ISO 5073:1985

Brown coals and lignites — Determination of humic acids

Charbons bruns et lignites — Dosage des acides humiques

Rjavi premogi in ligniti - Določevanje huminskih kislin

General Information

• Status: Withdrawn
• Publication Date: 10-Jul-1985
• Withdrawal Date: 10-Jul-1985
• ICS: 73.040 - Coals
• Technical Committee: ISO/TC 27 - Coal and coke
• Drafting Committee: ISO/TC 27 - Coal and coke
• Current Stage: 9599 - Withdrawal of International Standard
• Completion Date: 16-Dec-1999
• Ref Project: SIST ISO 5073:1998 - Brown coals and lignites -- Determination of humic acids

Relations

• Revised: ISO 5073:1999 - Brown coals and lignites — Determination of humic acids
• Effective Date: 15-Apr-2008

Standards Content (Sample)

International Standard
INTERNATIONAL ORGANIZATION FOR STANDARDIZATION.ME)I(C(YHAPOfiHAR OPTAHM3AL&lR fl0 CTAH~APTM3AL(MM~RGANISATION INTERNATIONALE DE NORMALISATION
Determination of humic acids
Brown coals and lignites -
Charbons bruns et lignites - Dosage des acides humiques
First edition - 1985-07-15
Ref l No. ISO 50734985 (E)
UDC 662.642 : 543.8 : 547.992.2
Descriptors : Chemical analysis, determination of content, humic acids.
minerals and ores, solid fuels, coal, lignite,
Price based on 3 pages

---------------------- Page: 1 ----------------------
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of
national Standards bodies (ISO member bedies). The work of preparing International
Standards is normally carried out through ISO technical committees. Esch 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, govern-
mental and non-governmental, in liaison with ISO, also take part in the work.
Draft International Standards adopted by the technical committees are circulated to
the member bodies for approval before their acceptance as International Standards by
the ISO Council. They are approved in accordance with ISO procedures requiring at
least 75 % approval by the member bodies voting.
International Standard ISO 5073 was prepared by Technical Committee ISO/TC 27,
Solid mineral fuels.
0 International Organkation for Standardkation, 1985
Printed in Switzerland

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ISO 50734985 (E)
INTERNATIONAL STANDARD
Determination of humic acids
Brown coals and lignites -
3.2 free humic acids: Humic acids obtained by a Single
1 Scope and field of application
Stage extraction of coal with a 1 % (mlm) sodium hydroxide
This International Standard specifies methods for the deter- Solution followed by precipitation with mineral acid.
mination of
3.3 total humic acid: Sum of the free humic acids and
a) total humic acids content, i.e. humic acids which are
humic acids bonded as salts (humates) extracted by an alkaline
bonded with the mineral matter of coai as humates, and free
sodium pyrophosphate Solution followed by extraction with a
hu mit acids ;
1 % (mlm) sodium hydroxide Solution and precipitation with
mineral acid.
b) free humic acids.
The humic acid content of brown coals and lignites varies with
4 Determination of total humic acids
the type of coal and petrographic composition.
4.1 Principle
This International Standard applies to the scientific
characterization of brown coal and lignites, and to their utili-
Action of an alkaline Solution of sodium pyrophosphate at am-
zation, for example for briquetting and agriculture.
bient temperature on an analytical Sample of coal from which
bitumens have been removed; Single Stage extraction of the
Sample with a hot sodium hydroxide Solution, precipitation of
2 References
humic acids with an excess of mineral acid, and weighing of the
precipitate.
ISO 975, Brown coals and lignites - Determination of the yield
of toluene soluble extract. 1 )
NOTE - For the purpose of this International Standard, “biturnen” is
synonymous with “toluene soluble extract” as determined in ISO 975.
ISO 1015, Brown coals and lignites - Determination of
moisture con tent - Direct volumetric method.
4.2 Reagents
ISO 1171, Solid mineral fuels - Determination of ash.
During the analysis, use only reagents of recognized analytical
grade and only distilled water or water of equivalent purity.
ISO 5068, Brown coals and lignites - Determination of
moisture con ten t - lndirect gravimetric method.
4.2.1 Toluene, e20 = 0,867 g/ml, boiling range 110 to
ISO !3069/2, Brown coals and lignites - Principles of sampling
111 OC. (At least 95 % should distil within this range.)
- Part 2: Sample preparation for determination of moisture
con ten t and for general analysis.
WARNING - Toluene is flammable and toxic by inhala-
tion, ingestion or skin absorption.
3 Definitions
4.2.2 Sodium hydroxide, 1 % (mlm) Solution.
For the purpose of this International Standard, the following
Dissolve 10 g of NaOH in water and make up to 1 000 ml.
definitions apply.
4.2.3 Alkaline sodium pyrophosphate, Solution.
3.1 humic acids: A group of amorphous condensed
polycarboxylic acids of high relative molecular mass which oc-
Dissolve 44,6 g of crystalline sodium pyrophosphate
cur as free humic acids and as salts (humates) of Calcium,
decahydrate (Na4P207m10H20) and 4 g of sodium hydroxide in
magnesium, iron, etc.
100 ml water.
1) At present at the Stage of draft. (Revision of ISO 9754975.)

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ISO 50734985 (EI
4.2.4 Hydrochlorit acid, 5 % ( V/ v). NOTE - The extraction of humic acids should be complete within 7 h.
4.52 Filter the contents of flask B into a 1 litre volumetric
4.3 Apparatus
flask and make up to the mark. Pipette 100 ml of the filtrate into
a beaker and add 60 ml of hydrochloric acid (4.2.4) to
Ordinary laboratory apparatus, and
precipitate the humic acids. Centrifuge the Suspension. Decant
the Solution. Wash the residue with water. Repeat the washing
4.3.1 Extraction apparatus, for bitumens Separation (sec
Operation until peptization of the humic acids begins, which is
ISO 975).
indicated by the formation of a gel or colloid. Add 5 ml of
hydrochloric acid (4.2.4) to the colloidal Solution to precipitate
the humic acids once again.
4.3.2 Drying oven, capable of being maintained at
90 $I 5 OC, or an infra-rd drying lamp.
Separate the resulting precipitate from the liquid by filtration
through an ashless filter Paper, previously dried to constant
4.3. 3 Centrifuge, capable of a minimum rate of rotation of
mass in the drying oven (4.3.2) at 90 k 5 OC. Transfer the filter
210 rad/s, with centrifuge tubes of at least 100 ml capacity.
Paper to a weighing bottle which has been heated to constant
mass in the drying oven (4.3.2) at 90 -t 5 OC. Dry the bottle
NOTE
- The RCF of the centrifuge should be sufficient to ensure
and precipitate at a temperature of 90 + 5 OC for 1 h. Remove
Separation of all precipitates or colloids from the corresponding sol-
the bottle from the oven, cool in
...

SLOVENSKI STANDARD
SIST ISO 5073:1998
01-februar-1998
5MDYLSUHPRJLLQOLJQLWL'RORþHYDQMHKXPLQVNLKNLVOLQ
Brown coals and lignites -- Determination of humic acids
Charbons bruns et lignites -- Dosage des acides humiques
Ta slovenski standard je istoveten z: ISO 5073:1985
ICS:
73.040 Premogi Coals
SIST ISO 5073:1998 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST ISO 5073:1998

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SIST ISO 5073:1998
International Standard
INTERNATIONAL ORGANIZATION FOR STANDARDIZATION.ME)I(C(YHAPOfiHAR OPTAHM3AL&lR fl0 CTAH~APTM3AL(MM~RGANISATION INTERNATIONALE DE NORMALISATION
Determination of humic acids
Brown coals and lignites -
Charbons bruns et lignites - Dosage des acides humiques
First edition - 1985-07-15
Ref l No. ISO 50734985 (E)
UDC 662.642 : 543.8 : 547.992.2
Descriptors : Chemical analysis, determination of content, humic acids.
minerals and ores, solid fuels, coal, lignite,
Price based on 3 pages

---------------------- Page: 3 ----------------------

SIST ISO 5073:1998
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of
national Standards bodies (ISO member bedies). The work of preparing International
Standards is normally carried out through ISO technical committees. Esch 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, govern-
mental and non-governmental, in liaison with ISO, also take part in the work.
Draft International Standards adopted by the technical committees are circulated to
the member bodies for approval before their acceptance as International Standards by
the ISO Council. They are approved in accordance with ISO procedures requiring at
least 75 % approval by the member bodies voting.
International Standard ISO 5073 was prepared by Technical Committee ISO/TC 27,
Solid mineral fuels.
0 International Organkation for Standardkation, 1985
Printed in Switzerland

---------------------- Page: 4 ----------------------

SIST ISO 5073:1998
ISO 50734985 (E)
INTERNATIONAL STANDARD
Determination of humic acids
Brown coals and lignites -
3.2 free humic acids: Humic acids obtained by a Single
1 Scope and field of application
Stage extraction of coal with a 1 % (mlm) sodium hydroxide
This International Standard specifies methods for the deter- Solution followed by precipitation with mineral acid.
mination of
3.3 total humic acid: Sum of the free humic acids and
a) total humic acids content, i.e. humic acids which are
humic acids bonded as salts (humates) extracted by an alkaline
bonded with the mineral matter of coai as humates, and free
sodium pyrophosphate Solution followed by extraction with a
hu mit acids ;
1 % (mlm) sodium hydroxide Solution and precipitation with
mineral acid.
b) free humic acids.
The humic acid content of brown coals and lignites varies with
4 Determination of total humic acids
the type of coal and petrographic composition.
4.1 Principle
This International Standard applies to the scientific
characterization of brown coal and lignites, and to their utili-
Action of an alkaline Solution of sodium pyrophosphate at am-
zation, for example for briquetting and agriculture.
bient temperature on an analytical Sample of coal from which
bitumens have been removed; Single Stage extraction of the
Sample with a hot sodium hydroxide Solution, precipitation of
2 References
humic acids with an excess of mineral acid, and weighing of the
precipitate.
ISO 975, Brown coals and lignites - Determination of the yield
of toluene soluble extract. 1 )
NOTE - For the purpose of this International Standard, “biturnen” is
synonymous with “toluene soluble extract” as determined in ISO 975.
ISO 1015, Brown coals and lignites - Determination of
moisture con tent - Direct volumetric method.
4.2 Reagents
ISO 1171, Solid mineral fuels - Determination of ash.
During the analysis, use only reagents of recognized analytical
grade and only distilled water or water of equivalent purity.
ISO 5068, Brown coals and lignites - Determination of
moisture con ten t - lndirect gravimetric method.
4.2.1 Toluene, e20 = 0,867 g/ml, boiling range 110 to
ISO !3069/2, Brown coals and lignites - Principles of sampling
111 OC. (At least 95 % should distil within this range.)
- Part 2: Sample preparation for determination of moisture
con ten t and for general analysis.
WARNING - Toluene is flammable and toxic by inhala-
tion, ingestion or skin absorption.
3 Definitions
4.2.2 Sodium hydroxide, 1 % (mlm) Solution.
For the purpose of this International Standard, the following
Dissolve 10 g of NaOH in water and make up to 1 000 ml.
definitions apply.
4.2.3 Alkaline sodium pyrophosphate, Solution.
3.1 humic acids: A group of amorphous condensed
polycarboxylic acids of high relative molecular mass which oc-
Dissolve 44,6 g of crystalline sodium pyrophosphate
cur as free humic acids and as salts (humates) of Calcium,
decahydrate (Na4P207m10H20) and 4 g of sodium hydroxide in
magnesium, iron, etc.
100 ml water.
1) At present at the Stage of draft. (Revision of ISO 9754975.)

---------------------- Page: 5 ----------------------

SIST ISO 5073:1998
ISO 50734985 (EI
4.2.4 Hydrochlorit acid, 5 % ( V/ v). NOTE - The extraction of humic acids should be complete within 7 h.
4.52 Filter the contents of flask B into a 1 litre volumetric
4.3 Apparatus
flask and make up to the mark. Pipette 100 ml of the filtrate into
a beaker and add 60 ml of hydrochloric acid (4.2.4) to
Ordinary laboratory apparatus, and
precipitate the humic acids. Centrifuge the Suspension. Decant
the Solution. Wash the residue with water. Repeat the washing
4.3.1 Extraction apparatus, for bitumens Separation (sec
Operation until peptization of the humic acids begins, which is
ISO 975).
indicated by the formation of a gel or colloid. Add 5 ml of
hydrochloric acid (4.2.4) to the colloidal Solution to precipitate
the humic acids once again.
4.3.2 Drying oven, capable of being maintained at
90 $I 5 OC, or an infra-rd drying lamp.
Separate the resulting precipitate from the liquid by filtration
through an ashless filter Paper, previously dried to constant
4.3. 3 Centrifuge, capable of a minimum rate of rotation of
mass in the drying oven (4.3.2) at
...

Nom
e internationale @ -5c 73
INTERNATIONAL ORGAN kLISATION
ION FOR STANDARDIZATlON*ME)K4YHAPOflHAR OPrAHM3AUMR Il0 CTAHflAPTM3AUMM.ORGANlSATlON INTERNATIONALE DE NO
bruns et lignites - Dosage des acides humi ues
-
es - Determination of humic acids
Brown coals and li!
Première éditil 1985-07-1 5
3.8 : 547.992.2 Réf. no : IS0 5073
1985 (FI
I
f Descripteurs : minér combustible solide, charbon, lignite, analyse chimique, dosage, acide humique.
Prix basé

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Avant-propos
L‘ISO (Organisation internationale de normalisation) est une fédération mondiale
d’organismes nationaux de normalisation (comités membres de I’ISO), L‘élaboration
des Normes internationales est confiée aux eomités techniques de I‘ISO. Chaque
comité membre intéressé par une étude a le droit de faire partie du comité technique
créé à cet effet. Les organisations internationales, gouvernementales et non gouverne-
mentales, en liaison avec I’ISO, participent également aux travaux.
Les projets de Normes internationales adoptés par les comités techniques sont soumis
aux comités membres pour approbation, avant leur acceptation comme Normes inter-
nationales par le Conseil de I’ISO. Les Normes internationales sont approuvées confor-
mément aux procédures de I‘ISO qui requièrent l’approbation de 75 % au moins des
comités membres votants.
La Norme internationale IS0 5073 a été élaborée par le comité technique ISO/TC 27,
Combustibles minéraux solides.
O Organisation internationale de normalisation, 1985
Imprimé en Suisse

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1 Objet et do aine d’application 3.2 acides humiques libres: Acides humiques
extraction unique du charbon avec une solution
La présente spécifie des méthodes de de sodium à 1 % (rnlm), suivie de leur précipita
détermination sence d’un acide minéral.
s, et des acides humiques libres;
d’un acide minéral.
humiques
4.1 Principe
culture.
2 Références
d’acide minéral, et pesée du précipité.
IS0 1015, bruns et lignites - Détermination de
NOTE - Dans le cadre de la présente Norme international
directe.
((bitume)) est synonyme d’«extrait soluble dans le toluèn
défini dans VISO 975.
minéraux solides - Détermination des
cendres.
4.2 Réactifs
IS0 5068, Charbons bruns et lignites - Détermination de
Au cours de l’analyse, utiliser uniquement des réa
l’humidité - Métho e gravimétrique indirecte.
lité analytique reconnue, et de l‘eau distillée ou
pureté équivalente.
IS0 506912, Charbo 6 bruns et lignites - Échantillonnage -
Partie 2: Préparation es échantillons pour la détermination de
I‘humidité et pour l’a alyse générale. 4.2.1 Toluène, ez0 = 0,867 glml, intervalle de
109 à 111 OC (au moins 95 YO du volume doit dist
intervalle).
3 Définitions
AVERTISSEMENT - Le toluène est un produi
Dans le cadre de la ésente Norme internationale, les défini-
ble et toxique par inhalation, ingestion et
cutanée.
tions suivantes sont pplicables.
I
pe d‘acides polycarboxyliques 4.2.2 Hydroxyde de sodium, solution à 1 % (ml
se moléculaire relative élevée,
acides humiques libres et sous Dissoudre 10 g d’hydroxyde de sodium dans de l’eau
um, de magnésium, de fer, etc. 1 O00 ml.
t. (Révision de I’ISO 975-1975.)

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IS0 5073-1985 (FI
chaque lavage et recueillir les liquides de lavage dans la fiole
4.2.3 Pyrophosphate de sodium, solution alcaline.
conique B. Remettre le résidu de charbon ainsi lavé dans la fiole
A. Ajouter 100 ml de la solution d'hydroxyde de sodium (4.2.2)
Dissoudre 44,6 g de pyrophosphate de sodium décahydraté
(Na4P2O7,10H201 et 4 g d'hydroxyde de sodium dans 100 ml et chauffer durant 2 h sur le bain d'eau bouillante (4.3.5). Lais-
ser refroidir, centrifuger le contenu de la fiole A jusqu'à tempé-
d'eau.
rature ambiante, puis centrifuger durant 15 min à 210 rad/s
(voir 4.3.3). Décanter la solution dans la fiole B. Laver deux fois
4.2.4 Acide chlorhydrique, solution à 5 % (if/ il.
le résidu non dissous avec 100 ml de la solution d'hydroxyde de
sodium (4.2.2). Centrifuger après chaque lavage et recueillir les
4.3 Appareillage
liquides de lavage dans la fiole B.
Matériel courant de laboratoire, et
NOTE - L'extraction devrait être complète en 7 h.
4.5.2 Filtrer le contenu de la fiole 6, recueillir le filtrat dans
Appareillage d'extraction, pour la séparation des
4.3.1
une fiole jaugée de 1 O00 ml et compléter jusqu'au trait. Pipet-
bitumes (voir IS0 9751.
ter 100 ml de filtrat dans un bécher et ajouter 60 ml de la solu-
tion d'acide chlorhydrique (4.2.41 pour précipiter les acides
4.3.2 Étuve, pouvant être maintenue à une température de
la suspension. Décanter la solution.
humiques. Centrifuger
90 f 5 OC, ou lampe à infrarouge.
Laver le résidu avec de l'eau. Répéter le lavage jusqu'à ce que la
peptisation des acides humiques commence, laquelle est signa-
lée par la formation d'un gel ou d'un colloïde. Ajouter 5 ml de la
4.3.3 Centrifugeuse, dont la vitesse angulaire minimale est
solution d'acide chlorhydrique (4.2.4) à la solution colloïdale
de 210 rad/s, avec éprouvettes d'au moins 100 ml de capa-
pour reprécipiter les acides humiques.
cité.
Séparer du liquide le précipité ainsi obtenu en le filtrant sur un
NOTE - La vitesse angulaire de la centrifugeuse doit être assez élevée
pour permettre de séparer tous précipités ou colloïdes de la solution papier filtre sans cendres préalablement séché jusqu'à masse
correspondante.
à 90 k 5 OC. Transférer le
constante dans l'étuve (4.3.21 réglée
papier filtre dans un vase à peser préalablement chauffé jusqu'à
masse constante dans l'étuve (4.3.2) réglée à 90 f 5 OC.
4.3.4 Agitateur mécanique.
Sécher le vase et le précipité à une température de 90 f 5 OC
durant 1 h. Retirer le vase de l'étuve, laisser refroidir d'abord
4.3.5 Bain d'eau bouillante.
durant 5 min à l'air, puis dans un dessiccateur contenant un
agent déshydratant app
...