SIST EN 889:2005
(Main)Chemicals used for treatment of water intended for human consumption - Iron (II) sulfate
Chemicals used for treatment of water intended for human consumption - Iron (II) sulfate
This document is applicable to iron (II) sulfate heptahydrate used for treatment of water intended for human consumption. It describes the characteristics of iron (II) sulfate heptahydrate and specifies the requirements and the corresponding analytical methods for iron (II) sulfate heptahydrate (analytical methods are given in Annex B) and gives information on its use in water treatment.
Produkte zur Aufbereitung von Wasser für den menschlichen Gebrauch - Eisen (II) sulfat
Diese Europäische Norm gilt für Eisen(II)sulfat-Heptahydrat zur Aufbereitung von Wasser für den menschlichen Gebrauch. Sie beschreibt die Eigenschaften von Eisen(II)sulfat-Heptahydrat und legt die Anforderungen sowie die entsprechenden Prüfverfahren für Eisen(II)sulfat-Heptahydrat fest. Sie gibt Informationen über die Anwendung von Eisen(II)sulfat-Heptahydrat in der Wasseraufbereitung.
ANMERKUNG Eine Übereinstimmung mit dieser Norm bedeutet keine gleichzeitige Annahme oder Zulassung des Produktes in einem der Mitgliedsländer der EU oder EFTA. Die Anwendung des in dieser Europäischen Norm beschriebenen Produktes unterliegt den jeweiligen Regelungen der nationalen autorisierten Stellen.
Produits chimiques utilisés pour le traitement de l'eau destinée a la consommation humaine - Sulfate de fer (II)
Kemikalije, ki se uporabljajo za pripravo pitne vode - Železov (II) sulfat
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN 889:2005
01-marec-2005
1DGRPHãþD
SIST EN 889:2000
Kemikalije, ki se uporabljajo za pripravo pitne vode - Železov (II) sulfat
Chemicals used for treatment of water intended for human consumption - Iron (II) sulfate
Produkte zur Aufbereitung von Wasser für den menschlichen Gebrauch - Eisen (II) sulfat
Produits chimiques utilisés pour le traitement de l'eau destinée a la consommation
humaine - Sulfate de fer (II)
Ta slovenski standard je istoveten z: EN 889:2004
ICS:
13.060.20 Pitna voda Drinking water
71.100.80 .HPLNDOLMH]DþLãþHQMHYRGH Chemicals for purification of
water
SIST EN 889:2005 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN 889:2005
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SIST EN 889:2005
EUROPEAN STANDARD
EN 889
NORME EUROPÉENNE
EUROPÄISCHE NORM
November 2004
ICS 71.100.80 Supersedes EN 889:1998
English version
Chemicals used for treatment of water intended for human
consumption - Iron (II) sulfate
Produits chimiques utilisés pour le traitement de l'eau Produkte zur Aufbereitung von Wasser für den
destinée à la consommation humaine - Sulfate de fer (II) menschlichen Gebrauch - Eisen (II) sulfat
This European Standard was approved by CEN on 30 September 2004.
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 Central Secretariat 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 Central Secretariat has the same status as the official
versions.
CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,
Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, 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
© 2004 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 889:2004: E
worldwide for CEN national Members.
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SIST EN 889:2005
EN 889:2004 (E)
Contents
Page
Foreword.3
Introduction .4
1 Scope .5
2 Normative references .5
3 Description .5
4 Purity criteria.7
5 Test methods.9
6 Labelling - Transportation - Storage.11
Annex A (informative) General information on iron (ll) sulfate.12
Annex B (normative) Analytical methods .17
Annex C (informative) Determination of cadmium, chromium, nickel and lead (inductively coupled
plasma optical emission spectrometry (ICP/OES)).30
Bibliography .32
2
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SIST EN 889:2005
EN 889:2004 (E)
Foreword
This document (EN 889:2004) has been prepared by Technical Committee CEN/TC 164 “Water supply”, the
secretariat of which is held by AFNOR.
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 May 2005, and conflicting national standards shall be withdrawn at the latest by
May 2005.
This document supersedes EN 889:1998.
Significant technical differences between this edition and EN 889:1998 are as follows:
a) replacement of the reference of to EU Directive 80/778 of 15 July 1980 with the latest Directive in force
(see[1]);
b) expansion of annex A by addition of A.2 "quality of commercial product";
c) deletion of annex D.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark,
Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,
Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
3
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SIST EN 889:2005
EN 889:2004 (E)
Introduction
In respect of potential adverse effects on the quality of water intended for human consumption, caused by the
product covered by this Standard:
a) this Standard provides no information as to whether the product may be used without restriction in any of the
Member States of the EU or EFTA;
b) It should be noted that, while awaiting the adoption of verifiable European criteria, existing national regulations
concerning the use and/or the characteristics of this product remain in force.
NOTE Conformity with the standard does not confer or imply acceptance or approval of the product in any of the Member
States of the EU or EFTA. The use of the product covered by this document is subject to regulation or control by National
Authorities.
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SIST EN 889:2005
EN 889:2004 (E)
1 Scope
This document is applicable to iron (II) sulfate heptahydrate used for treatment of water intended for human
consumption. It describes the characteristics of iron (II) sulfate heptahydrate and specifies the requirements and
the corresponding analytical methods for iron (II) sulfate heptahydrate (analytical methods are given in Annex B)
and gives information on its use in water treatment.
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.
EN ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696:1987).
ISO 3165, Sampling of chemical products for industrial use - Safety in sampling.
ISO 6206, Chemical products for industrial use - Sampling - Vocabulary.
ISO 8213, Chemical products for industrial use - Sampling techniques - Solid chemical products in the form of
particles varying from powders to coarse lumps.
3 Description
3.1 Identification
3.1.1 Chemical name
Iron (II) sulfate heptahydrate.
3.1.2 Synonym or common names
Ferrous sulfate, iron vitriol, copperas, green salt.
3.1.3 Relative molecular mass
278,02.
3.1.4 Empirical formula
FeSO . 7H O.
4 2
3.1.5 Chemical formula
FeSO . 7H O.
4 2
5
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SIST EN 889:2005
EN 889:2004 (E)
1)
3.1.6 CAS Registry Number
7782-63-0 (FeSO . 7H O).
4 2
7720-78-7 (FeSO ).
4
2)
3.1.7 EINECS reference
231-753-5 (FeSO ).
4
3.2 Commercial forms
The iron (ll) sulfate heptahydrate is available as wet crystals (a) or free-flowing crystals (b).
3.3 Physical properties
3.3.1 Appearance
The iron (ll) sulfate heptahydrate is a light green crystal.
3.3.2 Density
3
The density of iron (ll) sulfate heptahydrate is equal to 1,9 g/cm at 20 °C.
3
The bulk density of commercial form a) is equal approximately to 1 kg/dm and of commercial form b)
3
approximately to 0,8 kg/dm .
3.3.3 Solubility (in water)
The solubility of iron (II) sulfate heptahydrate is 487 g/l at 20 °C.
3.3.4 Vapour pressure
Not applicable.
3)
3.3.5 Boiling point at 100 kPa
Not applicable.
3.3.6 Melting point
For the iron (ll) sulfate heptahydrate the melting starts at approximately 64 °C, leading to decomposition.
3.3.7 Specific heat
Not known.
3.3.8 Viscosity (dynamic)
Not applicable.
1)
Chemical Abstracts Service Registry Number.
2)
European Inventory of Existing Commercial Chemical Substances.
3)
100 kPa = 1 bar.
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SIST EN 889:2005
EN 889:2004 (E)
3.3.9 Critical temperature
Not applicable.
3.3.10 Critical pressure
Not applicable.
3.3.11 Physical hardness
Not applicable.
3.4 Chemical properties
Iron (II) sulfate heptahydrate and especially solutions of iron (II) sulfate heptahydrate have acid and reducing
properties. They react by oxidation or hydrolysis (depending on the pH).
4 Purity criteria
4.1 General
This document specifies the minimum purity requirements for iron (II) sulfate used for the treatment of water
intended for human consumption. Limits are given for impurities commonly present in the product. Depending on
the raw material and the manufacturing process other impurities may be present and, if so, this shall be notified to
the user and when necessary to relevant authorities.
NOTE Users of this product should check the national regulations in order to clarify whether it is of appropriate purity for
treatment of water intended for human consumption, taking into account raw water quality, required dosage, contents of other
impurities and additives used in the product not stated in this product standard.
Limits have been given for impurities and chemical parameters where these are likely to be present in significant
quantities from the current production process and raw materials. If the production process or raw materials leads
to significant quantities of impurities, by-products, or additives being present, this shall be notified to the user.
4.2 Composition of commercial product
The product shall contain not less than a mass fraction of 82,1 % of FeSO . 7H O (i.e. not less than a mass
4 2
fraction of 16 % of Fe) and shall be within ± 3 % of the manufacturer's declared values.
4.3 Impurities and main by-products
The product shall conform to the requirements specified in Table 1.
The concentration limits refer to Fe (ll).
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SIST EN 889:2005
EN 889:2004 (E)
Table 1 — Impurities
Limit
Mass fraction of Fe (ll) content
Impurity
in %
Grade 1 Grade 2 Grade 3
Manganese max. 0,5 1 2
Insoluble matters :
- wet crystal form (a) max. 0,6 0,6 0,6
- free flowing form (b) max. 3 3 3
NOTE An excess of insoluble matters indicates the presence of
foreign matter. Iron as a component of the product will usually be
removed in the treatment process.
4.4 Chemical parameters
The product shall conform to the requirements specified in Table 2.
The concentration limits are specified in milligrams per kilogram of Fe (II).
Table 2 — Chemical parameters
Limit in
Parameter mg/kg of Fe (II)
type 1 type 2 type 3
Arsenic (As) max. 1 20 50
Cadmium (Cd) max. 1 25 50
Chromium (Cr) max. 100 350 500
Mercury (Hg) max. 0,1 5 10
Nickel (Ni) max. 300 350 500
Lead (Pb) max. 10 100 400
Antimony (Sb) max. 10 20 60
Selenium (Se) max. 1 20 60
-
NOTE Cyanide (CN),pesticides and polycyclic aromatic
hydrocarbons are not relevant since the raw materials used in the
manufacturing process are free of them. For maximum impact of iron (ll)
sulfate on trace metal content in drinking water see A.2.
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EN 889:2004 (E)
5 Test methods
5.1 Sampling
Observe the general recommendations of ISO 3165 and take into account ISO 6206. Prepare the laboratory
sample required by the relevant procedure described in ISO 8213.
5.2 Analyses
5.2.1 Main product
Iron (II) sulfate is determined as Fe (II) content in the test sample by titrimetry with potassium dichromate solution
(see B.1).
5.2.2 Impurities
5.2.2.1 Manganese
The manganese content shall be determined by flame atomic absorption spectrometry (FAAS) (see B.2).
5.2.2.2 Insoluble matters
The percentage mass fraction of the insoluble matters shall be determined in accordance with the method
described in B.3.
5.2.3 Chemical parameters
5.2.3.1 General
The contents of chemical parameters shall be determined by atomic absorption spectrometry (AAS).
5.2.3.2 Preparation of sample solution
5.2.3.2.1 General
Oxidation and wet digestion is used to bring the samples into a stable solution.
5.2.3.2.2 Principle
)
Oxidation with hydrogen peroxide (H O followed by digestion with hydrochloric acid (HCl).
2 2
5.2.3.2.3 Reagents
All reagents shall be of a recognized analytical grade and the water used shall conform to the grade 3 specified in
EN ISO 3696.
5.2.3.2.3.1 Hydrochloric acid (HCl), solution, mass fraction 30 %.
5.2.3.2.3.2 Hydrogen peroxide (H O ), solution, mass fraction 30 %.
2 2
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5.2.3.2.4 Apparatus
Ordinary laboratory apparatus and glassware together with the following
5.2.3.2.4.1 Analytical balance.
5.2.3.2.4.2 Graduated cylinder, capacity 50 ml.
5.2.3.2.4.3 Round flask with reflux condenser.
5.2.3.2.4.4 Hot plate.
5.2.3.2.4.5 Volumetric flask, capacity 200 ml.
5.2.3.2.5 Procedure
Dissolve with 20 ml of water 20,0 g of the iron salt. Add to iron (II)-samples 30 ml hydrogen peroxide solution
(5.2.3.2.3.2). After adding 50 ml hydrochloric acid (5.2.3.2.3.1) boil the solution for 15 min by using a reflux
condenser (5.2.3.2.4.3). Cool down the solution, transfer to a 200 ml volumetric flask (5.2.3.2.4.5) and fill up to the
mark with water. This is the sample solution.
5.2.3.3 Arsenic
The arsenic content shall be determined by hydride generation atomic absorption spectrometry (see B.4).
5.2.3.4 Cadmium
The cadmium content shall be determined by graphite furnace atomic absorption spectrometry (see B.6).
5.2.3.5 Chromium
The chromium content shall be determined by graphite furnace atomic absorption spectrometry (see B.6).
5.2.3.6 Mercury
The mercury content shall be determined by cold vapour atomic absorption spectrometry (see B.5).
5.2.3.7 Nickel
The nickel content shall be determined by graphite furnace atomic absorption spectrometry (see B.6).
5.2.3.8 Lead
The lead content shall be determined by graphite furnace atomic absorption spectrometry (see B.6).
5.2.3.9 Antimony
The antimony content shall be determined by hydride generation atomic absorption spectrometry (see B.4).
5.2.3.10 Selenium
The selenium content shall be determined by hydride generation atomic absorption spectrometry (see B.4).
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EN 889:2004 (E)
6 Labelling - Transportation - Storage
6.1 Means of delivery
In order that the purity of the product is not affected, the means of delivery shall not have been used previously for
any different product or it shall have been specially cleaned and prepared before use.
4)
6.2 Risk and safety labelling according to the EU Directives
Iron (II) sulfate is not subject to labelling regulations.
NOTE Annex I of the Directive 67/548/EEC on Classification, packaging and labelling of dangerous substances and its
amendments and adaptations in the European Union contains a list of substances classified by the EU. Substances not in this
Annex I should be classified on the basis of their intrinsic properties according to the criteria in the Directive by the person
responsible for the marketing of the substance.
6.3 Transportation regulations and labelling
5)
Iron (II) sulfate is not listed under a UN number .
Iron (II) sulfate is not classified as a dangerous product for road, rail, sea and air transportation.
6.4 Marking
The marking shall include the following information:
the name "iron (II) sulfate", trade name, commercial form, grade and type;
the net mass;
the name and the address of the supplier and/or manufacturer;
the statement "this product conforms to EN 889".
6.5 Storage
6.5.1 Long term stability
Commercial form a) : Depending upon conditions of storage discolouration can occur due to oxidation to the
ferric form. Storage time shall therefore be as short as possible. Normally it is made up into solution and used
promptly;
commercial form b) : Unlimited stability when it is stored at temperature not over 40 °C in a dry place.
6.5.2 Storage incompatibilities
Iron (II) sulfate heptahydrate and its solutions have an acid character similar to diluted solutions of sulfuric acid
and are therefore corrosive to most common metals, also to concrete. Contact with these materials has to be
avoided. Keep away from alkaline or oxidation agents. Avoid contact with agents capable of liberating chlorine.
4)
See [2].
5)
United Nations Number.
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SIST EN 889:2005
EN 889:2004 (E)
Annex A
(informative)
General information on iron (ll) sulfate
A.1 Origin
A.1.1 Raw materials
The product is manufactured from:
iron-titanium ore and sulfuric acid;
steel and sulfuric acid (pickle liquor).
A.1.2 Manufacturing process
Iron (ll) sulfate is produced by: Crystallization of oversaturated solutions of iron (II) sulfate heptahydrate in sulfuric
acid by cooling and separation of the crystals by centrifuges or filters.
For the commercial form b) : Additional removal of the moisture by drying.
A.2 Quality of commercial product
The three types of iron (II) sulfate specified in Table 2 reflect the quality of commercially available products.
Figures A.1 to A.3 show the maximum concentrations of trace metals that would be added to the raw water by the
addition of products corresponding to the purity levels specified in Table 2. It can be seen that the concentrations of
metal added are well below the Parametric Values given in the EU Directive 98/83/EC (see [1]) at typical product
doses. Furthermore, the figures overstate the concentrations of metals that would be present in the treated water
since a substantial proportion of the trace metals will be incorporated in the sludge. Users of this product should
select an appropriate grade and type to enable them to achieve treated water quality targets taking into account
raw water characteristics, required dosage, process plant conditions and other relevant factors.
12
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SIST EN 889:2005
EN 889:2004 (E)
Element
Drinking water limit ug/l
As
10
Cd
5
Cr
50
Hg
1
Ni
20
Pb
10
Sb
5
Se
10
Key
1 Maximum addition to water µg/l metal
2 Product dosage mg/l Fe - Typical dose
Figure A.1 — Maximum impact of iron (II) sulfate, type 1, on trace metal content of water
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EN 889:2004 (E)
Element
Drinking water limit ug/l
As
10
Cd
5
Cr
50
Hg
1
Ni
20
Pb
10
Sb
5
Se
10
Key
1 Maximum addition to water µg/l metal
2 Product dosage mg/l Fe - Typical dose
Figure A.2 — Maximum impact of iron (II) sulfate, type 2, on trace metal content of water
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SIST EN 889:2005
EN 889:2004 (E)
Element
Drinking water limit ug/l
As
10
Cd
5
Cr
50
Hg
1
Ni
20
Pb
10
Sb
5
Se
10
Key
1 Maximum addition to water µg/l metal
2 Product dosage mg/l Fe - Typical dose
Figure A.3 — Maximum impact of iron (II) sulfate, type 3, on trace metal content of water
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EN 889:2004 (E)
A.3 Use
A.3.1 Function
The product is used as primary coagulant.
A.3.2 Form in which it is used
The product is used saturated or highly concentrated, not lower than a mass fraction of 20 %. Over-diluted
solutions can hydrolyse and form a precipitate.
A.3.3 Treatment dose
3
The treatment dose is variable depending on raw water quality and corresponds to approximately 20 g/m to
3 3 3
50 g/m (corresponding to a treatment dose between 4 g/m and 10 g/m expressed as Fe).
A.3.4 Means of application
In order to use iron (II) sulfate heptahydrate as a coagulant, a previous or simultaneous oxidation to iron (III) state
should be necessary. The highly concentrated solution is normally dosed by acid-resistant metering pumps. To
promote a rapid dispersion a high turbulence at the point of addition is desirable.
A.3.5 Secondary effects
Increase of the sulfate content and chloride concentration if chlorine is used for oxidation. Reduction of alkalinity
and pH value.
A.3.6 Removal of excess product
The coagulation process includes the hydrolysis of the ferric ions to ferric hydroxide. This precipitate is removed by
sedimentation, flotation and/or filtration.
A.4 General rules relating to safety
A.4.1 Rules for safe handling and use
The supplier will provide current safety instructions.
A.4.2 Emergency procedures
A.4.2.1 First aid
In case of contact with skin, the affected area should be washed with water.
In case of contact with eyes, they should be immediately rinsed with water for at least 10 min, medical advice
should be sought.
If swallowed, provided patient is conscious, the mouth should be washed out with water and 5 % (m/m) sodium
bicarbonate solution followed by a demulcent such as milk should be given. Medical advice should be sought.
A.4.2.2 Spillage
As much solid product as possible should be removed. Then it should be rinsed with water.
A.4.2.3 Fire
Product is not combustible.
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EN 889:2004 (E)
Annex B
(normative)
Analytical methods
B.1 Determination of iron (II) : Fe (II)
B.1.1 General
This method applies to product with iron contents greater than a mass fraction of 0,2 %.
B.1.2 Principle
Iron is directly titrated with potassium dichromate solution.
B.1.3 Reagents
All reagents shall be of a recognized analytical grade and the water used shall conform to the grade 3 in
accordance with EN ISO 3696.
B.1.3.1 Sulfuric acid, H SO concentrated, density ρ = 1,84 g/ml.
2 4
B.1.3.2 Phosphoric acid, H PO concentrated, density ρ = 1,71 g/ml.
3 4
B.1.3.3 Barium diphenylamine sulfonate solution, c(Ba(C H -NH-C H SO ) ) = 8 mmol/l.
6 5 6 4 3 2
B.1.3.4 Potassium dichromate solution, c(K Cr O ) = 0,0166 mol/l.
2 2 7
B.1.4 Apparatus
Ordinary laboratory apparatus and glassware.
B.1.5 Procedure
B.1.5.1 Test solution
In a 500 ml conical flask, pour 200 ml of water, add 10 ml of sulfuric acid (B.1.3.1) and 10 ml of phosphoric acid
(B.1.3.2). Cool with water. Weigh to the nearest 0,1 mg, between 3 g and 10 g of the laboratory sample and
transfer to the conical flask containing the acid solution.
B.1.5.2 Determination
Titrate the test solution with potassium dichromate (B.1.3.4) with a volumetric burette and add five drops of barium
diphenylamine sulfonate (B.1.3.3) near the end-point.
End-point is achieved when a persistent purple colour appears, record the volume (V) of potassium dichromate
required for the complete titration.
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B.1.5.3 Expression of results
The iron (II) content, C expressed as mass fraction, is given by the following equation:
(II)
V ×0,558
C = (1)
(II)
m
where
V is the volume, in millilitres, of potassium dichromate required for the titration;
m is the mass, in grams, of the sample used for the test solution.
B.2 Determination of manganese
B.2.1 General
This method is applicable to iron salt with manganese content greater than a mass fraction of 0,05 %.
B.2.2 Principle
Iron salt is diluted in water. Manganese is determined in this diluted solution by direct injection of the solution into
the flame of an atomic absorption spectrometer. Manganese is converted to the atomic state by thermal
dissociation. The absorption of the atoms is measured in the light path of the FAAS at a wavelength specific to the
element. The concentrations are calculated by means of a calibration curve.
B.2.3 Reagents
All reagents shall be of a recognized analytical grade, water shall conform to the grade 3 in accordance with
EN ISO 3696 and ultra pure grade acid shall be used.
B.2.3.1 Hydrochloric acid (HCl), solution, mass fraction 30 %.
B.2.3.2 Manganese, standard stock solution, c (Mn) = 1 g/l.
0
B.2.3.3 Manganese, intermediate standard solution, c (Mn) = 100 mg/l : Pipette 10 ml of standard stock
1
solution (B.2.3.2) into a 100 ml volumetric flask (B.2.4.1), add 3 ml of hydrochloric acid (B.2.3.1) and dilute to the
mark with water .
B.2.3.4 Manganese, standard solution, c (Mn) = 0,5 mg/l : Pipette 0,5 ml of intermediate standard solution
2
(B.2.3.3) into a 100 ml volumetric flask (B.2.4.1) and dilute to the mark with water .
B.2.3.5 Manganese, standard solution, c (Mn) = 1 mg/l : Pipette 1 ml of intermediate standard solution
3
(B.2.3.3) into a 100 ml volumetric flask (B.2.4.1) and dilute to the mark with water .
B.2.3.6 Manganese, standard solution, c (Mn) = 2 mg/l : Pipette 2 ml of intermediate standard solution
4
(B.2.3.3) into a 100 ml volumetric flask (B.2.4.1) and dilute to the mark with water .
B.2.3.7 Manganese, standard solution, c (Mn) = 3 mg/l : Pipette 3 ml of intermediate standard solution
5
(B.2.3.3) into a 100 ml volumetric flask (B.2.4.1) and dilute to the mark with water .
B.2.3.8 Blank solution: Pipette 3 ml of hydrochloric acid (B.2.3.1) into a 200 ml volumetric flask (B.2.4.1) and
dilute to the mark with water.
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B.2.4 Apparatus
Ordinary laboratory apparatus and glassware together with the following.
B.2.4.1 Volumetric flasks, capacity 100 ml and 200 ml.
B.2.4.2 Analytical balance, having an accuracy of ± 0,1 mg.
B.2.4.3 Flame atomic absorption spectrometer.
B.2.4.4 Electrode-less discharge or hollow cathode lamp for the determination of manganese.
B.2.5 Procedure
B.2.5.1 Sample solution
Weigh, to the nearest 0,1 mg, 20 g of the laboratory sample, transfer into a 200 ml volumetric flask (B.2.4.1) and
dilute to the mark with water.
B.2.5.2 Spectrometer settings
The operating parameters of the flame atomic absorption spectrometer are adjusted in accordance with the
operating manual issued by the manufacturer.
The spectrometer is operated at the wavelength specific for manganese: 279,5 nm. The flame composition is the
following: Air: 13,5 l/min - Acetylene: 2,0 l/min.
B.2.5.3 Determination
B.2.5.3.1 Test solution
Pipette 5 ml of the sample solution (B.2.5.1) into a 100 ml volumetric flask (B.2.4.1), add 3 ml of hydrochloric acid
(B.2.3.1) and dilute to the mark with water.
B.2.5.3.2 Measurement
Inject the test solution (B.2.5.3.1) directly into the flame by aspiration through the nebuliser, setting the
spectrometer as described in B.2.5.2. Repeat the injection three times, record the absorbance and calculate the
mean.
B.2.5.4 Calibration function
To provide the calibration function, measure the absorbance of the four standard solutions (B.2.3.7, B.2.3.6,
B.2.3.5 and B.2.3.4) and the absorbance of the blank solution (B.2.3.8) respectively in the same way as the sample
solutions (see B.2.5.3.2). Calculate calibration function with the absorbance means, expressed in absorbance unit,
of each solutions on vertical axis and the concentrations, expressed in milligrams per litre, on the horizontal axis.
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SIST EN 889:2005
EN 889:2004 (E)
B.2.5.5 Expression of results
The manganese concentration (C ) in the test solution is calculated with the calibration function (B.2.5.4).
Mn
The manganese concentration of the iron salts (C ) expressed in milligrams per kilogram of iron product is
s
calculated as following:
C ×100× 200
Mn
C = =C × 4000 /m (2)
s Mn
5×m
where
C is the manganese concentration in the test solution in milligrams per litre.
Mn
m is the mass , in grams, of the sample used for the test solution.
B.3 Determination of insoluble matters
B.3.1 General
This method is applicable to the determination of insoluble matters in iron based coagulants. The measuring range
of insoluble matters is between a mass fraction of 0,002 % and 10 %.
...
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