FINAL DRAFT UGANDA 
STANDARD  
  FDUS EAS 148-4 
First  Edition  
2018-mm-dd 
 
 Reference number  
FDUS EAS 148-4: 2017 
© UNBS 201 8 
  
Cement  — Test Methods  — Part 4: Quantitative determination 
of constituents  
 FDUS EAS 148 -4:2017 
ii                © UNBS  2018  - All rights reserved  
 Compliance with this standard does not, of itself confer immunity from legal obligations  
A Uganda Standard does not purport to include all necessary provisions of a contract. Use rs are 
responsible for its correct application  
© UNBS 2018  
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilised in any 
form or by any means, electronic or mechanical, including photocopying and microfil m, without prior written 
permission from UNBS.  
Requests for permission to reproduce this document should be addressed to  
The Executive Director  
Uganda National Bureau of Standards  
P.O. Box 6329  
Kampala  
Uganda  
Tel: +256 41 7 333 2 50/1/2 
Fax: +256 41 4 286 123  
E-mail: info@unbs.go.ug  
Web: www.unbs.go.ug  
 FDUS EAS 148 -4:2018 
© UNB S 2018  - All rights reserved                 iii National foreword  
Uganda National Bureau of Standards (UNBS) is a parastatal under the Ministry of Trade, Industry and 
Cooperatives established under Cap 327, of the Laws of Uganda, as amended.  UNBS is mandated to co -
ordinate the elaboration of standards and is  
(a) a member of International Organisation for Standardisation (ISO) and  
(b) a contact point for the WHO/FAO Codex Alimentarius Commission on Food Standards, and  
(c) the Nat ional Enquiry Point on TBT Agreement of the World Trade Organisation (WTO).  
The work of preparing Uganda Standards is carried out through Technical Committees. A Technical 
Committee is established to deliberate on standards in a given field or area and con sists of representatives of 
consumers, traders, academicians, manufacturers, government and other stakeholders.  
Draft Uganda Standards adopted by the Technical Committee are widely circulated to stakeholders and the 
general public for comments. The committ ee reviews the comments before recommending the draft standards 
for approval and declaration as Uganda Standards by the National Standards Council.  
This Uganda Standard, US EAS 148 -4: 2017, Cement — Test methods — Part 4: Cement  — Test Methods  — 
Part 4: Qu antitative determination of constituents,  is identical with and has been reproduced from an East 
African Standard, EAS 148 -4: 2017 , Cement — Test methods — Part 4: Quantitative determination of 
constituents , and adopted as a Uganda Standard.  
The committee  responsible for this document is Technical Committee UNBS/TC 3, Building and construction .  
This standard cancels and replaces US 100 -4:2016, Cement — Test methods — Part 4: Quantitative 
determination of constituents (2nd Edition) , which has been technica lly revised.  
   EAS 148 -4: 201 7 
ICS 91.100.10  
© EAS 2017                                                                                                                           Second Edition  2017  
  
 
EAST AFRICAN STANDARD  
Cement  — Test Methods  — Part 4: Quantitative determination of 
constituents  
EAST AFRICAN COMMUNITY  EAS 148 -4: 201 7 
ii © EAC 2017  – All rights reserved  
 Copyright notice  
This EAC document is copyright -protected by EAC. While the reproduction of this document by 
participan ts in the EAC standards development process is permitted without prior permission from EAC, 
neither this document nor any extract from it may be reproduced, stored or transmitted in any form for 
any other purpose without prior written permission from EAC.  
Requests for permission to reproduce this document for the purpose of selling it should be addressed 
as shown below or to EAC’s member body in the country of the requester:  
© East African Community  2017  — All rights reserved  
East African Community  
P.O.Box 1096  
Arusha  
Tanzania  
Tel: 255 27 2504253/8  
Fax: 255 27 2504481/2504255  
E-mail: eac@eachq.org  
       Web: www.eac -quality.net  
Reproduction for sales purposes may be subject to royalty payments or a licensing agreement.  
Violators may be persecuted  EAS 148 -4: 201 7 
© EAC 2017 – All rights reserved  iii 
 Contents  Page 
Foreword  ................................ ................................ ................................ ................................ ............................  iv 
1 Scope  ................................ ................................ ................................ ................................ ......................  1 
2 Normative references  ................................ ................................ ................................ ............................  1 
3 General requirements for testing  ................................ ................................ ................................ .........  1 
3.1 Number of tests  ................................ ................................ ................................ ................................ ..... 1 
3.2 Determination of constant mass  ................................ ................................ ................................ ..........  2 
3.3 Expression  of masses and results  ................................ ................................ ................................ ...... 2 
3.4 Repeatability and reproducibili ty ................................ ................................ ................................ .........  2 
4 Preparation of a cement sample  ................................ ................................ ................................ ..........  3 
5 Reagents  ................................ ................................ ................................ ................................ ................  3 
6 Determinatio n of the constituent content of cements with more than three constituents  ............  3 
6.1 General  ................................ ................................ ................................ ................................ ...................  3 
6.2 Selective dissolution method  ................................ ................................ ................................ ...............  4 
6.2.1  Principle  ................................ ................................ ................................ ................................ .................  4 
6.2.2  Reagents  ................................ ................................ ................................ ................................ ................  4 
6.2.3  Apparatus  ................................ ................................ ................................ ................................ ...............  5 
6.2.4  Procedure  ................................ ................................ ................................ ................................ ...............  5 
6.2.5  Calculation of the contents of cement constituents  ................................ ................................ ..........  7 
6.2.5.2  Calculation of the contents of insoluble residues  ................................ ................................ .............  7 
6.2.6  Repeatability and reproducibility  ................................ ................................ ................................ .........  9 
6.2.7  Qualitative determination of th e type of cement.  ................................ ................................ .............  10 
7 Determination of the contents  of constituents for cements with three constituents  ..................  10 
7.1 General  ................................ ................................ ................................ ................................ .................  10 
7.2 Determination of the slag content  ................................ ................................ ................................ ..... 10 
7.2.1  Dense liquid separation method  ................................ ................................ ................................ ........  10 
7.2.2  Microscope  method  ................................ ................................ ................................ .............................  16 
7.3 Determination of the siliceous fly ash content  ................................ ................................ ................  19 
7.3.1  Selective dissolution method  ................................ ................................ ................................ .............  19 
7.4 Determination of the natural pozzolana content  ................................ ................................ ..............  21 
7.4.1  Selective dissolution method  ................................ ................................ ................................ .............  21 
7.4.2  Dense liquid separation method  ................................ ................................ ................................ ........  24 
 EAS 148 -4: 201 7 
iv © EAC 2017  – All rights reserved  
 Foreword  
Development of the East African Standards has been necessitated by the need for harmonizing requirements 
governing quality of products and services in th e East African Community. It is envisaged that through 
harmonized standardization, trade barriers that are encountered when goods and services are exchanged 
within the Community will be removed.  
In order to achieve this objective, the Community establishe d an East African Standards Committee mandated 
to develop and issue East African Standards.   
The Committee is composed of representatives of the National Standards Bodies in Partner States, together 
with the representatives from the private sectors and con sumer organizations. Draft East African Standards 
are circulated to stakeholders through the National Standards Bodies in the Partner States. The comments 
received are discussed and incorporated before finalization of standards, in accordance with the proc edures 
of the Community.  
East African Standards are subject to review, to keep pace with technological advances. Users of the East 
African Standards are therefore expected to ensure that they always have the latest versions of the standards 
they are implem enting .  
EAS 148-4 was prepared by Technical Committee EASC/TC /026, Cement, lime, clay and related products . 
In the preparation of this East African Standard, reference was made to the following standard:  
CEN /TR 196-4: 200 7; Methods testing cement - Part 4: Quantitative Determination of constituents.  
The assistance derived from the above source is hereby acknowledged with thanks . 
This second edition cancels and replaces the first edition (EAS  148-4:2000), which has been technically 
revised.  
EAS 148 consis ts of the following parts, under the general title Cements  — Test methods : 
 Part 1: Determination of strength  
Part 2: Chemical analysis of cement  
Part 3: Determination of setting times and soundness  
Part 4: Quantitative Determination of constituents  
Part 5: Pozzolanicity test for pozzolanic cement  
Part 6: Determinatio n of fineness  
 Part 7: Method of taking and preparing samples of cement  
 Part 8: Heat of hydration – Solution method   
 EAST AFRICAN STANDAR D EAS 148 -4: 201 7 
 
© EAC 2017  – All rights reserved  1 
 Cement  — Test Methods  — Part 4: Quantitative determination of 
constituents  
1 Scope  
This East African Standard describes the procedure s for determining the contents of the most of the 
constituents of cements that fall within the scope of FDEAS 18 -1. 
The method given in Clause 6 applies to all cements, whatever the number and nature of their constituents.  
In the case where the operator is  certain that the cement contains only, over and above the clinker and set 
regulator, blastfurnance slag, fly ash or pozzolana, the other methods given in Clause 7 can be applied.  
2 Normative references  
The following referenced documents are indispensable for the application of this document. For dated 
references, only the edition cited applies. For undated references, the latest edition of the referenced 
document (including any amendments) applies.  
EAS 18 -1, Cement — Part 1: Composition, specifications and  conformity criteria for common cements  
EAS 148 -2, Cements — Test Methods — Part 2: Chemical analysis of cement  
EAS 148 -7, Cements — Test Methods — Part 7: Methods of taking and preparing samples of cement  
ISO 385, Laboratory glassware — Burettes  
 ISO 835,  Laboratory glassware — Graduated pipettes  
3 Requirements  for testing  
3.1 Number of tests  
To carry out the calculation for the contents of the cement constituents, two tests shall be made for each. The 
following analytes are determined:  
a) for the method of c hoice by selective dissolution (clause 6): sulfuric anhydride and carbon dioxide 
contents, residues after EDTA and nitric acid dissolution and sulfide contents in the cement and in the 
EDTA residue;  
b) for the methods of analysis for cements with three consti tuents (clause 7): sulfuric anhydride and 
carbon dioxide contents, loss on ignition, calcium oxide, magnesium oxide and manganese oxide 
contents, sulfide contents, sulfide contents and insoluble residues. Depending on the method used, 
only some of these an alytes can be determined.  
If, for each analyte, the difference between the two values obtained is less than twice the standard deviation 
for repeatability for this analyte, the value to take for further calculations is the arithmetic mean of the two EAS 148 -4: 201 7 
2 © EAC 2017  – All rights reserved  
 values . If the difference between the two values is greater than twice the standard deviation for repeatability, a 
third test shall be carried out and the value to be taken for further calculations shall be arithmetic mean of the 
two closest values.  
Hence, for t he method of choice by selective dissolution, only one calculation shall be carried out for the 
quantitative determination of constituents, in particular for clinker.  
Likewise, for the methods of analysis for cements with three constituents, a single calcu lation will enable the 
context of hydraulic or pozzolanic constituent to be determined.  
The standard deviations for repeatability of the various analytes to be considered, most of which can be found 
in EAS 148 -2, are indicated in table 1.  
Table 1 —Standard  deviations for repeatability of the various analytes  
Analytes  Standard deviation for repeatability 
(Sr in % by mass)  
SO 3 0.07 
CO 2 0.07 
a (EDTA residue)  0.50 
b (HNO 3 residue)  0.11 
S2- 0.02 
CaO 0.18 
Mg 0.15 
MnO  0.003  
Insoluble residue  0.10 
Loss on  ignition  0.04 
 
3.2 Determination of constant mass  
Constant mass shall be determined by making successive 15 -min ignitions followed each time by cooling and 
then by weighing. Constant mass is reached when the difference between two successive weighing is less 
than 0.000 5 g.  
3.3 Expression  of masses and results  
3.3.1  Express masses in grams or the nearest 0.0001 g.  
3.3.2  Express the results of the tests, given by the mean of two determinations, as a percentage to one 
decimal place.  
3.3.3  If the difference between two determinations is greater than twice the standard deviation for 
repeatability, repeat the test and take the mean of the two closest values.  
3.4 Repeatability and reproducibility  
3.4.1  Repeatability  – Precision under repeatability conditions whe re independent test results are obtained 
with the same method on identical test items (material) in the same laboratory by the same operator using the 
same equipment within short intervals of time.  EAS 148 -4: 201 7 
© EAC 2017 – All rights reserved  3 
 3.4.2  Reproductivity  – Precision under reproductivity cond itions where test results are obtained with the 
same method on identical test items (material) in different laboratories with different operators using different 
equipment.  
3.4.3  Repeatability and reproductivity in this document are expressed as repeatabil ity standard deviation(s) 
and reproductivity standard deviation(s) in absolute percent and relate to clinker contents for the general 
method of determination of the constituents by selective dissolution and to hydraulic and pozzolanic contents 
for the meth ods of analysis of cement with three constituents  
4 Preparation of a cement sample  
Before analysis, the laboratory sample taken in accordance with the provisions of EAS 148 -7 shall be treated 
to obtain a test sample.   
5 Reagents  
5.1 Use only reagents of analytical quality  and distilled water of equal purity during the analysis.  
5.2 Unless otherwise stated, percent (%) means percentage by mass.  
5.3 The density “ ρ” of liquids is given at 20 °C. The densities of concentrated liquid reagents are expressed 
in grams per cubic centimetre.  
5.4 The degree of dilution is always given in the form of a volumetric sum, for example, hydrochloric acid (1 
+ 2) means 1 volume of  concentrated hydrochloric acid has to be mixed with 2 volumes of water.  
6 Determination of the constituent content of cements with more than three 
constituents  
6.1 General  
6.1.1  This method applies to cement with several constituents, that is  
a) clinker;  
b) hydraulic , pozzolanic or inert constituents; and  
c) set regulator(s) . 
6.1.2  The constituents determined by this method are classified as follows:  
a) set regulator;  
b) clinker;  
c) slag;  
d) (undifferentiated) calcareous constituents that is  combinations of any limestone, cha lk, or materials 
derived from the clinker production process; and  
e) (undifferentiated) siliceous constituents that is  combinations of any flint, natural pozzolana, siliceous 
fly ash, silica fume.   
6.1.3  Their number is therefore five, in principle, but:  EAS 148 -4: 201 7 
4 © EAC 2017  – All rights reserved  
 a) some  constituents, mainly calcareous or siliceous, can contain one or more components of the same 
nature although it may not be possible to identify them separately; and  
b) these same (undifferentiated) calcareous or siliceous constituents, could contain one or m ore of each 
type,  for example chalk can contain flint inclusions; some siliceous fly ashes and pozzolans have 
compositions similar to calcareous fly ashes. It is therefore not possible, using the method in this 
clause, to precisely identify the constituen ts of cement because of the possibility of the content of 
each type being modified by the other.  
Should there be a need to determine (differentiate) the nature of the calcareous or siliceous constituents more 
precisely, further enquiries should involve the  manufacturer of the cement as described in 6.2.5.4.  
The results obtained from the application of this method are quantitatively valid, whatever the relative 
importance of the constituents identified.  
6.2 Selective dissolution method  
6.2.1  Principle  
6.2.1. 1 Following preparation, one fraction of cement sample is treated with a solution containing 
triethanolamine (TEA), diethylamine (DEA) and EDTA. Another fraction is treated with dilute nitric acid (see 
Table 2).  
6.2.1. 2 The results from these two selective  dissolutions and the additional determinations of the sulfuric 
anhydride and carbon dioxide contents of the cement together with the sulfide contents of the cement and the 
residue from the dissolution in the EDTA solution enable the contents of the variou s constituents to be 
calculated.  
Table 2 — Reagents and their effects  
Reagent  Soluble  Insoluble  
EDTA solution  Set regulator(s)  
Clinker  
Calcareous constituent(s)  Slag 
Pozzolana  
Fly ash  
Siliceous constituent(s)  
Silica fumes  
Dilute nitric acid  Set regulator (s) 
Clinker  
Calcareous constituent(s)  
Slag Pozzolana  
Fly ash  
Siliceous constituent(s)  
Silica fumes  
 
6.2.2  Reagents  
6.2.2.1 Triethanolamine  (TEA):  N(CH 2CH 2OH) 3  [ρ =1.12  g/cm3] 
6.2.2.2 EDTA : dehydrate of the disodium salt of ethylene -diamine -tetracetic ac id C 10H14N2Na2O8.2H 2O 
6.2.2.3 Diethylamine  (DEA):  (C2H5)2NH 
6.2.2.4 Ethanol:   C2H5OH(ethyl alcohol)  
6.2.2.5 Concentrated nitric acid:   HNO 3 [ρ (1.40 - 1.42) g/cm3] EAS 148 -4: 201 7 
© EAC 2017 – All rights reserved  5 
 6.2.3  Apparatus  
6.2.3.1  Balance,  capable  of weighing to the nearest 0.000 1 g.  
6.2.3.2  Drying oven , controlled at 105 °C ± 5 °C.  
6.2.3.3  Apparatus, to check the temperature  at (20  ± 0.5) ºC 
6.2.3.4  Electrically controlled propeller stirrer , fitted with a glass propeller.  
6.2.3.5  Glass microfiber filter papers , with porosity of the order of 1 μm - 2 μm and a maximum 
diameter of at least 9 cm that fits the funnel of the filtration system. Insert above and below the filter a ring of 
polytetrafluoroethylene (PTFE) obtained from the supplier in order to improve the collection of particles on the 
filter. The filter shall be resistant to alcohol and alkalis and shall be dried to constant mass, at 105 °C.  
6.2.3.6  Filter paper , capable of retaining particles between 4 μm and 12 μm to use in case of particularly 
fine filtration. If necessary, two superimpos ed glass microfibre filters can be used.  
6.2.3.7  Vacuum filtration system, capable of being used with glass microfiber filter papers  
6.2.3.8  Desiccator,  containing anhydrous magnesium perchlorate  
6.2.3.9  Volumetric glassware , of analytical accuracy, that i s class  A as defined in ISO 385 and ISO 835.  
6.2.3.10  Ordinary glassware , beakers, flasks, watch glasses.  
6.2.3.11  Agate mortar  
6.2.3.12   Sieve , with a mesh aperture of 75 µm 
6.2.4  Procedure  
6.2.4.1  Preparation of the test sample  
Treat the cement sample ob tained in accordance with the provisions of FDEAS 148 -7 as follows:  
a) Prepare a laboratory sample of approximately 20 g using a sample divider or by quartering;  
b) Do not remove the iron from the sample at any stage in the operations;  
c) Grind the sample in the ag ate mortar (6.2.3.11), then pass it through the 75 µm sieve (6.2.3.12). If a 
residue remains, repeat the operation until all the sample passes through the 75 µm sieve;  
d) Collect and blend all that has passed through the sieve into a single sample; and  
e) Dry th e sample for 2 h in the oven (6.2.3.2) and allow it to cool in the desiccator (6.2.3.8)  
6.2.4.2  Preparation of the EDTA solution  
6.2.4.2.1  Mix 250 mL of triethanolamine (TEA) (6.2.2.1) with 500 mL water  in a 2 000 -mL beaker. Dissolve 
(93.00 ± 0.02) g of ED TA (6.2.2.2) in this mixture and allow to cool to ambient temperature. Transfer to a 1 
000-mL graduated flask.  
6.2.4.2.2   Place the flask under a fume -hood, add rapidly 173 mL of diethylamine (DEA) (6.2.2.3), stopper 
and allow to cool.  
6.2.4.2.3   Make up t o the mark with water.  EAS 148 -4: 201 7 
6 © EAC 2017  – All rights reserved  
 6.2.4.2.4  Promptly transfer the solution so obtained to a dark brown glass bottle fitted with an air -tight 
closure. The solution shall not be stored for more than one month.  
WARNING 1  Diethylamine (DEA) is a very volatile material wh ich can be toxic if inhaled in a 
concentrated form. Hence the need to prepare this solution under a fume -hood, away from any source 
of heat of flame, while wearing safety glasses and gloves, and carrying out all operations as quickly 
as possible.  
WARNING 2  During dissolution of the cement, the beaker should be covered in order to prevent any 
risk of inhalation and to avoid the loss of volatile constituents which can affect the buffering action of 
the EDTA solution. If an unpleasant smell escapes from the co vered beaker, it is recommended that 
work be carried out under a fume -hood, including the filtration procedures.  
6.2.4.3  Dissolution using the EDTA solution  
6.2.4.3.1  Using a pipette fitted with a filler, transfer 50 m L of the EDTA buffered  solution (6.2.4 .2) to a 1 
000-mL beaker and dilute with water to approximately 800  mL. 
6.2.4.3.2  Using the stirrer (6.2.3.4) stir the solution at approximately 300 r/min.  
6.2.4.3.3  Check that the temperature of the solution is (20 ± 0.5) ºC (6.2.3.3).  
6.2.4.3.4  Spread on to the surface of the solution (0.5000 ± 0.0200) g of dry cement accurately weighed to 
the nearest 0.0001 g ( m). The addition shall be progressive  during stirring in order to avoid formation of 
agglomerates which are difficult to disperse.  
6.2.4.3.5  After 5 min interrupt the stirring and check that no lumps of cement remain. If they do, break them 
up using the flattened end of a glass rod.  
6.2.4.3.6  Cover the beaker.  
6.2.4.3.7  Continue stirring for (120 ± 5) min, while maintaining  the temperature of the sol ution at (20 ± 0.5) 
º C. 
6.2.4.3.8   The filter paper should be prepared before filtration in order to avoid any errors due to loss of 
glass microfibres during subsequent handling. In order to do this, it is necessary to wash the filter paper with 
water, dr y it in the oven, allow it to cool in a desiccator until ambient temperature is reached and weigh it to 
the nearest 0.0001 g ( m1). 
6.2.4.3.9 Place the weighed filter paper flat on the vacuum  filtration apparatus (6.2.3.7) and, before fixing 
the upper part of the funnel, moisten it with water.  
6.2.4.3.10  Filter the extract solution through the moist filter paper or the conical filter paper (6.2.3.6) moisten 
as well, by applying suction such that the pressure in the filter is never less than 33.5 kPa (250 mm Hg). 
6.2.4.3.11  Wash the stirrer and the beaker with water  and if necessary use a glass rod with a rubber end to 
detach any adhering solids and transfer the total solid residue to the filter funnel. Rinse the sides five times 
with 10 mL of water, allowing the water to pass through completely between each rinsing. Finally rinse with 
ethanol (6.2.2.4)  
6.2.4.3.12  Carefully remove the filter paper from the funnel and place it on a weighing  dish (6.2.3.10) Dry the 
filter paper in the dish in the oven (6.2.3.2) f or 1 h.  
6.2.4.3.13 After cooling in the desiccators (6.2.3 8) for 15 min, weigh the filter paper plus the residue to the 
nearest 0.0001 g ( m2). 
6.2.4.3.14 Retain the filter paper plus residue in a sealed container so that, if required (6.2.4.7), the sulphi de 
content of the residue can be determined.  EAS 148 -4: 201 7 
© EAC 2017 – All rights reserved  7 
 6.2.4.4  Dissolution using dilute nitric acid  
6.2.4.4.1  Pour 120 m L distilled water into a 400 m L beaker. Stir using the stirrer (6.2.3.4). During stirring, 
add gradually (1.000 ± 0.0200) g of dry cement weighed to the nearest 0.0001 g ( m3). The addition shall be 
progressive in order to avoid the formation of agglomerates which are difficult to disperse. Stir for 5 min. 
Check that no lumps of cement remain. If they do, break them using the flattened end of a glass  rod. Continue 
to stir and whilst stirring, slowly add 80 m L of dilute nitric acid (1+9).  
6.2.4.4.2  Continue stirring for 30 min.  
6.2.4.4.3  If hydrogen sulphite (H 2S) is evolved, carry out this procedure under a fume -hood.  
6.2.4.4.4  Filter through a pre -weighed glass microfiber filter paper ( m4) (6.2.3.5).  
6.2.4.4.5  The preparation of the filter paper, the filtration procedures and washing of the residue are 
identical to those described in order to obtain the EDTA residue  (6.2.4.3).  
6.2.4.4.6  Dry the filter  paper  and the residue for 1 h in the oven (6.2.3.2). After cooling in the desiccators 
for 15 min, weigh the filter paper plus to the nearest 0.0001 g ( m5). 
6.2.4.5  Sulfuric anhydride content  
Determine the sulphuric anhydride content of the cement by the m ethod described in FD EAS 148 -2. 
6.2.4.6 Carbon dioxide content  
Determine the carbon dioxide content of the cement by the method described in FD EAS148 -2. 
6.2.4.7  Sulfide content  
Determine the sulphide contents of the cement (S 1) and of the residue obtained from the EDTA dissolution 
(S2) by the method described in FD EAS 148 -2. 
NOTE  In order to improve the accuracy of the determination of sulphide content, it is necessary that:  
a) S1 is determined by t aking a quantity of cement of ( 0.5000 ± 0.200) g  weighed to t he nearest 0.0001 
g for the  measurement;  
b) S2 is determined by taking the residue from the EDTA dissolution, including the filter paper (see 
6.2.4.3) and placing it all in a reaction flask for the measurement. The sample mass involved is then 
given as ( m2 – m1 ); and  
c)  the use of a larger test portion of cement, as suggested in the Note to FDEAS 1 48-2, is 
recommended when the sulphide content is low  
6.2.5  Calculation of the contents of cement constituents  
6.2.5.1  Calculation of the contents of insoluble resid ues 
Express all calculated values as percentages (%) of dry material. Calculate the content of insoluble residue,  𝖺, 
obtained from the EDTA dissolution from the formula : 
𝖺
1001 2mmm  (1) 
where  EAS 148 -4: 201 7 
8 © EAC 2017  – All rights reserved  
 m is the mass of cement;  
m1 is the mass of the fil ter paper; and  
m2 is the combined mass of the dried residue plus filter paper.  
Calculate the content of insoluble residue, b, obtained from the nitric acid dissolution from the formula:  
100.
34 5
mmmb
 (2) 
where  
m3 is the mass of cement;  
m4 is the mass of the filter; and  
m5 is the combined mass of the dried residue plus filter paper  
6.2.5.3   Calculation of contents of constituents  
Calculate the set regulator content, 𝖱, from the formula:  
R = 1.6 x s …(3)  
where  
s is the sulfuric anhydride content of the cement.  
Calculate the calcareous constituent content, C, from the formula:  
C = 2.0 x c if c > 1 (4a) 
C = 0 if c > 1 (4b) 
Where:  
c is the carbon dioxide content of the  cement.  
Calculate the siliceous constituent content, P, from the formula:  
P= 1.05x b if b>2 (5a) 
P= 0 if b≤ 2 (5b) 
Where  
b is the content of insoluble residue obtained from the nitric acid dissolution . 
Calculate the slag content, L, from the formula:  
L= 0 if (𝖺-b) ≤𝟣 (6a) 
L= 𝟣.0 (𝖺-b) if 𝟣 < (𝖺-b) <30  (6b) 
L= max (L1, L2) if (𝖺-b) <30  (6c) EAS 148 -4: 201 7 
© EAC 2017 – All rights reserved  9 
 where 
L1 = 1.05 ( a - b) (7) 
L2 = 100.  
a S
2) (1 baS  (8) 
This equation is valid if the condition 100 S1 ≥ a. S2 is satisfied  
If this is not the case, car ry out a new determination of S1, S2 and   
where  
, is the sulfide content of the cement;  
 is the sulfide content of the residue obtained from the EDTA dissolution.  
Calculate the clinker content,  K, from the formula:  
K = 100 - R- C – P - L 
NOTE  1 To obtain the contents of the various constituents expressed in relation to cement on the “set regulator free” 
basis, it is necessary to multiply the values obtained above by the factor: 100/(100 -R) 
NOTE 2  Clinker content, taking into consi deration that it is the principal constituent present in all types and classes of 
cement, is in effect always calculated as the difference between 100 % and the sum of the other constituents.  
6.2.5.4  Further investigations  
If results are anomalous, that is  when:  
a) some of the constituents quantified are different from those which should be present on the basis of the 
designated type/ or class declared by the supplier;  
b) the content measured for some constituents normally present in the cement leads to its ident ification 
within a type and/or class other than those declared by the supplier; and  
c) the use of a new constituent for which experience of the quantitative determination by the present method 
is considered as yet insufficient , 
an inspection body or, failing this, any independent body commissioned by the interested parties to carry out 
the analyses should proceed, prior to issuing a report of the analysis, to additional investigations with the 
cement manufacturer . 
6.2.6  Repeatability and reproducibility  
Precis ion estimates for repeatability and reproducibility have been determined for clinker content only because 
clinker is present in all types and classes of cement.  
Where  
(a - b)< 30;                            or  
(a - b)≥ 30                              and L= L1 
the standard deviation for repeatability is 1 %;  EAS 148 -4: 201 7 
10 © EAC 2017  – All rights reserved  
 the standard deviation for reproducibility is 2 %.  
where  
(a - b)≥ 30                              and L= L2 
the standard deviation for repeatability is 2 %;  
the standard deviation for reproducibility i s 4 %.  
6.2.7  Qualitative determination of the type of cement.  
Determine the type of cement under investigation by comparing the values obtained with the ranges given in 
table 1 of FDEAS 18-1 defining the different cement types.  
7 Determination of the conte nts of constituents for cements with three constituents  
7.1 General  
7.1.1  The different methods described in this clause apply only to cement with three constituents, that is  
a) clinker  
b) a single hydraulic or pozzolanic constituent (slag, pozzolana, siliceous  fly ash); and  
c) Set regulator (s)  
7.1.2 Therefore, they can only be used if an inspection body or, failing this, any independent body 
commissioned by the interested parties to carry out the analyses has a document from the cement producer 
certifying the abs ence of any constituent other than those listed above.  
7.1.3  Some of the methods in clause 7 are variations on the methods of choice whereas others are based 
on physical separation of constituents and different analytical principles.  
7.2 Determination of t he slag content  
7.2.1  Dense liquid separation method  
7.2.1.1  Principle  
7.2.1.1.1  Fractions of clinker and of slag are separated as cleanly as possible by means of dense liquids 
from a size fraction of cement  (see Figure 1).  
7.2.1.1.2  The concentrations of  tracer analysis present in the cement and in the fractions of clinker and 
slag are determined.  The sla g content of the cement is then calculated.  EAS 148 -4: 201 7 
© EAC 2017 – All rights reserved  11 
 
 
Figure 1  — Scheme of the separation using dense liquids  
7.2.1.2  Reagents  
7.2.1.2.1  Di-iodomethane  CH 2I2 (ρ = 3.31  g/cm3 - 3.32 g/cm3). This reagent is toxic and shall be handled 
with the greatest care using safety gloves in a fume cupboard fitted with an extractor.  
7.2.1.2.2  Dibutyl phthalate  C6H4 (COOC 4H9)2, (ρ = 1.04 g/cm3)  
7.2.1.2.3  Bromoform  CHBr 3, (ρ = 2.88 g/ cm3 - 2.89 g/cm3). This reagent is toxic and shall be handled with 
the greatest care using safety gloves in a fume cupboard fitted with an extractor.  
7.2.1.2.4  Ethanol  C2H5OH (absolute ethyl alcohol)  
7.2.1.2.5  Diethyl ether,  C2H5OC 2H5 
7.2.1.3  Apparatus  
7.2.1. 3.1 Balance,  capable of weighing to the nearest 0.000 1 g. 
7.2.1.3.2  Drying oven,  controlled at (105 ± 5) °C.  EAS 148 -4: 201 7 
12 © EAC 2017  – All rights reserved  
 7.2.1.3.3  Sintered glass filter,  with mean pore diameter less than 4 μm 
7.2.1.3.4  Centrifuge,  capable of at least 1 000 r/min  
7.2.1.3.5  Sieve,  with a minimum mesh aperture of 32 μm and maximum of 40 μm 
7.2.1.3.6  Sieve, with a mesh aperture of 75 μm as 6.2.3.12  
7.2.1.3.7  Polarizing microscope, fitted with source for transmit ted light with a minimum magnification of 
100. 
7.2.1.3.8  Desiccator, as 6.2.3. 8  
7.2.1.3.9  Volumetric glassware , see 6.2.3.9  
7.2.1.3.10  Ordinary glassware , see 6.2.3.10  
7.2.1.4  Procedure  
7.2.1.4.1  Preparation of the test sample  
The cement sample obtained ( approximately 2 kg) in accordance with the provisions of FD EAS 148 -7 shall be 
treated as follows:  
a) separate by dry sieving a sufficient quantity of cement to obtain at least 15 g of material in either the 
size fraction 32 μm - 75 μm or 40 μm - 75 μm; 
b)  re-sieve this fraction with ethanol on the finer sieve (32 μm or 40 μm) in order to remove fine 
particles, which would adhere to the larger grains; and  
c) wash once in diethyl ether and then dry the sample for 2 h in the oven (7. 2.1.3.2) and allow it to cool 
in the desiccator ( 7.2.1.3.8)  
7.2.1.4.2  Separation of the clinker and slag fractions (see Figure 1)  
7.2.1.4.2.1  Bring the size fraction into suspension in a liquid with a density of 2.98 g/ cm3 (a mixture of di -
iodomethane and  dibutyl phthalate or bromoform) at a concentration not exceeding 4 g of material in 100 mLof 
dense liquid).  
7.2.1.4.2.2  Remove iron particles by stirring with a magnet.  
7.2.1.4.2.3  Transfer the suspension into centrifuge tubes and centrifuge for 5 min. Se parate the residue 
from the supernatant by pouring the latter ( S1) into another centrifuge tube ( the use of a narrow necked tube 
my simplify this operation). Reserve the residue ( c1) for the purification of the clinker.  
7.2.1.4.2.4  Repeat the separation o peration at twice, restoring the supernatant ( S2) to suspension in a liquid 
with the same density and centrifuging it for 5 min. Reject the residues.  
7.2.1.4.2.5  Pour the last supernatant obtained ( S3) into a sintered glass filter (7.2.1.3.3), wash twice i n 
diethyl ether, dry for 30 min in the oven, and allow to cool in the desiccator to ambient temperature.  
7.2.1.4.3  Purification of the clinker fraction ( c4) (see Figure 1)  
7.2.1.4.3.1  Wash the residue ( c1) from the first centrifuging operation twice with d iethyl ether on a 
sintered glass filter. Dry for 30 min in the oven and allow cool in the desiccator to ambient temperature.  EAS 148 -4: 201 7 
© EAC 2017 – All rights reserved  13 
 7.2.1.4.3.2  Bring the powder so obtained into suspension in a liquid with a density of 3.10 g/cm3 (a 
mixture of di -iodomethane and dibutyl phthalate or bromoform) at a concentration not exceeding 4 g of 
material in per 100 m L of dense liquid. Transfer into centrifuge tubes and centrifuge for 5 min.  
7.2.1.4.3.3  Reject the supernatant and, using a sintered glass filter, recover the liqu id from the centrifuge 
tubes. Centrifuge the residue at least twice more for 5 min after having again suspended it in the liquid with a 
density of 3.10 g/cm3. Remove the supernatants.  
7.2.1.4.3.4  Pour the last residue obtained ( c4) into a sintered glass f ilter, wash twice with diethyl ether.  
7.2.1.4.3. 5 Dry for 30 min in the oven and allow cool in the desiccator to ambient temperature.  
7.2.1.4.3. 6 In order for the chemical analyses to be carried out, the final clinker fraction ( c4) shall weigh at 
least 4 g . 
7.2.1.4.3. 7 If this quantity has not obtained, sufficient separations shall be carried out so that the sum of 
each of the individual clinker fractions weighs a least 4 g.  
7.2.1.4.4  Purification of the slag fraction ( c7) (see Figure 1)  
7.2.1.4.4. 1 To obta in the slag fraction, restore the supernatant ( S3) to suspension in a liquid with a 
density of 2.87 g/cm3 - 2.89 g/cm3 (a mixture of di -iodomethane and dibutyl phthalate or bromoform) at a 
concentration not exceeding 4 g of material in 100 mL of dense liqu id. 
7.2.1.4.4. 2 When the quantity of slag collected is small, however, the use of a liquid with a lower density 
is permitted, but the latter shall never have a value below 2.84  g/cm3. 
7.2.1.4.4.3  Transfer into centrifuge tubes. Centrifuge for 5 min. Reject  the supernatant and, using a 
sintered glass filter, recover the liquid from the centrifuge tubes. Centrifuge the residue at least twice more for 
5 min after having again suspended it in the liquid of the same density as that used for the first separation.  
Reject the supernatants.  
7.2.1.4.4.4  Pour the last residue obtained ( c7) into a sintered glass filter and wash twice with diethyl 
ether.  
7.2.1.4.4.5  Dry for 30 min in the oven and allow cooling in the desiccator to ambient temperature.  
7.2.1.4.4.6   In order to carry out the chemical analyses, the final slag fraction ( c7) shall weigh at least 4 g.  
7.2.1.4.4.7  If this quantity has not been obtained, sufficient separations shall be carried out so that the 
sum of each of the individual slag fractions weighs at least 4 g  
7.2.1.4.5  Checking the purity of the clinker and slag fractions  
7.2.1.4.5.1  The purity of the fractions can be checked by the operator by observing them under a 
microscope (7.2.1.3.7).  
7.2.1.4.5.2  For this purpose, place a few milligrams of po wder on a slide, disperse in a drop of immersion 
oil, cover the sample with a cover slide and examine using the microscope (magnification X 100).  
7.2.1.4.5.3  The slag grains are bright, homogeneous, with a glassy fracture and they remain faint 
between cros sed nicols.  
7.2.1.4.5.4  The clinker grains are dark, granular with irregular contours and the facets reflect in polarized 
light when the microscope table is rotated.  
7.2.1.4.5. 5 If one of these phases is not considered sufficiently pure, carry out a furthe r separation.  EAS 148 -4: 201 7 
14 © EAC 2017  – All rights reserved  
 7.2.1.4.6  Determination  of the contents of the tracer analytes  
7.2.1.4.6.1  Determine in mass %, the contents of sulfuric anhydride ( ss), calcium oxide and other tracer 
analytes ( S2-, MgO or MnO), which are not present in the set regulator, in  the oven -dried cement , as well as 
in the fractions slag and clinker,( c7 ) and ( c4 ) respectively.  
7.2.1.4.6.2  Carry out analyses according to the methods described in FDEAS 148 -2. 
7.2.1.4.6.3  If the final result of the analysis has to be expressed on cal cined materials, it is necessary to 
determine the loss on ignition of the cement and of the slag and clinker fractions in accordance with the 
method described in Clause 7 of FDEAS 148-2. 
7.2.1.5  Calculation of the slag content of cement  
Calculate the sulfu ric anhydride content, S S, in the set regulator(s) from the formula:  
 
Z 0.7XZkCYkAXkS
Ss


 (10) 
where  
X = (C c - C1) (A 1 - Ak) - (Ac - A1) (C 1- Ck) 
Y = S (C 1 – Ck) + S k(Cc - C1) 
Z = S (A 1 – Ak) + S k(Ac - A1) 
where  
SS  is the sulfuric anhydride content of the set regulator(s);  
S is the sulfuric anhydride content of the cement ; 
Sk  is the sulfuric anhydride content of the clinker fraction;  
Cc is the calcium oxide content of the cement;  
C1 is the calcium oxide content of the slag fraction  
Ck is the calcium ox ide content of the clinker fraction;  
Ac is the tracer content of the cement (S2-, MgO or MnO);  
A1 is the tracer of the slag fraction (S2-, MgO or MnO);  and 
Ak is the tracer content of the clinker fraction (S2-, MgO or MnO).  
The calculated sulfuric anhydrid e content in the set regulator(s) shall be within limits corresponding to the 
extreme values existing under industrial conditions. These limits are considered to be equal to:  
– Maximum: S s = 58 % (SO 3 content of anhydride);  
– Minimum: S s = 32 % (SO 3 content of  gypsum containing 30 % impurities)  EAS 148 -4: 201 7 
© EAC 2017 – All rights reserved  15 
 If the calculated value of S s is not within these limits, repeat the determination.  
Among the tracer analytes meeting the above conditions, that which leads to the most precise final result is 
that for which the term f, defined as follows, is a minimum:  
kr
AASf
1
 
where S r  is the standard deviation for repeatability of the analytical determination of this tracer analyte (see 
3.1). 
Calculate the slag content of the cement from the following formulae:  
From the dry materials:  
 
)kSsS (0.7)sSk(C)a'i(C)c'sS (0.7)b'k(C)a'c(C
100L


 (11) 
  
Where  
 a’ = Ss – Sk 
 b’ = S s – S 
 C’ = S - Sk 
 
From the calcined materials:  
p) (100)1p (100
LL'


                 12) 
The slag content related to the sum of the slag and clinker is given by:  
From the dry mater ials: 
LkSb' 100La' 100l

                (14) 
From the calcined materials:  
kpb' 100)kpsS1p L(a'L)kSb' 100(100)1p L(100a' 100
l'


    (14 
where  
L  is the slag content of the cement;  
L‘  is the slag content of the calcined cement;  EAS 148 -4: 201 7 
16 © EAC 2017  – All rights reserved  
 l is the slag content of the (clinker+ cement)  
l‘ is the  slag content of the calcined (clinker+ slag);  
p1   is the loss on ignition of the slag fraction;  
p is the loss on ignition of the cement; and  
pk  is the loss on ignition of the clinker fraction.  
7.2.1.6  Repeatability and reproduc ibility 
The standard devia tion for repeatability is 1%.  
The standard deviation for reproducibility is 3%.  
These values are valid whatever the slag content.   
7.2.2  Microscope  method  
7.2.2.1  Princip le 
The blastfurnace slag content is measured by microscope counting. The sample, taken  from a particular 
cement size fraction, is examined in transmitted or reflected light.  
After counting a sufficient number of grains, ignoring the set regulator(s), calculate the ratio, LV, as a 
percentage from the formula:  
100
) clinker (slag grains of number Totalslag of grains of NumberLv 

 (15) 
The blastfurnace slag content of the cement is calculated using two corrections, for density (by calculation) 
and for distribution (by chemical analysis).  
7.2.2.2  Apparatus and materials . 
7.2.2.2.1  Air jet or mechanical sieve , with a sieve of mesh aperture 32 μm. 
7.2.2.2.2  Sieve,  with a mesh aperture of 40 μm.  
7.2.2.2.3  Polarizing microscope, as 7.2.1.3.7.  
7.2.2.2.4  Microscope  with source for reflected light with a magnification from 200 - 400. 
7.2.2.2.5  Canada balsam  
7.2.2.2.6  Equipment for preparing sections  
7.2.2.2.7  Synthetic resin  
7.2.2.2.8   Volumetric glassware, see 6.2.3.9  
7.2.2.2.9   Ordinary glassware, see 6.2.3.10  EAS 148 -4: 201 7 
© EAC 2017 – All rights reserved  17 
 7.2.2.3  Procedure  
7.2.2.3.1  Preparation of the test sample  
Using the air jet or mechanical sieve apparatus (7.2.2.2.1), first separate by sie ving the fraction of grains 
larger than 32 μm. Next, with the hand sieve (7.2.2.2.2), separate by sieving the fraction of grains larger than 
40 μm. Remove the iron particles by means of a magnet. The 32 μm - 40 μm fraction shall be at least 2 g.  
The cement sample obtained in accordance with the pr ovisions of FDEAS148 -7 shall be treated as follows:  
a) examination in transmitted light; and  
Disperse a sample of approximately 0.02 g of the fraction in Canada balsam (7.2.2.2.5). For this purpose, melt 
the Canada balsam on a microscope slide at a temperatur e of 130 °C - 150 °C. Cover with a cover slide.  
b) examination in reflect light  
Disperse a sample of  approximately  1 g of the sieved fraction in the synthetic resin. Wait until the synthetic 
resin  (7.2.2.2.7)  has solidified.  
Grind the surface of the sample, p olish and etch with water for about 30 s.  
7.2.2.3.2  Microscope counting  
Take care to ensure that the sample is not damaged when placed under the microscope.  
a) in transmitted light ; and  
Examine the sample in transmitted light (magnification 100). Count at lea st one thousand clinker and slag 
grains in all ignoring the set regulator.  
The grains of slag are clear, homogeneous, with a glassy fracture and they remain faint between crossed 
nicols.  
The grains of clinker are dark, granular, with irregular contours and  the facets reflect in polarized light when 
the microscope table is rotated.  
The grains of the set regulator (gypsum and anhydrite) are not very distinct in natural light, but the facets 
reflect in polarized light when the microscope table is rotated.  
NOTE  The observation is made easier by using a mica quarter wave plate.  
b) in reflect light  
Count at least one thousand clinker and slag grains in all under the microscope in reflected light ignoring the 
set regulator.  
After etching, the ferrite phase (C 4AF) of t he clinker appears white and the other clinker minerals (C 3S, C 2S 
and C 3A) appear dark in colour while the granulated blastfurnace slag grains are light grey in colour, which 
makes it easy to distinguish them from the clinker grains.  
NOTE   C4AF= (CaO) 4.Al2O3.Fe 2O3, tetracalcium aluminoferrite;  
   C3S= (CaO) 3.SiO 2, tricalcium silicate;  
   C2S= (CaO) 2. SiO 2, dicalcium silicate;  
   C3A= (CaO) 3. Al 2O3, tricalcium aluminate.  EAS 148 -4: 201 7 
18 © EAC 2017  – All rights reserved  
 7.2.2.3.3  Determination of the contents of the tracer  
7.2.2.3.3.1  Determine the conten ts of the tracers, CaO, SO 3 and the loss on ignition, in the cement and in 
the fraction examined by microscope, in accordance with the methods described  in FD EAS 148 -2.  
7.2.2.3.3.2  Express the CaO, SO 3 contents on the calcined material.  
7.2.2.4  Calculati on of the slag content of the cement  
Calculate successively:  
the result of the count:  
k 11
nnnLv
100
 (16) 
the correction for density:  
vL)1dk(dkd 100vL1d 100
ml


 (17) 
The densities of the slag and clinker can be estimated as 2.87 g/cm3 and 3 .15 g/cm3 respectively, hence 
equation 17 can be written:  
vv
mLLl28.0 315287
 (18) 
the correction distribution:  
PS 1.7 100S) 0.7c(C 100
mC

 (19) 
p'f's 1.7 100)f's 0.7f'(C 100
fC


 (20) 
The slag content, l’, on calcined (slag+ clinker) is then given by:  
23)fCm(C
100mll'

 (21) 
In this formula, it is assumed that the difference between the calcium oxide contents of the clinker and slag is 
23 %.  
The slag content, l, on the dry ( slag+ clinker) is given by:  
100P) (100l'l
 (22) 
where  
Lv is the slag content by volume of the fr action examined by microscope, in percent;  EAS 148 -4: 201 7 
© EAC 2017 – All rights reserved  19 
 Lm is the slag content of the slag and clinker mixture of the fraction examined by microscope, on dry 
cement.  
n1 is the number of slag grains ; 
nk is the number of clinker grains;  
d1 is the density of the slag, in grams per cubic centimetres;  
dk is the density of the clinker grams per cubic centimeters;  
Cc is the calcium oxide content of the cement;  
Cm is the calcium oxide content of the slag and clinker mixture;  
Cf’  is the calcium  oxide content of the fraction exa mined by microscope;  
Cf is the calcium oxide content of the fraction examined by microscope related to the calcined sample 
free of set regulator(s).  
S is the sulfuric anhydride content of the cement;  
S f ' is the sulfuric anhydride content of the fraction examined by microscope;  
P is the loss on ignition of the cement;  
p' is the loss on ignition of the fraction examined by microscope;  
l is the slag content of the slag and clinker mixture;  
l’ is the slag content of the calcined slag and clinker mixture;  
lm is the slag content of the slag and clinker mixture of the fraction  examined by microscope, on dry 
material, in percent.  
7.2.2.5  Repeatability  and reproducibility  
7.2.2.5.1  The standard deviation for repeatability is 1 %.  
7.2.2.5. 2 The standard deviation f or reproducibility is 3 %.  
7.2.2.5. 3 These standard deviations are valid whatever the slag content.  
7.3 Determination of the siliceous fly ash content  
7.3.1  Selective dissolution method  
7.3.1.1  Principle  
7.3.1.1.1  After drying in the oven, the cement is tr eated with a solution of hydrochloric acid in methanol 
containing salicylic acid.  
7.3.1.1.2  The clinker and a fraction of the set regulator (s) are, in principle, dissolved.  
7.3.1.1.3  The siliceous fly ash and the fraction remaining from the set regulator(s ) are not, in principle, 
dissolved.  EAS 148 -4: 201 7 
20 © EAC 2017  – All rights reserved  
 7.3.1.1.4  Weighing the residue obtained and also the determination of its sulfuric anhydride content and 
that of the cement allows the siliceous fly ash content of the cement to be calculated.  
7.3.1.2  Reagents  
7.3.1.2.1  Methanol,  CH 3OH (anhydrous methyl alcohol) ( ρ = 0.79 g/cm3) 
7.3.1.2.2  Concentrated hydrochloric acid , HCI ( ρ = 1.18 g/cm3 -1.19 g/cm3) 
7.3.1.2.3  Salicylic acid, C6H4(OH)  COOH  
7.3.1.2.4  Acid solution,  place 800 mL of the methanol into a graduated 1 000 -mL flask. Add 41.7 mL of 
hydrochloric acid and (50.00 ± 0.02) g of salicylic acid. Mix until the salicylic acid is completely dissolved. 
Make up to 1 000 mL with methanol.  
7.3.1.3  Apparatus  
7.3.1.3.1  Balance,  as 6.2.3.1  
7.3.1.3.2  Drying oven,  6.2.3.2  
7.3.1.3.3  Electrically controlled stirrer , as 6.2.3.4  
7.3.1.3.4  Filters, with a mean pore diameter less than 4 μm  
7.3.1.3.5  Desiccator,  as 6.2.3.8  
7.3.1.3.6  Volumetric glassware , as 6.2.3.9  
7.3.1.3.7  Ordinary glassware , as 6.2.3.10  
7.3.1.4  Procedure  
7.3.1.4.1  Preparation of the test sample  
The cement sample obtained in accordance with  the provisions of FDEAS 148 -7 shall be treated as follows:  
a) take 20 g of the sample using a sample -divider or by quartering; and  
b) Dry the sample for 2 h in the oven (7.3.1.3.2) and allow to cool in the desiccators (7.3.1.3.5.)  
7.3.1.4.2  Dissolution  using  acid solution  
7.3.1.4.2.1  Place 200 mL of the acid solution, (7.3.1.2.4), into a 400 –mL beaker. Stir using the stirrer, 
(7.3.1.3.3). Slowly add (2.0 ± 0.1) g of dry cement weighed to the nearest 0.0001 g ( m). The addition shall be 
progressive whilst stirr ing in order to avoid formation of lumps which are difficult to disperse. After 5 min 
interrupt the stirring and check that no lumps of cement remain. If they do, break them up using the flattened 
end of a glass rod.  
7.3.1.4.2.2  Continue stirring for 30 mi n. Allow the solution to settle for 5 min.  
7.3.1.4.2.3  Filter through a pre -weighed filter ( m1). Wash the insoluble residue six times with 
approximately 100 mL of methanol, allowing it to dry completely after each washing.  
7.3.1.4.2.4  Dry the filter and in soluble residue for 2 h in the oven. Allow the filter and the insoluble 
residue to cool in the desiccators to ambient temperature and weigh ( m2). EAS 148 -4: 201 7 
© EAC 2017 – All rights reserved  21 
 7.3.1.4.3   Determination of the sulphuric anhydride content  
Determine the sulphuric anhydride content of the i nsoluble residue, si (7.3.1.4.2) and also of the cement, s C, 
as described in FD EAS 148 -2. 
7.3.1.5  Calculation of the fly ash content of cement  
Calculate the fly ash content, V, of the dry cement from the formula:  
)i1 2s 1.813. (100
mm mV 
 (23) 
Calculate the f ly ash content, V, of the sum of the clinker and fly ash from the formula:  
c1.813s 100V.100
v
 (24) 
where  
V is the fly ash content of dry cement;  
v is the fly ash content of dry (clinker+ fly ash);  
m is the mass of the cement;  
m1 is the mass of the drie d filter;  
m2 is the mass of the dried filter plus insoluble residue;  
si is the sulfuric anhydride content of the insoluble residue; and  
sc  is the sulfuric anhydride content of the content of the cement.  
7.3.1.6  Repeatability and reproducibility  
7.3.1.6.1  The standard deviation for repeatability is 0.5 %.  
7.3.1.6.2  The standard deviation for reproducibility is 2 %.  
7.3.1.6.3  These standard deviations are valid whatever the fly ash content.  
7.4 Determination of the natural pozzolana content  
7.4.1  Selective d issolution method  
7.4.1.1  Principle  
7.4.1.1. 1 After drying in the oven, the cement sample is treated with a solution of hydrochloric acid in 
methanol containing salicylic acid.  
7.4.1.1.2  The clinker and a fraction of the set regulator(s) and the alkaline e arth carbonates of certain 
pozzolanas are, in principle, dissolved.  
7.4.1.1. 3 The natural pozzolanas (except the alkaline earth carbonates of some of them) and the remaining 
fraction from the set regulator(s) are not, in principle, dissolved.  EAS 148 -4: 201 7 
22 © EAC 2017  – All rights reserved  
 7.4.1.1. 4 Weighing the residue obtained and the determination of its sulfuric anhydride content, as well as 
the carbon dioxide content and sulfuric anhydride content of the cement, allows the pozzolana content of the 
cement to be calculated.  
7.4.1.2  Reagents  
7.4.1.2.1  Methanol,  as 7.3.1.2.1  
7.4.1.2.2  Concentrated hydrochloric acid, as 7.3.1.2.2   
7.4.1.2.3  Salicylic acid,  as 7.3.1.2.3  
7.4.1.2.4  Acid solution, as 7.3.1.2.4  
7.4.1.3  Apparatus  
7.4.1.3.1  Balance,  as 6.2.3.1  
7.4.1.3.2  Drying oven,  as 6.2.3.2  
7.4.1.3.3  Electric ally controlled stirrer, as 6.2.3.4  
7.4.1.3.4  Sintered glass filters,  with a mean pore diameter from 5 μm - 15 μm 
7.4.1.3.5  Desiccator,  as 6.2.3.8  
7.4.1.3.6  Volumetric glassware, see 6.2.3.9  
7.4.1.3.7  Ordinary glassware,  see 6.2.3.10  
7.4.1.4  Procedure  
7.4.1.4.1   Preparation of the test sample  
Treat the cement sample obtained in accordance with the provision s of FDEAS 148 -7 as follows:  
a) take approximately 20 g of the sample using a sample -divider or by quartering; and  
b) dry the sample for 2 h in the oven (7.4.1.3.2) and allow to cool in the desiccators (7.4.1.3.5).  
7.4.1.4.2  Dissolution using acid solution  
7.4.1 .4.2.1  Place 200 mL of the acid solution into a 400 -mL beaker. Stir using the stirrer (7.4.1.3.3). 
Slowly add (2.0 ± 0.1) g of dry cement weighed of the nearest 0.0001 g ( m). The addition shall be progressive 
whilst stirring in order to avoid formation of agglomerates which are difficult to disperse. After 5 min interrupt 
the stirring and check that no lumps of cement remain. If they do, break them up using the flattened end of a 
glass rod.  
7.4.1.4.2.2  Continue stirring for 30 min. Allow the solution to set tle for 5 min.  
7.4.1.4.2.3  Filter through a weighed filter ( m1). Wash the insoluble residue six times with approximately 
100 mL of methanol, allowing it to dry completely after each washing.  
7.4.1.4.2.4  Dry the filter and insoluble residue for 2 h in the o ven. Allow the filter and the insoluble 
residue to cool in the desiccators to ambient temperature and weigh ( m2). EAS 148 -4: 201 7 
© EAC 2017 – All rights reserved  23 
 7.4.1.4.3  Determination of the sulphuric anhydride content  
Determine the sulfuric anhydride content of the insoluble residue ( Si) and of the c ement ( Sc) according to the 
method described in FDEAS 148 -2. 
7.4.1.4.4  Determination of the carbon dioxide content  
Determine the carbon dioxide content, c, of the cement by the method described in FD EAS 148-2, using 
however, as the solution for dissolving the cement, the acid solution described in 7.4.1.2.4 and the quantities 
of cement and acid solution previously specified.  
7.4.1.5  Calculation of the pozzalana content of cement  
Calculate the calcium carbonate content of the cement, C’, from the equation:  
C’ = 2.273 x c  (25) 
The pozzolana content of the cement, PO, is given by:  
 'C s 1.813. 100
m1m2m
oPi 

 (26) 
The pozzolana content of the sum of the clinker and pozzolana, PO, is given : 
s 1.813 100P100.
opo

 (27) 
where  
 PO is the pozzolana  content of the cement:  
po is the pozzolana content of the sum of the clinker and pozzolana;  
C‘ is the calcium carbonate content of the cement;  
c is the carbon dioxide content of the cement;  
m is the mass of the cement;  
m1  is the mass of the filter;  
m2 is the mass of the filter and the insoluble  residue;  
si is the sulfuric anhydride content of the insoluble residue;  
s  is the sulfuric anhydride content of the cement.  
7.4.1.6  Repeatability and reproducibility  
7.4.1.6.1  The standard deviation for repeatability is 1 %.  
7.4.1.6.2  The standard deviation for reproducibility is 1.5 %.  
7.4.1.6.3  These standard deviations are valid whatever the pozzolana content within the range 0 % - 40 %.  EAS 148 -4: 201 7 
24 © EAC 2017  – All rights reserved  
 7.4.2  Dense liquid separation method  
7.4.2.1  Principle  
7.4.2.1.1  After drying in the oven, the ceme nt sample is dissolved in a solution of salicylic acid in methanol. 
The clinker silicates are, in principle, dissolved. The clinker aluminates and aluminoferrites as well as the 
pozzolanas are not, in principle, dissolved.  
7.4.2.1. 2 The clinker is isolated  by separating a size fraction of the cement using dense liquids. Possible 
contamination of this clinker can be corrected by dissolving it in a dilute acid. The clinker is selectively 
dissolved by a solution of salicylic acid in methanol enabling the clink er content to be determined and the 
pozzolana content to be calculated.  
7.4.2.2  Reagents  
7.4.2.2.1  Di-iodomethan e: as 7.2.1.2.1  
7.4.2.2.2  Bromoform : as 7.2.1.2.3  
WARNING  These reagent s are  toxic and should be handled with the greatest care using safety 
gloves in a fume cupboard fitted with an extractor .  
7.4.2.2.3  Methanol: as 7.3.1.2.1  
7.4.2.2.4  Ethanol:  as 7.2.1.2.4  
7.4.2.2.5  Salicylic acid : as 7.3.1.2.3  
7.4.2.3.6  Concentrated hydrochloric acid : as 7.3.1.2.2  
7.4.2.2.7  Dilute hydrochloric acid  HCl (1 + 100 ) 
7.4.2.2.8  Dilute hydrochloric acid HCl (1 + 500)  
7.4.2.2.9  Diethyl ether  C2H5OC 2H5, (ρ = 0.71 g/cm3) 
7.4.2.2.10  Acid solution : Place 800 mL of the methanol into a graduated 1 000 -mL flask. Add (170.00 ± 
0.02) g of salicylic acid. Mix until the salicylic acid is completely dissolved. Make up to 1 000 -mL with 
methanol.  
7.4.2.3  Apparatus  
7.4.2.3.1  Balance,  as 6.2.3.1  
7.4.2.3.2  Drying oven,  as 6.2.3.2  
7.4.2.3.3  Electrically controller stirrer, as 6.2.3.4  
7.4.2.3.4  Centrifuge,  as 7.2.1.3.4  
7.4.2.3.4  Sieve as 7.2.1.3.5  
7.4.2.3.5  Sieve  as 7.2.1.3.6  
7.4.2.3.6  Sintered glass filters  with mean pore d iameter of 5 μm - 15 μm  
7.4.2.3.7  Desiccator , see 6.2.3.8  EAS 148 -4: 201 7 
© EAC 2017 – All rights reserved  25 
 7.4.2.3.8  Volumetric glassware, see 6.2.3.9  
7.4.2.3.9  Ordinary glassware, see 6.2.3.10  
7.4.2.4  Procedure  
7.4.2.4.1  Preparation of the test sample  
Treat the cement sample obtained in accordance with the provisi ons of FD EAS 148 -7 as follows for, 
7.4.2.4.1a), the determination of insoluble residue in the salicylic acid solution and, 7.4.2.4.1 b), the separation 
of the clinker fraction:  
a) take approximately 20 g of the sample -divider or by quartering, dry it for 2 h in the oven (7.4.2.3.2) 
and allow to cool in the dessicator (7.4.2.3.8) ; and  
b) take a sample of approximately 2 kg, separate by dry sieving a sufficient amount of cement to obtain 
at least 15 g of material in either the size fraction 32 µm or 40 µm -75 µm, r e-sieve this fraction with 
ethanol on the finest sieve to remove the fine particles which would adhere to the larger grains, wash 
once in diethyl ether and then dry the sample for 2 h in the oven (7.4.2.3.2) and allow to cool in the 
desiccators (7.4.2.3.6) .  
7.4.2.4.2  Determination of the cement  residue insoluble in the salicylic acid solution  
7.4.2.4.2.1  Place 100 mL of the salicylic acid solution into a 200 -mL beaker. Stir using the stirrer 
(7.4.2.3.3). Slowly add (1.0 ± 0.1) g of the dry cement weighed t o the nearest 0.0001 g ( m). 
7.4.2.4.2. 2 The addition shall be progressive whilst stirring in order to avoid formation of agglomerates 
which are difficult to disperse. After 5 min, interrupt the stirring and check that no lumps of cement remain. If 
they do,  break them up using the flattened end of a glass rod.  
7.4.2.4.2. 3 Continue stirring for 60 min. Allow the solution to settle for 5 min.  
7.4.2.4.2.4   Filter through a sintered glass filter (7.4.2.3.7) previously dried in the oven and weighed ( m1). 
Wash the  insoluble residue six times with approximately 100 mL of methanol in all, allowing it to dry 
completely after each washing. Wash once in diethyl ether.  
7.4.2.4.2. 5 Dry the filter and the insoluble residue for 2 h in the oven (7.4.2.3.2). Allow the filter and the 
insoluble residue to cool in the desiccator (7.4.2.3.8) to ambient temperature and weigh ( m2). 
7.4.2.4.3  Determination of the sulfuric anhydride content  
Determine the sulfuric anhydride content (s) of the cement according to the method described in  FDEAS 148 -
2. 
7.4.2.4.4  Separation of the clinker fraction  
7.4.2.4.4.1  The clinker fraction obtained after separation by dense liquids shall weigh at least 3 g in order 
to carry out the determination of its residue insoluble in the salicylic acid. If this amount is not obtained, repeat 
the separation operations in order to obtain the required amount.  
7.4.2.4.4.2  Add the size fraction to a dense liquid with a density of 3.05 g/cm3 (a mixture of di -
iodomethane and bromoform) at a concentration not exceeding 4  g of material in 100 mL of dense liquid.  
7.4.2.4.2.3  Remove the metal particles using a magnet.  
7.4.2.4.2.4  Transfer the suspension into centrifuge tubes and centrifuge for 5 min at not less than 1 000 
r/min. Separate the supernatant from the residue and reject the supernatant.  EAS 148 -4: 201 7 
26 © EAC 2017  – All rights reserved  
 7.4.2.4.2. 5 Repeat the separation operation at least twice, putting the residue back into suspension in a 
liquid with the same density and centrifuging for 5 min. Reject the supernatants.  
7.4.2.4.2. 6 Rinse the last residue obtained  twice in methanol and once in diethyl ether; dry for 2 h in the 
oven and allow to cool to ambient temperature in the desiccator.  
7.4.2.4.2. 7 Suspend the powder obtained in a dense liquid of density 3.25 g/cm3 (mixture of di -
iodomethane and bromoform) at a  concentration not exceeding 4 g of material per 100 mL of dense liquid.  
7.4.2.4.2. 8 Transfer the suspension into centrifuge tubes and centrifuge for 5 min at not less than 1 000 
r/min. Separate the residue from the supernatant by pouring the supernatant into a new centrifuge tube. 
Reject the residue.  
7.4.2.4.2. 9 Repeat the separation operation at least twice, putting the supernatant back into suspension 
in a liquid of the same density and centrifuging for 5 min. Reject the residues.  
7.4.2.4.2.1 0 Rinse th e last supernatant obtained, twice in methanol and once in diethyl ether, dry for 2 h in 
the oven and allow cooling to ambient temperature in the desiccator.  
7.4.2.4.5  Determination of the clinker residue insoluble in the salicylic acid solution  
7.4.2.4.5. 1 Place 100 mL of the salicylic acid solution into a 200 -mL beaker. Stir using the stirrer 
(7.4.2.3.3).Slowly add (1.0 ± 0.1) g of the clinker fraction prepared in accordance with 7.4.2.4.4.4 and weighed 
to the nearest 0.0001 g ( m3). Continue stirring for 60 min. Allow the solution to settle for 5 min.  
7.4.2.4.5. 2 Filter through a sintered glass filter (7.4.2.3.7) previously dried in the oven and weighed ( m4). 
Wash the insoluble residue six times with approximately 100 mL of methanol, allowing it to dry com pletely 
after each washing. Wash once in diethyl ether.  
7.4.2.4.5. 3 Dry the filter and the insoluble residue for 2 h in the oven (7.4.2.3.2). Allow the filter and the 
insoluble residue to cool in the desiccator (7.4.2.3.8) to ambient temperature and weigh (m5). 
7.4.2.4.6  Determination of the clinker residue insoluble in hydrochloric acid  
7.4.2.4.6.1  Place in a 250 -mL beaker (1.0 ± 0.1) g of the clinker fraction  prepared according to 7.4.2.4.4 
and weighed to the nearest 0.0001 g ( m6). Add 100 mL of water an d disperse. Pour in 40 mL of dilute 
hydrochloric acid (1 + 100) and 60 mL of water and stir for 30 min.  
7.4.2.4.6. 2 Filter through a sintered glass filter (7.4.2.3.7) previously dried in the oven and weighed (m7). 
Wash the insoluble residue with 50 mL of d ilute hydrochloric acid (1 + 500) previously heated to 70 °C. Rinse 
with 10 mL of water, then with methanol and with diethyl ether.  
7.4.2.4.6. 3 Dry the filter and the insoluble residue for 2 h in the oven (7.4.2.3.2). Allow the filter and the 
insoluble res idue to cool to ambient temperature in the desiccators (7.4.2.3.8) and weigh ( m8). 
7.4.2.5  Calculation of the pozzolana content of cement  
Calculate successively the insoluble residue as percentage from the formulae:  

mm m100 R1 2
c
 (28) 

34 5
g
mm m100 R
 (29) EAS 148 -4: 201 7 
© EAC 2017 – All rights reserved  27 
 

67 8
f
mmm100I (30) 
 
S) 1.7 (100S 1.7 R100 Rckp

 (31) 

)I (100IR100 R
ff g
k

 (32) 
The pozzolana content of the sum of the clinker and pozzolana , po, is given by:  

kk kp
0R99R R100 p

 (33) 
NOTE  In this formula, it is assumed that the in soluble residue of the pozzolana in salicylic acid solution is 99 %.  
where  
Rc is the cement residue insoluble in salicylic acid solution;  
Rg is the residue of 3.05 - 3.25 fraction insoluble in salicylic acid solution;  
If is the residue of the 3.05 - 3.25 f raction  insoluble in hydrochloric acid solution;  
Rkp is the cement residue free from set regulator(s) insoluble in salicylic acid solution;  
Rk is the clinker residue insoluble in salicylic acid solution corrected for any contamination;  
S is the sulfuric an hydride content of the cement;  
m is the mass of the cement;  
m1 is the mass of filter;   
m2 is the combined mass of the filter and the insoluble residue;  
m3 is the mass of the clinker;  
m4 is the mass of the filter;  
m5 is the combined mass of the filter and the insoluble residue;  
m6 is the mass of the clinker;  
m7 is the mass of the filter;  
m8 is the combined mass of the filter and the insoluble residue;  
po  is the pozzolana content of the sum of the clinker and pozzolana constituents of the cement.  
7.4.2.6  Repeatability  and reproducibility  
7.4.2.6.1  The standard deviation for repeatability is 1.5 %.  
7.4.2.6. 2 The standard deviation for reproducibility is 3 %.  EAS 148 -4: 201 7 
28 © EAC 2017  – All rights reserved  
 7.4.2.6. 3 These standard deviations are valid for pozzolana contents of cement within the range 0 % - 40 
%. 
 EAS 148 -4: 201 7 
© EAC 2017 – All rights reserved  29 
 Bibliography  
CEN /TR 196-4: 200 7; Methods testing cement - Part 4: Quantitative Determination of constituents.  EAS 148 -4: 201 7   
 
© EAC 2017  – All rights reserved