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EN ISO 26845:2008 Análisis químico de refractarios. Requisitos generales para análisis 2008-03-01
químicos en vía húmeda, espectrometría de absorción atómica y
espectrometría de emisión atómica con plasma de acoplamiento
inductivo (ISO 26845:2008) (Ratificada por AENOR en mayo de 2008.)

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EUROPEAN STANDARD EN ISO 26845

NORME EUROPÉENNE
EUROPÄISCHE NORM March 2008

ICS 81.080 Supersedes ENV 955-4:1997

English Version

Chemical analysis of refractories - General requirements for wet

chemical analysis, atomic absorption spectrometry (AAS) and
inductively coupled plasma atomic emission spectrometry (ICP-
AES) methods (ISO 26845:2008)

Analyse chimique des matériaux réfractaires - Exigences Chemische Analyse feuerfester Erzeugnisse - Allgemeine
générales pour les méthodes d'analyse chimique par voie Anforderungen an die nasschemische Analyse,
humide, par spectrométrie d'absorption atomique (AAS) et Atomabsorptionsspektrometrie-(AAS-)Verfahren und
par spectrométrie d'émission atomique avec plasma induit Verfahren mit induktiv gekoppeltem Plasma (ICP) (ISO
par haute fréquence (ICP-AES) (ISO 26845:2008) 26845:2008)

This European Standard was approved by CEN on 16 February 2008.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European
Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national
standards may be obtained on application to the CEN Management Centre or to any CEN member.

This European Standard exists in three official versions (English, French, German). A version in any other language made by translation
under the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as the
official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,
Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.

EUROPEAN COMMITTEE FOR STANDARDIZATION

COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG

Management Centre: rue de Stassart, 36 B-1050 Brussels

© 2008 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 2[Link] E
worldwide for CEN national Members.

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EN ISO 26845:2008 (E)

Contents Page

Foreword..............................................................................................................................................................3

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EN ISO 26845:2008 (E)

Foreword
This document (EN ISO 26845:2008) has been prepared by Technical Committee ISO/TC 33 "Refractories" in
collaboration with Technical Committee CEN/TC 187 “Refractory products and materials” the secretariat of
which is held by BSI.

This European Standard shall be given the status of a national standard, either by publication of an identical
text or by endorsement, at the latest by September 2008, and conflicting national standards shall be
withdrawn at the latest by September 2008.

Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.

This document supersedes ENV 955-4:1997.

According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech
Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia,
Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain,
Sweden, Switzerland and the United Kingdom.

Endorsement notice

The text of ISO 26845:2008 has been approved by CEN as a EN ISO 26845:2008 without any modification.

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ISO 26845:2008(E)

Contents Page

Foreword............................................................................................................................................................ iv
Introduction ........................................................................................................................................................ v
1 Scope ......................................................................................................................................................1
2 Normative references ............................................................................................................................1
3 Terms and definitions ...........................................................................................................................2
4 Apparatus ...............................................................................................................................................2
5 Reagents.................................................................................................................................................6
6 Sampling ...............................................................................................................................................11
7 Sample mass ........................................................................................................................................12
8 Basic procedure...................................................................................................................................12
9 Determination of loss on ignition (gravimetric)................................................................................12
10 Expression of test results...................................................................................................................13
11 Examination and adoption of test results .........................................................................................13
12 Test report ............................................................................................................................................14

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ISO 26845:2008(E)

Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies
(ISO member bodies). The work of preparing International Standards is normally carried out through ISO
technical committees. Each member body interested in a subject for which a technical committee has been
established has the right to be represented on that committee. International organizations, governmental and
non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the
International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.

International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.

The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.

Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.

ISO 26845 was prepared by Technical Committee ISO/TC 33, Refractories.

It is to be used in conjunction with ISO 10058-1, ISO 10058-2 and ISO 10058-3, ISO 20565-1, ISO 20565-2
and ISO 20565-3, ISO 21079-1, ISO 21079-2 and ISO 21079-3, and ISO 21587-1, ISO 21587-2 and
ISO 21587-3.

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ISO 26845:2008(E)

Introduction
This International Standard gives the general requirements common to the standards used for the chemical
analysis of refractories and refractory products, i.e.:

ISO 10058, Chemical analysis of magnesite and dolomite refractory products (alternative to the X-ray
fluorescence method):
⎯ Part 1: Apparatus, reagents, dissolution and gravimetric silica
⎯ Part 2: Wet chemical analysis
⎯ Part 3: Flame atomic absorption spectrometry (FAAS) and inductively coupled plasma emission
spectrometry (ICP-AES)

ISO 20565 Chemical analysis of chrome-bearing refractory products and chrome-bearing raw materials
(alternative to the X-ray fluorescence method) —
⎯ Part 1: Apparatus, reagents, dissolution and gravimetric silica
⎯ Part 2: Wet chemical analysis
⎯ Part 3: Flame atomic absorption spectrometry (FAAS) and inductively coupled plasma emission
spectrometry (ICP-AES)

ISO 21079 Chemical analysis of refractories containing alumina, zirconia and silica — Refractories containing
5 % to 45 % of ZrO2 (alternative to the X-ray fluorescence method) —
⎯ Part 1: Apparatus, reagents and dissolution
⎯ Part 2: Wet chemical analysis
⎯ Part 3: Flame atomic absorption spectrometry (FAAS) and inductively coupled plasma emission
spectrometry (ICP-AES)

ISO 21587 Chemical analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence
method) —
⎯ Part 1: Apparatus, reagents, dissolution and gravimetric silica
⎯ Part 2: Wet chemical analysis
⎯ Part 3: Inductively coupled plasma and atomic absorption spectrometry methods

These International Standards give wet chemical, AAS and ICP methods for the analysis of refractory
materials and products. They are to be used as an alternative to ISO 12677, when the laboratory does not
have an XRF instrument or its instrument does not meet the requirements of ISO 12677: Chemical analysis of
refractory products by XRF — Fused cast bead method.

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INTERNATIONAL STANDARD ISO 26845:2008(E)

Chemical analysis of refractories — General requirements for

wet chemical analysis, atomic absorption spectrometry (AAS)
and inductively coupled plasma atomic emission spectrometry
(ICP-AES) methods

1 Scope
This International Standard specifies apparatus, reagents, sampling, sample preparation, terms and
definitions, basic procedures, loss on ignition and reporting of results applicable to the following standards,
which are used for the chemical analysis of refractory products and raw materials by wet chemical, AAS and
ICP-AES:

ISO 10058-1, ISO 10058-2 and ISO 10058-3;

ISO 20565-1, ISO 20565-2 and ISO 20565-3;

ISO 21079-1, ISO 21079-2 and ISO 21079-3;

ISO 21587-1, ISO 21587-2 and ISO 21587-3.

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.

ISO 31-0, Quantities and units — Part 0: General principles

ISO 836, Terminology for refractories

ISO 3310-1, Test sieves — Technical requirements and testing — Part 1: Test sieves of metal wire cloth

ISO 5022, Shaped refractory products — Sampling and acceptance testing

ISO 6286, Molecular absorption spectrometry — Vocabulary — General — Apparatus

ISO 6353-1:1982, Reagents for chemical analysis — Part 1: General test methods

ISO 6353-2, Reagents for chemical analysis — Part 2: Specifications — First series

ISO 6353- 3, Reagents for chemical analysis — Part 3: Specifications — Second series

ISO 6955, Analytical spectroscopic methods — Flame emission, atomic absorption, and atomic
fluorescence — Vocabulary

ISO 8656-1, Refractory products — Sampling of raw materials and unshaped products — Part 1: Sampling
scheme

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ISO 26845:2008(E)

3 Terms and definitions

For the purposes of this document, the terms and definitions given in ISO 836 and the following apply.

3.1
dry unshaped refractories
particles and/or powder of unshaped refractories without liquid (mortar and mixture of refractory aggregate
and pitch or resin)

3.2
wet unshaped refractories
particles and/or powder of unshaped refractories with liquid (mortar and mixture of refractory aggregate and
pitch or resin)

3.3
alumina-zirconia-silica refractories
refractories in which aluminium oxide (1 % to 80 % by mass), zirconium oxide (including hafnium oxide) (5 %
to 50 % by mass) and silicon(IV) oxide (0,1 % to 45 % by mass) are used as chemical components

4 Apparatus
Standard laboratory apparatus and the following.

4.1 Spectrometers

4.1.1 Atomic absorption (AA) spectrometer, conforming to the requirements of ISO 6955. An instrument
which can be operated using a dinitrogen oxide/acetylene flame for the determinations of aluminium oxide and
calcium oxide is appropriate.

4.1.2 Flame emission spectrophotometer, comprising a stand-alone flame emission instrument or an AA

spectrometer used in emission mode.

4.1.3 Inductively coupled plasma atomic emission (ICP-AE) spectrometer.

4.1.4 Molecular absorption spectrometer, conforming to the requirements of ISO 6286.

4.1.5 Photometer, with a 1 cm cell.

4.2 Heaters

4.2.1 Burner, such as a Mecker burner or a Bunsen burner.

4.2.2 Electric muffle furnace, suitable for use above 1 150 °C.

4.2.3 Sand bath, comprising an electrically heated or burner-heated iron plate with sand, which can be
heated to the temperature at which white smoke of sulfuric acid occurs.

4.2.4 Steam bath, electric- or burner-type, which can be controlled at the appropriate temperature.

4.3 Devices

4.3.1 Analytical electronic balance, readable to the nearest 0,1 mg.

4.3.2 Magnetic stirrer, comprising a stirring system using a magnetic rotating bar coated with ethylene-4-
fluoride resin.

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ISO 26845:2008(E)

4.3.3 Filter paper, ashless, medium pore.

4.3.4 Cation-exchange resin column, consisting of plastic wool (10 mm) packed into a plastic tube
(diameter 12 mm × 200 mm) with a funnel attached to the top and an eluent outlet sharp-pointed to the
bottom.

Pour a slurry (18 ml) of the water-expanded strongly acidic cation-exchange resin [divinylbenzene 8 % (DVB),
75 µm to 150 µm] into the column. Adjust the flow rate to 1,0 ml to 1,5 ml per minute by the packing condition
of the plastic wool. Wash the column with hydrochloric acid (1+2, 120 ml) and water (70 ml). An example of a
normal column is shown in Figure 1.

Dimensions in millimetres

Key
1 polypropylene funnel
2 cation-exchange resin
3 polypropylene wool

Figure 1 — Example of a cation-exchange resin column

4.4 Platinum ware

The platinum apparatus may be of platinum or platinum alloy.

4.4.1 Platinum crucible, with a volume of 20 ml or 30 ml.

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ISO 26845:2008(E)

4.4.2 Platinum dish, with the diameters of the base and wall almost the same, and a height of
approximately half the diameter. 75 ml or 150 ml volume are commonly used sizes.

4.5 Glassware

4.5.1 Burette, with a 0,1 ml scale and a maximum volume of 50 ml.

4.5.2 Conical flask, capable of holding a volume of 500 ml and 1 l.

4.5.3 Desiccator, containing dried silica gel as the drying agent.

4.5.4 Erlenmeyer flask, capable of holding a volume of 500 ml.

4.5.5 Glass beakers, with a range of appropriate volumes (100 ml, 200 ml, 300 ml, 400 ml, 500 ml, etc.).

4.5.6 One-mark pipette, suitable for the transfer of each sample solution or standard solution.

4.5.7 Reflux steel head, comprising a funnel, with a long leg capable of being bent so that the end touches
the inside wall of a flask (see Figure 2).

Dimensions in millimetres

a) Steel head b) Steel head setting

Key
1 steel head
2 erlenmeyer flask
3 head that contacts internal wall

Figure 2 — Steel head for reflux

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ISO 26845:2008(E)

4.5.8 Separating funnels, 250 ml and 500 ml, with stoppers.

4.5.9 Volumetric flasks, made of glassware (100 ml, 250 ml, 500 ml, 1 000 ml, etc.) as appropriate for
each solution.

4.5.10 Volumetric pipette, of capacity 5 ml.

4.5.11 Watch glass, of diameter 75 mm.

4.6 Porcelain ware

4.6.1 Porcelain basin, with a diameter of 125 mm.

4.6.2 Porcelain crucible, capable of holding a volume of 15 ml.

4.7 Plastic ware

4.7.1 Plastic beaker, of capacity 100 ml.

4.7.2 Polyethylene tetrafluoride beaker, of capacity 200 ml. Heat in nitric acid for at least 2 h and wash in
water.

NOTE Instead of a polyethylene tetrafluoride beaker, a 150 ml platinum dish can be used.

4.7.3 Volumetric flasks, made of plastic, as appropriate for each solution, and calibrated as follows. Either

a) wash a plastic flask thoroughly, invert it and allow it to stand to dry naturally, or

b) wash a plastic flask with water, ethanol and diethylether and dry it by blowing air into it.

Cut 20 graduations from a sheet of section paper (1 mm squares) into a strip and attach it to the marked line
of the plastic flask, so that the line coincides with the central line of the paper. Weigh the flask to the nearest
milligram.

Add water at approximately room temperature up to the lower end (B) of the strip, and weigh the flask. Then
add more water up to the upper end (A) of the strip, and weigh the flask. Separately, measure the water
temperature, in degrees Celsius, the room temperature, in degrees Celsius and the atmospheric pressure, in
kilopascals, and obtain the correct marked line, S, the number of graduations counted from the bottom edge
(B) of the graduation paper, using the following equation:

⎡ 1 000 000 − ( m + m′) ⎤

⎢ f ⎥ − mB
S= ⎣ ⎦
m A − mB
20

where

mA is the mass of water up to the top edge (A) of the graduated paper, in milligrams, [i.e. (mass obtained
by second weighing) – (mass of Erlenmeyer flask)]; mA = mB + [mass of water from (A) to (B)];

mB is the mass of water up to to bottom edge (B) of the graduated paper, in milligrams, [i.e. (mass
obtained by first weighing) – (mass of Erlenmeyer flask)] ;

m is the correction value, in milligrams, at 20 °C room temperature, and 101,325 kPa {760 mmHg}
atmospheric pressure;

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ISO 26845:2008(E)

m′ is the correction value, in milligrams, due to deviation from a room temperature of 20 °C, and an
atmospheric pressure of 101,325 kPa [760 mmHg]; it is ± 4,0 mg per ± 1 °C room temperature, and
± 1,3 mg per ± 0,133 kPa (1 mmHg) atmospheric pressure;

100
f is a constant given by
normal capacity of plastic flask to be calibrated

Mark the new line on the strip.

NOTE When the correct line is shown on the flask, the strip can be removed.

4.8 Miscellaneous

4.8.1 Electric muffle furnace, capable of being controlled at temperatures up to at least 1 100 °C.

4.8.2 Desiccator.

4.8.3 pH meter, with a glass electrode.

5 Reagents
During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only
distilled water or water of equivalent purity.

Reagents should conform to the requirements of ISO 6353-1，ISO 6353-2 and ISO 6353-3, as appropriate.
Specific requirements for reagents are given in the appropriate clause.

5.1 Stock reagents

5.1.1 Acetic acid, concentrated, (ISO 6353-2, R 1) minimum mass fraction 99,7 %.

5.1.2 Aluminium chloride solution, Al (25 mg/ml). Dissolve 123,5 g of aluminium chloride in water and
dilute to 1 l with water.

5.1.3 Aluminium oxide solution, Al2O3, 10 mg/ml. Weigh 5,3 g of aluminium (minimum mass fraction
99,9 %) in a 300 ml beaker and cover with a watch glass. Then add 250 ml of hydrochloric acid (1+1) and
heat on a steam bath until dissolved. Remove the watch glass and evaporate to 30 ml to remove excess
hydrochloric acid. After cooling, add water and dilute to 1 000 ml in a volumetric flask with water.

5.1.4 Ammonia solution, concentrated (ISO 6353-2, R 3), minimum mass fraction 25 %.

5.1.5 Ammonia solution (1+1). Add 1 volume of ammonia solution (concentrated) to 1 volume of water.

5.1.6 Ammonia solution (1+9). Add 1 volume of ammonia water (concentrated) to 9 volumes of water.

5.1.7 Ammonium acetate buffer solution. Add 120 ml of acetic acid to 500 ml of water, followed by 74 ml
of ammonia solution (concentrated) (5.1.4). Dilute to 1 l.

5.1.8 Ammonium acetate solution, 100 g/l. Dissolve 100 g of ammonium acetate in water and dilute to 1l.

5.1.9 Ammonium acetate solution, 200 g/l. Dissolve 200 g of ammonium acetate in water and dilute to 1 l.

5.1.10 Ammonium chloride.

5.1.11 Ammonium chloride solution, 20 g/l. Dissolve 10 g of ammonium chloride in 500 ml of water, add a
drop of methyl red solution and drop in ammonia solution (1+9) (5.1.6) until the colour turns yellow. If the
colour becomes red again due to heating, drop in ammonia solution (1+9).

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ISO 26845:2008(E)

5.1.12 Ammonium ceric nitrate solution, 10 g/l. Dissolve 5 g of ammonium ceric nitrate in about 200 ml of
water. Cautiously add 7 ml of sulfuric acid, cool, dilute to 500 ml with water and mix.

5.1.13 Ammonium molybdate solution, 100 g/l. Dissolve 10 g of ammonium molybdate tetrahydrate in
100 ml of water, and filter if necessary. Store in a plastic bottle. Discard after 4 weeks.

5.1.14 Ammonium molybdate solution, 80 g/l. Dissolve 40 g of ammonium molybdate tetrahydrate in

500 ml of water, and filter if necessary. Store in a plastic bottle. Discard after 4 weeks or earlier if any visible
deposit of molybdic acid is observed.

5.1.15 Ammonium molybdate solution, 20 g/l. Dissolve 2 g of ammonium molybdate tetrahydrate in 20 ml

of hot water, filter if necessary and dilute to 100 ml with the addition of 60 ml of sulfuric acid (1+1) and water.

5.1.16 L(+)-ascorbic acid solution, 100 g/l. Dissolve 10 g of L (+)-ascorbic acid in water and dilute to
100 ml. This solution shall be kept in the dark and at a low temperature. Discard after 2 weeks.

5.1.17 Boric acid, H3BO3.

5.1.18 Boric acid solution, 40 g/l. Dissolve 40 g of boric acid in water and dilute to 1 l.

5.1.19 Buffer solution, (pH 10). Dissolve 70 g of ammonium chloride in 570 ml of ammonia solution
(concentrated) (5.1.4) and dilute to 1 000 ml with water.

5.1.20 Chloroform, (ISO 6353-2, R7) minimum mass fraction 99 %.

5.1.21 Chromium(III) oxide solution, Cr2O3 10 mg/ml. Weigh 6,8 g of chromium (minimum mass fraction
more than 99,9 %) in a 300 ml beaker and cover with a watch glass. Add 250 ml of hydrochloric acid (1+1)
and heat until dissolved on a steam bath. Remove the watch glass and evaporate until 30 ml remains, to
remove excess hydrochloric acid. Cool and transfer to a 1 000 ml volumetric flask and dilute to the mark with
water.

5.1.22 Cupferron, 60 g/l. Dissolve 6 g of cupferron in 100 ml of water. Filter if necessary. Prepare this
solution freshly when required. Store the solid reagent in a tightly stoppered bottle, in the presence of a piece
of ammonium carbonate to prevent decomposition.

5.1.23 CyDTA solution, 8 g/l. Add 4,6 ml of sodium hydroxide solution, 100 g/l, to 2 g of
cyclohexanediamine tetraacetate hydrate and dissolve by heating. After cooling, dilute to 250 ml with water.

5.1.24 Diantipyrylmethane (DAM) solution, 10 g/l. Dissolve 1 g of diantipyrylmethane monohydrate in

30 ml of hydrochloric acid (1+50), and dilute to 100 ml with water.

5.1.25 Diethyl ether.

5.1.26 Diphenylcarbazide solution, 10 g/l. Dissolve 0,1 g of diphenylcarbazide in 10 ml of acetone. It is

essential to prepare this solution immediately before use.

5.1.27 Eluent A, 0,8 mol/l hydrofluoric acid, 0,65 mol/l boric acid. Dissolve 40 g of boric acid in 960 ml of
water, pour the solution into a plastic vessel (1 l) and add 35 ml of hydrofluoric acid (minimum mass fraction
46 %). Mix by shaking.

5.1.28 Eluent B. Combine 995 ml of water and 5 ml of hydrofluoric acid (minimum mass fraction 46 %) in a
suitably sized plastic vessel and mix by shaking.

5.1.29 Filter-paper pulp, powdery.

5.1.30 Ethanol, minimum mass fraction 95 %.

5.1.31 Fusion mixture. Mix anhydrous sodium and potassium carbonates in equimolar proportions.

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ISO 26845:2008(E)

5.1.32 Hexamethylenetetramine (hexamine).

5.1.33 Hydrazinium dichloride solution, 150 g/l. Dissolve 15 g of hydrazinium dichloride in water and dilute
to 100 ml.

5.1.34 Hydrochloric acid, concentrated, (ISO 6353-3, R 13), minimum mass fraction 35 %.

5.1.35 Hydrochloric acid (1+1). Add 1 volume of hydrochloric acid, concentrated (5.1.32) to 1 volume of
water.

5.1.36 Hydrochloric acid (1+2). Add 1 volume of hydrochloric acid, concentrated (5.1.32) to 2 volumes of
water.

5.1.37 Hydrochloric acid (1+3). Add 1 volume of hydrochloric acid, concentrated (5.1.32) to 3 volumes of
water.

5.1.38 Hydrochloric acid (1+4). Add 1 volume of hydrochloric acid, concentrated (5.1.32) to 4 volumes of
water.

5.1.39 Hydrochloric acid (1+9). Add 1 volume of hydrochloric acid, concentrated (5.1.32) to 9 volumes of
water.

5.1.40 Hydrochloric acid (1+20). Add 1 volume of hydrochloric acid, concentrated (5.1.32) to 20 volumes of
water.

5.1.41 Hydrochloric acid (1+50). Add 1 volume of hydrochloric acid, concentrated (5.1.32) to 50 volumes of
water.

5.1.42 Hydrochloric acid (1+150). Add 1 volume of hydrochloric acid, concentrated (5.1.32) to 150 volumes
of water.

5.1.43 Hydrofluoric acid, concentrated, (ISO 6353-3, R 67), minimum mass fraction 40 % to 48 %.

5.1.44 Hydrofluoric acid (1+9). Add 1 volume of hydrofluoric acid, concentrated (5.1.41) to 9 volumes of
water. Store in a plastic container.

5.1.45 Hydrogen peroxide solution, minimum mass fraction 30 %.

5.1.46 Hydrogen peroxide solution, minimum mass fraction 6 %.

5.1.47 Hydroxyammonium chloride solution, 100 g/l. Dissolve 10 g of hydroxyammonium chloride in

warm water, filter if necessary, cool and dilute to 100 ml.

5.1.48 Iron(III) oxide solution, Fe2O3, 10 mg/ml. Weigh 7,0 g of iron (minimum mass fraction 99,9 %) in a
300 ml beaker and cover with a watch glass. Then add 250 ml of hydrochloric acid (1+1) and heat until
dissolved on a steam bath. Remove the watch glass and evaporate until 30 ml remains, to remove excess
hydrochloric acid. After cooling, transfer to a 1 000 ml volumetric flask, and dilute to the mark with water.

5.1.49 Iron(III) chloride solution. Dissolve 1 g of iron(III) chloride hexahydrate in 100 ml of hydrochloric acid
(1+50) (5.1.39).

5.1.50 Lanthanum solution, 50 g/l. Weigh 50 g of lanthanum(III) oxide into a 1 000 ml beaker. Carefully add
200 ml of hydrochloric acid (1+1) and dissolve while heating. Dilute to 1 000 ml with water. If the reaction is
too violent on addition of hydrochloric acid (1+1), move the beaker into flowing water to cool.

5.1.51 Magnesium oxide solution, MgO, 10 mg/ml. Weigh 6 g of magnesium metal (minimum mass
fraction 99,9 % and a mass fraction of Si less than 0,001 %), transfer to a 500 ml beaker and cover with a
watch glass. Add 100 ml of hydrochloric acid (1+1), and heat on a steam bath until dissolved. After cooling,
transfer to a 1 000 ml volumetric flask, and dilute to the mark with water.

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ISO 26845:2008(E)

5.1.52 DL-mandelic acid.

5.1.53 Mixed acid. Mix sulfuric acid (1+1) and phosphoric acid with a 1:1 ratio.

5.1.54 Nitric acid, concentrated, minimum mass fraction 65 %.

5.1.55 Nitric acid (1+1). Add one volume of nitric acid, concentrated (5.1.52) to one volume of water.

5.1.56 Nitric acid (1+3). Add one volume of nitric acid, concentrated (5.1.52) to three volumes of water.

5.1.57 Nitric acid (1+20). Add one volume of nitric acid, concentrated (5.1.52) to twenty volumes of water.

5.1.58 2,2′, 2″-Nitrilotriethanol (1+1). Add 1 volume of 2,2′, 2″-nitrilotriethanol to one volume of water.

5.1.59 Perchloric acid, concentrated, minimum mass fraction 70 %.

5.1.60 1,10-Phenanthrolinium chloride solution, 1 g/l. Dissolve 0,1 g of 1,10-phenanthrolinium chloride

monohydrate in water, dilute to 100 ml, and keep in a dark and cool place. Discard the solution if it becomes
coloured during storage.

5.1.61 1,10-Phenanthrolinium chloride solution, 10 g/l. Dissolve 1 g of 1,10-phenanthrolinium chloride

monohydrate in 100 ml of water, and keep in a dark and cool place. Discard the solution if it becomes
coloured during storage.

5.1.62 Ortho-phosphoric acid, minimum mass fraction 98 %.

5.1.63 Phosphoric acid, concentrated, minimum mass fraction 85 %.

5.1.64 Phosphoric acid (2+3). Add 2 volumes of phosphoric acid, concentrated (5.1.61) to 3 volumes of
water, then mix and leave to cool.

5.1.65 Phosphoric acid (1+9). Add 1 volume of phosphoric acid, concentrated (5.1.61) to 9 volumes of
water, then mix and leave to cool.

5.1.66 Partially hydrolysed polyacrylamide, aqueous solution, 20 g/l.

5.1.67 Polyethylene oxide solution, 2,5 g/l. Add 0,5 g of polyethylene oxide to 200 ml of water slowly while
stirring, preferably on a mechanical stirrer, until dissolved. Discard after two weeks.

5.1.68 Polyethylene oxide solution, 0,5 g/l. Add 0,1 g of polyethylene oxide to 200 ml of water slowly while
stirring, preferably on a mechanical stirrer, until dissolved. Discard after two weeks.

5.1.69 Potassium hydroxide solution, 250 g/l. Dissolve 250 g of potassium hydroxide in water, cool and
dilute to 1 l. Store in a polyethylene bottle.

5.1.70 Potassium chloride.

5.1.71 Potassium disulfate, pure.

5.1.72 Potassium periodate.

5.1.73 Potassium permanganate solution, 3 g/l. Dissolve 0,6 g of potassium permanganate in 200 ml of
water. Store in the dark.

5.1.74 Silver nitrite solution, 10 g/l. Store the reagent in a brown bottle.

5.1.75 Sodium azide solution, 20 g/l. Dissolve 2 g of sodium azide in 100 ml of water and mix.

5.1.76 Sodium carbonate, anhydrous.

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ISO 26845:2008(E)

In some brands of this agent, a minute quantity of calcium oxide is included. When determining calcium oxide
by inductively coupled plasma atomic emission spectrometry (ICP-AES), a pure high-quality agent should be
used.

5.1.77 Sodium diethyldithiocarbamate solution, 100 g/l. Dissolve 5 g of sodium diethyldithiocarbamate

cupferron in 50 ml of water. Filter if necessary. Prepare this solution freshly when required.

5.1.78 Sodium diphenylamine-4-sulfonate solution, 2 g/l.

5.1.79 Sodium hydroxide solution, 100 g/l. Cautiously, to avoid a vigorous reaction, dissolve 20 g of
sodium hydroxide in 150 ml of water, while stirring and cooling. After cooling, dilute to approximately 200 ml.

5.1.80 Sodium sulfide solution, 100 g/l. Dissolve 1 g of sodium sulfide nonahydrate in 10 ml of water.
Prepare this solution freshly when required.

5.1.81 Sulfuric acid, concentrated, (ISO 6353-2, R 37), minimum mass fraction 95 %.

5.1.82 Sulfuric acid solution (1+1). Cautiously add, while stirring, 200 ml of sulfuric acid, concentrated
(5.1.79) to 200 ml of water, while cooling the solution.

5.1.83 Sulfuric acid solution (1+3). Cautiously add, while stirring, 200 ml of sulfuric acid, concentrated
(5.1.79) to 600 ml of water, while cooling the solution.

5.1.84 Sulfuric acid solution (1+4), Cautiously add, while stirring, 50 ml of sulfuric acid, concentrated
(5.1.79) to 200 ml of water, while cooling the solution.

5.1.85 Sulfuric acid solution (1+5). Cautiously add, while stirring, 50 ml of sulfuric acid, concentrated
(5.1.79) to 250 ml of water, while cooling the solution.

5.1.86 Sulfuric acid solution (1+9). Cautiously add, while stirring, 20 ml of sulfuric acid, concentrated
(5.1.79) to 180 ml of water, while cooling the solution.

5.1.87 Sulfuric acid solution (1+15). Cautiously add, while stirring, 20 ml of sulfuric acid, concentrated
(5.1.79) to 300 ml of water, while cooling the solution.

5.1.88 Sulfuric acid solution (1+150). Cautiously add, while stirring, 5 ml of sulfuric acid, concentrated
(5.1.79) to 750 ml of water, while cooling the solution.

5.1.89 L(+)-tartaric acid solution, 100 g/l. Dissolve 100 g of L(+)-tartaric acid with water and dilute to 1 l.

5.2 Indicators

5.2.1 Barium diphenylamine sulfonate.

5.2.2 Bromophenol blue, 1 g/l solution. Dissolve 0,4 g of sodium hydroxide in 100 ml of water to make
NaOH 4 g/l. Grind 0,1 g of bromophenol blue with 1,5 ml of sodium hydroxide solution (4 g/l), dilute to 100 ml
with water and mix.

5.2.3 Calcein indicator (screened), (3,3′-bis[N,N′-bis(carboxylmethyl) aminomethyl fluorescein). Mix, by

grinding together, 0,2 g of calcein, 0,12 g of thymolphthalein and 20,0 g of potassium chloride.

5.2.4 2,4-Dinitrophenol, saturated solution. Dissolve 1 g of 2,4-dinitrophenol in 100 ml of hot water, cool
and filter.

5.2.5 Dithizone indicator, 0,25 g/l. Dissolve 0,012 5 g of dithizone in 50 ml of ethanol (mass fraction
95 %). The solution will keep for at least a week.

5.2.6 Eriochrome Black T solution, 2 g/l. Dissolve 0,20 g of Eriochrome Black T in 100 ml of ethanol and
add 0,5 g of hydroxylammonium chloride. Store in a black glass bottle with a stopper.

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ISO 26845:2008(E)

5.2.7 Methyl orange solution, 0,5 g/l. Dissolve 0,05 g of methyl orange in 100 ml of hot water, cool and
filter.

5.2.8 Methyl thymol blue complexone indicator. Mix, by grinding together, 0,2 g of methyl thymol blue
complexone and 20 g of potassium nitrate.

5.2.9 Methyl orange solution, 0,4 g/l. Dissolve 0,10 g of methyl orange C.I. 13025 in 50 ml of ethanol
(minimum volume fraction 95 %) and dilute to 250 ml with water in accordance with ISO 6353-1:1982, 4.3.5.
Keep this solution in a dark glass bottle.

5.2.10 Methyl red solution, 0,1 g/l. Warm 25 mg of finely powdered methyl red C.I. 13020 with 0,95 ml of
sodium hydroxide solution (2 g/l) and 5 ml of ethanol (mass fraction 95 %), and dilute to 250 ml with water in
accordance with ISO 6353-1:1982, 4.3.6. Keep this solution in a dark glass bottle.

5.2.11 p-Nitrophenol solution, 2 g/l. Dissolve 0,20 g of p-nitrophenol in 100 ml of water.

5.2.12 Solochrome Black 6B indicator, (as Eliochrome Blue-Black B). Mix, by grinding together, 0,5 g of
Solochrome Black 6B and 20 g of sodium chloride.

5.2.13 Xylenol orange solution, 1 g/l. Dissolve 0,10 g of the xylenol orange with water and dilute to 100 ml.
Keep this solution in the dark in a refrigerator. Discard after 4 weeks.

6 Sampling

6.1 General

Take a laboratory sample in accordance with ISO 5022 for shaped, fired refractory products, and with
ISO 8656-1 for unshaped refractory products and raw materials, or by a procedure agreed between the
parties concerned.

6.2 Refractory brick or its raw material

Crush the laboratory sample obtained in 6.1 to pass through a 6,7 mm sieve, conforming to the requirements
of ISO 3310-1, and reduce to 100 g by riffling or quartering. Grind the reduced sample to pass through a
300 µm sieve conforming to the requirements of ISO 3310-1.

6.3 Unshaped refractory products

6.3.1 Dry unshaped refractory products

Carry out the procedures specified in 6.1 and 6.2.

6.3.2 Wet unshaped refractory products

Spread the laboratory sample obtained in 6.1 on a heat-resistant plate that will not react with the sample (e.g.
polyethylene tetrafluoride plate) to form a charge of 10 mm thickness. Dry in an air-bath at 110 °C ± 5 °C for at
least 10 h. Crush the sample as described in 6.2.

6.4 Preparation of the test sample

Reduce the sample prepared using the procedure specified in 6.1 to about 10 g by quartering, and grind the
sample to pass through a 106 µm sieve conforming to the requirements of ISO 3310-1. This is the test sample
for analysis.

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ISO 26845:2008(E)

Transfer the sample into a container (e.g. flat weighing bottle, 50 mm × 30 mm), spread it in a thin layer and
dry it in a drying oven at 110 °C ± 5 °C for at least 2 h.

Cool and store in a desiccator.

7 Sample mass
Weigh the required quantity of the test portion for each chemical analysis to the nearest 0,1 mg.

8 Basic procedure

8.1 Number of determinations

Carry out each chemical analysis twice.

8.2 Blank test

During each chemical analysis, carry out a blank test. The result of the blank test is deducted from the
determination in each case, to give the test result.

9 Determination of loss on ignition (gravimetric)

9.1 Principle

A sample is heated at 1 025 °C ± 25 °C to constant mass and the loss or gain of mass is measured.

9.2 Procedure

Heat a platinum or a porcelain crucible to 1 025 °C ± 25 °C, using the furnace for 15 min. Cool in a desiccator
and weigh, using an electronic balance, to the nearest 0,1 mg.

Transfer 1,0 g of the dry sample, prepared in accordance with 6.1, into the crucible and weigh the crucible and
sample to the nearest 0,1 mg.

Place the crucible without a lid in an electric muffle furnace and raise the temperature to 1 025 °C ± 25 °C.
Maintain this temperature for 30 min and allow to cool with a lid. Weigh the mass of the crucible plus the
ignited sample to the nearest 0,1 mg. Repeat this loss on ignition at 15 min intervals until constant mass is
reached.

9.3 Calculation of results

Calculate the loss on ignition, LOI, as a percentage by mass, using the following equation:

m 2 − m3
LOI = × 100
m 2 − m1

where

m1 is the mass of the empty crucible, in grams;

m2 is the mass of the crucible and sample, in grams;

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ISO 26845:2008(E)

m3 is the mass of the crucible and ignited sample, in grams.

NOTE If a gain on ignition is observed, a minus sign is added before the numerical value.

10 Expression of test results

Calculate the test results as a percentage composition on a dry basis, and express the result as the mean of
the two determinations in accordance with ISO 31-0, as follows:

a) if an integer part of the percentage is two digits, express the result to one decimal place;

b) if an integer part of the percentage is one digit, express the result to two decimal places.

11 Examination and adoption of test results

If the absolute difference between the two test results is less than the error margin given in Table 1, the mean
test result is reported as the final value.

If the absolute difference between the two test results is equal to, or greater than, the error margin given in
Table 1, test two further samples. If the absolute difference between the two test results is equal to, or less
than, the values given in Table 1, report the arithmetical mean of the four test results as the final value. If the
range of four test results exceeds the values given in Table 1, report the median of the test results as the final
value.

Table 1 — Permissible difference in test values

Component
Mass % by mass
fraction
MnO
% LOI SiO2 Al2O3 Fe2O3 TiO2 or CaO MgO Na2O K2O HfO2 ZrO2 P2O5 B2O3
Cr2O3

Under 0,1 0,02 0,02 0,02 0,01 0,01 0,01 0,02 0,02 0,02 0,02 0,01 0,02 0,02 0,02
∼ 0,2 0,05 0,02 0,02 0,02 0,02 0,02 0,05 0,05 0,05 0,05 0,02 0,02 0,05 0,05

∼ 0,5 0,05 0,05 0,05 0,03 0,03 0,05 0,05 0,05 0,05 0,05 0,05 0,03 0,05 0,05

∼2 0,05 0,05 0,05 0,04 0,04 0,05 0,05 0,05 0,05 0,05 0,05 0,05 0,05 0,05

∼5 0,10 0,10 0,10 0,05 0,05 0,1 0,10 0,10 0,10 0,10 0,10 0,1 0,10

∼ 10 0,20 0,20 0,20 0,20 0,2 0,2 ― 0,20 0,20 0,20 0,20 0,2 ―

∼ 20 0,2 0,20 0,2 0,2 ― 0,2 ― 0,2 0,20 0,20 0,2 0,2 ―

∼ 50 0,2 0,20 0,2 0,2 ― 0,4 ― 0,2 ― ― 0,4 0,4 ―

Over 50 0,2 0,3 0,3 ― ― ― ― 0,2 ― ― 0,2 ― ―

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ISO 26845:2008(E)

12 Test report

The test report shall contain, as a minimum, the following information:

a) all information necessary for identification of the sample tested;

b) a reference to this International Standard (ISO 26485:2008);

c) the method used (wet chemical analysis, ICP or AAS), with reference to the appropriate parts of the other
International Standards giving the test methods, i.e. ISO 10058-1, ISO 10058-2 and ISO 10058-3,
ISO 20565-1, ISO 20565-2 and ISO 20565-3, ISO 21079-1, ISO 21079-2 and ISO 21079-3, and
ISO 21587-1, ISO 21587-2 and ISO 21587-3;

d) the results of the tests, including the results of the individual determinations and their means, calculated
as specified in each method and expressed in accordance with Clause 10;

e) any deviations from the procedure specified;

f) any unusual features (anomalies) observed during the test;

g) the date of the test.

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