‫ﻫﻴﺌﺔ ﺍﻟﺘﻘﻴﻴﺱ ﻟﺩﻭل ﻤﺠﻠﺱ ﺍﻟﺘﻌﺎﻭﻥ ﻟﺩﻭل ﺍﻟﺨﻠﻴﺞ ﺍﻟﻌﺭﺒﻴﺔ‬

STANDARDIZATION ORGANIZATION FOR G.C.C (GSO)

GSO ISO 760:1988

ISO 760 :1978

– ‫ﺍﻟﺘﺒﻎ ﻭﻤﻨﺘﺠﺎﺘﻪ‬
(‫ﺘﻘﺩﻴﺭ ﻤﺤﺘﻭﻯ ﺍﻟﻤﺎﺀ )ﻁﺭﻴﻘﺔ ﻜﺎﺭل ﻓﻴﺸﺭ‬
TOBACCO AND TOBACCO PRODUCTS -
DETERMINATION OF WATER CONTENT -
KARL FISCHER METHOD

ICS:65.160
 TOBACCO AND TOBACCO PRODUCTS -
DETERMINATION OF WATER CONTENT -
KARL FISCHER METHOD

Date of GSO Board of Directors Approval : 1409(H)-04-17 (1988-11-26)

Issuing Status : Technical Regulation
GSO STANDARD GSO ISO 760:1988

INTRODUCTION

The STANDARDIZATION ORGANIZATION FOR G.C.C (GSO)has adopted the

international standard No. 760/78 “Determination of Water Content - Karl Fischer Method”
issued by the International Organization for Standardization (ISO).
The text of this international standard has been translated into Arabic language without any
technical modifications with view to its approval as a Gulf standard.

1
GSO STANDARD GSO ISO 760:1988

TOBACCO AND TOBACCO PRODUCTS -

DETERMINATION OF WATER CONTENT -
KARL FISCHER METHOD

1- SCOPE AND FIELD OF APPLICATION

This Gulf standard specifies a general method known as the Karl Fischer method
suitable for the determination of free water or water of crystallization in most
solid or liquid chemical products, both organic and inorganic.

Two methods of titration, depending on whether the end point is detected visually
or electrometrically, are specified. The visual method can be used when no
electrometric apparatus is available but is applicable only to colourless solutions;
it is always a direct titration. The electrometric method, on the other hand, may
involve either a direct titration or a back-titration. The electrometric method,
whether by direct titration or back-titration, is the more accurate, and for this
reason it is recommended.

2- PRINCIPLE
Reaction of any water present in a test portion with a solution of iodine and
sulphur dioxide in a pyridine/methanol mixture (Karl Fischer Reagent),
previously standardized by titration with an exactly known mass of water (items
6.1, 7.1 and 8.1).
NOTE: Methanol may be replaced by 2-methoxyethanol (ethylene glycol monomethyl ether). With
this solvent, a more constant titration volume is obtained and the reagent can be used with
aldehydes and ketones, without using any special technique.

3- REACTIONS
H2O + I2 + SO2 + 3C5H5N 2C5H5N.HI + C5H5N.SO3

C5H5N.SO3 + ROH C5H5NH.OSO2OR

4- REAGENTS AND MATERIALS

During the analysis, use only reagents of recognized analytical grade and only
distilled water or water of equivalent purity.

4.1 Methanol, not containing more than 0.05% (m/m) of water. If the reagent
contains more than this quantity of water, dry it by distillation from magnesium
turnings activated with iodine. Collect the distillate in a receiver protected from
atmospheric moisture by means of a guard tube filled with the desiccant (item
4.9).

4.2 2-Methoxyethanol (Ethylene glycol monomethyl ether), not containing more than
0.05% (m/m) of water. If the reagent contains more than this quantity of water,
dry it by distillation, rejecting the first portion of distillate, which contains the
water.

2
GSO STANDARD GSO ISO 760:1988

4.3 Pyridine, not containing more than 0.05% (m/m) of water. If the reagent contains
more than this quantity of water, dry it by distillation, rejecting the first portion of
distillate, which contains the water.

4.4 Sample solvent: either a mixture containing 4 parts by volume of the methanol
(item 4.1) and 1 part by volume of the pyridine (item 4.3), or (preferably for
determinations with compounds containing carbonyl groups) a mixture containing
4 parts by volume of the 2-methoxyethanol (item 4.2) and 1 part by volume of the
pyridine (item 4.3).

4.5 Karl Fischer Reagent

Place 670 ml of the methanol (item 4.1) or the 2-methoxyethanol (item 4.2) in a
dry brown glass flask, fitted with a ground glass stopper.

Add about 85 g of iodine. Stopper the flask and shake it occasionally until the
iodine is completely dissolved. Then add approximately 270 ml of the pyridine
(item 4.3), stopper the flask again and mix thoroughly. Using the method
described below, dissolve 65 g of sulphur dioxide in this solution, cooling to
ensure that the temperature of the liquid does not exceed 20oC.
NOTE: As the reaction is exothermic, it is necessary to cool the flask from the beginning and to
maintain it at about 0oC, for example by immersing it in an ice bath or in crushed solid carbon
dioxide.

Replace the ground glass stopper by an attachment for introducing sulphur

dioxide, consisting of a cork bearing a thermometer and a glass inlet tube 6
mm x 8 mm, reaching to within 10 mm of the bottom of the flask, and a small
capillary tube for connecting to the atmosphere.

Place the whole assembly with the ice bath on a balance and weigh to the nearest
1 g. Connect the inlet tube to a cylinder of sulphur dioxide by means of a flexible
connection and a drying tube filled with the desiccant (item 4.9) and gently open
the tap on the cylinder.

Adjust the rate of flow of sulphur dioxide so that all the gas is absorbed without
the liquid showing any sign of rising in the inlet tube.

Maintain the equilibrium of the balance by gradually increasing the tare, and
ensure that the temperature of the liquid does not rise above 20oC. Close the tap
on the cylinder as soon as the increase in mass reaches 65 g.

Immediately remove the flexible connection and reweigh the flask and its inlet
attachment. The mass of dissolved sulphur dioxide should be between 60 and 70
g. A slight excess is not harmful.

Stopper the flask, mix the solution and leave for at least 24 hours before using it.
In fact, as the result of imperfectly understood reactions which occur in the fresh
reagent, the water equivalent of the reagent decreases rapidly to begin with and
then much more slowly.

3
GSO STANDARD GSO ISO 760:1988

This water equivalent is between 3.5 and 4.5 mg/ml. It shall be determined daily
if methanol has been used, but may be determined less frequently if 2-
methoxyethanol has been used.

It is possible to prepare Karl Fischer reagent having a lower water content by

diluting the solution prepared as described above with the sample solvent (item
4.4).

Store the reagent in the dark and protected from atmospheric moisture. It should
preferably be stored in the reagent bottle (item 5.1.1.5).

4.6 Sodium tartrate dihydrate.

4.7 Water/methanol, standard solution corresponding to 10 g of water per litre.

Using a microburette or a pipette, place 1 ml of water in a perfectly dry 100 ml

one-mark volumetric flask containing approximately 50 ml of the methanol (item
4.1). Dilute to the mark with the methanol and mix. [For standardization of the
Karl Fischer reagent (item 4.5) with this solution, see annex A, clause A.1 or A.2,
depending on whether the visual method or the direct electrometric method is
used].

1 ml of this standard solution contains 10 mg of water.

4.8 Water/methanol, standard solution corresponding to 2 g of water per litre

Using a microburette or a pipette, place 1 ml of water in a perfectly dry 500 ml

one-mark volumetric flask containing approximately 100 ml of the methanol (item
4.1). Dilute to the mark with the same methanol and mix. (See the
correspondence by volume of this solution with the Karl Fischer reagent (item
8.2.2).

1 ml of this standard solution contains 2 mg of water.

4.9 Aluminium sodium silicate, anhydrous, in the form of granules of diameter 1.7
mm, for use as a desiccant. The granules may be regenerated by washing with
water and drying at 350oC for at least 48 hours.

Alternatively, activated silica gel may be used as a desiccant.

4.10 Silicone-base grease, for lubricating the ground glass joints.

5- APPARATUS
All the glassware used shall be previously dried for 30 minutes in an oven
controlled at approximately 130oC, then allowed to cool and stored in a desiccator
containing the desiccant (item 4.9).

5.1 For direct titration (by visual method or electrometric method)

5.1.1 A suitable form of apparatus for this method is given in annex B, should no
commercial apparatus be available. This standard apparatus comprises the parts
described below:

4
GSO STANDARD GSO ISO 760:1988

5.1.1.1 Automatic burette, of capacity 25 ml, with a fine point, graduated in 0.05 ml and
protected from atmospheric moisture by a guard tube filled with the desiccant
(item 4.9).

5.1.1.2 Titration vessel, of effective capacity 100 ml, connected to the tap of the
automatic burette (item 5.1.1.1) by a ground glass joint and having two sides
tubes, one permitting the introduction of platinum electrodes if the electrometric
method is used and the other fitted with a “Vaccine Cap”, to permit the
introduction of liquid test portions by means of syringe without opening the
vessel.

5.1.1.3 Platinum electrodes (see figures 1 and 2, annex B), fused to a glass tube enabling
them to be introduced into the bottom of the titration vessel (item 5.1.1.2) and
joined to two copper wires which in turn are connected to the device for the
electrometric detection of the end-point (item 5.1.1.7). (These are omitted in the
case of the visual method).

5.1.1.4 Electromagnetic stirrer, operating at a rotational frequency of 150 to 300/minute,

with a mild steel bar coated with glass or polytetrafluorethylene (PTFE), and fixed
on a base of adjustable height.

5.1.1.5 Reagent bottle for the Karl Fischer reagent, of capacity approximately 3 litres, of
brown glass, in which the filling tube of the automatic burette (item 5.1.1.1) is
immersed through the ground glass stopper.

5.1.1.6 Rubber bulb, connected to a Drechsel bottle filled with the desiccant (item 4.9),
for the admission of dry air under pressure into the reagent bottle (item 5.1.1.5) in
order to fill the automatic burette (item 5.1.1.1).

5.1.1.7 Device for the electrometric detection of the endpoint, shown diagrammatically in
figure 3, annex B. (This is omitted in the case of the visual method).

5.1.2 Medical syringes, of suitable capacity, the volume of which is calibrated.

5.1.3 Small glass tube, closed at one end and fitted at the other with a rubber stopper,
used for weighing and introducing into the titration vessel, for example, the mass
of sodium tartrate (item 4.6) (approximately 0.250 g) used to standardize the Karl
Fischer reagent (item 4.5), or possibly test portions of solid products.
5.2 For electrometric back-titration method

5.2.1 A suitable form of apparatus for this method is given in annex C, should no
commercial apparatus be available. This standard apparatus comprises the parts
described below.

5.2.1.1 Two automatic burettes, of capacity 25 ml, with fine points, connected directly to
their filling containers, one of brown glass for the Karl Fischer reagent (4.5) and
the other for the standard water/methanol solution (item 4.8).

5.2.1.2 Titration vessel, of effective capacity 100 ml, connected to the automatic burettes
(item 5.2.1.1) by means of ground glass joints and having two side tubes, one
permitting the introduction of platinum electrodes and the other fitted with a

5
GSO STANDARD GSO ISO 760:1988

“Vaccine Cap”, to permit the introduction of liquid test portions by means of a

syringe without opening the vessel.

5.2.1.3 Drying tube, connecting the filling containers of the burettes (item 5.2.1.1) and
the stopper of the titration vessel (item 5.2.1.2) by a closed circuit.

5.2.1.4 Platinum electrodes (see figures 4 and 5, annex C), fused to a glass tube enabling
them to be introduced into the bottom of the titration vessel (item 5.1.1.2) and
joined to two copper wires which in turn are connected to the device for the
electrometric detection of the endpoint (item 5.2.1.6).

5.2.1.5 Electromagnetic stirrer, operating at a rotational frequency of 150 to 300/minute,

with a mild steel bar coated with glass or polytetrafluorethylene (PTFE), and fixed
on a base of adjustable height.

5.2.1.6 Device for the electrometric detection of the endpoint, shown diagrammatically in
figure 3, annex B.

5.2.2 Medical syringes, of suitable capacity, the volume of which is calibrated.

5.2.3 Small glass tube, closed at one end and fitted at the other with a rubber stopper,
used for weighing and introducing into the titration vessel, for example, the mass
of sodium tartrate (item 4.6) (approximately 0.250 g) used to standardize the Karl
Fischer reagent (item 4.5), or possible test portions of solid products.

6- VISUAL TITRATION
6.1 Principle for the detection of the end-point

Development of colour in the test portion by addition of the first drop of excess
Karl Fischer reagent, coloured with iodine which gradually becomes colourless on
addition to the test portion containing the water to be determined.

6.2 Procedure

6.2.1 Standardization of the Karl Fischer reagent

6.2.1.1 Assemble the apparatus as shown in annex B, lubricating the joints with the
grease (item 4.10). Introduce by means of a syringe (item 5.1.2) 25 ml of the
methanol (item 4.1) into the titration vessel (item 5.1.1.2) through the “Vaccine
Cap”. Switch on the electromagnetic stirrer (item 5.1.1.4). In order to cause
reaction of the traces of water present in the methanol, add the Karl Fischer
reagent (item 4.5) from the automatic burette (item 5.1.1.1) until a brown colour is
obtained.

6.2.1.2 In the small glass tube (item 5.1.3), weigh to the nearest 0.0001 g, approximately
0.250 g of the sodium tartrate (item 4.6). Place this in the titration vessel very
quickly, removing the “Vaccine Cap” for a few seconds, then weigh the small
glass tube, so as to determine, by difference, the mass (m1) of the sodium tartrate
used.

6
GSO STANDARD GSO ISO 760:1988

Standardization may also be effected by introducing a mass (m2) of water of

approximately 0.040 g from a dropping bottle, weighed before and after
introduction into the titration vessel.

Titrate the know quantity of water introduced with the Karl Fischer reagent (item
4.5) to be standardized until the same brown colour as in (item 6.2.1.1) is
obtained, and note the volume (V1) of reagent used.

6.2.2 Determination

Empty the titration vessel (item 5.1.1.2) by means of its drain tap. Place in it 25
ml (or the volume specified in the procedure for the product to be analyzed) of the
methanol (item 4.1) or other solvent (item 4.3 or 4.4), using a syringe (item 5.1.2)
passing through the “Vaccine Cap”. Switch on the electromagnetic stirrer (item
5.1.1.4). In order to cause reaction of the traces of water present in the methanol,
add the Karl Fischer reagent (item 4.5) from the automatic burette (item 5.1.1.1)
until a brown colour is obtained.

Introduced the specified test portion by means of a syringe in the case of a liquid,
or weighed to the nearest 0.0001 g in the small glass tube (item 5.1.3) in the case
of a solid powder. Titrate with the Karl Fischer reagent until the same brown
colour is obtained.

Note the volume (V2) of Karl Fischer reagent used for the determination.
NOTE: It is advisable to use a test portion such that its water content corresponds to a volume of
Karl Fischer reagent that can be measured with sufficient accuracy. If necessary, increase in
proportion the quantities of solvent and test sample used and then use a titration vessel of suitable
capacity.

6.3 Expression of results

6.3.1 Water equivalent of the Karl Fischer reagent

The water equivalent T of the Karl Fischer reagent (item 4.5), expressed in
milligrams of water per milliliter of reagent is given by the formula:

m1 x 0156
. 6 m2
T = or T =
V1 V1

Where:
m1 is the mass, in milligrams, of the sodium tartrate (item 4.6) introduced if this
reagent is used for the standardization (item 6.2.1.2);
m2 is the mass, in milligrams, of water introduced if pure water is used for the
standardization (item 6.2.1.2);

7
GSO STANDARD GSO ISO 760:1988

V1 is the volume, in milliliters, of the Karl Fischer reagent (item 4.5) used for the
standardization;
0.156 6 is the factor for calculation of the water of the sodium tartrate dihydrate.
6.3.2 Water content of the sample
The water content of the sample, expressed as a percentage by mass, is given by
the formula:

V2 x T V2 x T
or
m o x 10 Vo x d x 10

Where:
mo is the mass, in grams, of the test portion (in the case of solid products);
Vo is the volume, in milliliters, of the test portion (in the case of liquid products);
d is the density of the sample, in grams per milliliter, at 20oC (in case of liquid
products);
V2 is the volume, in milliliters, of the Karl Fischer reagent (item 4.5) used for the
determination (item 6.2.2);
T is the water equivalent, in milligrams per milliliter, of the Karl Fischer reagent,
calculated in accordance with (item 6.3.1).

7- DIRECT ELECTROMETRIC TITRATION

7.1 Principle of the detection of the end-point
Immersion in the solution of two platinum electrodes subjected to a potential
difference: While water is present in the solution, the polarization of the cathode
opposes the passage of a current. Indication of the end-point of the titration by
the depolarization of the cathode accompanied by a sudden increase in current
(which is shown by a suitable electrical device).
7.2 Procedure
7.2.1 Standardization of the Karl Fischer reagent
7.2.1.1 Assemble the apparatus as shown in figure 1, annex B, lubricating the joints with
the grease (item 4.10). Introduce by means of a syringe (item 5.1.2) 25 ml of
the methanol (item 4.1) into the titration vessel (item 5.1.1.2) through the
“Vaccine Cap”. Switch on the electromagnetic stirrer (item 5.1.1.4) and close the
circuit of the device for the electrometric detection of the end-point (item 5.1.1.7).

8
GSO STANDARD GSO ISO 760:1988

Adjust the apparatus so that a potential difference of 1 to 2 V is applied to the

electrodes and the galvanometer shows a low current, usually a few
microamperes. In order to cause reaction of the traces of water present in the
methanol, add the Karl Fischer reagent (item 4.5) until the galvanometer shows a
sudden increase in current of about 10 to 20 µA, which remains stable for at least
1 minute.
7.2.1.2 In the small glass tube (item 5.1.3), weigh, to the nearest 0.001 g, approximately
0.250 g of the sodium tartrate (item 4.6). Place this in the titration vessel very
quickly, removing the “Vaccine Cap” for a few seconds; then weigh the small
glass tube, so as to determine, by difference, the mass (m3) of the sodium tartrate
used.
Standardization may also be effected by introducing a mass (m4) of water of
approximately 0.040 g from a dropping bottle, weighed before and after
introduction into the titration vessel.
Titrate the known quantity of water introduced with the Karl Fischer reagent (item
4.5) to be standardized, until the same deflection of the pointer of the
galvanometer is reached and remains stable for at least 1 minute. Note the
volume (V3) of reagent used.
7.2.2 Determination
Empty the titration vessel (item 5.2.1.2) by means of its drain tap. Place in it 25
ml (or the volume specified in the procedure for the product to be analysed) of the
methanol (item 4.1) or other solvent (item 4.3 or 4.4), using a syringe (item 5.1.2)
passing through the “Vaccine Cap”. Switch on the electromagnetic stirrer (item
5.1.1.4). In order to cause reaction of the traces of water present in the solvent
used, add the Karl Fischer reagent (item 4.5), proceeding as specified in (item
7.2.1) until there is sudden and constant deflection lasting for at least 1 minute.
Introduce the specified test portion by means of syringe in the case of a liquid, or
weighed to the nearest 0.0001 g in a small glass tube (item 5.1.3) in the case of a
solid powder. Titrate with the Karl Fischer reagent using the same electrometric
procedure for detecting the end-point of the reaction.
Note the volume (V4) of Karl Fischer reagent used for the determination.
NOTE: It is advisable to use a test portion such that its water content corresponds to a volume of
Karl Fischer reagent that can be measured with sufficient accuracy.

If necessary, increase in proportion the quantities of solvent and test sample used
and then use a titration vessel of suitable capacity.
7.3 Expression of results
7.3.1 Water equivalent of the Karl Fischer reagent
The water equivalent T of the Karl Fischer reagent (item 4.5), expressed in
milligrams of water per millilitre of reagent, is given by the formula:

9
GSO STANDARD GSO ISO 760:1988

m 3 x 01566
. m4
T = or T =
V3 V3

Where:
m3 is the mass, in milligrams, of the sodium tartrate (item 4.6) introduced if this
reagent is used for the standardization (item 7.2.1);
m4 is the mass, in milligrams, of water introduced if pure water is used for the
standardization;
V3 is the volume, in milliliters, of the Karl Fischer reagent (item 4.5) used for the
standardization;
0.156 6 is the factor for calculation of the water of the sodium tartrate dihydrate.
7.3.2 The water content of the sample, expressed as a percentage by mass, is given by
the formula:

V4 x T V4 x T
or
m o x 10 Vo x d x 10

Where:
mo is the mass, in grams, of the test portion (in the case of solid products);
Vo is the volume, in milliliters, of the test portion (in the case of liquid products);
d is the density of the sample, in grams per milliliter at 20oC (in the case of liquid
products);
V4 is the volume, in milliliters, of the Karl Fischer reagent (item 4.5) used for the
determination (item 7.2.2);
T is the water equivalent, in milligrams per milliliter, of the Karl Fischer reagent,
calculated in accordance with (item 7.3.1).

8- ELECTROMETRIC BACK-TITRATION
8.1 Principle for the detection of the end-point
Addition of an excess of Karl Fischer reagent which is then back-titrated with a
standard water/methanol solution. Subjection of the electrodes to a very slight
potential difference but sufficient to cause a large deflection of the galvanometer
pointer at the start of the back-titration. Indication of the end-point of the titration
by the polarization of the cathode accompanied by the sudden interruption of the
current (which is shown by a suitable electrical device).

10
GSO STANDARD GSO ISO 760:1988

8.2 Procedure
8.2.1 Standardization of the Karl Fischer reagent
8.2.1.1 Assemble the apparatus as shown in annex C, lubricating the joints with the
grease (item 4.10). Place in the titration vessel (item 5.2.1.2) sufficient Karl
Fischer reagent (item 4.5) from one of the automatic burettes (item 5.2.1.1) to
cover the electrodes (item 5.2.1.4). Switch on the electromagnetic stirrer (item
5.2.1.5) and close the circuit of the device for the electrometric detection of the
end-point (item 5.2.1.6). Allow the standard water/methanol solution (item 4.8)
to flow from the second automatic burette (item 5.2.1.1) until the pointed of the
galvanometer moves suddenly to zero.
8.2.1.2 In the small glass tube (item 5.2.3), weigh to the nearest 0.0001 g, approximately
0.250 g of the sodium tartrate (item 4.6). Place this in the titration vessel very
quickly, removing the “Vaccine Cap” for a few seconds, then weigh the small
glass tube, so as to determine, by difference, the mass (m5) of the sodium tartrate
used.
Standardization may also be effected by introducing a mass (m6) of water of
approximately 0.040 g from a dropping bottle, weighed before and after
introduction into the titration vessel.
Then add a known excess volume (V5) of the Karl Fischer reagent, stopping when
the solution becomes brown in colour. Wait for 30 seconds and back-titrate this
excess, using the standard water/methanol solution (item 4.8), until the pointer of
the galvanometer moves suddenly to zero. Note the volume (V6) of this solution
(item 4.8) used.
8.2.2 Correspondence between the Karl Fischer reagent and the standard
water/methanol solution
Partially empty the titration vessel (item 5.2.1.2), leaving the electrodes
submerged in the liquid neutralized as specified in (item 8.2.1).
Add 20 ml of the Karl Fischer reagent (item 4.5), measured in the first automatic
burette (item 5.2.1.1), and titrate with the standard water/methanol solution (item
4.8) contained in the second automatic burette, until the pointer of the
galvanometer moves suddenly to zero. Note the volume (V7) of this solution
(item 4.8) used.
8.2.3 Determination
Empty the titration vessel (item 5.2.1.2) by means of its drain tap. Place in it 25
ml (or the volume specified in the procedure for the product to be analysed) of the
methanol (item 4.1), using a syringe (item 5.2.2) passing through the “Vaccine
Cap”. Switch on the electromagnetic stirrer (item 5.1.1.5).

11
GSO STANDARD GSO ISO 760:1988

In order to cause reaction of the traces of water present in the methanol, add a
slight excess (approximately 2 ml) of the Karl Fischer (item 4.5) and then add the
standard water/methanol solution (item 4.8) until the pointer of the galvanometer
moves suddenly to zero.
Introduce the specified test portion by means of syringe in the case of a liquid or
weighed to the nearest 0.0001 g in a small glass tube (item 5.2.3) in the case of a
solid powder.
Add a known excess volume (V8) of the Karl Fischer reagent, stopping when the
solution becomes brown in colour. Wait for 30 seconds and back-titrate this
excess, using the standard water/methanol solution (item 4.8) until the pointer of
the galvanometer moves suddenly to zero.
Note the volume (V9) of this solution (item 4.8) used.
NOTE: It is advisable to use a test portion such that its water content corresponds to a volume of
Karl Fischer reagent that can be measured with sufficient accuracy. If necessary, increase in
proportion the quantities of methanol and test sample used and then use a titration vessel of
suitable capacity.

8.3 Expression of results

8.3.1 Water equivalent of the Karl Fischer reagent
The water equivalent T of the Karl Fischer reagent (item 4.5), expressed in
milligrams of water per milliliter of reagent, is given by the formula:

m5 x 0156
. 6 m6
T = or T =
20 20
V5 − ( V6 ) V5 − ( V6 x )
V7 V7

Where:
m5 is the mass, in milligrams, of the sodium tartrate (item 4.6) introduced if this
reagent is used for the standardization (item 8.2.1.2);
m6 is the mass, in milligrams, of water introduced if pure water is used for the
standardization (item 8.2.1.2);
V5 is the known excess volume, in milliliters, of the Karl Fischer reagent (item 4.5)
added in (item 8.2.1.2);
V6 is the volume, in milliliters, of the standard water/methanol solution (item 4.8)
used in (item 8.2.1.2) for the back-titration;
V7 is the volume, in milliliters, of the standard water/methanol solution (item 4.8)
used in (item 8.2.2) (correspondence with the Karl Fischer reagent);
0.156 6 is the factor for calculation of the water of the sodium tartrate dihydrate.

12
GSO STANDARD GSO ISO 760:1988

8.3.2 Water content of the sample

The water content of the sample, expressed as a percentage by mass, is given by
the formula:
20 T
[ V8 - ( V9 x )] x
V7 m o x 10

Or

20 T
[ V8 - ( V9 x )] x
V7 Vo x d x 10
Where:
mo is the mass, in grams, of the test portion (in the case of solid products);
Vo is the volume, in milliliters, of the test portion (in the case of liquid products);
d is the density of the sample, in grams per milliliter, at 20oC (in the case of liquid
products);
V7 is as defined in (item 8.3.1);
V8 is the known excess volume, in milliliters, of the Karl Fischer reagent (item 4.5)
added in (item 8.2.3);
V9 is the volume, in milliliters, of the standard water/methanol solution (item 4.8)
used in (item 8.2.3) for the back-titration;
T is the water equivalent, in milligrams per milliliter, of the Karl Fischer reagent,
calculated in accordance with (item 8.3.1).

9- TEST REPORT
The test report shall include the following particulars:
a) An identification of the sample;
b) The reference of the method used;
c) The results and the method of expression used;
d) Any unusual features noted during the determination;
e) Any operation not included in this Gulf standard or regarded as optional.

13
GSO STANDARD GSO ISO 760:1988

ANNEX A

STANDARDIZATION OF KARL FISCHER REAGENT

WITH STANDARD WATER/METHANOL SOLUTION

A.1 VISUAL METHOD

A.1.1 If the standard water/methanol solution (item 4.7) is used instead of the sodium
tartrate (item 4.6) to standardize the Karl Fischer reagent (item 4.5), sub-clause
(item 6.2.1.2) relating to visual titration is amended as follows:
Using a syringe (item 5.1.2), add 10.0 ml of the methanol (item 4.1) to the
titration vessel; titrate with the Karl Fischer reagent (item 4.5) until the same
brown colour as in (item 6.2.1.1) is obtained, and note the volume (V10) of reagent
used.
In the same way, add 10.0 ml of the standard water/methanol solution (item 4.7).
Titrate the known quantity of water thus introduced with Karl Fischer reagent
(item 4.5) to be standardized, until the same brown colour is obtained, and note
the volume (V11) of reagent used.
A.1.2 In addition, sub-clause (item 6.3.1) is amended as follows:
The water equivalent T of the Karl Fischer reagent (item 4.5), expressed in
milligrams of water per millilitre of reagent is given by the formula:

100
T =
V11 − V10

Where:
100 is the mass, in milligrams, of water contained in 10 ml of the standard
water/methanol solution (item 4.7).
V10 is the volume, in millilitres, of the Karl Fischer reagent (item 4.5) used for the
titration of the 10 ml of the methanol (item 4.1).
V11 is the volume, in millilitres, of the Karl Fischer reagent (item 4.5) used for the
titration of the 10 ml of the standard water/methanol solution (4.7).

A.2 ELECTROMETRIC METHOD – DIRECT TITRATION

A.2.1 If the standard water/methanol solution (item 4.7) is used instead of the sodium
tartrate (item 4.6) to standardize the Karl Fischer reagent (item 4.5), sub-clause
(item 7.2.1.2) relating to direct electrometric titration is amended as follows:

14
GSO STANDARD GSO ISO 760:1988

Using a syringe (item 5.1.2), add 10.0 ml of the methanol (item 4.1) to the
titration vessel; titrate with the Karl Fischer reagent (item 4.5) until the same
deflection of the pointer of the galvanometer is reached and remains stable for at
least 1 minute, and note the volume (V12) of reagent used.
In the same way, add 10.0 ml of the standard water/methanol solution (item 4.7).
Titrate the known quantity of water thus introduced with the Karl Fischer reagent
(item 4.5) to be standardized until the same deflection of the pointer of the
galvanometer is reached and remains stable for at least 1 minute. Note the
volume (V13) of reagent used.
A.2.2 In addition, sub-clause (item 7.3.1) is amended as follows:
The water equivalent T of the Karl Fischer reagent (item 4.5), expressed in
milligrams of water pe millilitre of reagent, is given by the formula:

100
T =
V13 − V12

Where:
100 is the mass, in milligrams, of water contained in 10 ml of the standard
water/methanol solution (item 4.7).
V12 is the volume, in millilitres, of the Karl Fischer reagent (item 4.5) used for the
titration of the 10 ml of the methanol (item 4.1).
V13 is the volume, in millilitres, of the Karl Fischer reagent (item 4.5) used for the
titration of the 10 ml of the standard water/methanol solution (4.7).

15
GSO STANDARD GSO ISO 760:1988

ANNEX B

TYPICAL APPARATUS FOR

VISUAL OR DIRECT ELECTROMETRIC TITRATION
(for visual titration, omit the electrodes and the associated electrical equipment).

16
GSO STANDARD GSO ISO 760:1988

17
GSO STANDARD GSO ISO 760:1988

ANNEX C
TYPICAL APPARATUS FOR ELECTROMETRIC BACK-TITRATION

18
GSO STANDARD GSO ISO 760:1988

19