EN ISO 6326-5:1997

Natural gas - Determination of sulfur compounds - Part 5: Lingener combustion method (ISO 6326-5:1989)

Specifies a method for the determination of total sulphur in natural gas. It is applicable to gases with sulphur contents between 0,5 mg/m3 and 1 000 mg/m3. With a total sulphur content of more than 0,1 mg sulphur in the absorption solution, visual titration with an indicator can be chosen, whereas for lower contents turbidimetric titration is preferable.

Erdgas - Bestimmung von Schwefelverbindungen - Teil 5: Verbrennung nach dem Lingener-Verfahren (ISO 6326-5:1989)

Dieser Teil von ISO 6326 legt ein Verfahren für die Bestimmung des Gesamtschwefelgehaltes in Erdgas fest. Das Verfahren ist anwendbar auf Gase mit Schwefelgehalten zwischen 0,5 mg/m3 und 1000 mg/m3. Bei einem Gesamtschwefelgehalt von mehr als 0,1 mg in der Absorptionslösung kann die visuelle Titration mit einem Indikator gewählt werden, während bei niedrigeren Gehalten die Trübungstitration vorzuziehen ist.

Gaz naturel - Détermination des composés soufrés - Partie 5: Méthode de combustion Lingener (ISO 6326-5:1989)

La présente partie de l'ISO 6326 prescrit une méthode pour la détermination de la teneur totale en soufre du gaz naturel. Cette méthode est applicable aux gaz dont la teneur totale en soufre est comprise entre 0,5 mg/m3 et 1 000 mg/m3. Le titrage visuel avec indicateur peut être choisi lorsque la teneur totale en soufre est supérieure à 0,1 mg dans la solution absorbante, le titrage turbidimétrique étant préférable pour les teneurs inférieures. --
NOTE Dans toutes les parties de l'ISO 6326, 1 m3 de gaz est exprimé pour les conditions normales (0 °C; 101,325 kPa).

Zemeljski plin - Določevanje žveplovih spojin - 5. del: Metoda sežiga po Lingenerju (ISO 6326-5:1989)

General Information

• Status: Withdrawn
• Publication Date: 16-Dec-1997
• Withdrawal Date: 11-Feb-2020
• ICS: 75.060 - Natural gas
• Technical Committee: CEN/TC 238 - Test gases, test pressures and categories of appliances
• Drafting Committee: CEN/SS N21 - Gaseous fuels and combustible gas
• Current Stage: 9960 - Withdrawal effective - Withdrawal
• Completion Date: 12-Feb-2020
• Ref Project: SIST EN ISO 6326-5:2000 - Natural gas - Determination of sulfur compounds - Part 5: Lingener combustion method (ISO 6326-5:1989)

Standards Content (Sample)

SLOVENSKI STANDARD
01-december-2000
=HPHOMVNLSOLQ'RORþHYDQMHåYHSORYLKVSRMLQGHO0HWRGDVHåLJDSR/LQJHQHUMX
,62
Natural gas - Determination of sulfur compounds - Part 5: Lingener combustion method
(ISO 6326-5:1989)
Erdgas - Bestimmung von Schwefelverbindungen - Teil 5: Verbrennung nach dem
Lingener-Verfahren (ISO 6326-5:1989)
Gaz naturel - Détermination des composés soufrés - Partie 5: Méthode de combustion
Lingener (ISO 6326-5:1989)
Ta slovenski standard je istoveten z: EN ISO 6326-5:1997
ICS:
75.060 Zemeljski plin Natural gas
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

ISO
INTERNATIONAL
6326-5
STANDARD
First edition
1989-07-01
Determination of Sulfur
Natura1 gas -
compounds -
Part 5 :
Lingener combustion method
Determination des composh soufr& -
Gaz naturel -
Partie 5 : MMode de combustion Lingener
Reference number
ISO 6326-5 : 1989 (El
ISO 6326-5 : 1989 (El
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. 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. ISO
collaborates closely with the International Electrotechnical Commission (1 EC) on all
matters of electrotechnical standardization.
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 6326-5 was prepared by Technical Committee ISO/TC 158,
Analysis of gases.
Na tural gas -
ISO 6326 consists of the following Parts, under the general title
Determination of Sulfur compounds :
-
Part 7 : General in troduction
- Part 2: Gas chromatographic method using electrochemical detector for the
an
determina tion o f odoriferous Sulfur compounds
-
Part 3: Determination of hydrogen sulfide, mercaptan Sulfur and carbonyl
sulfide Sulfur by po ten tiometry
-
Part 4: Determination of individual Sulfur compounds chroma tograph y
bY WS
with a flame pho tometric detector
Part 5: Lingener combustion method
Annex A of this part of ISO 6326 is for information only.
0 ISO 1989
All rights reserved. No part of this publication may be reproduced or utilized in any form or by any
means, electronie or mechanical, including photocopying and microfilm, without Permission in
writing from the publisher.
International Organization for Standardization
Case postale 56 l CH-121 1 Geneve 20 l Switzerland
Printed in Switzerland
ii
ISO 6326-5 : 1989 (El
Introduction
The standardization of several methods for the determination of Sulfur compounds in
natura1 gas is necessary in view of the diversity of these compounds [hydrogen sulfide,
carbonyl sulfide, thiols (mercaptans), tetrahydrothiophene (THT), etc.] and the pur-
poses of the determinations (required accuracy, measurement at the drilling head or in
the transmission pipes, etc. ).
In Order to enable the user to choose the method most appropriate to his needs and to
perform the measurements under the best conditions, ISO 6326 has been prepared in
several Parts.
ISO 6326-1 gives a rapid comparison of standardized
methods and therefore provides
information for the choice of the method.
The other Parts of ISO 6326, including this Part, describe in detail the various stan-
dardized methods.
The determination of total Sulfur is specified in ISO 4260 : 1987, Petroleum products
and hydrocarbons - Determination of Sulfur content - Wickbold combustion
me thod.
. . .
Ill
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ISO 6326-5: 1989 (E)
INTERNATIONAL STANDARD
Determination of Sulfur compounds -
Natura1 gas -
Part 5 :
Lingener combustion method
1 Scope 3 Principle
This part of ISO 6326 specifies a method for the determination A measured volume sf gas is burnt with air at atmospheric
of total Sulfur in natura1 gas. The method is applicable to gases
pressure in a glass combustion apparatus. The resulting Sulfur
with Sulfur contents between 0,5 mg/m3 and ‘l 000 mg/m3. oxides are converted into sulfuric acid by absorption in
With a total Sulfur content of more than 0,l mg Sulfur in the
hydrogen peroxide solution. Depending on the Sulfur content
absorption Solution, visual titration with an indicator tan be of the test gas, the sulfate ions in the absorption Solution are
Chosen, whereas for lower contents turbidimetric titration is
determined using either visual titration with an indicator or tur-
preferable. bidimetric titration.
NOTE - In all Parts of ISO 6326, 1 m3 of gas is expressed at normal
conditions (0 OC; 101,325 kPa).
4 Reagents and materials
2 Normative rederences
During the analysis, use only reagents of recognized analytical
grade and only distilled water or water sf equivalent purity.
The following Standards contain provisions which, through
reference in this text, constitute provisions of this part of
4% Hydrogen Peroxide, IO % (rnlrn) aqueous Solution,
ISO 6326. At the time of publication, the editions indicated
Sulfur-free, as absorbing liquid for the Sulfur oxides.
were valid. All Standards are subject to revision, and Parties to
agreements based on this part of ISO 6326 are encouraged to
investigate the possibility of applying the most recent editions
4.2 Activated carbsn, for adsorption of Sulfur impurities
of the Standards listed below. Members of IEC and ISO main-
from the combustion air.
tain registers of currently valid International Standards.
4.3 Absorbing liquid :
ISO 385-1 : 1984, Laborstory glassware - 5urettes - Part 7 : 30 % Onl~n) aqueous Solution of
General requiremen ts. potassium hydroxide, for the purification of the combustion air.
ISO 648 : 1977, Laborstory glassware - he-mark pipettes.
One-mark 5 Apparatus
ISO 1042 : 1983, Laboratory glassware -
volume tric flasks.
The schematic layout of the apparatus is shown in figure 1.
ISO 3585 : 1976, Glass plant, Pipeline and fittings - Properties
Ordinary laboratory apparatus and
of borosilicate glass 3.3.
ISO 6326-5 : 1989 (El
Air
Combustion device
Pressure-equalizing vessel
Capillary flow meter
U-tube manometer
Dry gas meter with thermometer
Condensate separator
Vacuum pump
-
Figure 1 Schematic layout of the apparatus
5.3 Capillary flow meter (C), measuring range 10 I/min to
5.1 Combustion device (AI
30 I/min.
The combustion device is manufactured of borosilicate glass
complying with ISO 3535. lt consists of the Parts shown in
5.4 U-tube manometer (D), arm length 500 mm.
figure 2,
5.5 Dry gas meter (E)
5.1.1 Receiver with cooling jacket (see figure 3).
The range of the meter shall be appropriate for the quantity of
5.1.2 Flame tube (see figure 4)
Sample to be burned and the meter shall have been recently
calibrated. The gas meter shall be equipped with a thermometer
The outer diameter of the flame tube is determined by the in-
for the measurement of the gas temperature. The thermometer
side diameter of the receiver with cooling jacket and the annular
shall have a measuring range of 0 OC to at least 30 OC. The
gap shown in figure 2.
scale intervals shall be not less than 0,5 OC.
5.1.3 Burner (see figure 5)
NOTE - The gas meter should be flushed with the gas to be analysed
before the combustion, in particular when analysing gases with dif-
ferent Sulfur contents, to avoid disturbance by adsorption and desorp-
For the combustion of natura1 gases a universal burner with a
tion phenomena.
needle valve is often preferable.
5.1.4 Intermediate piece (see figure 6) 5.6 Condensate separator (FL
The thermometer shall have a measuring range of 0 OC to at
5.7 Vacuum pump (GI
least 100 OC. The scale interval shall be not less than 1 OC.
The suction capacity of the vacuum pump shall be at least
51.5 Reitmeyer attachment (see figure 7).
25 I/min. lt is recommended that a drying tower with a drying
agent be included between the condensate separator (F) and
the vacuum pump (G) to protect the oil in the vacuum pump.
5.2 Pressure-equaliming vessel (BL
ISO 6326-5 : 1989 (E)
Dimensions in millimetres
Tube8x l-
Tube 10 x l-
I
II
I
II
I
I
I
I
Il
I
I
I
II
I
I
II
I
I
Il
ll
l
Ir
1’
3,2’o,z
I’
I
I
I
I
Annular gap
h /--- Centred flame-tube
l
ek
I
l
I
I
/
I
11 I 11
Ii
1 JI *
Figure 2 - Combustion vessel
ISO 6326-5 : 1989 (E)
Dimensions in millimetres
Dimensions in millimetres
Spherical joint-cup 29/ 15-,
Conical joint-socket 60/46~
\
Conical joint-
socket socket 45/40 45/40
Hose connectionY
L Conical Conical joint- joint-
cone cone 60146 60146
Tube Tube 40 40 x x 1,6 1,6
iTube54x 1,8
/
/
C
s
Tube 75 x 2,2
r,
/
\Tube44x 1,6
f’
r Eight holes @ 2+ir5
/
- uniformly distributed
over the periphery
LOne-way cock
Figure 4 - Flame tube
Figure 3 - Receiver with cooling jacket

ISO 6326-5 : 1989 (El
Dimensions in millimetres
Three apertures
Spherical joint-cup-\ k-4
f-----q 9,5 k 0,5
Gas jet apertu
@ 0,l + 0,05
Dimensions in millimetres
. Tube4Oxl ,6-\
79n-Y
Thermometer
iV--
Extension
displaced
rearward
joint-socket 14/23
by 90° --
Spherical joint-cup-
Spherical joint-cup
/
Conical joint-cone
45/40
Spherical joint-ball-’
/
l-
Tube 1Ox
Figure 6 - Intermediate piece
Figure 5 - Burner
Dimensions in millimetres
Bent rearward through 90°
i-
Conical joint-
socket 14/23
A
-0
+
-8
Spherical joint-ball 29/15i
Figure 7 - Reitmeyer attachment
ISO 6326-5 : 1989 (El
7 Analytical determination
6 Procedure
With a total Sulfur content of more than 0,l mg Sulfur in the ab-
61 . Preparation for combustion
sorption Solution, visual titration with an indicator tan be
Chosen, whereas for lower contents turbidimetric titration is
Draw air, which if necessary should be cleaned of Sulfur im-
preferable.
purities with activated carbon (4.2) and/or absorbing liquid
(4.31, through the combustion apparatus with the aid of the
vacuum pump (GI, with a required volumetric flow about
7.1 Determination of Sulfur content by visual
20 I/min. Remove the burner (5.1.3) and pour sufficient
titration
hydrogen peroxide Solution (4.1) into the receiver (5.1.1) to rise
around the flame tube (5.1.2) to the height of the burner tip
7.1.1 Reagents
throughout the period of combustion. After connection of the
cooling water, the combustion apparatus is ready for use.
During the analysis, use only reagents of recognized analytical
grade and only distilled water or water of equivalent purity.
6.2 Combustion
7.1.1.1 ZPropanol (Isopropyl alcohol).
With a preliminary pressure of about 2 kPa on the U-tube
manometer (D), ignite the gas at the removed burner. Carefully
introduce the burner, with the flame directed downwards, into
7.1 .l.2 Barium perchlorate, Standard volumetric Solution.
the flame tube and note the reading on the gas meter (EI. The
air flow and cooling water flow may have to be adjusted. The
Dissolve 1,7 g of barium perchlorate [Ba(C10,)21 in 200 ml of
temperature and pressure of the gas shall be read during the
water in the 1 000 ml one-mark volumetric flask (7.1.2.11, make
combustion period. The exhaust gas temperature on the ther-
up to the mark with the 2-propanol (7.1.1 .l) and adjust to
mometer shall be kept between 50 OC and 70 OC. As soon as
pH 3,5 with perchloric acid. Standardize the Solution
the required quantity of gas, up to 500 litres depending on
against a Standard reference Solution of sulfuric acid,
Sulfur content (sec clause 7) has been burnt, shut off first the
c(H+O~) = 0,005 mol/l.
gas supply and then the vacuum pump. Drain the absorbing
Solution into a beaker (7.1.2.5 or 7.2.2.61, rinse the receiver
1 ml of this Standard volumetric Solution is equivalent to
with water and note the reading on the gas meter (E).
approximately 0,16 mg sf S.
6.3 Determination of gas volume
7.1.1.3 Thorinl), 0,2 % (mlm) aqueous indicator solution.
ifference in readings
The volume of gas burnt, shown by the d
Store in a silica glass or polyethylene bottle.
3n the gas meter, shall be reduced to nor mal conditions :
7.1.1.4 Methylene blue, 0,Ol % (mlm) aqueous indicator
v _ v *n hnb + Pe)
Solution.
n-
Pn T
Store in a silica glass or polyethylene bottle.
where
7.1.2 Apparatus
V is the volume of the gas Sample measured in accordance
with 6.2 at temperature T (kelvins) and pressure Pamp + pe
Ordinary laboratory apparatus and
(kilopascals);
Tn is the thermodynamic temperature, in kelvins, at nor-
7.1.2.1 One-mark volumetric flask, of capacity 1 000 ml,
mal ambient conditions (273,15 K);
complying with ISO 1042.
T is the thermodynamic tempera ture, in kelvins, of the gas
7.1.2.2 One-mark pipette, of capacity 20 ml, complying
Sample;
with ISO 648.
is the pressure, in kilopascals, at normal conditions
Pn
7.1.2.3 Conical flask, wide neck, of capacity 250 ml.
(101,325 kPa);
in kilopascals, measured
is the atmospheric pressure,
Pamb
7.1.2.4 Burette, of capacity 25 ml, graduated in 0,05 ml,
during gas sampling;
complying with ISO 385-1, or an automatic titrator.
in ki measured with
is the excess pressure, lopascals,
Pe
7.1.2.5 Beaker, of capacity 250 ml.
the water manom eter during sampling.
WS
1) Thorin is the registered trade name for disodium-4-[(2-arsonophenyl)-azol
...