 6,0 25

NOTE 5 Within 1 hour the precipitate should be filtered. Any longer results in high yields.

NOTE 6Quantities of KBrO3 -KBr standard solution should use the following list
(requirements, not notes):

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Table 8 ̶ Comparison of MgO content with the amount of standard solution
Amount of KBrO3 - KBr
Estimated MgO content,
standard solution, mL
%
0-1 10
1-2 15
2-3 20
3-4 25
4-5 30
5-6 35

7.1.4.2.4 Blangko

Make a blanket determination, using the same procedure and amount of reagent, and correct
the results obtained in the analysis.

7.1.4.2.5 Calculations

Calculate the percentage of MgO with an accuracy of 0.1 as follows:

% MgO = E (V1 R - V2 ) x 200

Description:
E is the equivalence of MgO to Na S O223 solution,
grams/mL; V1 is the milliLiter of KBrO3 - KBr solution used;
R is the ratio of the strength of KBrO3 - KBr solution to Na S O223 solution; V2 is
the Na S O223 solution used, mL;
200 is 100 divided by the weight of the sample used (0.5 grams).

NOTE V1 R indicates the volume of Na S O223 solution equivalent to the volume of KBrO3 -KBr
solution used, V2 indicates the amount of Na S O223 .required by the excess KBrO3 -KBr not reduced
by magnesium oxyquinolate.

7.1.4.3 Titanium dioxide

7.1.4.3.1 Test method summary

The dioxide test method (TiO2 ) is determined colorimetrically by comparing the color
intensity of the titanium peroxide solution in the sample with the color intensity of the titanic
sulfate book peroxide solution.

7.1.4.3.2 Disorder

The disturbing elements in the peroxide method for TiO2 are vanadium, molybdenum and
chromium. In small amounts they can cause interference to other elements in the cement
therefore melting with Na2 CO3 7.1.4.3.5 item d) and extraction with water is necessary.

7.1.4.3.3 Cholorim

eter Equipment
The equipment should consist of a colorimeter of the Kennicou or Duboscq type, or another
colorimeter or spectrometer designed to measure light transmittance, and usable for
measurements at wavelengths of 400 nm-450 nm.

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7.1.4.3.4 Reagents

a) Ammonium chloride (NH4 Cl).


b) Ammonium nitrate (NH4 NO3 20 grams/L).
c) Iron(II) sulfate solution (1 mL = 0.005 grams Fe O23 ).
Dissolve 17.4 grams of iron(II) sulfate (FeSO4 .7H2 O) in water containing 50 mL of H2
SO4 and dilute to 1L. One milliLiter is equivalent to 1% Fe O23 in 0.5 grams of sample.
d) Hydrogen peroxide (30%).
Concentrated hydrogen peroxide
(H O22 ).
e) Sodium carbonate (20 g/L Na2 CO3 ).
f) Sodium or potassium pyrosulfate (Na S O227 or K S O227 ).
g) Standard solution of titanic sulfate (1 mL = 0.000 2 g TiO2 ).
- Use standard TiO2 provided by the National Bureu of Standars (standard sample
154 or its substitute). Dry for 2 hours at (105-110)o C. Transfer TiO2 weighing (0.20-
0.21) grams to 125 mL philips beaker.
- Add 5 grams of ammonium sulfate ((NH4)2 SO4 ) and 10 mL of H2 SO4 to the beaker
and insert a short-stemmed glass separatory funnel into the mouth of the beaker.
- Heat the mixture continuously until it boils while the flask is rotated over the flame.
Continue heating until the solution is completely dissolved effectively and no part of
the material sticks to the walls of the flask.

NOTE Although there is a small amount of TiO residue2 , it will not interfere if this procedure
is carried out properly.
- Cool and immediately pour the solution into 200 mL of cold water while stirring
vigorously.
- Rinse the flask and funnel with H2 SO4 (1+19), stir, then let the solution and wash
water stand for at least 24 hours. Strain into a 1 liter volumetric flask, wash the filter
thoroughly with H2 SO4 (1+19), dilute to the limit with H2 SO4 (1+19), and shake.

Calculate the TiO equivalence2 , of titanic sulfate solution, grams/mL, as follows:

AB
E=
1 000

Description:
E is the equivalence of TiO2 , from a solution of Ti(SO )42 , grams/mL;
A is the gram of TiO2 , the raw material used (correction for loss on drying;
B is the percentage of rawTiO2 as stated in the certificate issued by the National
Bureau of Standards (NBS), divided by 100;
1 000 is milliliters of solution in a measuring flask.

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7.1.4.3.5 Procedure

a) Thoroughly mix 0.5 grams of cement sample and 0.5 grams of NH4 Cl in a 50 mL
beaker, cover the beaker with a watch glass, and carefully add 5 mL of HCl.
Let the acid flow down over the lip of the lidded beaker.
After the chemical reaction subsides, remove the cover, stir the mixture with a glass
stirring rod, re-cover (NOTE 1) during the pendigestant time, stir the contents once more
breaking up any lumps still present to facilitate complete decomposition of the cement.
Quickly place a medium-porous filter paper into the funnel and transfer the sediment
onto the filter paper. Rub the wall in the chemistry classroom with a rubber policeman
and rinse the beaker and policeman.
Wash the filter paper two or three times with hot HCl (1+99), and then with a little hot
water ten or twelve times, allowing the water to run off each time.

NOTE 1 A hot plate can be used instead of a steam bath. If the appliance is equipped with a
temperature control so that the heat generated is close to that of a steam bath.

b) Transfer the filter paper and residue to a crucible (NOTE 2), dry and gently incandesce
until the carbon from the filter paper burns completely without flame.
Treat the SiO2 obtained with 0.5 mL-1 mL of water, 10 mL of HF, and 1 drop of H2 SO4 ,
and evaporate carefully to dryness. (NOTE 3).

NOTE 2 When a shorter procedure is desired for purposes other than the referee test method,
usually with little regard to the rigor of the procedure such as 7.1.4.3.5 item b) may be omitted.

NOTE 3 When the determination of SiO2 is desired in addition to the determination of TiO2 , SiO2
may be treated with HF as in 7.1.3.2.1.3 to 7.1.3.2.1.4.

c) Heat the filtrate to boiling and add NH4 OH until the solution becomes completely
alkaline, indicated by an ammoniacal odor.
Add a small amount of filter paper pulp to the solution and boil for (50-60) seconds.
Allow the precipitate to form, filter through medium-porous filter paper, and wash twice
with hot NH4 NO3 solution (20 g/L).
Place the precipitate in a crucible where the SiO2 has been treated with HF and gently
incandesce it until the carbon from the filter paper is exhausted.

NOTE 4 When determination of the ammonium hydroxide group is desired in the addition at TiO2
temperature, precipitation and fumigation may be made as in 7.1.3.3.3 items a) to 7.1.3.3.3 item
d). However, the crucible should contain residues from the treatment of SiO2 with HF unless
circumstances permit to omit this as indicated in NOTE 58.

d) Add 5 grams of Na2 CO3 , to a crucible and melt for (10-15) minutes (see "Interference").
Cool, separate the melt from the crucible and transfer into a small beaker.

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Wash the crucible with hot water using rubber policemen. Digest the melt and wash until
the melt disintegrates then filter through 9 cm diameter medium porous filter paper and
wash several times with Na2 CO3 (20 grams/L).
Discard the filtrate, place the precipitate in a crucible and gently incandesce it until the
carbon from the filter paper is completely burned off. Add 3 grams of Na S O227 or K S
O227 to the crucible and heat to incandescence until the residue dissolves in the melt
(NOTE 5).
Cool and dissolve the fused pool in water containing 2.5 mL of H2 SO4 .
If necessary reduce the volume of solution (NOTE 6), filter into a 100 mL volumetric flask
through 7 cm diameter medium porous filter paper and wash with hot water. Add 5 mL of
H3 PO4 and cool the solution with water, and shake well.

NOTE 5 Start heating carefully as pyrosulfate (also known as fused bisulfate) splashes at the
start of heating due to H2 SO4 . Avoid unnecessarily high temperatures or prolonged heating as
the pyrosulfate fused can damage the platinum. Use pyrosulfate that does not splatter by
providing partial heating of the pyrosulfate in a crucible to remove excess H2 SO4 . and destroy
the cold fused mass.

NOTE 6 If the solution is evaporated to a small volume and allowed the contents to cool, it may
cause the sulfate precipitate to be difficult to redissolve. In the event of excessive evaporation, do
not allow the contents to cool, but add hot water and digest on a steam bath or need heating until
all the precipitate is redissolved, with the possibility of a small amount of insoluble SiO2 remaining.

NOTE 7 From time to time hydrogen peroxide will decompose. Its strength can be determined by
adding a certain amount to 200 mL of cold water and 10 mL of H2 SO4 . (1+1) and then titrated
with a standard solution of potassium permanganate (KMnO4 ) prepared according to 7.1.3.9.2
item b). If the standard solution contains 0.005 635 7 grams of KMnO4
/mL, then 49.5 mL of this solution is required by 0.50 mL of H O22 30%.

e) Prepare a reference standard solution of Ti(SO4 ) standard solution2 or a series of


reference standard solutions in a 100 mL volumetric flask, depending on the type of
colorimeter used.
To each solution, add 3 grams of Na S O227 or K S O227 dissolved in water, then add an
amount of Fe2 SO4 solution equivalent to Fe O23 containing 0.5 grams of cement, 2.5 mL
of H2 SO4 and 5 mL of H3 PO4 solution (NOTE 8). When the solution is at room
temperature, add 1.0 mL of 30% H O22 , dilute to the limit with water and shake well
(NOTE 9).

NOTE 8 The coloration caused by the Fe2 (SO )43 solution is partly the effect of the H2 SO4 ,
H3 PO4 and alkali salts on the iron ion and peritanic ion. The sequence must be followed to obtain
high accuracy. However, if a shorter procedure is desired for purposes other than referee
analysis, the addition of pyrosulfate, FeSO4 and H3 PO4 solutions to the comparison solution can
be omitted when Fe O23 in the cement sample is less than 5%. This may result in slightly reduced
precision.

NOTE 9 Color develops quickly and is stable for some time, but if the peroxide solution is left for
a long time, oxygen bubbles will appear and interfere with the color comparison. When the
contents of the first tube are swirled, fine bubbles may form which should be allowed to clear
before the comparison is made. The comparison between the standard solution and the sample
should be done not more than 30 minutes after the addition of H O22 .

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f) Compare the color, light transmittance or absorbance of the sample solution with the
reference standard solution.
The method of comparing colored solutions or measuring transmittance or absorbance
depends on the type of equipment (see 7.1.4.3.5 item g to 7.1.4.3.5 item i) and should
be in accordance with the manufacturer's instructions for use.
When the cement peroxide solution is compared to a single standard peroxide solution,
remember that this single standard solution cannot cover all the required TiO2 content
regions. The difference in volume or depth for the two liquids should not be more than
50% of the smallest price.
All solutions shall contain H2 SO4 , H3 PO4 , Fe2 (SO )43 and persulfate in the
concentrations specified, except where circumstances in accordance with NOTE 10 are
desired.

NOTE 10 Although there is a small amount of TiO residue2 , it will not interfere if this procedure is
carried out properly.

g) Kennicott type colorimeter


Using a piston (plunger) in a reservoir of standard peroxide solution, adjust the amount
of solution through which light passes until it gives the same color intensity as the
sample peroxide solution.

h) Duboscq type colorimeter


Raise or lower the torch from the bowl so that both solutions give the same color
intensity when viewed from above. Color comparison can be done visually or
photoelectrically.

i) A colorimeter designed to measure light transmittance


Measurements should be made at wavelengths of 400 nm-450 nm and can be made
either visually or photoelectively. In most colorimeters of this type, the equipment is
calibrated with a standard solution and the calibration curve shows the relationship
between light transmittance or absorbance and TiO content2 (which has been prepared
in advance).

7.1.4.3.6 Blangko

Make a blank determination, following the same procedure and amount of reagent and
correct the results obtained in the analysis.

7.1.4.3.7 Calculations

Calculate the percentage of TiO2 with an accuracy of 0.01. If a colorimeter designed to


measure the transmittance of light is used: read the percentage of TiO2 from the calibration
curve showing the relationship of light intensity to TiO content2 .
When the sample peroxide solution is compared with one of the reference standard
solutions, calculate the percentage of TiO2 as follows.
For kennicott type colorimeters:

%TiO2 = (100 VE/S) x (D/C)

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For the duboscq type colorimeter:

%TiO2 = (100 VE/S) x (F/G)

Description:
V is milliLiters of Ti(SO )42 standard solution in the standard peroxide
solution; E is the TiO2 equivalence of the Ti(SO )42 standard
solution, grams/mL;
S is the gram of sample used;
C is the total volume of the peroxide reference standard solution, mL;
D is the volume of peroxide reference standard solution comparable to the sample peroxide
solution, mL;
F is the depth of the reference standard peroxide solution through which light passes;
G is the depth of the sample peroxide solution through which the light passes.

NOTE The difference between D and C or between F and G should not exceed 50% of the
smallest price.

7.1.4.4 Phosphorus pentaoxide

7.1.4.4.1 Test method summary

In this method, phosphorus is determined volumetrically by precipitating phosphorus as


ammonium phosphomolybdate and diluting with NaOH and H2 SO4 .

7.1.4.4.2 Reagents

a) Ammonium molybdate solution


Prepare the solution in accordance with 7.1.3.5.3 item a).
b) Ammonium nitrate (NH4 NO )3
c) Potassium nitrate solution (10 g/L)
Dissolve 10 grams of potassium nitrate (KNO3 ) in water that is free of CO2 , dilute to 1
liter (water freed from CO2 by boiling).
d) Standard solution, sodium hydroxide (0.3 N)
- Dissolve 12 grams of sodium hydroxide (NaOH) in 1 liter of cold water that is free of
CO2 (water is freed from CO2 by boiling).
- Add 10 mL of fresh, filtered barium hydroxide (Ba(OH)2 ) saturated solution.
- Shake the solution regularly for a few hours, and filter.
- Take care of CO contamination2 from the air.
- Standardize the solution to potassium phthalic acid (sample standard No. 84) or
benzoic acid (sample standard No. 39) provided by National Berau Standards in
accordance with the instructions accompanying the standard material.
- Calculate the equivalence of phosphorus pentaoxide (P O25 ) from solution

(grams/L), as follows: E = N x 0.003 086

Description:
E is the equivalence of P O25 with NaOH solution,
grams/mL; Nadalah normality of NaOH solution;
0.003 086 is the equivalence of P O25 to 1N NaOH solution, grams/mL.

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NOTE The value of the solution is based on the assumption that phosphorus in cement is
precipitated as Ammonium phosphomolybdate (2(NH )43 PO4 , 12 MoO3 ) and the precipitate
reacts with the NaOH solution:

2 (NH )43 PO4 , 12MoO3 + 46 NaOH = 2 (NH )42 HPO4 + (NH )42 MoO4 + 23 Na2 MoO4 +
22 H2 O.

The number 0.003 086 is obtained by dividing the molecular weight of P O25 (141.96) by mm
46 (46 is the amount of NaOH in the reaction equation) and by 1 000 (the number of
milliliters in 1 liter). Since the actual composition of the precipitate is affected by the
precipitation conditions, it is therefore important to pay careful attention to the sequence of
procedures as described.

e) Sodium nitrite (NaNO2 50 g/L)

f) Standard solution, sulfuric acid (0.15 N)


Dilute 4.0 mL of H2 SO4 to 1 L with freshly boiled cold water. Standardize against the
NaOH standard solution. Determine the ratio of the concentration of H2 SO4 standard
solution to the volume of NaOH solution by dividing the volume of NaOH solution by the
volume of H2 SO4 solution used in the titration.

7.1.4.4.3 Procedure

a) Weigh (1-3) grams of sample (NOTE 1) and 10 g of NH4 NO3 into a 150 mL beaker.
Stir the mixture, add 10 mL of HNO3 , and stir rapidly, using a flat-tipped stir bar to break
up the cement lumps, until the cement is completely decomposed and the thick gel of
silica (SiO2 ) is broken.
Cover the beaker with a watch glass, place it on a water bath or heating plate at
approximately 100o C for (15-20) minutes, and stir the contents occasionally during
heating.
Add 20 mL of hot water to the beaker and stir the contents.
If the cement contains sufficient manganese to show a red or brown residue, add a few
milliliters of NaNO2 (50 g/L) to dissolve the residue.
Bring the contents of the beaker to a boil until all the nitrous vapor is gone.
This procedure should be carried out in no more than 5 minutes, and water should be
added to replace the part lost due to evaporation.
Filter, using medium-porous filter paper, into a 400 mL beaker under a suction and with a
platinum cone to support the filter paper. Wash the SiO2 residue with hot water until the
volume of filtrate and wash water is approximately 150 mL.

NOTE 1 The amount of sample and reagent used depends on the phosphorus content of the
cement. The minimum amount is required when the cement contains 0.5% P O 25 or greater. The
maximum amount is required when the specified level of P O25 is 0.1% or less.

b) Heat the solution at (69-71)o C, remove from the heat source, and immediately add (50-
100) mL of ammonium molybdate solution.
Stir the solution vigorously for 5 minutes, wash the inner side of the beaker with cold
KNO3 (10 g/L) solution, cover the beaker with a watch glass and leave for 2 hours.

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Using a suction, filter the precipitate (NOTE 2) decant the solution with as little
disturbance of the precipitate as possible. Stir the precipitate in a beaker with a stream of
cold KNO solution3 , decant the liquid, then wash the precipitate over the filter.
Rub the stirring bar and beaker with policeman, wash and pour the contents over the
filter. Wash the precipitate until acid-free (NOTE 3), allowing each addition of washing
solution to be completely sucked up before the next addition.

NOTE 2 The filter may be medium porous filter paper supported by a platinum cone or a small
hirsch funnel using suitably cut filter paper and a thin layer of acid-free washed pulp or asbestos
pulp. Filtering should be done with care that it has been washed acid-free. Screening should be
done carefully to avoid loss of sediment. The sieve should be absolutely precise, and suction
should be carried out before sieving and maintained until the washing is complete.

NOTE 3 Approximately 10 washes are expected. Test the 10th wash water with a drop of
phenophtalein indicator and one drop of NaOH standard solution. If a pink color appears and is
visible for at least 5 minutes, the precipitate is completely acid-free, otherwise the washing should
be continued.

c) Transfer the filter and sediment to the beaker used for settling, using small pieces of
damp paper to clean the funnel and remove any parts of the sediment that may be in the
funnel.
Add 20 mL of cold CO-free water2 to the beaker and crush the filter paper with the
policeman used to scrub the beaker.
Add excess 0.3 N NaOH solution, stir the contents of the beaker until the yellow color
spots disappear, wash the policeman and the beaker walls with 50 mL of cold CO-free
water2 , and add 2 drops of neutral phenolphatalein indicator solution.
Treat the solution with 0.15 N H2 SO4 solution, in a measured amount, sufficient to
completely remove the pink color.
Complete the titration with NaOH solution until a slight pink color persists for at least 5
minutes.

7.1.4.4.4 Blangko

Make a blank determination, following the same procedure and amount of reagent, correcting
the results obtained in the analysis.

7.1.4.4.5 Calculations

Calculate the percentage of P O25 to an accuracy of 0.01 as follows:

% P O25 = [E(V -V12 R)/S] x 100

Description:
E is the equivalence of P O25 to NaOH solution, g/L; V1
is the milliLiter of NaOH solution used;
V2 is the milliliters of H2 SO4 used;
R is the ratio of the strength of H2 SO4 solution to NaOH solution;
S is the gram of sample used.

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7.1.4.5 Manganese oxide

7.1.4.5.1 Test method summary

In the test method, manganese oxide is determined volumetrically by titration by potassium


permanganate solution.

7.1.4.5.2 Reagents

a) Potassium permanganate standard solution (0.18 N)


Prepare a solution of potassium permanganate (KMnO4 ) and treat as described in
7.1.3.9.2 item b), except that manganese oxide (Mn O23 ) solution equivalence is
calculated with potassium oxide (CaO) equivalence.
Calculate the equivalence of Mn2 O in solution as

follows: E = (B x 0.353 4)/A

Description:
E is the equivalence of Mn O23 to KMnO4 solution, g/mL; Bad is
the gram of Na C O224 used;
A is the milliLiter of KMnO4 solution required in the titration of Na C
O2240.353 4 is the molecular ratio of 3Mn23 to 10 Na C O224 .

b) Zinc oxide (ZnO) powder

7.1.4.5.3 Procedure

a) Place 2 grams of sample in a 250 mL beaker and add approximately 50 mL of water.


Stir the mixture until suspension occurs and then add 15 mL of HCl. Heat the mixture carefully
until the solution forms as completely as possible.
Add 5 mL of HNO3 and 50 mL of water to the solution and boil until some of the chlorine
has escaped.
If necessary, add hot water to maintain a volume of  100 mL.
Stop boiling and add ZnO powder to the solution until it is acid-free.
Add (3-5) grams of excess ZnO powder to the solution and boil for a few minutes.
b) Without filtering, and while keeping the solution heated (90-100)o C with intermittent or
continuous heating, titrate with 0.18 N KMnO4 standard solution, until the addition of 1
drop of KMnO4 causes a pink color that does not disappear anymore.
Near the end point of the titration, allow the precipitate to drop slightly, and observe the
color of the solution layer from the side of the beaker.

7.1.4.5.4 Blangko

Make a blank determination, following the same procedure and amount of reagent and
correct the results obtained in the analysis.

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7.1.4.5.5 Calculations

Calculate the percentage of Mn O23 to an accuracy of 0.01 as follows:

% Mn O23 = E V x 50

Description:
E is the equivalence of Mn O23 to KM On4 solution, grams/mL;
V is the milli liter of KMnO solution4 used;
50is 100 divided by the weight of the sample used (2 grams).

7.1.4.6 Free calcium oxide

7.1.4.6.1 Test method summary

This test method is a rapid way test to determine free calcium oxide in fresh slag.
If old cement or slag is used, the possible presence of calcium hydroxide should be kept in
mind, as this method does not distinguish between free CaO and free Ca(OH)2 .
Two test methods are provided. First, alternative test method A is a modification of the franke
procedure in which free lime is titrated with a dilute solution of perchloric acid after the
solution has been in an ethyl acetosdetate-isobutyl alcohol solvent.
Second, alternative test method B is the titration of ammonium acetate-alcohol glycerin
against free lime with Sr(NO )32 as an accelerant.

7.1.4.6.2 Franke modified test method (Alternative test

method A) 7.1.4.6.2.1 Equipment

a) Reflux equipment
Consists of a short-necked flat-bottomed Erlenmeyer flask, 250 mL capacity.
A water-cooled reflux condenser with a minimum length of 300 mm. The flask and the
reflux condenser are connected with a glass connector.
The reflux condenser should be equipped with an absorbent tube containing a desiccant,
such as silica gel, and a material for separating CO2 , such as ascarite.
The absorbent tube is attached by rubberizing the top of the reflux column.

b) Burette

The capacity is 10 mL and the scale should not be greater than 0.05 mL.

c) Vacuum filter equipment.

It consists of a Gooch cup of size No. 3, capacity 25 mL in which is placed a suitable


filter paper, size 21 mm, Walter cup holder, 500 mL suction flask and vacuum suction
source. The cup is filled halfway with compacted paper pulp.

d) Glass boiling stone granules.

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7.1.4.6.2.2 Solvents required

a) Ethyl acetoacetate-isobutyl alcohol solvent


Three volume parts of ethyl acetoacetate and 20 volume parts of isobutyl alcohol.
b) Thymol blue indicator
Dissolve 0.1 gram of thymol blue indicator powder in 100 mL of isobutyl alcohol.
c) Perchloric acid standard solution
- A 22 mL solution of perchloric acid (70 - 72) % to 1 L with isobutyl alcohol.
- Standardize this solution as follows: Incinerate 0.100 0 grams of calcium carbonate
primary raw material in a crucible at (900 - 1 000)o C.
- Cool the crucible and its contents in a desiccator and weigh with an accuracy of
0.000 1 gram to a fixed weight.
- Perform weighing quickly to prevent absorption of water and CO2 .
- Transfer the unmilled CaO immediately into a clean, dry erlenmeyer flask, and
reweigh the empty crucible to the accuracy of 0.000 1 gram, to determine the
amount of CaO added. Then follow the procedure starting with "Add 70 mL of ethyl
acetoacetate-isobutyl alcohol etc." from 7.1.4.6.2.3 item a).
- Calculate the equivalence of CaO to perchloric acid standard solution in grams per
milliLiter by dividing the weight of CaO used by the volume of perchloric acid
required for the titration.

7.1.4.6.2.3 Procedure

a) Weigh 1,000 grams of the pulverized sample and transfer it to a dry and clean 250 mL
Erlenmeyer flask.
Add four to five glass boiling stones.
Add 70 mL of the prepared ethyl acetoacetate-isobutyl alcohol solvent. Swirl the flask
until the sample is dispersed.

NOTE Careful smoothing of the sample is essential for the liberation of free lime grains which are
often trapped in the tricalcium silicate crystals in cement. However, contact of the sample with air
should be kept as small as possible to avoid carbonation of the free lime. In particular, direct
breathing into the sample should be avoided. The sample should be fine enough to easily pass a
no. 200 (75 µm) sieve but sieving is not recommended. If the sample is not tested immediately, it
should be stored in an airtight container to avoid unnecessary contact with air.

b) Connect the flask to the reflux condenser and treat the sample to boiling. Reflux for 15
minutes.
c) Separate the condenser flask, stopper it, and cool it immediately to room temperature.
d) Filter the sample and solution using vacuum equipment. Wash the flask and residue in
10-15 mL increments with isobutyl alcohol until the total volume of washing solution is 50
mL.
e) Add 12 drops of thymol blue indicator to the filtrate and titrate with 0.2 N perchloric acid
until a clear color change occurs.

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7.1.4.6.2.4 Calculations

Calculate the percent of free calcium oxide with an accuracy of 0.1%:

EV x 100
% free CaO =
W

Description:
E is the equivalence of CaO to perchloric acid, grams/mL;
V is the milliLiter of perchloric acid solution required by the sample;
W is the weight of the sample, grams.

7.1.4.6.3 Sr(NO rapid test method )32 (alternative test

method B) 7.1.4.6.3.1 Reagents

a) Ammonium acetate standard solution (1 mL = 0.005 g CaO)


- Prepare a standard solution of ammonium acetate (NH C H4232 ) Oby dissolving 16
grams of ammonium acetate (previously stored in a desiccator) in 1 liter of ethanol
in a dry and clean closed botot.
- Standardize this solution by the same procedure as in 7.1.4.6.3.2 item a) except for
subsequent use as a sample substitute, incandescent to a fixed weight of ± 0.1
gram of CaCO3 with a platinum crucible at (900 - 1 000)o C. Cool the contents in a
desiccator and weigh to the accuracy of 0.000 1 gram.
- Weigh quickly to prevent absorption of water and CO2 . Immediately transfer the
unrefined CaO into a 250 mL boiling flask (containing glycerin-ethanol solvent and
Sr(NO )32 , and weigh the empty crucible again to determine the weight of CaO with
an accuracy of 0.000 1 gram.
- Proceed according to items 7.1.4.6.3.2 item a) and 7.1.4.6.3.2 item b).
- Calculate the equivalence of CaO to ammonium acetate in grams per milliLiter by
dividing the weight of CaO used by the volume of solution required.
b) Phenoltphalein indicator

Dissolve 1.0 gram of phenolpthalein in 100 mL of ethanol (formula 2 B)

c) Glycerin - ethanol solvent (1+2)


- Mix 1 part glycerin volume with 2 parts ethanol volume (formula 2 B).
- To each Liter of this solution, add 2.0 mL of phenolphthalein indicator solution.

NOTE Denatured ethanol according to formula 2 B (99.5% ethanol and 0.5% benzol) is
preferable but can be substituted with reagent grade isopropyl alcohol.

d) Strosium nitrate Sr(NO )32 , reagent grade.

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7.1.4.6.3.2 Procedure

a) Transfer 60 mL of glycerin-ethanol solvent into a 250 mL flat bottom boiling flask, clean
and dry.
Add 2 grams of anhydrous strontium nitrate (Sr(NO )32 ), and adjust the solvent to a
slightly alkaline state by dropwise addition of dilute and fresh NaOH solution in alcohol
until a slightly pink color is formed.
Weigh 1,000 grams of pulverized sample into a flask, insert a magnetic stirring rod, and
immediately connect it to a water-cooling condenser (using a 24/40 connecting cup).

NOTE Denatured ethanol according to formula 2 B (99.5% ethanol and 0.5% benzol) is preferable
but can be replaced with reagent grade isopropyl alcohol.
Simmer the solution in the flask on a magnetically stirred hot plate for 20 minutes at a
medium stirring speed.

b) Remove the condenser and filter the contents of the flask with a polypropylene buchner
funnel under suction, using a 250 mL flask with tubular sides to filter.
Treat the filtrate to boiling and immediately titrate with ammonium acetate standard
solution until the end point of the titration is colorless.

7.1.4.6.3.3 Calculations

Calculate the percent of free calcium oxide with an accuracy of 0.1% as follows:

% free CaO = EV x 100

Description:
E is the equivalence of CaO to ammonium acetate solution, grams/mL;
V is the milliLiter of ammonium acetate solution required by the sample.

7.2 Physics test method

7.2.1 Auxiliary materials and equipment

7.2.1.1 Auxiliary materials

a) The temperature of the testing room is set at (23 ± 1.7)o C, while the humidity of the
relative humidity test laboratory room is not less than 50%.
b) What is meant by a humid room is a room with a relative humidity of around 95%.
c) If water is used in the test, then water means distilled water.
d) By cold water, we mean water that has a room temperature.
e) Measurement of the amount of water is sufficient with a measuring cup that has a scale
division of 1 mL.
f) Weighing with accuracy to 0.01 grams must be carried out with scales with a capacity
of at most 500 grams.
g) Weighing with accuracy to 10 grams must be carried out with scales with a capacity
of at most 5 000 grams.

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7.2.1.2 Equipment

a) Standard sieve size 150 um (no. 100) and 850 um (No. 20)
Wire mesh for standard sieves should be made of brass, bronze or suitable wire. The
wire is fixed firmly to the frame to a depth of 50 mm from the top of the frame.
The joints between the frame and the wire mesh should be filled with solder to prevent
cement from remaining in the joints.
The strainer frame should be round with a diameter of 203 mm equipped with a pan and
cover.

b) Scales
Analytical scales have a capacity of no more than 200 grams with an accuracy of 0.000
1 or scales with a constant load and can be read directly. Scales must be able to
produce repeat readings with a difference of no more than 0.000 2 grams and must have
an accuracy of 0.000 2 grams. Scales with direct reading must have a sensitivity of no
more than 0.000 1 gram. Conventional scales with 2 pans must have a maximum
difference of 0.000 3 grams if weighing is done with pan exchange.

c) Weighing stone
Weighing stones must be checked at least once a year or if necessary readjusted at
least within the tolerances permitted for class III. For this purpose, each laboratory must
be able to maintain accuracy or must have standard weighing stones from 50 grams to
10 mg that comply with at least class III specifications and must calibrate them.

d) Brush
A soft-bristled brush is required for the purpose of cleaning the 150 um (No. 100) sieve.

7.2.2 Smoothness testing with blaine tool and turbidimeter

7.2.2.1 With the blaine tool

Testing with the blaine tool aims to determine the fineness expressed in the specific surface
area of Portland cement, calculated as the sum of the total surface area cm 2 /gram, or m2 /kg
of Portland cement.

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7.2.2.1.1 Equipment

(1) Blaine tool


The blaine tool basically consists of a device that draws a certain amount of air through a
prepared portland cement base with a certain porosity, which is a function of particle size
and determines the air flow rate through the base.
This tool is shown in Figure 3 and consists of the following parts:
a) Cell permeability
The permeability cell consists of a rigid cylinder with an inner diameter of (12.70 ±
0.10) mm fabricated from austenitic stainless metal.
i. The inside of the cell should be smooth (0.81 um fineness)
The top of the cell should be perpendicular to the main axis of the cell.
The bottom of the cell must be able to form an airtight connection with the upper
end of the manometer, so that no air leakage occurs between the contact areas.
ii. The ledge is (0.5-1.0) mm wide and is the part of the cell that attaches firmly to
the cell, at a distance of (55 ± 10) mm, from the top of the cell to hold the
perforated metal disk.
The top of the permeability cell should be equipped with a protruding outer part,
to facilitate the removal of the cell from the manometer.
b) Plates
i. The disk is made of stainless metal with a thickness of (0.9 ± 0.1) mm
perforated with (30-40) holes with a diameter of 1 mm and spread evenly.
ii. The disk should fit inside the cell, the center of one side of the disk should be
marked or scratched legibly, so that the tester always knows to stick that side at
the bottom when inserting it into the cell.
c) Torak
i. The piston is made from austenitic stainless steel which must fit precisely into
the cell with a tolerance of no more than 0.1 mm.
ii. The base of the piston must be perfectly flat and perpendicular to the main axis.
iii. The piston must be equipped with an air vent, which is a flat section of (3.0 ±
0.3) mm wide on one side.
iv. The top of the piston is equipped with a protruding outer part, so that when the
piston is inserted into the cell and the protruding part of the cell contacts the top
of the cell, the distance between the base of the piston and the top of the disk
should be (15 ± 1) mm.
d) The filter paper should have medium airflow resistance, be circular with flat edges
and have a diameter equal to the inner diameter of the cell.

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e) Manometer
The manometer is made from a U-shaped glass tube with an outer diameter of 9
mm, as shown in Figure 3.
The top of one of the arms should form an airtight connection with the permeability
cell. The manometer arm to which the permeability cell is connected shall be
marked by a line encircling the tube at a distance of (125-145) mm below the top
discharge, and also by other lines at a distance of (15 ± 1) mm, (70 ± 1) mm, and
(110 ± 1) mm above this line.
The discharge should be placed at a distance of (250-305) mm above the base of
the manometer, used for emptying the air in the manometer arm connected to the
permeability cell.
The manometer shall be equipped with a positive airtight valve or clamp located at a
distance of not more than 50 mm from the manometer arm.
The manometer should be firmly fixed in such a way that both arms are
perpendicular.

Figure 3 ̶ Blaine tool

f) Manometer fluid
The manometer should be filled to the center line of the tube with a non-volatile,
non-hygroscopic, low viscosity and density liquid, such as dibutyl pthalate (dibutyl
1,2 benzene dicarboxylate) or a light mineral oil.

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g) Timekeeping device
Timekeeping devices must be equipped with buttons for starting and stopping, and
must be readable to 0.5 seconds or less.
For time ranges from 0 seconds to 60 seconds. Timekeepers should have a
maximum accuracy of 0.5 seconds, and for time spans between 60 seconds and
300 seconds should have an accuracy of 1% or less.

(2) Other equipment.


a. A suitable small funnel.
b. Small fluffy brush (No. 7).
c. Weighing cup.
d. Analytical balance that conforms to specifications.

7.2.2.1.2 Tool calibration

7.2.2.1.2.1 Example of standard cement

For calibration of the blaine tool, standard cement from NIST, Standard Reference Material
No. 114 must be used. The cement sample must first be adjusted to room temperature.

7.2.2.1.2.2 Determination of cement layer (bed) volume


Determination of the volume of the cement layer is done by transferring mercury as follows:
a) Place two circular pieces of filter paper in a cell slightly smaller in diameter than the cell,
until all the filter paper is flat on the metal disk then fill the cell with mercury, ACS grade
or better, to remove air bubbles attached to the cell wall.
Use tweezers (pliers) when carrying the cell. If the cell is of a material that will be
amalgamated with mercury, the inside of the cell should be given a very thin protective
layer of oil before adding the mercury.
Then fill the cell with mercury.
Smooth the surface with the top edge of the cell using a glass plate pressed gently
against the mercury surface, until you are sure there are no air bubbles or voids between
the mercury surface and the glass plate.
Remove the mercury from the cell, weigh and record the weight.
Remove one of the filter papers from the cell, then place a layer of cement on top of the
remaining filter paper, which is made by inserting approximately 2.80 grams of cement
(standard cement is not required) and then placing the removed filter paper on top of the
cement.
Then press this cement layer with a piston until the piston neck contacts the cell surface.

NOTE The preparation of the cement paste should be compact. If it is too loose or the cement
cannot be pressed to the bottom with the desired volume, adjust the amount of cement used in
the experiment. The empty cell space above the cement layer is then filled with mercury, and
leveled as described above. Remove the mercury, weigh and record the weight.

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b) Calculate the volume of portland cement base to an accuracy of 0.005 cm3 with the
formula:

Wa - Wb ....................... (1)
V= D

Description:
V is the volume of the portland cement layer, cm3 ;
Wa is the weight of mercury required to fill the cell without the portland cement
layer, grams;
Wb is the weight of mercury required to fill the empty part of the cell occupied by
the portland cement layer, grams.
The density of mercury at the test temperature, grams/cm3 .

c) The determination of the volume of the Portland cement layer must be made at least
twice, and for each determination the cement layer is compacted separately. The cement
layer volume price used for the average calculation shall be derived from two
determination prices with a maximum difference of  0.005 cm3 . The ambient
temperature of the cell shall be recorded at the beginning and end of the experiment.

7.2.2.1.2.3 Sample preparation

Put a sample of standard cement from the ampoule into a bottle whose volume is
approximately 120 cm3 shake vigorously for two minutes to break the clots. Leave the bottle
standing and closed for two minutes, then open the lid and stir gently, to even out the
particles that must be homogenized.

7.2.2.1.2.4 Standard sample weight

The weight of the standard sample for calibration shall be taken in such a way as to obtain a
standard cement layer having a porosity of 0.500 ± 0.005 and calculated by the formula:

W = ρ v (1 - e )... ...... (2)

Description:
W is the weight of the standard sample required, grams;
ρis the density of Portland cement test samples, the value used is 3.15 Mg/m3 or
3.15 g/cm3 ;
vvolume of standard cementitious coating determined in the manner described in
7.2.2.1.2.2, cm3 ;
e is the desired porosity of the standard cementitious layer (0.530 ± 0.005).

NOTE Porosity is the ratio of the volume of voids to the overall volume in a cementitious layer.

7.2.2.1.2.5 Preparation of cement layer


Place the metal disk at the bottom of the cell, place a filter paper on the metal disk and press
down with a rod whose diameter is slightly smaller than the diameter of the cell, so that the
disk and filter paper are in the right position.
Weigh a quantity of cement with accuracy to 0.001 gram whose weight is determined in
accordance with the aforementioned calculation, in item 7.2.2.1.2.4, and put it into the cell.

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Gently knock on the outer cell wall to flatten the cement layer inside. Place a piece of filter
paper on top of this cement layer and press with the piston until the piston neck contacts the
cell surface.
Pull the piston slightly upwards, rotate 90 degrees, press again and then slowly pull the
piston out of the cell.

7.2.2.1.2.6 Determination of permeability of cement layer


Each time the permeability of the cement layer is determined, a new filter paper should be used.
a) Connect the permeability cell to the manometer tube with an airtight connection in such a
way that it does not disturb the prepared cement layer (NOTE 1).

NOTE 1 Apply a small amount of grease to the manometer connecting tap, close one arm of the
manometer, open it slightly and close it again. A continuous pressure drop indicates a leak in the
system.

b) Slowly remove the air in one of the manometer tubes until the manometer liquid reaches
the top line mark, then close the valve tightly.
c) Run the timer when the bottom of the liquid miniscus reaches the second line mark from
the top, stop when the bottom of the liquid miniscus reaches the third line mark. Record
the observed time span (seconds) and the test temperature (o C).
d) In calibrating the blaine device, make at least three flow time determinations, each time
using a different layer of standard cement. Calibration should be carried out by the same
tester who performed the fineness test (NOTE 2).

NOTE 2 Samples are cleaned of brush hairs and reused, provided they are kept dry and all tests
are carried out within 4 hours after opening the sample.

7.2.2.1.2.7 Recalibration
The blaine tool must be recalibrated when :
a) At a certain time span, which is necessary for correction of possible wear of the piston or
permeability cell.
b) There is a loss of fluid inside the manometer.
c) If other types and grades of filter paper are required.

NOTE It is recommended to prepare and use a secondary standard used as a fineness


standard to calibrate the tool between calibrations with standard cement samples.

7.2.2.1.3 Procedure

a) The temperature of the tested cement sample should be the same as the room temperature at
the time of testing.
b) The weight of the sample to be tested shall be equal to the weight of the standard
cement for calibration as described in 7.2.2.1.2.4, except when determining the fineness
of type III or other finer types of cement, where the weight of the contents is so great that
pressure with the thumb alone cannot cause the neck of the piston to contact the top of
the cell.
The required sample weight shall be such that the cement sample layer has a porosity of
0.530 ± 0.005.

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c) Preparation of cement layer
Preparation of cement in accordance with 7.2.2.1.2.2.
d) Permeability testing
Permeability testing in accordance with 7.2.2.1.2.6 except in determining the flow time
only once.

7.2.2.1.4 Specific face area calculation


a) The specific face area is calculated with the following formulas:

S Ts
S = .................................................................................................................... (3)
Ts

Ss T
S = ....................................................................................................................
s (4)
Ts 

S=Ss (b - e )s s T ........................................................................ (5)


e3
(b - e)
s3
e Ts

S=Ss (b - e )s e3 s T......................................................................... (6)



e s3 Ts
 (b-e)

S =Ss ρs (b - e )s e3 T .............................................................................. (7)


Ts
ρ(b - e) es 3

e3
s T
S = Ss ρs (b - e )s............................................................................................... (8)

ρ(b - e)es
3
Ts 

Description:
S is the specific surface area of the tested cement sample, cm2 /gram;
Ss is the specific surface area of the standard cement sample used in the calibration, cm2
/gram;
T is the time span of the pressure drop in the manometer for the tested portland cement
sample, seconds;
Ts is the time span of the pressure drop in the manometer for the standard cement
sample used in the calibration, seconds;
ηis the viscosity of air at the testing temperature of the cement sample under test, poise;
ηs is the air viscosity at the testing temperature of the standard cement sample used for
calibration, poise;
e is the porosity of the tested cement sample layer;
es is the porosity of the standard cement sample layer used in the calibration;
ρis the density of the standard cement sample tested (value set at 3.15);
ρs is the density of the standard cement sample used in the calibration (considered 3.15
mg/m3 or 3.15 grams/cm3 );
is a constant (for portland cement 0.9).

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NOTE  , and obtained from Tables 9, 10, and 11, respectively.
Rat
e3
e T

1. Equation (3) and equation (4) are used to calculate the fineness of the portland cement
sample that is packed to the same porosity as the standard cement sample used for
calibration.
Equation (3) is used when the experimental temperature differs by a maximum of 3o C from
the calibration experimental temperature and equation (4) when the experimental
temperature differs by more than 3o C from the calibration experimental temperature.
2. Equation (5) and equation (6) were used to calculate the fineness of portland cement
samples obtained to achieve porosity different from the standard cement samples used for
calibration.
Equation (5) is used when the temperature difference in the calibration experiment is a
maximum of 3o C and equation (6) is used when the temperature of the calibration
experiment differs by more than 3o C.
3. Equation (7) and equation (8) are used to calculate the fineness of materials other than
Portland cement. Equation (7) is used when the experimental temperature differs by ±3o C
from the calibration experimental temperature and equation (8) is used when the
experimental temperature differs by more than 3o C from the calibration experimental
temperature.
b) To calculate the specific surface area in m2 /kg, multiply the surface area in cm2 /gram by
a factor of 0.1.
c) Round prices in cm2 /gram to the nearest tenth while for m2 /kg round to the nearest
unity.
EXAMPLE 3 447 cm2 /gram rounded to 3 450 cm2 /gram or 345 m2 /kg.

7.2.2.1.5 Report

a) For cement and cement-based materials, a one-time determination is sufficient.


b) For each high-fineness material with a long time interval, report the average fineness of
the two permeability tests, provided that the difference is no more than 2%. If the
difference is outside the above provisions, repeat the test until the difference meets the
provisions.

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Table 9 ̶ Specific gravity of mercury, air viscosity (η) andη at a given temperature

Room Specific gravity of Air viscosity, η η


temper mercury (Mg/m (µPa.s)
ature (O )3
C)
18 13,55 17,98 4,24
20 13,55 18,08 4,25
22 13,54 18,18 4,26
24 13,54 18,28 4,28
26 13,53 18,37 4,29
28 13,53 18,47 4,30
30 13,52 18,57 4,31
32 13,52 18,67 4,32
34 13,51 18,76 4,33

Table 10 ̶ Porosity values of cementitious coatings


Porosity of cement layer e3
E
0,496 0,349
0,497 0,350
0,498 0,351
0,499 0,352
0,500 0,354
0,501 0,355
0,502 0,356
0,503 0,357
0,504 0,358
0,505 0,359
0,506 0,360
0,507 0,361
0,508 0,362
0,509 0,363
0,510 0,364
0,525 0,380
0,526 0,381
0,527 0,383
0,528 0,384
0,529 0,385
0,530 0,386
0,531 0,387
0,532 0,388
0,533 0,389
0,534 0,390
0,535 0,391

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Table 11 ̶ Air flow time range
T T T T T T T T T T T T
26 5,10 51 7,14 76 8,72 101 10,05 151 12,29 201 14,18
26,5 5,15 51,5 7,18 76,5 8,75 102 10,10 152 12,33 202 14,21
27 5,20 52 7,21 77 8,77 103 10,15 153 12,37 203 14,25
27,5 5,24 52,5 7,25 77,5 8,80 104 10,20 154 12,41 204 14,28
28 5,29 53 7,28 78 8,83 105 10,25 155 12,45 205 14,32
28,5 5,34 53,5 7,31 78,5 8,86 106 10,30 156 12,49 206 14,35
29 5,39 54 7,35 79 8,89 107 10,34 157 12,53 207 14,39
29,5 5,43 54,5 7,38 79,5 8,92 108 10,39 158 12,57 208 14,42
30 5,48 55 7,42 80 8,94 109 10,44 159 12,61 209 14,46
30,5 5,52 55,5 7,45 80,5 8,97 110 10,49 160 12,65 210 14,49
31 5,57 56 7,48 81 9,00 111 10,54 161 12,69 211 14,53
31,5 5,61 56,5 7,52 81,5 9,03 112 10,58 162 12,73 212 14,56
32 5,66 57 7,55 82 9,06 113 10,63 163 12,77 213 14,59
32,5 5,70 27,5 7,58 82,5 9,08 114 10,68 164 12,81 214 14,63
33 5,74 58 7,62 83 9,11 115 10,72 165 12,85 215 14,66
33,5 5,79 58,5 7,65 83,5 9,14 116 10,77 166 12,88 216 14,70
34 5,83 59 7,68 84 9,17 117 10,82 167 12,92 217 14,73
34,5 5,87 59,5 7,71 84,5 9,19 118 10,86 168 12,96 218 14,76
35 5,92 60 7,75 85 9,22 119 10,91 169 13,00 219 14,80
35,5 5,96 60,5 7,78 85,5 9,25 120 10,95 170 13,04 220 14,83
36 6,00 61 7,81 86 9,27 121 11,00 171 13,08 222 14,90
36,5 6,04 61,5 7,84 86,5 9,30 122 11,05 172 13,11 224 14,97
37 6,08 62 7,87 87 9,33 123 11,09 173 13,15 226 15,03
37,5 6,12 62,5 7,91 87,5 9,36 124 11,14 174 13,19 228 15,10
38 6,16 63 7,94 88 9,38 125 11,18 175 13,23 230 15,17
38,5 6,20 63,5 7,97 88,5 9,41 126 11,22 176 13,27 232 15,23
39 6,24 64 8,00 89 9,43 127 11,27 177 13,30 234 15,30
39,5 6,28 64,5 8,03 89,5 9,46 128 11,31 178 13,34 236 15,36
40 6,32 65 8,06 90 9,49 129 11,36 179 13,38 238 15,43
40,5 6,36 65,5 8,09 90,5 9,51 130 11,40 180 13,42 240 15,49
41 6,40 66 8,12 91 9,54 131 11,45 181 13,45 242 15,56
41,5 6,44 66,5 8,15 91,5 9,57 132 11,49 182 13,49 244 15,62
42 6,48 67 8,19 92 9,59 133 11,53 183 13,53 246 15,68
42,5 6,52 67,5 8,22 92,5 9,62 134 11,58 184 13,56 248 15,73
43 6,56 68 8,25 93 9,64 135 11,62 185 13,60 250 15,81
43,5 6,60 68,5 8,28 93,5 9,67 136 11,66 186 13,64 252 15,87
44 6,63 69 8,31 94 9,70 137 11,70 187 13,67 254 15,94
44,5 6,67 69,5 8,34 94,5 9,72 138 11,75 188 13,71 256 16,00
45 6,71 70 8,37 95 9,75 139 11,79 189 13,75 258 16,06
45,5 6,75 70,5 8,40 95,5 9,77 140 11,83 190 13,78 260 16,12
46 6,78 71 8,43 96 9,80 141 11,87 191 13,82 262 16,19
46,5 6,82 71,5 8,46 96,5 9,82 142 11,92 192 13,86 264 16,25
47 6,86 72 8,49 97 9,85 143 11,96 193 13,89 266 16,31
47,5 6,89 72,5 8,51 97,5 9,87 144 12,00 194 13,93 268 16,37
48 6,93 73 8,54 98 9,90 145 12,04 195 13,96 270 16,43
48,5 6,96 73,5 8,57 98,5 9,92 146 12,08 196 14,00 272 16,49
49 7,00 74 8,60 99 9,95 147 12,12 197 14,04 274 16,55
49,5 7,04 74,5 8,63 99,5 9,97 148 12,17 198 14,07 276 16,61
50 7,07 75 8,66 100 10,00 149 12,21 199 14,11 278 16,67
50,5 7.11 75,5 8,68 100,5 10,02 150 12,25 200 14,14 280 16,73

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7.2.2.2 With a turbidimeter

7.2.2.2.1 Equipment

7.2.2.2.1.1 Standard equipment

The main Wagner turbidimeter consists of a light source maintained at a fixed intensity and
arranged so that a parallel beam of light passes through the cement suspension under test
and strikes a sensitive photoelectric plate. The electric current generated by the cell is
measured by a microammeter and the reading indicated is a measure of the turbidity of the
suspension. Primary estimates indicate that turbidity is an intermediate measurement of the
surface area of the suspended cement sample. The apparatus shall consist of the specific
parts described in 7.2.2.2.1.2 to 7.2.2.2.1.7 and shall be arranged in accordance with the
complete design and dimensional requirements shown in Figure 4 to Figure 7 and Table 12,
except for those made of wood or metal.

Figure 4a ̶ Front view of the turbidimeter with the door open

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̶ Front view of turbidimeter with door open

Figure 5 - Turbidimeter rear view

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Figure 7 - Turbidimeter electrical


Figure 6 - Time burette

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Table 12 ̶ Turbidimeter equipment dimensions
Units in millimeters
Image description Dimensions
A 445
B 438
C 381
D 105
E 3,0
F 28,6
G 85,7
H 33,3
I 102
J 39,7
K 55,6
L 65,1
M 28,6
N 3,0
O 51
P 51
Q 3,0
R 61,1
S 69,8
T 51
U 22,2
V 34,9
W 13
X 38
Y 15,9
Z 38 ± 0,76
AA 51 ± 2,5
AB 267
AC .....
AD ......
E 39,7
AF 55,6
AG 66,7
AH 203
AI 23,6
AJ 1,38 A
AK cmA
NOTE
A
The number is the actual number that is part of the goal and the
number that connects the parts;
is consequently unrelated to the column heading.

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7.2.2.2.1.2 Turbidimeter

Installed in a wooden or metal box with the following fittings:

a) Light source
The light source in Figure 4b consists of an electric lamp with a filament concentrated
between (3-6) candela operated by a source with a constant emf. The lamp must be
firmly fixed in the socket. A clean and shiny parabolic metal reflector should be firmly
fixed opposite the lamp, focused such that approximately parallel beams of light pass
through the sedimentation tank and hit the photoelectric cell. The light intensity should
be regulated by means of two rheostats of approximately 6 ohms and 30 ohms and the
rheostats should be of such characteristics that uniform changes in light intensity are
obtained over the full range of resistance. The rheostats should be installed in parallel
with each other and in series with the lamp.

b) Heat-absorbing equipment

The light must pass through a heat absorbing equipment before entering the
sedimentation tank as long as the heat radiation from the light beam must be absorbed,
the equipment can be:
i. water cells or;
ii. special heat-absorbing glass filter.

The water cell should be made of seamless brass pipe having an outer diameter of 76
mm, wall thickness of 3 mm and length of 102 mm with a glass window glued at the end.
The cell shall have a hole for filling distilled water. The hole must be closed with a metal
plug. The cell when mounted on a movable stand shall have the cover either in the upper
or lower position. The heat absorbing equipment should be arranged so that all light rays
from the lamp enter the sedimentation tank through the heat absorbing equipment.

c) Tools for inhibitors

Glass for light reduction shall be provided to reduce the light intensity from 100 µA to 20
µA to 30 µA. The light intensity shall be reduced uniformly over the entire cell section
subjected to the light beam during the test. The inhibitor shall be mounted in a frame that
can be swung out of the light path using a holder.

d) Sedimentation tank

The sedimentation tank must be:

i. Plates of (5-6) mm glass or boro silicate glass cemented or glued together to


form a square tank or;
ii. A molded glass tank that has walls of approximately 5 mm thickness with a flat
surface.

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The dimensions of the tank should be 51 mm long, 38 mm wide and 203 mm high.
mm. Permissible variations for the inside dimensions of the tank are length ± 2.5 mm
and width ± 0.76 mm. The 51 mm face of the tank must have an equal clearance of 0.25
mm at all points. A mark shall be placed on the side of the tank to indicate the volume
content of 335 mL which is the limit of the tank content during the test. A tank filled with
clear kerosene up to the mark and placed in the light beam of the turbidimeter, will yield
a uniform microameter reading of ±0.1 μA, for the entire usable portion of the tank.

e) Photoelectric cell

The equipment used to measure light intensity should be a sensitive photoelectric cell
that is directly connected to the microameter. A horizontally slotted cover 13 mm high, 35
mm wide shall be fitted over the photoelectric cell. The front of the cover should be (25 ±
1) mm in front of the cell face. The cell face should be parallel to the tank face with a
distance of 0.5 mm.

f) Protector

The metal shield uses a slot 16 mm high, 38 mm wide. Should be placed between the
heat sink and the sedimentation tank.

g) Lifting device

The light source, heat absorber, photoelectric cell, filter blocker and shield shall be
assembled on a movable stand that can be raised or lowered by two interconnected
screws and can be accurately adjusted so that the turbidity of the suspension can be
determined at the desired depth. The center of the light source, heat absorbing
equipment, photocell, slot center of the metal shield, and cover must be in a straight line
parallel to the stand. The sedimentation tank should be mounted on a platform that is not
affected by the location of the equipment so that the tank can be free from vibration
caused by the movement of the stand. The stand shall be level at all elevation points and
the tank shall be normal to the stand. The distance between the tank and the opening
surface of the stand shall not vary by more than 0.4 mm between the "30 - 50" and "0"
positions. The level of the light beam with reference to the solution surface is indicated
by a pointer which will move along a scale mounted on the box. Point 0 of the scale
indicates the position where the center line of the hole for the light beam is at the same
height as the liquid surface in the tank when filled to the limit of 335 mL. The lines on the
scale marked 7.5; 10; 15; 20; 25; and 30 to 50 indicate the depth of suspension, h, in
Table 13. The scale when compared to a standard scale with an accuracy of 0.1 mm at
all points shall not show a deviation at any point greater than 0.25 mm and indicates the
position where the pointer was located when the turbidity reading for h was taken. The
interior of the turbidimeter cabinet and the outer mounting surface, parabolic reflector,
heat absorbing equipment, shield, photoelectric cell cover shall be painted using a solid
black color.

NOTE The 0-50 marking requirement on the scale is used only for new turbidimeters and not for
used equipment that meets the other requirements of this method.

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7.2.2.2.1.3 Microameter

a) D'Arsonval type microammeters have a range of 0 μA - 50 μA and must be readable to


0.1 μA. New microammeters must be accurate to ± 0.5% of the full scale value for the
value portion of the scale at 25o C. For microammeters already in use the accuracy shall
be the same as for new instruments except that the accuracy at 40 μA and 50 μA shall
be ± 1% of full scale. The internal resistance of the microameter is between 50 ohms
and 150 ohms. The microameter should not be installed on a work surface containing or
consisting of iron or steel, or near magnetic influences.

b) Digital microameter

NOTE An apparatus with a range of 199.9 μA can be used and allows the operator to read the
theoretical Io directly without the use of additional equipment. The high internal resistance of a digital
microameter should not affect the linearity of the readings at beam intensity levels encountered in
fineness determination using a Wagner turbidimeter.

7.2.2.2.1.4 Current source

A 6V car battery and an emergency light battery or emf source can be used as current
sources.

7.2.2.2.1.5 Sieve

The sieve shall meet the requirements of ASTM C 430-08, Standard Test Method for
Fineness of Hydraulic Cement by the 45-µm (No 325) Sieve.

7.2.2.2.1.6 Stirring equipment

The stirring equipment should consist of:


a) A cylindrical brush, with a diameter of 19 mm and a length of approximately 45 mm with
the tip approximately fitted around the base of the test tube with a diameter of 22 mm.
b) Other stirring equipment is equally efficient at dispersing as measured using specific
surface determination for a standard sample. The stirring equipment should rotate at a
speed of approximately 3 500 revolutions/minute.

7.2.2.2.1.7 Burette time

The settling time of particles of different sizes can be obtained using a burette filled with
kerosene. The burette should consist of a glass tube with a capillary pipe at the lower end.
The top of the burette should be large to serve as a funnel to feed kerosene into the tube.
The burette should meet certain dimensions given in Table 14. The lines on the burette
should be round (circular). A 45 μm wire filter (No. 325) can be used with the burette and the
burette should be closed when not in use.

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7.2.2.2.1.8 Scales

Must meet the requirements in 7.2.1.2 item b).

Table 13 ̶ Values of h, d and h/d2 used in calibration of turbidimeter equipment

Particle diameter, Suspension depthof, h


h/d2
d (µm) (cm)
50 15 0,006 00
45 15 0,007 41
40 15 0,009 38
35 15 0,012 24
30 15 0,016 67
25 13,1 0,0210
20 10 0,0250
15 6,6 0,0293
10 3,3 0,0330
7,5 2,1 0,0373

Table 14 ̶ Burette dimensions


Dimensi Allowable variation, cm
Descri on,
ption cm
Tube length (large) 38 ±4
Tube inner diameter (large) 1,9 ± 0,2
Capillary length 17,5 ± 2,5
Capillary diameter 0,09 ± 0,005
0 mark on the top of the burette 7 ±1

7.2.2.2.2 Material

Suspending liquid
Clear kerosene can be used for turbidimeter equipment. Kerosene must not be reused.

7.2.2.2.3 Test piece

Size of the test sample


Select the size of the cement sample for testing so that the initial microameter reading is
between 12 μA and 20 μA.

NOTE The following approximations will help quickly in sample size selection: 0.25 grams for
normal cement fineness and 0.2 grams for high cement fineness.

7.2.2.2.4 Turbidimeter calibration

Calibrate the turbidimeter equipment based on the procedure below:

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7.2.2.2.4.1 Calibrate the burette

For calibration of the burette scale, use kerosene of known viscosity and specific gravity at
the temperature at which the calibration is performed. The specific gravity and viscosity of the
kerosene must be determined. Calculate the flow time of the burette in relation to the settling
time for different particle sizes using the following equation:

t = [1 837 000η/(ρ1 - ρ2 )] x (h/d )2

Description:
t is the settling time or flow time in seconds;
η is the viscosity of kerosene at the calibration temperature, p;
ρ1 is the specific gravity of cement particles (grams/cm3 ) = 3.15 for Portland cement
(NOTE 1);
ρ2 is the specific gravity of kerosene at the calibration
temperature, Mg/m3 ; is the depth of suspension to light level in cm;
is the particle diameter, μm.
The h/d2 numbers are given in the Table of h, d and h/d2 values used in the
calibration of the Turbidimeter equipment (Table 13).

Fill the burette with kerosene at the calibration temperature, start time counting as soon
as the kerosene in the burette passes the zero point, and make marks on the burette
for the level reached with decreasing kerosene for each time interval, t, calculated as
described above. For these marks, place a permanent line and number on the burette
indicating the corresponding diameter (NOTE 2). The construction and distribution of
the burette shall be such that at the calibration temperature the time taken for the
kerosene to pass through the line on the burette corresponds to the settling time
calculated within 1%, except that the allowable variation shall not be less than 1
second.

NOTE 1 The specific gravity of Portland cement should not vary too much and for this work it is
estimated to have a fixed value of 3.15. A variation of 0.15 from this value when substituted
using Stoke's law gives a variation of 2.5% for the measured particle diameter.

NOTE 2 Using a calibrated burette, the apparatus can be used within the normal range of room
temperature without further correction, the change in kerosene flow rate from the burette
automatically compensating for the change in viscosity of the suspension. The temperature of
the suspension and kerosene in the burette should be maintained equal within 0.5o C. This
condition will exist if the supply of kerosene is maintained in the same room as the apparatus. It
is necessary to ensure that only clear kerosene is used in the burette, and in addition the
capillary tube should be checked frequently to ensure that there are no pieces of gauze or other
materials clogging in it.

7.2.2.2.4.2 Calibration of 45 μm sieve (No. 325)

Calibration shall be made using ASTM C 430-08, Standard Test Method for Fineness of
Hydraulic Cement by the 45-µm (No 325) Sieve, which is based on correcting the sieve
percentage on the difference between the test residual obtained and the resulting residual
value indicated by the electronically formed sheet sieve fineness specified for the standard
sample, expressed as a percentage of the test residual.

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7.2.2.2.4.3 Setting the right light intensity, Ir
a) Fill the sedimentation tank to the limit mark with clear kerosene.
b) For turbidimeters equipped with a digital microammeter with a range of 199.9 μA, place
a sedimentation tank containing clear kerosene on a tank stand in the turbidimeter. Set
the light intensity so that the microammeter reads 100.00 μA. Readjust the light
intensity until equilibrium is obtained at this reading. Place the filter blocker in the path
of the beam. When equilibrium is obtained, record the reading of the measuring
instrument as Ir . The gauge reading becomes the reference value for the beam
intensity. Measuring instrument readings are also taken at the beginning and end of
each test through the slow filter lamp itself to check the requirements of 7.2.2.2.5.2 item
(3)h).
c) For turbidimeters equipped with a D'Arsonval type microameter, place a sedimentation
tank containing clear kerosene on a tank stand in the turbidimeter. Set the beam
intensity such that the microameter reads 50.0 μA with the beam blocking filter
removed from the beam path. Readjust the beam intensity until equilibrium is obtained
at this reading. Connect a resistance or combination of resistances as illustrated in
Figure 4a so that the reading of the measuring instrument is reduced to a balance
value between 23.0 μA and 25.0 μA. Increase the beam intensity so that the balance
beam reading obtained between 23.0 μA and 25.0 μA is doubled for sure. Adjust the
beam intensity again until a balance is obtained at the reading level of the doubled
measuring instrument. Place the beam reduction filter on the beam path. Remove the
resistor from the measuring instrument circuit. When the balance is obtained, record
the reading of the measuring instrument as Ir . This value becomes the reference value
for the lamp intensity. Set the rheostat at the start of each test to give the gauge
reading through the filter plus a clean kerosene tank. This gauge reading corresponds
to a gauge reading of 100.00 μA through the tank of clean kerosene using the lamp
strainer removed from the lamp path. Gauge readings are also taken at the start and
end of each test through the self beam to check the requirements of 7.2.2.2.5.2 item
(3)h).

NOTE 1 A ½ watt carbon resistance with a 5% tolerance limit can be used to obtain the desired
gauge reading. The shunt resistance or combination resistance shown in Figure 4a has a
resistance value between 85% and 100% of the internal resistance value of the gauge printed
on the card inside the gauge cover. The series resistance has a resistance value equal to the
difference between the internal resistance of the measuring instrument and the calculated
resistance of the measuring instrument and the shunt combination.

NOTE 2 An uncertain but acceptable test method for determining the gauge setting
corresponding to a current of 100.0 μA through the gauge with the beam filter removed from the
beam path can be obtained by removing the series resistance in the gauge circuit. The inner
resistance of the photocell is large enough to cause a small error of approximately 0.5% of the
desired setting when series resistance is omitted from the circuit.
d) Example: When the internal resistance of the instrument is 90 ohms, and the
measuring instrument is coupled with a 470 ohm resistance parallel to the 100 ohm
resistance, the combined resistance of the measuring instrument and the displacer, will
be reduced to 43 ohms. This will reduce the reading of the measuring instrument, from
50.0 μA to the calculated value of 23.9 μA.

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7.2.2.2.4.4 Determination of the K value in the specific surface equation

Determine the value of K in the specific surface equation in 7.2.2.2.7 item (1) by dividing the
specific surface of the given standard sample by the value obtained for the statement in [ ].
Repeat this calibration procedure 2 more times. Average the three K value results.

7.2.2.2.4.5 Calibration frequency

The turbidimeter should be calibrated 6 months prior to the cement sample test.

NOTE The three K values (before averaging) established during calibration should not vary by more
than 1.5% from their average value.

7.2.2.2.5 Procedure

7.2.2.2.5.1 Sieve designation

Place 1 gram of cement sample on sieve no. 325 (45 μm). Record the percentage of cement
passing the sieve as r.

7.2.2.2.5.2 Suspension preparation

(1) Sample dispersion


a) Place the semen sample into the test tube together with (10-15) mL of kerosene
and 5 drops of dispersing agent i.e. oleic acid or long-stored lin oil (NOTE 1).
b) Stir the mixture for 1 minute with a stirrer.
c) Then transfer it to the sediment tank
d) Wash the stirrer and tubes and tubes with clear kerosene and put the wash into the
sediment tank.
e) Add kerosene to the tank to exactly 335 mL (NOTE 2).

NOTE 1 Oleic acid shall be of a grade with a b.j between (0.948 - 0.953) grams/cm3 . The
dispersing agent should be light and have little or no effect on the viscosity of the kerosene.
The dispersing agent will change when stored for a long time or exposed to heat or light.
Therefore, it should be stored in dark-colored glass bottles and sealed. Dropper bottles
should be emptied, cleaned, dried and refilled periodically. When oleic acid is no longer
able to disperse or when foam appears in the suspension (there may be a little water in the
kerosene), long-stored lin oil should be used as dispersing agent. The same dispersing
agent should be used for tool calibration and fineness determination.

NOTE 2 It is important that the liquid limit in the tank is equal to the 0 mark on the
apparatus, this corresponds to a suspension volume close to 335 mL. This can be obtained
by using a measuring cup calibrated to obtain 335 mL of the entire kerosene boost
suspension volume; or by using a meter consisting of a flat plate approximately (50 - 63)
mm to the center to which is vertically attached a metal pin of a specified length, when the
plate is placed in position above the tank, the pin point is at the 335 mL level. Both
methods should ensure that the liquid limit is within 1/10 mm.

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(2) Stirring of the suspension
Immediately before placing the tank into the light beam path, shake it to distribute the
suspension evenly. Cover the tank with the glass lid and move 180° about the horizontal
axis through the center of the tank, rotating the tank up and down approximately every
second for 1 minute (NOTE 3). Be careful not to allow kerosene to escape (NOTE 4).
The suspension is ready to be placed in its holder in the path of the light beam.

NOTE 3 The procedure described for stirring the suspension should be followed carefully. The
procedure for mixing drinks should not be followed.

NOTE 4 The tank lid should be tight so that no kerosene flows off the tank surface. The surface of
the glass tank should be clean when the suspension is added, and care should be taken to avoid
unnecessary cleaning until the determination is complete.

(3) Turbidimeter operating procedure


Operate the turbidimeter equipment according to the following working procedure:
a) Using a slow filter in a sedimentation tank containing approximately 100 mL of clear
kerosene in a light path, set the light intensity Ir as described in the light intensity
setting procedure Ir by repeating the readings at 1 minute intervals until no change in
the reading occurs indicating that the lamp and photoelectric cell are in equilibrium.
Remove the tank, check and record the light intensity.

NOTE 5 To protect microameters, the lamp is only switched on when the suspension or slow
light intensity reducing filter is at the microameter range value. The chargeable battery
should be disconnected occasionally to reduce the voltage to a fixed value. If the
microameter shows continuous fluctuations, check for broken lamp cables and photoelectric
cell circuits, see that the rheostat connections are clean, and make sure that the lamp,
socket and reflector are properly seated.
b) Weigh a sample of cement to a specified weight, and record to the nearest 0.000 2
grams. Prepare the suspension according to the above procedure.
c) Place the shelf limit pointer at the (30-50) μm position.
d) Fill the burette to a certain height with kerosene of the same lot and temperature as
the kerosene used in making the suspension, and start agitating the tank containing
the suspension in accordance with 7.2.2.2.5.2 item (2). Continue the oscillatory
movement process until the kerosene in the burette reaches zero and stop the
agitation process. Immediately place the tank in the beam path position.
e) Immediately move the beam-reducing filter out of the way of the light and close the
toolbox door.
f) Read the microameter to the nearest value of 0.1 μA as the kerosene passes the
50, 45, 40, 35, and 30 marks.
g) Raise the rack successively until the 25, 20, 15, 10 and 7.5 marks on the scale, the
micrometer reading at each position being like the reading when the kerosene is
emptied from the burette.
h) Lower the rack to the (30-50) μm position. Replace the filter in the light beam path,
move the tank, and check the lamp intensity. If the microameter reading shows a
shift of more than 0.3 μA from the initial setting through the filter alone, then the test
should be repeated.

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7.2.2.2.6 Data logging

For data recording and specific surface calculations, Table 15 is recommended.

7.2.2.2.7 Calculations

(1) How to calculate the specific surface

a) Calculate the specific surface using the following equation:

 ( − log I 50 ) 
S=K  
1,5 + 0.75 log I 7.5 + log I10 log I15 + ....... + log I 45 − 9.5 log I 50 

Description:
This is the specific surface of the sample, m2 /kg;
Times the calibration factor as described in section 7.2.2.2.4.4;
r is the percent of sample weight corrected by the sample passing a 45 μm (No. 325)
sieve (NOTE 1) and I , I , I7,51015 , ..... I50 are microameter readings
corresponding to particle diameters of 7.5 μm, 10 μm, 15 μm, ......50 μm, μA.

NOTE 1 The K value determined using 7.2.2.2.4.3 is used only for materials having a
specific gravity equal to that of Portland cement (approximately 3.15 grams/cm3 ). For
other materials, the values are obtained by calculation using the derivative of the
equation, which varies inversely with particle diameter (grams/cm3 ).

b) To calculate the specific surface in m2 /kg, multiply the surface area in cm2 /gram
by a factor of 0.1.
c) Round numbers in cm2 /gram to the nearest 10 units (for m2 /kg to the nearest
value)

For example:
Identify an example: Example
X:
Passing sieve 45 μm (No. 325)r, corrected, T 90,4
Calibration factor 33,9

The m reading on the filter, μA:


Before testing: 17,5
After testing: 17,5
Sample weight, gram 0,25

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Table 15 ̶ Example of recording turbidimeter test data and specific surface
calculations

Particle size, μm I, μm Log I


50 17,3 ....... 1,238A
45 17,4 1,241
40 17,6 1,246
35 17,9 1,253
30 18,4 1,265
25 19,1 1,281
20 20,1 1,303
15 21,6 1,334
10 23,9 1,378
7,5 25,6 ....... 1,408A
0,75 x 1,408 = 1,056
1,500
Total = 12,857
9,5 x 1,238 = 11,761
Difference = 1,096
S = (33.9 x 90.4 x 0.762)/1.096 = 2131 cm /grams2
Rounded to 2130 cm2 /g or 213 m /gram2
NOTES:
A
For ease of calculation, Log I50 and Log I7,5 are recorded in separate columns.

(2) Specific surface of the first turbidimeter reading I50 .

This method can be used for successive determinations for the same plant, with the
same sample size used, and no significant changes in fineness, color or other cement
properties. Under these conditions the specific surface of the sample can be calculated
from the first turbidity reading I50 , using the following equation:
S = c (2 - log I )50
Description:
This is the specific surface of the sample, m2 /kg;
I50 is a microameter reading that corresponds to a particle diameter of 50
μm;
c is the transmittance constant for a particular plant.

NOTE 2 The transmintance constant can be evaluated by substituting into the above equation the
known values of S and 2 - log I50 as determined using complete turbidimeter testing. An average
is made with a minimum of 5 c values determined from the complete test.

(3) If the fineness of the sample determined by 7.2.2.2.7 item (2) fails to meet the
requirements for fineness, retesting shall be carried out using the complete procedures
of 7.2.2.2.5.2 item (3), 7.2.2.2.6 and 7.2.2.2.7.

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7.2.2.2.8 Precision and bias

(1) Single operator precision


The variation coefficient of a single operator is 2.6%. Therefore, the results of 2 tests
performed by the same operator for the same sample, the average should not differ by
more than 7.3%.

(2) Multilaboratory precision


The multi-laboratory coefficient of variation is 3.8%. Therefore, the results obtained from
two different laboratories for the same sample should not average more than 10.6%.

NOTE The numbers representing the D1S% and D2S% limits are described in ASTM C 670-13,
Standard Practice for Preparing Precision and Bias Statements for Test Methods for Construction
Materials.

(3) When there is no accepted reference material suitable for the determination of bias in
accordance with this method, it is not made.

7.2.3 Normal consistency testing

This test method includes checking the normal consistency of hydraulic cement.

7.2.3.1 Purpose and use

This test method is used to determine the amount of water required in the preparation of
hydraulic cement paste for testing.

7.2.3.2 Equipment

a) Scales and weighing stones must meet specifications


b) Measuring cup with a capacity of 200 mL or 250 mL, according to specifications
c) Vicat tool

Figure 8 - Vicat tool

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The vicat tool shall consist of a frame A (Figure 8) having a movable rod B, weighing
300 grams, one end of a piston C of 10 mm diameter, spaced at least 50 mm apart,
and the other end of a disassembled needle D of 1 mm diameter and 50 mm length.
The rod B can be used alternately and can be fixed in several positions with the
adjusting screw E and has an adjustable indicator F, movable on a scale (indicated in
mm) whose scale is attached to the frame A. The cement paste to be tested is inserted
into the ring G, which is rigidly conical, placed on a non-absorbent flat plate H, the
width of each side of which is ± 100 mm.
Rod B is made of stainless steel having a hardness of not less than 35 HRC and must
be straight with the tip of the piston perpendicular to the axis of the rod.
B. The ring is made of non-corroding, non-water-absorbing material having a bottom
inner diameter of 70 mm and a top of 60 mm with a height of 40 mm.
In addition to the above, the vicat tool must comply with the following specifications:
a. Movable rod weight (B) (300 ± 0.5) grams.
b. Diameter of piston rod end (C) (10 ± 0.05) mm.
c. Needle diameter (1 ± 0.05) mm.
d. Inner diameter of the bottom ring (70 ± 3) mm.
e. Inner diameter of top ring (60 ± 3) mm.
f. Ring height (40 ± 1) mm.
g. Scale division
The scale division, when compared to a standard scale whose accuracy is 0.1
mm at each point, must not show a deviation greater than 0.25 mm.

d) Stirring machine, mixer, mixing bowl, and rake.


e) Stirring knife, triangular knife with straight edge size (100 - 150) mm

7.2.3.3 Temperature and humidity

a) The ambient air temperature of the table where dry cement, molds and base plates are
mixed should be maintained between (20 - 27.5) C.o
b) Humid room humidity in accordance with 7.2.1.1 items a) and b)

7.2.3.4 Procedure

7.2.3.4.1 Preparation of cement paste

Mix 650 grams of cement with measured water, according to the procedure described in
Appendix C.
Place the mixer and dry bowl in the mixing position of the mixer. Then put the ingredients into
the bowl and mix them in the following way:
Put all the mixed water into the bowl. Add the cement to the water and wait for 30 seconds
for the mixed water to be absorbed. Start the mixer and mix at low speed (140 ± 5)
revolutions per minute for 30 seconds.

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Stop the mixer for 15 seconds and during this time collect the paste that sticks to the walls of
the bowl.
Run the mixer at medium speed (285 ± 10) revolutions per minute and mix for 1 minute.

7.2.3.4.2 Test piece molding

Immediately form the prepared cement paste according to the grains as above, into a ball
with both hands (wearing rubber gloves) and throw it 6 times from one hand to the other at a
distance of approximately 15 cm.
Press the pasta ball in one hand into the large hole of the vicat ring, which is held in the other
hand.
Take it out with one stroke of the palm. Place the ring with the large hole on the glass plate,
remove the excess paste in the small ring hole with a single motion using the edge of a
triangular stirring knife, with a slightly oblique motion towards the apex of the ring, smooth the
surface, if necessary gently tapping with the tip of the stirring knife.
During cutting and smoothing work avoid pressing on the paste.

7.2.3.4.3 Consistency determination

Center the paste in the ring under the launching rod B, stick the end of the launching rod C on
the paste surface and lock the screw E.
Then fix the F indicator at the zero mark of the scale, and release the launcher rod at most 30
seconds after the completion of paste making.
The tool must be free from vibration during the test.

Normal consistency of the paste is achieved when the launching rod penetrates to a limit (10
± 1) mm below the paste surface within 30 seconds after release. Carry out the above
experiment using different percentage of water until normal consistency is achieved. Use
fresh cement in each experiment.

7.2.3.5 Calculations

Percent consistency is expressed in terms of paste moisture content and is calculated by the
formula:

Wa
%W=
Ws
Description:
W is the consistency expressed in paste moisture content,
%; Wa is the weight of water, grams;
Ws is the weight of dry cement, grams.

Calculate the amount of water required for normal consistency rounded up to 0.1% and
report the weight of dry cement rounded up to 0.5%.

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7.2.4 Binding time testing

7.2.4.1 Equipment

a) Scales
Scales and weighing stones must meet specifications
b) 200 or 250 mL capacity measuring cup, according to specifications

7.2.4.2 Temperature and humidity

The ambient air temperature of the table where dry cement, molds and base plates are
mixed shall be maintained at (23 ± 3.0)o C. The temperature of the mixing water and moist
room shall be maintained at 23.0 ± 2.0 C.o
The humidity of the laboratory room and the damp room where the test specimens are stored
shall not be less than 50%.

7.2.4.3 Preparation of cement paste

Mix 650 grams of cement with the percentage of mixing water required for normal
consistency according to the procedure described in Appendix C.
In testing it is recommended to use distilled water but in referee testing and joint testing it
must use distilled water.
Test specimens used to determine normal consistency can also be used for the
determination of bonding time with a vicat needle in accordance with the procedure
described in 7.2.4.4.

7.2.4.4 Bonding time testing with manual vicat tool (method A)

This method is intended for the determination of the bonding time of hydraulic cement using
a vicat needle.

7.2.4.4.1 Specialized equipment

Manual vicat tool (method A) in accordance with 7.2.3.2 item c) and Figure 8.

7.2.4.4.2 Procedure

7.2.4.4.2.1 Test piece molding

Molding of test specimens in accordance with 7.2.3.4.2. Immediately after molding, store the
test specimens in a damp room and leave them until the setting of the bonding time.
The test specimen shall be in a molding ring with a glass plate H during the test time.
Samples for binding time and autoclave testing may be made from the same sample.

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7.2.4.4.2.2 Determination of binding time

Leave the specimen in a moist chamber for 30 minutes after molding, then penetrate with a 1
mm diameter needle and every 15 minutes thereafter (for type III cements every 10 minutes)
until it reaches penetration at 25 mm or less.
For penetration tests, lower needle D until it rests on the surface of the cement paste.
Tighten screw E, and set indicator F at the upper end of the scale. Fix it at zero on the scale.

Free the rod by rapidly loosening screw E and allow the needle to descend for 30 seconds,
then read the scale to determine penetration (if the paste appears thin, the initial descent of
rod B may be slowed to prevent bending the needle 1 mm).
The distance between penetration points is not less than 5 mm against the inner wall of the
mold and the distance between 2 penetration points is not less than 10 mm. Record the
results of the penetration test. By interpolation determine the time at which 25 mm
penetration is obtained. This is the initial bonding time. The final bonding time is when the
needle does not appear to be immersed in the paste.

Attention:
- During penetration testing the equipment must be vibration-free.
- Keep the 1 mm diameter needle straight and clean because clumps of cement sticking to
the side of the needle will slow down penetration, when cement sticks to the tip of the
needle it will speed up penetration.
- The bonding time is not only affected by the percentage of water temperature used, the
amount of paste received, but also caused by air temperature and humidity.

7.2.4.4.3 Precision

a) Based on the results of the experiment by a single operator (within laboratory) the
standard deviation for the initial binding was 12 minutes within the range of (49-202)
minutes. The standard deviation for the final bonding was 20 minutes within the range of
(185-312) minutes. Therefore the test results performed by the same operator should not
differ by more than 34 minutes for initial bonding and 56 minutes for final bonding of the
same paste.
b) Based on the results of the multi laboratory experiment (between laboratories) the
standard deviation for the initial binding was 16 minutes in the range of (49-207)
minutes. The standard deviation for the final binding was 43 minutes within the range of
(185-312) minutes. Therefore the test results conducted by 2 different laboratories, the
difference should not be more than 45 minutes for initial binding and 122 minutes for
final binding of the same paste.

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7.2.4.5 Bonding time testing with automatic vicat tool (method B)

7.2.4.5.1 Specialized equipment

a) Automatic vicat needle equipment


The equipment shall be equipped with a standard vicat needle. The needle shall have a
diameter of (1.0  0.05) mm and a minimum length of 50 mm. The total weight that can
be supported by the needle tip at the time of measurement is (300  0.5) grams. The
instrument shall be able to automatically complete and record the penetration
measurements of a sample test at intervals of not more than 10 minutes and run each
penetration test at least 5 mm away from the previous penetration and at least 10 mm
away from the inside of the mold.

b) Sample mold
The cement paste is held in a conical ring with a height of (40  1) mm and a movable
flat plate. The test surface has a minimum diameter of (60  3) mm.

7.2.4.5.2 Working procedure

7.2.4.5.2.1 Printed samples

Quickly formed from cement paste, prepared as described in the section on preparation of
cement paste into a ball shape using gloved hands and thrown six times from one hand to
the other, keeping the hands 150 mm apart. Press the ball, leaving it in the palm until the
large end of the conical ring, is held with the other hand, thoroughly filling the ring with paste.
Transfer the remainder to the larger end with a single movement of the palm. Place the larger
end on a flat plate. Use a sharp trowel with a sharp edge to remove the remaining paste on
top of the mold. Hold the trowel on a slope 30o with the front edge raised and starting from
closest to the center of the mold, smooth the paste by pulling the trowel over the top of the
mold with a saw; repeat the procedure for the other parts of the surface. Then smooth the
surface to the top of the mold by making a steady, complete motion across the surface using
the dragging edge of the trowel. oRepeat the cutting and smoothing steps but at 90° to the
previous cut. Repeat the steps as required to create a flat surface with the top of the mold.
Usually the paste is leveled in two stages, but sometimes up to three stages if needed. Avoid
excessive pressure and compaction. Since automatic vicat tools refer to the top of the mold
rim, it is very important that the top of the paste surface is uniform and flat with the top of the
mold.

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7.2.4.5.2.2 Setting time determination

By following the manufacturer's instructions and completing the required instrument


calibration and zeroing procedures. Set the instrument to measure for not less than 10
minutes (NOTE 1). Place the printed sample in the automatic vicat apparatus and start the
measurement (NOTE 2).

NOTE 1 Automated equipment is usually capable of more frequent measurements than once in every
10 minutes and more frequent measurements will minimize interpolation.

NOTE 2 The initial setting time is based on method A which is determined based on the elapsed time
required to obtain a penetration of 25 mm and the final engagement as the total elapsed time at which
the needle does not enter clearly into the paste. The endpoints are established using a qualified
automatic vicat test method that deviates significantly from the endpoints specified in method A, and
requires standardization for correct inclination.

7.2.4.5.2.3 The period of applicability of a method should be determined using the


average setting time of cement used for qualification and standardization, and should be
limited to 30 minutes greater than the maximum, and 30 minutes less than the minimum.

7.2.4.5.2.4 Calculation and reporting

Complete all calculations to the nearest 1 minute, and the report produces a value to the
nearest 5 minutes. The report should indicate that the test was conducted using method B.

7.2.4.5.3 Performance requirements (qualifications) for automatic vicat

instruments 7.2.4.5.3.1 Scope

When the time of setting results from automatic vicat equipment are used for acceptance or
rejection tests of cement, the methods used shall comply with the qualification requirements
of this section. The method is expected to consist of specific instrument procedures and
molding procedures meeting the requirements of this standard, which are used consistently
by a particular laboratory.

7.2.4.5.3.2 Example of portland cement required


Portland cement that complies with the requirements specified in the quality requirements of
this standard and such samples when tested according to method A, shall include the
following:
a) The cement has an initial initial bonding time of less than 110 minutes.
b) Cement with an initial early setting time greater than 150 minutes.
c) Cement with a final setting time of less than 180 minutes.
d) Cement with final binding time greater than 210 minutes

NOTE Laboratories are advised to provide sufficient cement for further qualification and
standardization.

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7.2.4.5.3.3 Testing

Using the method to be qualified and entering the standardization formula as described in the
standardization section, obtain a single determination of the initial and final setting times of
each of the three cements. On the same day, perform adjacent time to setting determinations
based on method A. Make a single determination of normal consistency for each cement,
and use the same amount of water for all mock batches. Complete three sets of tests on
different days, and repeat all the steps in the method. Perform qualification tests on samples
prepared separately from the standardization tests.

7.2.4.5.3.4 Calculations

Calculate the average of three series for the initial and final binding times for each cement
using the method. A method conforms to the initial binding time qualification requirements if
there is a difference between the mean value of the initial binding time for method A and the
corresponding mean value of method B that is not greater than 25 minutes for any sample,
and the range of three mock tests using method B does not exceed 30 minutes. Likewise, a
method complies with the final binding time qualification requirements if the difference
between the mean value of the final binding time for method A and the corresponding mean
value for method B is not greater than 45 minutes for any sample, and the range of three
mock tests by method B does not exceed 30 minutes. An example of qualification data is
given in Appendix B.

7.2.4.5.3.5 Standardization

When standardization is required with the aim of obtaining agreement between method A
and method B, it can be applied to other initial binding times, final binding times, or both. A
standardization formula should be based on a comparison of test results obtained using
method A and the selected method using an automated instrument (method B). Test results
from at least five different hydraulic cements are required for standardization. The cement
shall have a minimum range of 60 minutes initial setting time and a minimum range of 90
minutes final binding time when tested according to method A. If desired, three cements may
be used for instrument qualification, but resulting in a new determination. Use the same
method as used in instrument qualification, including all the same steps. Validation of
standardization formulas should be mathematically derived and applicable to all samples.
NOTE In general, automated instruments are computer-operated equipment, and can be easily
adopted for standardization calculations.

7.2.4.5.4 Re-qualification of methods


Requalification of a method is conducted at least once a year, and when any of the following
conditions occur:
a) The instrument is noticeably modified
b) The instrument is substantially improved
c) Substantial evidence shows that the method does not provide data that meets the
performance requirements.

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d) The averages of the laboratory reference cement and concrete samples differ from the
values obtained using the method by more than 45 minutes for the initial time or final
setting time.
7.2.4.5.5 Rigor and bias

7.2.4.5.5.1 Rigor

No rigor data are available at this time. A laboratory is advised to develop its own precision
data for the methods and instruments used. Based on the qualification requirements, the
precision of a method should not be greater than the precision of method A.

7.2.4.5.5.2 Bias

Since there is no suitable reference material for bias determination for the procedures in this
test method, no bias statement is presented.

7.2.4.6 Binding time testing with gillmore needle tool

7.2.4.6.1 Specialized equipment

Gillmore needle equipment


A gillmore tool that must meet the following requirements:
a) Initial binding needle:
- Weight : (113.4 ± 0.5) grams.
- Diameter : (2.12 ± 0.05) mm.

b) Final binding needle:


- Weight : (453.6 ± 0.5) grams.
- Diameter : (1.06 ± 0.05) mm.

The needle should be cylindrical with a length of (4.8 ± 0.5) mm. The tip of the needle should
be flat and located exactly on the axis and the rod (see Figure 9).

Figure 9 - Gilmore tool

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7.2.4.6.2 Procedure

7.2.4.6.2.1 Test piece molding

Form the cement paste into a slab approximately 75 mm in diameter and 13 mm thick on a
square glass.
The surface is flattened and the edges are beveled (Figure 10).
In making this slab, first place a lump of cement paste on the glass, level the surface and
then form the slab by moving the stirring spoon around in the direction from the outer edge,
to the center of the paste lump.

7.2.4.6.2.2 Determination of binding time

When determining the bonding time, hold the needle in the vertical position and penetrate the
"initial" needle (vertical position).
When the "initial" needle has no marks on the mold surface, record the time and count the
start of mixing cement and water as the initial bonding time.
Do the above using the "final" needle and count it as the final binding time.

Figure 10 - Cement paste slab shape

7.2.5 Expansion testing with autoclave

This test method involves determining the autoclave expansion of portland cement by testing
the specimens.

7.2.5.1 Purpose and use

Autoclave expansion testing to determine the potential index of slow expansion caused by
hydration of CaO, MgO or both.

7.2.5.2 Equipment

a) Scales and weighing stones, according to specifications.


b) Measuring cup, 200 mL or 250 mL capacity, according to specifications.
c) The mold measures: (25 x 25 x 285) mm (Figure 11).

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Figure 11 - Prism mold

d) Stirring knife, triangular knife with straight edge size (100-150) mm


e) Autoclave, consisting of a high pressure steam vessel equipped with a wall thermometer.
The autoclave shall be equipped with an automatic pressure regulator and a rupture disk
with a bursting pressure of 2.4 MPa ± 5%. In locations where explosive pressure using a
rupture disk is not permitted, the autoclave shall be equipped with a safety valve. In
addition, the autoclave shall be equipped with a discharge valve that can release air
during the initial heating period and release the remaining vapor pressure at the end of a
cooling period.

The pressure gauge shall have a nominal capacity of 4.0 Mpa (600 psi), shall not be
larger or smaller, a dial with a nominal diameter of 115 mm and shall have a scale from
(0-4.0) Mpa ((0 - 600) psi) with a scale division of not more than 0.03 MPa. The
measurement error shall not exceed ±0.03 MPa at an operating pressure of 2 MPa.
The capacity of the heating unit shall be such that the maximum saturated vapor
pressure load in the autoclave can be raised until the pressure gauge indicates 2 MPa
for (45 - 75) minutes from the time heating starts.
Automatic pressure regulators should be able to maintain the pressure at (2 ± 0.07) MPa
for at least 3 hours. The autoclave pressure should be designed so that the pressure
drops from 2 MPa to less than 0.07 MPa within 1.5 hours after the heating is stopped.
The breakable disk should be made of materials that have a tensile strength that is
relatively insensitive to temperature (20-216) C.o

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f) Length comparison
Length comparator used to measure the change in length of the test piece and
meet specifications (see Figure 12).

Figure 12 - Comparator

7.2.5.3 Temperature and humidity

7.2.5.3.1 Room temperature

Maintain room temperature, dry cement and reagent water, in accordance with 7.2.1.1 item a).

7.2.5.3.2 Humidity

Keep the humidity of the damp room in accordance with 7.2.1.1 item b).

7.2.5.4 Safety warning

a) The pressure gauge must have a capacity of 4.0 Mpa (600 psi).

Gauges with capacities that are too small or too large can pose a hazard. When the
working pressure is greater than the capacity of the gauge, the needle is out of scale,
and conversely with a larger gauge capacity, the needle is too small. For this reason, the
tester must be sure that the needle pointer does not cross the maximum scale section.

b) Pressure gauges must be tested for proper operation.

The thermometer should used together with measuring devices pressure which is
always ,
The purpose is to complete the detection of pressure gauge deviation from proper
operation.

c) The automatic pressure regulator must function at all times.

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d) Set the safety valve so that it will operate at a pressure (6 - 10) % above the maximum
pressure of 2.1 MPa, the specification set forth in this test method which is
approximately 2.3 Mpa (330 psi). If the manufacturer provides special instructions on
maintenance of the safety valve, follow them, otherwise check the safety valve
t w i c e a year. Check the safety valve to be open or set to be open at a
pressure of ± 2.3 Mpa (330 psi). Keep the discharge direction of the safety valve away
from the tester.

NOTE Unexpected circumstances may occur. For example, in one instance the automatic
pressure regulator malfunctioned, the safety valve jammed and the pressure regulator pointer that
was showing O suddenly rose beyond the maximum limit and stopped in the wrong position. The
condition of the pressure regulator was eventually discovered and the unknown pressure was
released before equipment damage occurred.

e) Testers wear leather gloves to prevent hand burns when removing the top of the
autoclave at the end of the test, keep the direction of the drain valve away from the
tester.
When removing the autoclave lid, tilt it so that the vapor to be released is away from the
tester.
Testers should take care to prevent burns caused by hot water that has been used in the
autoclave.

f) Be aware that in most autoclaves, the return of the needle to its original point or the
starting point does not necessarily indicate that the pressure inside the autoclave is zero,
there may still be a dangerous amount of pressure remaining.

7.2.5.5 Number of test pieces

Make at least one test piece.

7.2.5.6 Test mold preparation

Prepare the test piece mold according to Figure 10.

7.2.5.7 Test piece preparation

7.2.5.7.1 Cement paste mixing

Prepare a paste consisting of 650 grams of cement and sufficient water to obtain a paste of
normal consistency. Mix the paste mixture according to the procedure described in Appendix
C. Both test specimens for determination of binding time and test specimens for testing by
autoclave can be made from the same mix. If the paste used for the determination of the
binding time is a sample of the paste that has been used for the determination of the normal
consistency, as described in 7.2.3.4.2, then the specimens for the test by autoclave can be
prepared immediately from the paste that is still available.

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7.2.5.7.2 Test piece molding

Immediately after completion of the preparation of the test specimens for the binding time
test, mold the test specimens in two stages. Each stage is compacted with the thumb or
forefinger by pressing the paste towards the corners of the mold and along the mold surface,
until it produces a well-mixed specimen.

The surface is compacted, excess paste is cut off to be flush with the mold surface using a
stirring knife, and smooth the surface with a few strokes of the stirring knife. During mixing
and molding both hands are protected with rubber gloves.

7.2.5.7.3 Test piece preparation

Immediately place the mold filled with paste in a humid room for at least 20 hours.
If removed from the mold before 24 hours, the specimens should be kept in a humid room
until the time of the test.

7.2.5.8 Procedure

a) At 24 hours ± 30 minutes after molding, the test specimens were removed from the moist
chamber, immediately measured the length of each test specimen with a length
comparison tool and put into an autoclave must contain enough water at a temperature
of (20 - 28)o C, to keep the steam saturated during the test.
b) To allow air to escape from the autoclave during the preheating period leave the
discharge valve open until water vapor begins to escape (see safety warning).
The valve is then closed and the autoclave temperature is gradually increased to a vapor
pressure of 2 MPa over a period of (45 - 75) minutes from the start of heating. The
pressure is maintained at (2 ± 0.07) MPa for 3 hours.
At the end of the 3-hour period, heating is stopped and the autoclave is cooled gradually
until it reaches a pressure of less than 0.07 MPa in approximately 1.5 hours. At the end
of the 1.5 hour period, gradually the remaining pressure was gradually released by
opening the discharge valve until atmospheric pressure was reached.
Then the autoclave is opened, the test piece is taken out and then immersed in hot water
at a temperature above 90o C.
Within 15 minutes, cool the water around the test specimen gradually by adding cold
water until the water temperature drops to 23 C.o
Keep water around the specimen at 23o C for 15 minutes, then the surface of the
specimen is dried and the length is measured again with a length comparison tool.

NOTE If readings at 27o C are desired, it is recommended that the specimens after being
removed from the humid chamber be placed in water whose temperature is maintained at 27o C
for at least 15 minutes, remove and measure the length of each specimen with a length
comparison tool, then heat in an autoclave. After completion, remove from the autoclave and cool
the specimens with water to a temperature of 27O C within 15 minutes. Maintain the test
specimens at that temperature in water for as long as possible and then measure the length of
each test specimen with a length comparison tool.

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7.2.5.9 Calculations

Calculate the change in length of the test specimen before and after autoclave testing in %
(percent) with an accuracy of 0.01.
Report the percentage increase in length as the expansion of the autoclave. Express the
reduction in length with a minus sign in front of the percent.

7.2.6 Determination of compressive strength of hydraulic cement mortar

This test method involves the determination of the compressive strength of hydraulic cement
mortar using a cube mold with a side size of 50 mm.

7.2.6.1 Test method summary

The mix used consists of 1 part by weight of cement and 2.75 parts by weight of sand.
Portland cement is mixed with water with a certain cement water factor.
The dough that has been put into the cube is compacted by stacking when the cube is half
filled and fully filled, the test specimen is left in the mold in a humid room for 1 day, open the
mold in a humid room for 1 day, open the mold and the test specimen is immersed in water
containing lime until the test time.

7.2.6.2 Purpose and use

This test method is used for the determination of the compressive strength of hydraulic
cement mortars and the results can be used to determine whether the cement meets the
specifications. Furthermore, the test method is used as a reference by a number of other
specifications and test methods. Be careful if the results of this mortar test are to be used to
predict the compressive strength of concrete.

7.2.6.3 Equipment

(1) Weights and scales


The scales must conform to the specifications. The scales shall be evaluated for
accuracy and deviation at a total load of 2 000 grams.

(2) Measuring cup


A measuring cup with a specified capacity (preferably large enough to measure the
water mixture in a single operation) to produce the indicated volume at a temperature
of 20o C. The allowable variation is  2 mL. The measuring cup is divisible by at least 5
mL, except for a negligible line for the smallest volume of 10 mL for a 250 mL
measuring cup and the smallest volume of 25 mL for a 500 mL measuring cup. The
main indicating lines must circle the measuring cup and be numbered.

(3) Sample mold


For cube molds with a side of 50 mm, it must be firmly fixed. The mold should have no
more than 3 compartments and be separated into no more than two parts. The parts of
the mold when assembled become a strong unit. The mold is made of strong metal that
is not affected by cement mortar. For new molds the Rockwell Hardness number of the
metal should not be less than 55 HRB. The sides of the mold should have rigidity that
prevents widening or bending. The inner side of the mold should be flat and meet the
tolerances in Table 16.

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Table 16 ̶ Allowable variation of molding dies (mm)
50 mm cube mold
Parameters New Already in use
Side flatness < 0,025 < 0,05
Distance between opposite sides 50  0,13 50  0,50
Height of each compartment 50 + 0,25 - 0,13 50 + 0,25 - 0,38
Angle between adjacent surfaces*) 900  0.5 0 900  0.5 0
NOTES:
*) Measured at a point displaced slightly from the intersection. Measured separately for each
compartment between all inner faces and adjacent faces and between faces
the inside and the top and bottom of the plane of the mold.

(4) Stirring machine, mixer and mixing bowl


Machi stirrer power-driven equipped with a stirrer
ne
and bowl. See Figure 13, Figure 14 and Figure 15.

Figure 13 - Mixer machine

Figure 14 - Stirrer
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Figure 15 - Bowl

(5) Flow table and flow mold (see Figure 16)

Figure 16 - Flow table

(6) Pounder
Made of non-absorbent, non-abrasive, non-brittle materials, such as rubber compounds
that have a hardness of 80  10 shore A scale or teak wood made non-absorbent, non-
abrasive, by soaking in paraffin for 15 minutes at temperature
 200o C and should have a cross section of (13 x 25) mm, approximately (5 - 6) inches
or (120-150) mm long. The face of the pounder should be flat and perpendicular to the
handle.

(7) Stirring knife, triangular knife with straight edge size (100-150) mm.

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(8) Compressive strength machine
A compressive strength machine of either hydraulic or screw type, which has sufficient
openings between the upper pressing plane and the lower anvil to permit testing of
different sizes of specimens. The load applied to the specimen shall be accurate to
 1.0%. The upper pressing plane shall have a circular holder, a hard metal block firmly
attached to the center of the top of the machine.
The center of the circle should be located in the middle of the block surface during
contact with the test piece. The block shall be securely fixed in the circular holder, but
shall move freely in each direction.
The diagonal or diameter of the anvil surface should be slightly larger than the diagonal
of the test piece cube to facilitate proper placement of the test piece in the center of the
anvil a hard block should be used under the test piece to reduce wear of the machine
plate.
The surface of the anvil block in contact with the test piece should have a Rockwell
hardness number of not less than 60 HRC.
The surface of the block anvil must be perfectly flat with a slope of no more than 0.013
mm if the block is new and must be maintained with an allowable variation of 0.025 mm.

NOTE The anvil block diameter is 79.4 mm, which is sufficiently wide for testing 75 mm x 150 mm
cylinders, provided that the lower anvil block has a diameter greater than the diagonal of a 50 mm
cube but not greater than 74 mm and is mounted upright with the upper anvil block and installed
in the proper position.

7.2.6.4 Standard sand


The sand used should meet the requirements contained in Table 17 for the purpose of
grading, sand sourcing and loss of undesirable airborne characteristics.

Table 17 ̶ Standard sand requirements


Characteristics
Sand 20-30 Rated sand
Assessment, percentage that passes
the sieve
No. 16 (1.18 mm) 100 100
No. 20 (850 m) 85 - 100
No. 30 (600 m) 0-5 96 - 100
No. 40 (425 m) 65 - 75
No. 50 (300 m) 20 - 30
No. 100 (150 m) 0-4
Difference in air content of mortar made 2,0 1,5A)
using washed and unwashed sand, %
maximum air

Sand source Ottawa, 1 L or Ottawa, 1L


Les Suer, Mn
NOTE
A)
The compressive strength of Portland cement is made to the specification of blended Portland
cement, the cement being reduced by approximately 4% of the respective percentage of air in
the compressed cube A total of three washed sand tanks and three unwashed sand tanks are
required for the cube.
detected a strength difference of 7% between washed and unwashed mortar sands.

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7.2.6.5 Temperature and humidity

7.2.6.5.1 Temperature

The temperature of the air around the mixing board, dry materials, molds, flat plates and
mixing bowl should be maintained between 20o C and 26o C. The temperature of the mixing
water, room humidity and water in the storage tank should be set at (23  2).
oC.

7.2.6.5.2 Humidity

The relative humidity of the laboratory should not be less than 50%.

7.2.6.6 Test piece

For each test, 3 or more test pieces should be made.

7.2.6.7 Test mold preparation

a) Using a greased or oiled cloth, make a thin coating on the inside of the mold and the
base of the non-absorption plate. Wipe the mold face and plate base with the cloth as
necessary to remove excess coating and to make the inner surface thin. If sprayed
lubricant is used, spray it directly on the mold face and plate base at a distance of (150-
200) mm to obtain complete coverage. After spraying, if necessary wipe the surface
with a cloth to remove excess sprayed lubricant. Adherent coating is considered
adequate if finger pressure makes an impression.
b) Cover the surfaces of the parts to be joined with grease while the two molds are joined.
The amount should be sufficient while the two parts are firmly joined together. Remove
excess grease with a cloth.
c) After attaching the mold to the plate base (if the clamp type is bolted) carefully remove
with a dry cloth any excess oil or grease from the surface of the mold and plate base
using waterproof coatings, as coatings are paraffin, microcritaline wax, or a mixture of 3
parts paraffin and 5 parts rosin by weight. Melt the coating by heating between (110 -
120)o C. The outer contact area between the mold and the plate base is made
watertight by using the melted coating.
NOTE 1 Since spray-on lubricants evaporate, the mold should be checked for coating shortly
before use. If spraying has taken a long time, it needs to be sprayed again.

NOTE 2 The use of straight paraffin is permissible if watertight joints are guaranteed, due to the
low strength of paraffin, when the mold is not bonded to the slab base a mixture of paraffin and
rosin should be used. The paraffin and rosin mixture may be difficult to remove when the mold is
cleaned and a watertight joint may be secured with paraffin alone, by slightly heating the mold
and plate base before rubbing the joint. The aforementioned mold should be allowed to return to
its original temperature.

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7.2.6.8 Procedure
7.2.6.8.1 Composition of mortar

a) The proportional ratio of standard mortar is one part by weight of cement to 2.75 parts by
weight of standard graded sand. The water-cement factor is 0.485 for all types of
Portland cement and 0.460 for air-entrained types of Portland cement. The amount of
mixing water for other types of cement is such as to produce a flow rate of 110  5 and is
expressed as percent by weight to cement.
b) The quantities of materials to be mixed at the same time in a mortar batch to make six
and nine test samples are as follows:

Table 18 ̶ Composition of mortar


Number of test pieces
Material
6 9
s
Cement (gram) 500 740
Sand (gram) 1 375 2 035
Water (mL)
- Portland 242 359
-Portland containing air 230 340
-Other (with a flow rate of 110  5) --- ---

7.2.6.8.2 Preparation of mortar

Mechanically mixed according to the procedure in Appendix C.

7.2.6.8.3 Flow assignment

Wipe, clean and dry the flow table top carefully, and place the flow mold in the middle. Place
a layer of mortar with a thickness of  25 mm in the mold and pound it 20 times with a
pounder. The pounding pressure should be adjusted so that it fills the mold completely.
Then fill the mold with mortar and mash as in the first layer. Slice the mortar to get a flat
surface, level the top of the mold by using the straight side of the stirring knife (almost
perpendicular to the mold) in a sawing motion on the top of the mold.
Wipe the flow table clean and dry, taking care to remove water from around the corners of
the mold. Remove the mold from the mortar 1 minute after the work is completed.
Immediately lower the table to a height of 13 mm 25 times in 15 seconds. Flow is the result of
increasing the average diameter of the mortar pile, measured in at least 4 measurement
sites, expressed as a percentage of the original base diameter.
Experiment with mortars of varying water percentage until the desired flow is obtained. Use a
new mortar each time.

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7.2.6.8.4 Test piece molding

a) Leave the mortar in the mixing bowl, stirring for 90 seconds without a lid. During the first
15-second interval, immediately remove any mortar that sticks to the bowl wall.
Then stir again for 15 seconds at medium speed.
As soon as the stirring is complete, the stirrer is shaken to remove the adhering mortar
and put it into the bowl.

b) If duplicates are desired, return the mortar from the flow table to the bowl. Immediately
remove any that are stuck to the bowl walls and then re-mix the entire batch for 15
seconds at medium speed.
After mixing is complete, the mixer should be shaken to remove excess mortar in the
bowl.

c) If duplicate mixes are required for additional tests, the flow test is omitted and the mortar
is left in the mixing bowl for 90 seconds uncovered. During the last 15 seconds,
immediately wipe off the mortar adhering to the bowl wall. Then stir again for 15 seconds
at medium speed, after the stirring is finished, shake the stirrer to drop the mortar that
sticks to the stirring bowl.

d) Start molding the test specimens with no more than 2 minutes and 30 seconds after
completion of stirring. Place  25 mm thick layer of mortar (approximately ½ the depth of
the mold) on all cube mold chambers. Pound the mortar in each cube chamber for (4 X
8) rounds within 10 seconds, the pounding in the 2nd round of the next round, shall be
perpendicular to the previous round of pounding and consist of 8 rounds adjacent to
each other on the surface of the specimen, as described in Figure 17. The pounding
pressure shall be sufficient to ensure uniform filling of the mold. A pounding consisting of
4 rounds (32 impacts) shall be completed for one cube before proceeding to another.
When the pounding of the first layer in all cube spaces has been completed, fill the cube
with the remaining mortar and then pound as for the first layer. During the pounding of
the layers, try to keep the mortar sticking out of the mold, returning to the mold after
each round of pounding is completed, by using gloves. After each round of pounding, the
top of the cube should be slightly higher than the top of the mold. Pick up the mortar
sticking out of the mold with the poke knife and level the mold with the flat part of the
poke knife, once through the top of each cube in a motion perpendicular to the length of
the mold. Then, for the purpose of leveling the mortar sticking out of the mold and
making it all the same thickness, slice the flat part of the poke knife once more along the
length of the mold. Slice the mortar again until it is level with the top of the mold by
slicing the straight side of the poke knife (almost perpendicular to the mold) in a sawing
motion along the length of the mold.

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A. First and third order of B. Second and fourth order
impact of impact
Figure 17 - Collision sequence

e) Storage of test specimens

Immediately after the molding of the test specimen is completed, place the test
specimen in a humid chamber, keeping the test specimen immediately after molding in
the mold stored in the
on a plate basis inside moist room for (20-72) hours, with surface
The top is in contact with moist air but should be kept away from water droplets.
When the test piece is of the mold before 24 Keep test piece always
removed hours,
in a humid chamber until the test period is 24 hours.
Then soak (except for 24-hour testing) in storage room which is
made of non-rusting materials and filled with saturated lime water, keep the water in the
chamber clear, if necessary change the water.

f) Determination of compressive strength

Carry out the test immediately after removing the test specimens from the humid chamber
especially
to test piece for um r 24-hour testing from the bath water for testing-
life testing others, tested for tan the press until it breaks with the provisions
robustnes
s
time as follows:

Table 19 ̶ Testing time tolerance


Testing Tolerance allowed
Lifespan
24 hours  0.5 hours
3 days  1 hour
7 days  3 hours
28 days  12 hours

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If more than one specimen is simultaneously removed from the damp chamber, for 24-
hour tests protect each specimen with a wet cloth until the time of the test. For tests with
other test ages, if more than one specimen is simultaneously removed from the soaking
water for testing, maintain the specimens in water at a temperature of (23  2)o C and
each specimen is fully submerged until the test is performed. Wipe each test specimen
to a surface dry condition and remove any loose grains of sand or rough coating from the
surface that will contact the anvil block of the testing machine.
Check the surface using a straightedge (NOTE 1). If there are any indentations, rub the
surface flat or discard the specimen, periodically inspect the cross-section of the
specimen.

NOTE 1 The surface of the tested specimen will be lower than actual if the surface is not
completely flat. Therefore, the test specimen mold must be kept clean, otherwise irregular
surfaces will be formed. To prevent wear, use a mold cleaning tool that is softer than the mold
metal. In case the surface of the test specimen needs to be smoothed, it can be done by rubbing
the test specimen with fine emery paper or with a cloth attached to the surface plane using a little
pressure. Rubbing of uneven surface areas of test specimens larger than a few hundredths of a
mm is difficult, in which case the test specimens should be discarded.

Apply a load to the surface of the test piece that is in contact with the flat surface of the
mold.
Carefully place the test piece on the testing machine just below the center point of the
top anvil block. Before testing each cube, ensure that the circular mounting block is free
to move. No bearings should be used.
The initial load, at the desired rate of pressing, can be applied up to half of the maximum
load of a test specimen that is estimated to have a maximum load greater than 13.3 KN.
Do not apply a starting load to test specimens that are expected to have a maximum
load of less than 13.3 KN.
Set the rate of pressing such that the remainder of the load (or the entire load in case the
maximum load is estimated to be less than 13.3 KN), is applied without stopping, until it
breaks at a rate of pressing such that the maximum load will be reached, not less than
20 seconds, nor more than 80 seconds from the time pressing starts.
Do not make changes to the controls of the compressive strength testing machine while
the specimen is being pressed and has not yet broken.

NOTE 2 It is recommended to apply a thin coating of a good quality light mineral oil on the circular
seat of the top block anvil.

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7.2.6.9 Calculations

Record the total maximum load indicated by the testing machine, and calculate the compressive
strength based on the formula below:

Fm = P/A
Description:
Fm is the compressive strength in psi or
MPa; P is the total maximum load in
N;
A is the area of the loaded surface in mm2 .
For the 50 mm cube mold used for determination of compressive strength, either inch-pound
units or International System units are used. In any case, the unit provisions for load and
area must be used to calculate the compressive strength in the selected units. If the cross-
sectional area of a mold varies by more than 1.5% of the number, use the actual area for the
compressive strength calculation. The compressive strengths of all mold acceptance tests
made from the same sample and tested at the same period shall be averaged and reported
to the nearest value of 10 psi (0.1 MPa).

7.2.6.10 Test piece failure and retest

a) In the determination of compressive strength, don't bother with molds that are obviously wrong.
b) The maximum allowable deviation between molds of the same mortar bin, at the same
test time is 8.7% of the average value when three cubes represent an age test and 7.6%
when two cubes represent an age test.

NOTE The possible increase in range is 1 in 100 when the bath coefficient varies within 2.1%.
The 2.1% value is the average value for laboratories participating in the Portland cement and
masonry cement reference sample program of the Cement and Concrete Reference Laboratory.

c) If the range of three prints exceeds the maximum specified in 7.2.6.10 item b), discard
the result that differs most from the average and check the range of the remaining boxes
of prints. Make a retest of the sample if less than two molds remain after discarding
defective molds or discarding tests that fail to conform to the maximum allowable range
of two molds.

7.2.6.11 Accuracy and deviation

The accuracy of this test method is listed in Table 20 and is based on results from the
reference laboratory cement and concrete reference sample program. The accuracy is
developed from data where a test produces an average of the compressive strength tests of
three cubes cast from a single mortar bed and tested at the same age. A noticeable change
in accuracy cannot be obtained when the test results are an average of two cubes, unlike
when an average of 3 cubes is used.

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Table 20 ̶ Rigor
Coefficient Acceptable range of test
Portland cement with Test life
of variation results within 2 seconds
fixed water:cement factor (days) %A
1 sec
%A
Lab. Single 1 3,1 8,7
3 3,9 10,9
7 3,9 10,9
28 3,8 10,6
Average 3,7 10,4
Multi Lab. 1 7,3 20,4
3 6,8 19,0
7 6,6 18,5
28 6,5 18,2
Average 6,6 18,5
Portland cement mix Fixed
mortar flow rate
Lab. Single 3 4,0 11,3
7 3,8 10,7
28 3,4 9,6
Average 3,8 10,7
Multi Lab. 3 7,8 22,1
7 7,6 21,5
28 7,4 20,9
7,6 21,5
Mansory cement
Fixed mortar flow
rate
Lab. Single 7 7,9 22,3
28 7,5 21,2
Average 7,7 21,8
Multi lab. 7 11,8 33,4
28 12,0 33,9
Average 11,9 33,7
NOTE
A
represents each of (1S %) and (d2s %) as described in ASTM Practice C 670.

The accuracy statement can be used for mortars made from cementitious mixes, and tested
at the ages recorded. The exact limits are usually larger for tests at younger ages and slightly
smaller for tests at older ages.
The procedure deviations of this test method have no deviations, as the values of the
compressive strength are defined in the requirements of the test method.

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7.2.7 Rapid rigid testing of portland cement (paste method)

This test method includes the determination of the rapid stiffening of portland cement.

7.2.7.1 Limitations

Rapid stiffening is the progression to stiffening that occurs earlier in the working
characteristics of portland cement paste, mortar or concrete. This limitation includes apparent
stiffening and rapid stiffening.

a) Pseudo-bonding: rigid development occurring early in the working characteristics of


portland cement paste, mortar or concrete without the evolution of much heat, whose
rigidity can be removed and plasticity regained by further stirring without the addition of
water.
b) Rapid bonding: rigid development occurring early in the working characteristics of
portland cement paste, mortar or concrete, usually with rather large heat evolution,
whose rigidity cannot be removed and whose plasticity cannot be regained by further
stirring without the addition of water.

7.2.7.2 Test method summary

A paste is prepared from the cement to be tested, using a sufficient amount of water to give
the required initial penetration, measured using a vicat tool, within a specified amount of time
after mixing is complete.

The second penetration, also called the final penetration, is measured in a predetermined
amount of time.
The ratio between final penetration and initial penetration is calculated in the presentation.

7.2.7.3 Purpose and use

a) This test method is to determine the degree of rapid rigid development of smeen paste
or to establish whether or not the cement meets the rapid rigid specification limit.

b) When used to ensure that the cement meets the specified specification limits, the
required specification is normally expressed in terms of the minimum permissible final
penetration price, in percent, calculated in accordance with 7.2.7.8. When used to
estimate the relative rapid stiffening tendency of cement, additional information on the
price can be obtained if the re-stirring procedure described in 7.2.7.7 is carried out.
Under some conditions, to differentiate between the less consistent and less obvious
tendency towards rapid stiffening and cements that have a more consistent and more
obvious tendency towards rapid stiffening, it is necessary to compare the properties of
the re-stirred conditions of the two cements.

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c) The rapid apparent binding of cement can cause handling and casting difficulties, but
this will not occur if the concrete is stirred for longer than usual, which is usually done
during transporting the concrete or if it is stirred before casting, as is commonly done at
the foundry.

The stiffness of the cement due to rapid false binding is immediately apparent when the
concrete is stirred for a short time in a stationary mixer and brought to the casting site
without stirring devices, as in pavement work.

d) Cements with very fast apparent binding usually require slightly more water to produce
the same consistency, which can result in slightly lower compressive strength and
increased shrinkage.

e) Rapid bonding will cause difficulties in handling and casting the concrete which will
usually cause the cement to fail to meet the bonding time requirements.

7.2.7.4 Equipment
a) Vicat tool, in accordance with 7.2.3.2 item c).
b) Knife, triangular knife with straight edge measuring (100-150) mm.
c) Mixer, bowl, stirrer, rake.
d) Measuring cup, according to specifications.

7.2.7.5 Reagents
Mixing water, distilled water

7.2.7.6 Temperature and humidity

a) The temperature of the chamber, dry ingredients, stirrer, bowl, ebonite ring and base
plate was 23.0 ± 3o C. The temperature of the mixed water was conditioned at 23.0 ± 2.0
C.o
b) The humidity of the damp room shall comply with 7.2.1.1 item b).

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7.2.7.7 Procedure

7.2.7.7.1 Preparation of cement paste

Cement paste mix


Mix 500 grams of cement with sufficient water to produce a paste with an initial penetration of (32 ±
4) mm using the following procedure:
a) Install the stirrer and dry bowl on the stirring machine.
b) Put all the mixing water in a bowl.
c) Add cement and leave for 30 seconds so that the water is absorbed.
d) Start the mixer and mix at low speed (140 ± 5) rpm for 30 seconds.
e) Stop stirring for 15 seconds and during this time remove any mortar that may have stuck
to the walls of the bowl.
f) Run the stirrer at medium speed (285 ± 10) rpm and mix for 2.5 minutes.

7.2.7.7.2 Test piece molding

Immediately form the cement paste into balls with the gloved hand. Press the ball located in
one palm, insert it into the larger end of the ebonite ring G, held in the other hand, continue
filling the paste into the ring.
Remove the excess paste on the larger end of the ring with a single stroke of the palm. Place
the larger end of the ring on the glass plate, H, and slice off the excess paste on the smaller
end at the top of the ring with a single motion of a sharp triangular knife held at a slight angle
to the top surface of the ebonite ring.
If necessary, smooth the top of the test piece, with one or two touches with the tip of the
stirring blade. During cutting and smoothing do not press the paste.

7.2.7.7.3 Determination of initial penetration

Place the paste in the ebonite ring on the glass plate H, under the rod B (Figure 8),
approximately 1/3 of the diameter of the edge of the launcher tip, C, should be in contact with
the paste chamber and tighten the screw E.
Then set the F indicator at the top zero mark of the scale, and launch the rod exactly 20
seconds after completion of stirring.
The apparatus should be free from vibration during the test. If the rod has slid (32 ± 4) mm
below the paste surface within 30 seconds after launching, the paste has reached the right
consistency. Continue to test the paste with different percentage of water until the right
consistency is obtained.
This consistency is the initial penetration. During the 30 second interval for initial penetration
setting return the excess paste to the bowl and then cover the bowl and stirrer.

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7.2.7.7.4 Determination of final penetration

After completing the initial reading, remove the launcher from the paste, clean it and then the
ring and plate are set back in their new positions.
This should be done with as little disturbance to the paste in the vicat ring as possible. Then
the launcher is touched to the paste surface, tighten the screw and set the F indicator exactly
at the top of the scale.
Release the launcher for the second time 5 minutes ± 10 seconds after completion of stirring
and record the final penetration 30 seconds after the rod is launched.

7.2.7.7.5 Determination of re-stirring penetration

When penetration has been determined by the above procedure and the cement stiffens
instantly, information on the rapid stiffening properties can be obtained by the following tests:
a) After completing the 5-minute penetration measurement, immediately return the paste
to the bowl.
b) Start the mixer, raise the bowl towards the mixing position and mix the contents of the
bowl again at medium speed, (285 ± 10) rpm for 1 minute.
c) Fill the ring and record the penetration by following the procedures set out in test
specimen molding and initial penetration determination items 7.2.7.7.2 and 7.2.7.7.3.

7.2.7.8 Calculations

Calculate the percent final penetration, based on the ratio of final penetration to initial
penetration, as follows:

B
%P= x 100
A
Description:
The final penetration percent;
A is the initial penetration, mm;
Badalah final penetration, mm.

7.2.7.9 Report

Report the test results as follows: Initial


penetration... .................................. mm.
Final penetration... ......................... mm.
Percent final penetration ................. %.
Re-stirring penetration..................... mm.

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7.2.8 Determination of heat of hydration

This test method includes determining the heat of hydration of hydraulic cement by
measuring the dissolution heat of dry cement and the dissolution heat of cement that has
been hydrated for 7 days and 28 days, the difference between these prices being the heat of
hydration during the respective hydration times.

7.2.8.1 Equipment

(1) The calorimeter apparatus (see Figure 18) consists of


a) Calorimeter, consisting of a wide-mouthed flask, with a cork lid, the inner walls of
which are lined with hydrofluoric acid-resistant material. The temperature of the
contents of the flask shall not change by more than 0.001o C/min for each degree
of difference in room temperature when filled with 425 grams of acid as specified in
7.2.8.3 item (2), closed and left without stirring for 30 minutes.
The temperature at the check should be close to the initial temperature at the
determination.
b) The insulation box contains an insulating layer of cotton or similar material, is at
least 25 mm thick and encloses the walls and base of the flask, but allows easy
removal of the flask.
c) Differential thermometers and differential thermometer comparators that can be
adjusted Beckmann type, with a scale division of 0.01o C and has a range of 6o C.
The thermometer should be set so that the limits of the scale are close to room
temperature.
The part of the thermometer that will enter the calorimeter must be protected with a
coating that is resistant to hydrofluoric acid.
The thermometer is equipped with a special reading lens.
The Beckmann thermometer at zero can be determined by dipping in the liquid and
comparing it with a comparison thermometer.
An accurate benchmarking thermometer with a range of 0.1o C was placed near
the calorimeter and used for temperature readings and to place the zero point of
the Beckmann thermometer.
d) Funnel
The funnel used to insert the sample in the calorimeter is made of glass or plastic
and has a stem with a length of ± 76 mm with an inner diameter of not less than 6
mm.
e) Stirrer
The stirrer consists of three propeller blades made of polyethylene having the size
shown in Figure 19 and should enter the calorimeter as close as possible to the
bottom of the calorimeter. The motor should have a constant speed of at least 1/20
hp (37 W) and should be equipped with a speed reduction gear so as to set a
constant speed between (350 - 700) rev/min.

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Figure 18 - Calorimeter apparatus

Figure 19 - Calorimeter stirrer

NOTE The stirrer as shown in Figure 19 is manufactured from commercial materials


comprising
of 3 polyethylene propeller blades has a propeller diameter of 34 mm, a shaft diameter of 6 mm,
a shaft length of 455 mm. The function of the stirrer is to keep the temperature of the entire
liquid uniform and provide sufficient stirring to provide to maintain the temperature of the liquid.
solid part suspended in mixed acid. It is important to maintain speed
constant stirring because this stirring generates heat.

(2) Mixer machine


A medium-speed mixer can be used for mixing cement and water to form an all-round
paste.

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(3) A mortar, ± 200 mm in diameter, and a pounder for pulverizing partially hydrated
samples.
(4) Plastic bottle, measuring ± (80 x 25) mm, with lid.
(5) Drying oven, which can maintain the temperature of (100 - 110)o C.
(6) Weighing bottle, ±40 mm high and ±25 mm wide, with lid.
(7) Timing device.
(8) Sieve No. 100 (150 µm) and No. 20 (850 µm).
(9) Crucible, 30 mL capacity, with lid for incandescent loss determination.
(10) A suitable furnace that is capable of maintaining a temperature of (900 - 950)o C.
(11) Scales and weighing stones according to specification items.

7.2.8.2 Reagents and materials

a) Hydrofluoric acid (b.j 1.15)


b) Nitric acid (2.00 N)
c) Nitric acid (HNO3 2.00 N) used for the calorimeter, must be prepared and standardized
in large quantities, alternatively dilute HNO3 can be made by dissolving 127 mL of
concentrated nitric acid per liter of solution, provided that each determination of heat
capacity is carried out with HNO3 that has been prepared.
d) Candles
Paraffin wax or other suitable wax, for sealing bottle caps.
e) Zinc oxide (ZnO) should be heated at (900-950)o C for 1 hour then cooled in a
desiccator, grinded to pass a No. 100 sieve (150 µm) and stored before determining
the heat capacity, immediately heat 7 grams of ZnO at (900-950)o C for no more than 5
minutes, cool to room temperature in a desiccator, and weigh it carefully to put it in the
calorimeter.

7.2.8.3 Procedure for determining the heat capacity of the appliance

(1) To determine the heat capacity of the system (i.e. the number of calories I or Joules
required to increase the temperature of the calorimeter and its contents by 1o C),
measure the corrected temperature rise obtained by dissolving 7 grams of the ignited
ZnO in the acid mixture specified in 7.2.8.3 items (2) to 7.2.8.3 item (5).
(2) Transfer into a vacuum bottle ± 400 grams of HNO3 2 N, which has been cooled to the
lower temperature indicated on a Beckmann thermometer (usually about (4 - 5)o C
below room temperature), add 8 mL of HF (b.j 1.15), weigh and add enough HNO3 2 N
to make the total weight of the solution 425 grams.
Then install the calorimeter and start the stirring motor. Keep the propeller or wall from
touching the thermometer.
The bottom funnel should be ±6 mm below the bottom surface of the cover and at least
12 mm above the liquid surface.
The upper end of the beckman thermometer bulb should be at least 38 mm below the liquid
surface.

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These conditions should be the same in all determinations. After an initial stirring period
of at least 20 minutes to bring the temperature of the system to the same, record the
room temperature to the accuracy of 0.1o C, the acid temperature to the accuracy of
0.001o C record the time and then feed the ZnO through the funnel at the same all-
round speed (NOTE 1).
In no less than one minute and no more than two minutes insert the ZnO. Brush with a
brush any ZnO attached to the funnel rod into the acid mixture.

NOTE 1 The temperature of the sample should match the room temperature when the sample is
loaded into the calorimeter.

(3) After the sample was inserted, the temperature with an accuracy of 0.001 °C at 20

minutes later
at 40 minutes. The first 20-minute period covers the dissolution period which is the
temperature rise without correction, while the second 20-minute period is the
continuation period. The temperature difference between 20 minutes and 40 minutes is
the correction that needs to be added or subtracted from the temperature rise,
according to whether the calorimeter temperature rises or falls during the continuation
period.
a) Calculate the corrected temperature rise as follows:

R0 = Q20 - Q 0
R = R0 - ( Q40 - Q )20

Description:
R0 is the observed temperature rise,o C;
Q20 is the temperature of the calorimeter at the end of the
dissolution period; Q0 is the temperature of the calorimeter
when the sample is introduced; The correction temperature
rise rate,o C;
Q40 is the temperature of the calorimeter at the end of the continuation period.

b) Calculate the heat capacity of the calorimeter and its contents as follows (NOTE 2):

W [ 1072 + 0.4 (30 - t ) + [ 0.5( T - t ) ]


C=
R
Description:
C is the heat capacity, kJ/o C;
W is the weight of ZnO, grams;
Tis the final temperature of the final calorimeter, (Q20 + the temperature at the
time the beckmann thermometer reading was zero),o C;
Tis the temperature of ZnO (room temperature), when it was put into the calorimeter,o C;
Radis the corrected temperature rise, C.o

NOTE 2 The heat of a ZnO solution is 256.1 cal/g at 30o C. This value increases by 0.1 cal/g for
each degree of temperature drop below 30o C. The heat capacity of ZnO is 0.12 cal/go C. The
heat required to bring the ZnO to the final temperature of the calorimeter must be included in the
effective heat of the solution.

(4) If enough ZnO is found to stick to the funnel or lid when the calorimeter is opened the
test is canceled.

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(5) Redetermine the calorific capacity of the calorimeter at the following times:
a) When the Beckmann thermometer is reset.
b) When a new coating is applied to a thermometer, stirrer or flask.
c) When a new thermometer, new flask and/or new stirrer is used.
d) If a new acid solution is used (HNO3 ).
e) When deemed necessary by the operator.

7.2.8.4 Procedure for determining the heat of hydration

a) Preparation of cement paste


Before paste preparation, place the cement and mixing water in a fixed temperature
room, at (23 ± 2)o C, until the cement and water are the same temperature as the room
temperature.
Mix 150 grams of cement and 60 mL of distilled water with a spatula, and stir the mixture
vigorously with a mechanical stirrer for 5 minutes.
Dispense equal portions of the paste into four or more plastic bottles evenly until it
reaches approximately 13 mm from the top and seal immediately (the sealed bottles
should be sealed with melted wax).
The bottles were stored in an upright position in a water bath at room temperature (23 ±
2)o C until the time of testing.
b) Preparation of partially hydrated sample material for solution heat testing. At the
specified test age, remove from storage a bottle containing partially hydrated sample
material. During the initial 20 minutes of stirring of the calorimeter, the plastic bottle is
broken and the sample is immediately crushed in a mortar with a pounder until the
sample passes an 850 micron sieve (No. 20), immediately put into a sealed weighing
bottle.
c) Be careful, especially with 7-day partially hydrated sample materials, to keep the
influence of air as small as possible, so that the influence of CO 2 or moisture loss from
the sample is as small as possible.

7.2.8.5 Calorimetric determination of hydration heat of dry cement

Determine the heat of hydration of the dry cement sample as done in 7.2.8.3 item (1) but use
3 grams of sample (weighed to an accuracy of 0.001 grams) of dry cement instead of ZnO.
Calculations and result reports are based on samples for which loss of glow has been
determined. Test partially hydrated samples for 7 days.

NOTE The heat of a ZnO solution is 256.1 cal/g at 30o C. This value increases by 0.1 cal/g for each
degree of temperature drop below 30o C. The heat capacity of ZnO is 0.12 cal/go C. The heat required
to bring the ZnO to the final temperature of the calorimeter must be included in the effective heat of the
solution.

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7.2.8.6 Determination of heat of hydration for partially hydrated samples

For the determination of solution heat of partially hydrated samples follow the dry cement
procedure as in 7.2.8.5 but use (4.18 ± 0.05) grams of partially hydrated cement samples.
Weigh to an accuracy of 0.001 grams. Calculations are expressed based on examples that
have been determined to have lost their glow.

7.2.8.7 Missing incandescence

Immediately before and after the samples for calorimeter determination of the heat of
hydration are weighed, weigh the same number of samples in a crucible for determination of
the loss of incandescence.
The missing incandescent value used is the average result of two determinations.

For determination of loss of incandescence of dry cement, incandesce a sample of dry


cement at a temperature of (950 ± 50)o C for at least 1.5 hours, then after that immediately
transfer it to a desiccator, let it stand until room temperature, and immediately weigh it.
When determining the loss of incandescence of hydrated cement, first dry the weighed sample
in an oven at (100-110)o C for 1 hour, transfer it to a furnace at (950 ± 50)o C for 1 night, or on
a suitable heater for not less than 5 hours, cool it in a desiccator to room temperature and then
weigh it. Calculate the weight of the incandescent base sample inserted in the calorimeter as
follows:

A x W
Wi =
B

Description:
Wiis the weight of the sample calculated on the basis of the incandescent inserted in the
calorimeter, grams;
A is the weight of the sample after it has been refined, grams;
The weight of the sample before it was refined, grams;
W is the weight of the sample inserted in the calorimeter, grams.

In addition to the lost-flare procedure for portland cement, the lost-flare determination can be
determined using the referee method as given in the test method in 7.1.3.12 for portland
cement slag and slag cement.
a) Determine the SO content3 using the referee method corresponding to the test method
in 7.1.3.11.1. Also determine the SO content3 of unrefined cement using the same
method.
b) Calculate the weight percentage obtained from sulfur sulfide as follows: G

= 0.8 (S1 - S )2

Description:
The weight percent obtained in the refined sample; S1 is SO3 in the
refined sample;
S2 is SO3 in the unquenched sample; 0.8 is the
molecular weight ratio 4(O)/SO3 .

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c) Calculate the weight of a dry calorimetric sample on the basis of the following:

(A-BG/100) W
Wi =
B

Description:
Wiis the weight of the dry sample, on an incandescent basis, grams;
A is the weight of the dry sample that was incinerated, grams;
B is the weight of the dry sample before spinning, grams;
G is the weight percentage obtained from sulphur sulfide, and; W
is the weight of the dry calorimetric sample, grams.

d) Calculate the weight of a partially hydrated calorimetric example on an incandescent


basis as below:

A.W(1-G/100)B
Wi =
Description:
Wi is the weight of the dry calorimetric sample, on an incandescent basis, grams;
A is the weight of the partially hydrated sample after spinning, grams;
B is the weight of the partially hydrated sample before spinning, grams;
Gad is the weight percentage obtained from sulfur sulfide;
W is the weight of the dry calorimetric sample, grams.

NOTE The assumption is made in the calculations that the percent sulfide is the same
as before sparging for partially hydrated samples as specified in the cement.

7.2.8.8 Calculations

7.2.8.8.1 Dissolution calorific of dry cement

Calculate the corrected temperature rise as in 7.2.8.3 item (3)a) and 7.2.8.3 items
(3)b). Also correct the dissolution heat value if the temperature differs from the temperature
of the calorimeter when the sample was introduced. Thus, for dry cement which has a
specific heat of about 0.8 kj/kg.K, if the final temperature of the calorimeter exceeds the
temperature at which the cement sample was introduced, add a correction of 0.8 kj/kg.K, to
the heat of that temperature when calculating the dissolution heat. Calculate the dissolution
heat of dry cement as follows:

H1 = (RC/Wi ) - 0.8 (T - t )d

Description:
H1 is the dissolution heat of dry cement, kJ/kg;
is the corrected temperature rise,o C; C is the heat
capacity, kJ/°C;
Wi is the weight of the sample calculated on an
incandescent basis, grams; T is the room temperature at the
time the sample is introduced,o C;
td is the final temperature of the calorimeter at the end of the dry cement measurement,o C.

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7.2.8.8.2 Calor of dissolution of partially hydrated materials
Calculate the dissolution heat of partially hydrated samples the same as for dry cement,
except that the following corrections are made:
Because every 1o C increase in temperature during the dissolution heat test causes a
decrease in the solution heat of approximately 1.3 kJ/kg. So if the temperature of the partially
hydrated dissolution heat test exceeds the dry cement determination temperature, add a
correction of 1.3 kJ/kg to the dissolution heat value obtained for the partially hydrated
example.
Also, correct the calorific value of the solution if the final calorimeter temperature differs from
the calorimeter temperature at the time of the test.
For example partially hydrated cement from incandescent cement has a specific heat of
about 1.7 kJ/kg. If the final calorimeter temperature exceeds the sample temperature at the
time of insertion, add a correction of 1.7 kJ/kgo C when calculating the heat of dissolution.

H2 = (RC/Wi ) - 1.7 (T-th ) - 1.3 (td - t )h

Description:
H2 is the dissolution heat of the partially hydrated sample,
kJ/kg; R,C,Wi ,T and td are as in 7.2.8.8.1;
th is the calorimeter temperature at the end of measurement of the partially hydrated
example,o C.

7.2.8.8.3 Calor of hydration

The final calorimeter temperature of 25o C should be considered as the basic reference heat
of hydration, and it is important to remember the effect of variations at this temperature in the
consideration of test results. An increase in final temperature increases the heat of hydration
by approximately 0.4 kJ/kg.K, of incandescent cement.
For example, if the final temperature is 27o C, 0.8 kJ/kg must be deducted from its heat of
hydration in order to refer to the result of 25 C.o
The observation for the final calorimeter temperature is about 25o C, be careful in the
observation of the final temperature. Calculate the heat of hydration of cement carefully as
follows:

H= H1 - H2 - 0.4 (th - 25.0)

Description:
H is the heat of hydration of incandescent cement, kJ/kg;
H1 is the heat of dry cement solution, 7.2.8.8.1;
H2 is the heat of partially hydrated cement solution 7.2.8.8.2; th
is the same value as in 7.2.8.8.2.

7.2.8.9 Retest

In case of failing to meet the 28-day hydration heat requirement, the reserve paste sample
can be tested at the next age and corrected by 2.1 kJ/kg per day for each additional age. To
carry the calculation result of solution heat at 28 days.

The excess period for which this correction is made shall be limited to 4 days. In case of failing
to meet the requirement of 7 days, retest entirely including stirring of the paste.

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7.2.8.10 Accuracy and bias

7.2.8.10.1 Thoroughness

7.2.8.10.1.1 Single operator precision

The standard deviation of a single operator is 12.2 kJ/kg (1 second) and 14.8 kJ/kg (1
second) for dissolution heat and hydration heat respectively. Therefore, the results of two
tests performed by the same operator for samples of the same cement should not differ by
more than 34 kJ/kg in the determination of the heat of dissolution or 42 kJ/kg in the
determination of the heat of hydration.

7.2.8.10.1.2 Multi-laboratory rigor

The multi-laboratory standard deviation is 18.5 kJ/kg for dissolution heat and 16.9 kJ/kg for
hydration heat. Therefore, for two tests carried out for two different laboratories for samples
of the same cement should not differ by more than 52 kJ/kg for the determination of
dissolution heat or 48 kJ/kg for the determination of hydration heat.

7.2.8.10.2 Bias

There is no statement on bias as there is no acceptable reference material.

7.2.9 Sulfate-induced expansion testing

This test method, used only for Portland cement, involves determining the expansion of
mortar bars made from a mixture of Portland cement and gypsum in such proportions that
the sulfur trioxide (SO3 ) content in the mixture is 7.0% by weight. Values are specified in mm
per gram and are expressed as standards.

7.2.9.1 Purpose and use

This test method is intended primarily for use by those interested in research on potential
determination methods of sulfate resistance of Portland cement. This method is also used to
ensure that the sulfate resistance of Portland cement meets the requirements in Table 4.

7.2.9.2 Equipment

a) Scales and weighing stones must be within specifications.


b) Flow table, must meet the specification requirements (See Figure 16).
c) The mixer, bowl and stirrer must meet the specifications in Appendix C.
d) Stirring knives, triangular knives, pounder must meet specifications.
e) Measuring cups, molds and length comparators must meet specifications.

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7.2.9.3 Temperature and humidity

a) The temperature of the molding room, dry ingredients and stirring water should be
maintained at 23.0
± 4 °C.
b) The humidity of the printing room should not be less than 50%.

7.2.9.4 Ingredients

a) The sand used to make the test mortar shall meet the sand quality requirements as per
7.2.6.4.
b) Gypsum used for addition to Portland cement must be high quality natural gypsum with
100% passing a 150 µm sieve (no. 100), at least 94% passing a 75 µm sieve (no. 200)
and at least 90% passing a 45 µm sieve.
(no. 325).
Calculate the percentage of cement and gypsum required so that the mixture
containing 7.0% by weight of SO3 as follows:

% cement= [ ( g - 7.0 ) / ( g - c ) ] x 100


% gypsum = [ (7.0 - c ) / ( g - c ) ] x 100

Description:
c is the SO content3 in Portland cement, %;
girl is the SO content3 in gypsum, %;
7.0 is the SO content3 of the cement - gypsum mixture, %.

7.2.9.5 If the SO3 content of the gypsum is unknown, the gypsum shall be analyzed for its
SO3 content using the SO3 chemical analysis method of cement. The SO3 content shall be
determined with an accuracy of 0.1%.

7.2.9.6 Number and size of test specimens

a) For each cement sample, two mixes were made, each mix for 3 specimens. The size of
each specimen was (25 x 25 x 285) mm.
b) In routine testing, test specimens with a size of (25 x 25 x 160) mm can be used, but in
the case of disputes, the results obtained must be based on the size of the test
specimen (25 x 25 x 285) mm.

7.2.9.7 Procedure

7.2.9.7.1 Test mold preparation

a) The mold should be prepared according to Figure 11.


b) The amount of dry ingredients required for each mix shall be 400 grams (cement plus
gypsum) and 1 100 grams of sand. The amount of mixing water should be 194 mL for all
types of Portland cement.
c) Mix the mortar according to the mortar mixing procedure of Appendix C, except after
putting the mixing water into the bowl, add the gypsum and mix at low speed for 15
seconds, then stop mixing, add the cement, and continue as described in Appendix C.

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7.2.9.7.2 Test piece molding

Immediately after the flow test is completed, transfer the mortar back to the bowl, remove any
mortar stuck to the bowl wall, and mix again at medium speed (285 ± 10) rpm for 15
seconds. Remove the mixer and bowl from the mixer and put the excess mortar from the
mixer into the bowl. Fill the mold in two layers, each layer compacted with a pounder.

Push the mortar into the corners, around the bolts, and along the mold surface by pounding
until a homogeneous test piece is obtained.
After the top layer is solidified, cut off the excess mortar until it is flush with the top surface of
the mold and smooth the mold surface several times with a triangular stirring knife.

7.2.9.7.3 Test specimen storage

7.2.9.7.3.1 Initial storage

Moisten the test specimen in the mold in a humid cabinet at (23 ± 2) o C for (22-23) hours,
then remove the test specimen from the mold, marked accordingly and place it in water at
(23 ± 2)o C for at least 30 minutes before the initial measurement.

7.2.9.7.3.2 Advanced storage

After the test piece rod has been removed from its mold and has been measured,
horizontally place the test piece in water at a temperature of (23 ± 2) C. o
The placement of each test specimen shall be at least 6 mm apart on all sides except for
necessary supports.
All test specimens shall be submerged in water at least 13 mm deep. The ratio of the volume
of water to the volume of test specimens shall not be more than 5: 1 to prevent excessive
lime solubility.
Replace the bath water with fresh water every 7 days for the first 28 days and every 28 days
after that.

7.2.9.7.4 Length gauge

Measure the length of the specimen using a length comparison tool. Remove the specimens
from the water bath one by one, and wipe them with a damp cloth before measurement.

Take the first measurement at 24 hours ± 15 minutes from the time of mixing cement and
water. Measure the specimens again at the age of 14 days.

NOTE Addition of data from measured prices can be obtained by re-soaking the specimens after the
14-day test and taking additional measurements at a later age.

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7.2.9.8 Calculations

Calculate the difference in length of the specimens at 24 hours and 14 days with an accuracy
of 0.001% of the effective length and report it as the expansion of the specimens during that
period. All test specimens remaining for 14 days shall consist of 1 set of at least three test
specimens with allowable bushels depending on the number of test specimens remaining, as
follows:

Table 21 ̶ Deviation
Maximum allowable length
Number of test
deviation (%)
pieces
3 0,010
4 0,011
5 0,012
6 0,012

7.2.9.9 Report

Report the average length of a batch of test specimens meets the above conditions with an
accuracy of 0.001%.

7.2.10 Mortar air content testing

The purpose of testing with this method is to determine the air content in the mortar.

7.2.10.1 Equipment and materials

a) Flow tables, molds and calipers, as per 7.2.6.3.


b) The measuring instrument is a cylinder with an inner diameter of (76 ± 2) mm with a
depth of 88 mm standardized with (400 ± 1) mL water at a temperature of (23 ± 2)o C.
c) For the purpose of this test the capacity of the gauge is expressed in mL which is the
weight of water divided by 0.997 6. No correction for weight due to foam is made. The
gauge shall have an even wall thickness, a wall and base thickness of not less than 2.9
mm and a total empty weight of not more than 900 grams. The gauge shall be made of
metal material that is not damaged by cement.
d) Stirring machine, mixing bowl.
e) Slicing and leveling knife.
Slicing and grading knives are made of steel with a length of not less than 200 mm and a
thickness of 1.5 mm to 3.5 mm with a straight edge.
f) Scales that have a capacity of 2 kg with an accuracy of 1 gram.
g) 250 mL measuring cup with 2 mL measurement accuracy.
h) Pounder.
i) The metal spoon has a length of 230 mm and a bend length of 100 mm.

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7.2.10.2 Temperature and humidity

The room and dry material are kept at (23 ± 4)o C with room humidity not less than 50%.
Stirring and measurement water conditions at (23 ± 2) °C.

7.2.10.3 Standard sand

The standard sand used is Ottawa sand (standard sand 20-30) with the following grain
gradation:

Table 22 ̶ Ottawa sand grain gradation


Sieve hole diameter Sieve pass, (%)
1.18 mm 100
850 microns (85 - 100)
600 microns (0 - 5)

7.2.10.4 Procedure

7.2.10.4.1 Mixture arrangement

Portland cement :350 grams


Standard sand gradation 20-30 1 400 grams
Enough water to give a spread of (87.5 ± 7.5)%.

7.2.10.4.2 Stirring mortar

Install the stirrer and dry mixing bowl on the stirrer in the stirring position. Then put the
ingredients for one stirring into the bowl as follows:
a) Put the mixing water into the bowl.
b) Add the cement to the water, then start the mixer and stir at low speed (140 ± 5) rpm for
30 seconds.
c) Add all the sand slowly in 30-second intervals, while stirring at low speed (140 ± 5) rpm.
d) Stop the mixer, switch to medium speed (285 ± 10) rpm, and mix for 30 seconds. Stop
the mixer and leave the mortar for 1.5 minutes. During the first 15 seconds of this time,
immediately wipe off the mortar that sticks to the inner wall of the bowl, then close the
bowl.
e) Continue final stirring for 1 minute at medium speed (285 ± 10) rpm.
f) If necessary, at each interval when re-stirring is required, any mortar adhering to the
inner wall of the bowl should be removed immediately with a rake before re-stirring.

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7.2.10.4.3 Determination of mortar spread

Place the mold in the center of the flow table, which is first wiped dry. Fill the mold to a height
of 25 mm. Compact the mixture with a pounder for 20 times. The pounding pressure must be
sufficient so that the filling is completely flat. Fill the mold again to the brim and compact it
like the first layer. Then level the top of the mortar with a leveling knife in two perpendicular
directions.
Clean and dry the surface of the flow table on the outside of the mold. Remove the mold from
the mortar 1 minute after completion, tap the flow table from a height of 12.7 mm 10 times
within 6 seconds. The average spread that occurs is measured with a caliper from 4
measurements at different angles.
The measurement results are expressed in percent of the initial diameter. Repeat the work
as above with different amounts of water, until the desired spread is achieved. Each
repetition uses new mortar.

7.2.10.4.4 Determination of air content

If you have obtained the intended distribution, weigh the remaining 400 mL of mortar. Put the
mortar with a spoon into the measuring instrument in 3 layers. Each layer is compacted by
puncturing with a leveling knife 20 times along the inside of the mold. In puncturing the first
layer, the puncture should not hit the bottom of the mold. The second and last puncture is
enough to penetrate each layer of mortar. To remove air retained in the mortar, tap the side
of the gauge gently with a pounding stick at 5 different points around the gauge, one for each
mortar. To remove air retained in the mortar, tap the side of the gauge slowly with the
pounding stick at 5 different points around the gauge, 1 tap each.
Flatten the surface of the mortar in the gauge with a leveling knife in two perpendicular
directions. If during leveling any sand grains come out of the mortar and cause scratches, the
equipment should be repeated. All this work should be completed within 1.5 minutes. Clean
the mortar and water out of the gauge. Weigh the gauge and its contents and calculate the
weight of the mortar in grams.

7.2.10.5 Calculation of air content

Calculate the air content of the mortar with the formula below: Air

content = 100 - W [(182.7 + P)/(2 000 + 4 P)]

Description:
W is the weight of 400 mL of mortar, grams;
It is the percentage of water to the weight of cement used.

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8 Test pass requirements

Portland cement tested is declared unqualified if:


a) Cement fails to meet any of the quality requirements as listed in article 5.
b) A retest may be conducted on cement in storage in silos that will be shipped for a period
of more than 6 months. If the result of the retest fails to meet any of the quality
requirements as listed in Article 5, the cement shall be declared not to have passed the
test.
c) Certification of portland cement test results as qualified only applies to the sample group.

9 Packaging

9.1 Portland cement can be traded in packaged and bulk form. Unless otherwise specified,
packaged Portland cement shall be packed in bags with a net weight of 25 kg, and or 40 kg,
and or 50 kg for each bag.

9.2 Weight deficiency should not exceed 2% of the weight stated on each package.

10 Marking requirements

The packaging must include the code, brand/trade mark, type, company name and net
weight. For bulk portland cement the marking is included in the shipping document.

11 Storage and transportation

a) Semen when stored or transported must be maintained in a manner that allows for
easy inspection and identification.

b) Bulk cement is stored in weather-tight buildings/storages, which protects the cement


from moisture and avoids cement caking during storage and transportation.

c) Storage and transportation of cement in bags is done in such a way that it is protected
from the effects of weather.

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Appendix A
(informative)
Example of chloride determination record form

Table A.1 - Example of equivalent point determination form in chloride determination

Column 1 Column 2 Column Column


AgNO3 , Potential, mV 
3 mVA 4
 2mVB
mL
1,60 125,3
5,8
1,80 119,5 1,4
7,2
2,00 112,3 1,3
8,5
2,20 103,8 1,3
9,8
2,40 94,0 0,6
9,2
2,60 84,8 2,3
6,9
2,80 77,9 0,8
6,1
3,00 71,8 1,3
4,8
3,20 67,0

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Appendix B
(informative)
Example of qualification result

Table B.1 - Initial bonding time


units in minutes
Initial Average
Initial binding of
Cement Series binding of difference
method A
method B (spec. max 45)

A 1 95 105 ...

A 2 90 105 ...

A 3 95 90 ...

Julat
5 15 ...
(spec. 30 Max)

Average 93,3 100,0 6,7

B 1 100 120 ...

B 2 105 95 ...

B 3 85 95 ...

Julat
20 25 ...
(Spec. 30 Max)

Average 96,7 103,3 6,7

C 1 155 170 ...

C 2 155 160 ...

C 3 145 155 ...

Julat
10 15 ...
(spec. 30 Max)

Average 151,7 161,7 10,0

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Table B.2 - Final bonding time

units in minutes
Final Average
Final binding of
Cement Series binding of difference
method A
method B (spec. max 45)

A 1 150 150 ...

A 2 145 150 ...

A 3 170 125 ...

Julat
25 25 ...
(spec. 30 max)

Average 155,0 141,7 13,3

B 1 185 180 ...

B 2 200 180 ...

B 3 185 155 ...

Julat
15 25 ...
(spec. 30 max)

Average 190,0 171,7 18,3

C 1 235 225 ...

C 2 240 220 ...

C 3 240 215 ...

Julat
5 10 ...
(spec. 30 max)

Average 238,3 220,0 18,3

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Appendix C
(informative)
Mechanical stirring of hydraulic cement paste and
plastic consistency of mortar

C.1 Scope

This practical method involves mechanically stirring the hydraulic cement paste and plastic
consistency of the mortar.

C.2 Purpose and use

This method is intended for use in mechanized stirring of pastes and mortars for hydraulic
cement testing.

C.3 Equipment

C.3.1 Mixer machine

The stirring machine must be an epicyclic type mechanical stirring machine, which has an
electrically driven device that can move the stirrer to rotate horizontally and circulate.
The stirrer must have two speeds that can be adjusted mechanically. The first speed, a low
speed that can drive the agitator at (140 ± 5) rpm with a circular motion of the agitator blades
at (285 ± 10) rpm with a circular motion of the agitator rods at approximately 125 rpm. The
electric motor power must be at least 124 watts (1/6 hp).
The mixer shall be equipped with a spacer holding device as shown in Figure 12 which shall
be used to keep the distance between the bottom of the mixer and the bottom of the bowl no
greater than 2.5 mm, but no smaller than 0.8 mm (approximately equal to the diameter of
Ottawa sand (20 - 30) when the bowl is in the stirring position.

C.3.2 Stirrer

The stirrer should be easily disassembled, made of stainless steel, and the basic design as
described in Figure 13. If in the stirring position following the shape of the bowl used, the
closest distance between the stirrer tip and the inner wall of the bowl should be ±4.0 mm but
not less than 0.8 mm.

C.3.3 Mixing bowl

The demountable mixing bowl shall have a nominal capacity of 4.73 L. It shall have the
dimensions shown in Figure 14, and shall be made of stainless steel. The bowl shall be
equipped with a part that can be firmly attached to the stirring equipment in a firm position
during stirring.

Must be equipped with a lid made of non-absorbent material and not damaged by cement.

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C.3.4 Verifier

The scraper shall consist of a semi-rigid rubber blade fitted with a handle that is ±150 mm
long. The blade shall be ± 75 mm long, 50 mm wide and tapered to a thin side section of ± 2
mm.

C.3.5 Additional equipment

Scales, weighing stones, measuring cups other tools used in the measurement and
preparation of mortar materials before stirring shall meet the corresponding requirements.

C.4 Temperature and humidity

C.4.1 One room, dry ingredients, stirrers and bowls should be kept between (20 -
27.5)o C. Mixing water temperature should be (23 ± 1.7) C
̊ .

C.4.2 Laboratory humidity is at least 50%. Temperature and humidity in accordance with
7.2.1.1.

C.5 Ingredients, proportions and consistency

C.5.1 Requirements

The ingredients, proportions and consistency of the ingredients and their quantities must
meet the requirements of the particular method by which the paste or mortar is prepared.

C.5.2 Paste stirring procedure

C.5.2.1 Install the stirrer and the dry bowl on the stirrer in the stirring position. Then put the
ingredients for one stirring into the bowl as follows:
a) put all the mixing water into a bowl;
b) add cement into water and let stand 30 seconds, for water absorption;
c) Run the mixer at a low speed of 140 rpm ± 5 rpm for 30 seconds.

C.5.2.2 Stop the mixer for 15 seconds and during this time clean the inner walls of the bowl
of any stuck-on paste.

C.5.2.3 Run the mixer at medium speed at (285 ± 10) rpm and mix for 1 minute.

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C.5.3 Mortar stirring procedure

C.5.3.1 Install the stirrer and dry mixing bowl on the stirrer in the stirring position. Then
put the ingredients of one stirring into the bowl as follows:
a) put the mixing water in a bowl;
b) add cement to the water, then run the mixer while stirring at a low speed of 140 rpm ± 5
rpm for 30 seconds;
c) add all the sand slowly in 30-second intervals, while stirring at a low speed of 140 rpm ± 5
rpm.

C.5.3.2 Stop the mixer, switch to medium speed (285 ± 10) rpm, and mix for 30 seconds.

C.5.3.3 Stop the mixer and leave the mortar for 1.5 minutes. During the first 15 seconds of
this interval, immediately wipe off the mortar that sticks to the inner wall of the bowl, then
close the bowl.

C.5.3.4 Continue final stirring for 1 minute at medium speed (285 ± 10) rpm.

C.5.3.5 If necessary, at each interval when re-stirring is required, any mortar adhering to
the walls of the bowl section should be removed immediately with a rake before re-stirring is
carried out.

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Bibliography

ASTM C 150/C150M-12, Standard Specification for Portland Cement


ASTM C114-13, Standard Test Methods for Chemical Analysis of Hydraulic Cement
ASTM C109/C109M-13, Standard Test Method for Compressive Strength of Hydraulic
Cement Mortars (Using 2-in. or [50-mm] Cube Specimens)
ASTM C 151/C151M-09, Standard Test Method for Autoclave Expansion of Portland
Cement.
ASTM C 186-13, Standard Test Method for Heat of Hydration of Hydraulic Cement.
ASTM C 187-11e1, Standard Test Method for Amount of Water Required for Normal
Consistency of Hydraulic Cement Paste
ASTM C 191-13, Standard Test Method for Time of Setting of Hydraulic Cement by Vicat
Needle
ASTM C204-11, Standard Test Methods for Fineness of Hydraulic Cement by Air Permeability
Apparatus
ASTM C115/C115M-10e1, Standard Test Method for Fineness of Portland Cement by the
Turbidimeter
ASTM C 266-13, Standard Test Method for Time of Setting of Hydraulic Cement Paste by
Gillmore Needles
ASTM C 451-13, Standard Test Method for Early Stiffening of Hydraulic Cement (Paste
Method).
ASTM C185-08, Standard Test Method for Air Content of Hydraulic Cement Mortar
ASTM C 778-13, Standard Specification for Standard Sand
ASTM C 183-13, Standard practice for sampling and the amount of testing of hydraulic
cement.
BS 12-2008, Specification for portland cement
ASTM C452/C452M-10, Standard Test Method for Potential Expansion of Portland-Cement
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