SIST EN 24159:1997

Ferromanganese and ferrosilicomanganese - Determination of manganese content - Potentiometric method (ISO 4159:1978, ed. 1)

No scope available

Bestimmung des Mangangehaltes von Ferromangan und Ferrosilicomangan - Potentiometrisches Verfahren (ISO 4159:1978, Ausg.1)

Ferromanganese et ferro-silico-manganese - Dosage du manganese - Méthode potentiométrique (ISO 4159:1978, éd. 1)

Feromangan in ferosilikomangan - Določevanje mangana - Potenciometrična metoda (ISO 4159:1978)

General Information

• Status: Published
• Publication Date: 30-Nov-1997
• ICS: 77.100 - Ferroalloys
• Technical Committee: IFEK - Ferrous metals
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 01-Dec-1997
• Due Date: 01-Dec-1997
• Completion Date: 01-Dec-1997
• Mandate: M/BC/CEN/87/15 - ECISS - 2nd programme
• Ref Project: EN 24159:1989 - Ferromanganese and ferrosilicomanganese - Determination of manganese content - Potentiometric method (ISO 4159:1978, ed. 1)

Relations

• Corrected By: SIST EN 24159:1997/AC1:1997 - Ferromanganese and ferrosilicomanganese - Determination of manganese content - Potentiometric method (ISO 4159:1978, ed. 1)
• Effective Date: 22-Dec-2008

Overview

EN 24159:1989 (identical to ISO 4159:1978) specifies a potentiometric method for the determination of manganese content in ferromanganese and ferrosilicomanganese alloys. The procedure is designed for high‑manganese ferroalloys (typical manganese content 55–95 % m/m) and uses a controlled redox titration with potassium permanganate in a pyrophosphoric medium, with the endpoint detected potentiometrically.

Key topics and technical requirements

• Analytical principle: oxidative titration of manganese in a pyrophosphoric medium; potentiometric detection of the KMnO4 endpoint (sudden potential increase ≥ 100 mV).
• Sample preparation: precise test portion (small, highly weighed sample) is attacked/dissolved using a combination of hydrochloric, hydrofluoric and perchloric acids (procedures differ slightly for ferromanganese and ferrosilicomanganese).
• Reagents: analytical‑grade acids, potassium permanganate (recrystallized and standardized), sodium pyrophosphate (pyrophosphoric medium), and controlled dilutions of HCl for pH adjustment.
• Apparatus: volumetric glassware, reflux condenser, sintered‑glass filters, magnetic stirrer, pH meter, and potentiometer or equivalent electrometric setup (platinum and calomel electrodes).
• Procedure highlights:
  • Acid digestion with controlled heating until perchloric fumes/oxidation products form.
  • Dilution and pH adjustment to about 6.5–7 using diluted HCl.
  • Potentiometric titration with standardized KMnO4; a blank determination and parallel standardization of KMnO4 are required.
• Quality and reporting: recommended duplicate titration on a second aliquot; stated reproducibility for experienced operators: 95% confidence limits ≈ ±0.20 %.
• Safety note: special precautions with perchloric acid when heated (fuming) and with hydrofluoric acid.

Applications and users

• Practical for quality control and composition verification in ferroalloy production and processing.
• Used by:
  • Metallurgical and chemical analysis laboratories
  • Ferroalloy manufacturers and smelters
  • Materials testing and specification compliance teams
  • Purchasing/inspection departments verifying supplier alloy composition
• Common uses: batch release testing, incoming material inspection, process control, and certification of alloy chemistry.

Related standards and references

• ISO 3713 (sampling and preparation of ferroalloy samples) is referenced for sample preparation.
• EN 24159:1989 is the CEN adoption of ISO 4159:1978 - useful to cite both when documenting test methods.

Keywords: EN 24159:1989, ISO 4159:1978, ferromanganese, ferrosilicomanganese, manganese determination, potentiometric method, potassium permanganate, pyrophosphate, alloy quality control.

Standards Content (Sample)

SLOVENSKI STANDARD
01-december-1997
)HURPDQJDQLQIHURVLOLNRPDQJDQ'RORþHYDQMHPDQJDQD3RWHQFLRPHWULþQD
PHWRGD,62
Ferromanganese and ferrosilicomanganese - Determination of manganese content -
Potentiometric method (ISO 4159:1978, ed. 1)
Bestimmung des Mangangehaltes von Ferromangan und Ferrosilicomangan -
Potentiometrisches Verfahren (ISO 4159:1978, Ausg.1)
Ferromanganese et ferro-silico-manganese - Dosage du manganese - Méthode
potentiométrique (ISO 4159:1978, éd. 1)
Ta slovenski standard je istoveten z: EN 24159:1989
ICS:
77.100 Železove zlitine Ferroalloys
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

INTERNATIONAL STANDARD
INTERNATIONAL ORGANIZATION FOR STANDARDIZATIONWE~YHAPO~HAR OPrAHM3ALWlR I-IO CTAH~APTM3Al@lbWORGANISATION INTERNATIONALE DE NORMALISATION
Ferromanganese and ferrosilicomanganese - Determination
of manganese content - Potentiometric method
Ferro-manganese et ferro-silico-manganke - Dosage du manganese - JWthode potentiom&rique
First edition - 1978-12-15
iii
-
UDC 669.15-198 : 543.257.1 : 546.711 Ref. No. ISO 4159-1978 (E)
Descriptors : ferroalloys, ferromanganese, Chemical analysis, determination of content, manganese, potentiometric analysis.
Price based on 3 pages
0 (the International Organization for Standardization) is a worldwide federation
of national Standards institutes (ISO member bodies). The work of developing
International Standards is carried out through ISO technical committees. Every
member body interested in a subject for which a technical committee has been set
up has the right to be represented on that committee. International organizations,
gowernmental and non-governmental, in liaison with ISO, also take part in the work.
International Standard EO 4159 was developed by Technical Committee
!SO/TC 132, FerroaDoys, and was circulated to the member bodies in October 1977.
p ‘11
‘@ has been approved by the member bodies of the fokMng countries :
Austral ia Iran South Africa, Rep. sf
Austria
I taly Spain
Bulgaria Japan Sweden
Canada Korea, Rep. of Turkey
Cnechoslovakia Mexico klnited Kingdom
France Norway U.S.A.
Germany, F. R. Philippines U.S.S.R.
Romania
India Yugoslavia
2 member body of the following country expr disapproval of the document
rechnical grounds :
Poland
63 International Organkation for Standardkation, 1978 l
Printed in Switzerland
INTERNATIONAL STANDARD ISO4159=1978(E)
Ferromanganese and ferrosilicomanganese - Determination
of manganese content - Potentiometric method
1 SCOPE AND FIELD OF APPLICATION 4.5 Hydrochlorit acid, p 1,19 g/ml, diluted 1 i- 4.
This International Standard specifies a potentiometric
method for the determination of the manganese content of
4.6 Sodium pyrophosphate, saturated Solution.
ferromanganese and ferrosilicomanganese.
Dissolve 145 g of sodium pyrophosphate (P207Na4.10H20)
The method is applicable to alloys containing from 55
in a 2 litre conical flask, with about 1 litre of hot water;
to 95 % (mlm) of manganese.
heat without exceeding, even locally, the temperature
of 60 OC, until the salt is completely dissolved. Cool.
2 REFERENCE
Prepare this Solution at the time of use.
ISO 37 13, Ferroalloys - Sampling and preparation of
samples - General wies. 1)
4.7 Potassium permanganate, recrystal I ized.
Place 50 g of pure analytical grade potassium permanganate
3 PRINCIPLE
in the conical flask (5.1), and dissolve it in 200 ml of warm
distilled water (70 to 80 “CL
Dissolution of a test Portion with hydrochloric, hydro-
f luoric and perchloric acids.
Fit the reflux condenser (5.2) to the flask and boil the
Potentiometric determination (see note) of manganese with Solution for 20 min. Filter the warm Solution quickly under
vacuum through a sintered glass funnel (5.3).
potassium permanganate in a pyrophosphoric medium at a
controlled pH, according to the reaction :
Cool the filtrate in iced water, stirring vigorously, and
allow the fine, crystalline precipitate to settle for 10 min.
4 Mn2+ -l- MnO,- + 8 H+ + 15 (P207H2)2-
Decant the Solution; then, using a glass spatula, transfer the
-+ 5 Mn(P20,H2),3- + 4 H,O
crystalline mass into a funnel with a filter plate, porosity 4,
NOTE - The method may be completed by any other electrometric
and place under suction for a few minutes to remove most
method : amperometric titration, dead-stop, etc.
of the mother liquor.
Dissolve the crystalline mass in 160 ml of distilled water
4 REAGENTS
(deionized water is not permitted for this Phase), and
repeat the recrystallization.
During the analysis, use only reagents of recognized ana-
lytical grade, and only distilled water or water of equivalent
After filtering and placing under suction for approximately
purity, except where otherwise specified.
5 min, transfer the crystalline mass onto a 150 mm dia-
meter watch glass using a glass spatula, and dry it in air,
4.1 Perchlorit acid2), p 1,61 g/ml.
protected from light and dust. When the crystalline mass no
longer agglomerates when crushed with the spatula, dry it
4.2 Hydrofluoric acid, p 1 ,14 g/ml. at 110 “C for 2 h, then transfer it to a weighing bottle
fitted with a ground glass stopper.
4.3 Hydrochlorit acid, p 1 ,19 g/ml.
Store in the dark.
This salt contains 34,76 % (mlm) of Mn.
4.4 H
...