EN ISO 3405:2000

SLOVENSKI STANDARD
01-julij-2000
1DIWQLSURL]YRGL'RORþHYDQMHGHVWLODFLMVNLK]QDþLOQRVWLSULWODþQLDWPRVIHUL,62

Petroleum products - Determination of distillation characteristics at atmospheric pressure
(ISO 3405:2000)
Mineralölerzeugnisse - Bestimmung des Destillationsverlaufes bei Atmosphärendruck
(ISO 3405:2000)
Produits pétroliers - Détermination des caractéristiques de distillation a pression
atmosphérique (ISO 3405:2000)
Ta slovenski standard je istoveten z: EN ISO 3405:2000
ICS:
75.080 Naftni proizvodi na splošno Petroleum products in
general
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EUROPEAN STANDARD
EN ISO 3405
NORME EUROPÉENNE
EUROPÄISCHE NORM
March 2000
ICS 75.080
English version
Petroleum products - Determination of distillation characteristics
at atmospheric pressure (ISO 3405:2000)
Produits pétroliers - Détermination des caractéristiques de Mineralölerzeugnisse - Bestimmung des
distillation à pression atmosphérique (ISO 3405:2000) Destillationsverlaufes bei Atmosphärendruck (ISO
3405:2000)
This European Standard was approved by CEN on 1 March 2000.
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 Management Centre 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 Management Centre has the same status as the official
versions.
CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,
Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, 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
© 2000 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 3405:2000 E
worldwide for CEN national Members.

Page 2
Foreword
Corrected 2001-05-09
The text of the International Standard ISO 3405:2000 has been prepared by Technical
Committee ISO/TC 28 "Petroleum products and lubricants" in collaboration with Technical
Committee CEN/TC 19 "Petroleum products, lubricants and related products", the secretariat
of which is held by NEN.
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 September 2000, and conflicting
national standards shall be withdrawn at the latest by September 2000.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of
the following countries are bound to implement this European Standard: Austria, Belgium,
Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy,
Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United
Kingdom.
Endorsement notice
The text of the International Standard ISO 3405:2000 was approved by CEN as a European
Standard without any modification.
NOTE: Normative references to International Standards are listed in annex ZA (normative).

Page 3
Annex ZA (normative)
Normative references to international publications
with their relevant European publications
This European Standard incorporates by dated or undated reference, provisions from other
publications. These normative references are cited at the appropriate places in the text and the
publications are listed hereafter. For dated references, subsequent amendments to or revisions
of any of these publications apply to this European Standard only when incorporated in it by
amendment or revision. For undated references the latest edition of the publication referred to
applies (including amendments).
NOTE Where an International Publication has been modified by common modifications,
indicated by (mod.), the relevant EN/HD applies.
Publication Year Title EN Year
ISO 3170 1988 Petroleum liquids - Manual sampling EN ISO 3170 1998
(including Amendment 1:1998)
ISO 3171 1988 Petroleum liquids - Automatic pipeline EN ISO 3171 1999
sampling
INTERNATIONAL ISO
STANDARD 3405
Third edition
2000-03-01
Petroleum products — Determination of
distillation characteristics at atmospheric
pressure
Produits pétroliers — Détermination des caractéristiques de distillation à
pression atmosphérique
Reference number
ISO 3405:2000(E)
©
ISO 2000
ISO 3405:2000(E)
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ii © ISO 2000 – All rights reserved

ISO 3405:2000(E)
Contents Page
1 Scope .1
2 Normative references .1
3 Terms and definitions .2
4 Principle.3
5 Apparatus .3
5.1 General.3
5.2 Distillation flasks .3
5.3 Condenser tube and cooling bath.4
5.4 Metal shield or enclosure for flask (manual apparatus only).8
5.5 Heat source .8
5.6 Flask-support .8
5.7 Graduated cylinders .8
5.8 Temperature measurement system .9
5.9 Centring device.10
5.10 Barometer.10
6 Samples and sampling.11
7 Preparation of apparatus .12
8 Apparatus verification.14
8.1 Level follower.14
8.2 Electronic temperature-measurement devices.14
9 Procedure .15
10 Calculations.17
11 Expression of results .20
12 Precision.20
12.1 General.20
12.2 Repeatability.21
12.3 Reproducibility.21
12.4 Bias .23
13 Test report .23
Annex A (normative) Thermometer specifications.24
Annex B (normative) Determination of temperature-sensor lag times and specified distillation data.25
Annex C (informative) Examples of data calculations.27
Annex D (informative) Bias between manual and automated results.31
Annex E (informative) Emulation of emergent-stem errors .33
ISO 3405:2000(E)
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. Each 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, governmental and non-governmental, in
liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical
Commission (IEC) on all matters of electrotechnical standardization.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3.
Draft International Standards adopted by the technical committees are circulated to the member bodies for voting.
Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote.
Attention is drawn to the possibility that some of the elements of this International Standard may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights.
International Standard ISO 3405 was prepared by Technical Committee ISO/TC 28, Petroleum products and
lubricants.
This third edition cancels and replaces the second edition (ISO 3405:1988), of which it constitutes a technically
revision.
Annexes A and B form a normative part of this International Standard. Annexes C, D and E are for information only.
iv © ISO 2000 – All rights reserved

INTERNATIONAL STANDARD ISO 3405:2000(E)
Petroleum products — Determination of distillation
characteristics at atmospheric pressure
WARNING — The use of this International Standard may involve hazardous materials, operations and
equipment. This International Standard does not purport to address all of the safety problems associated
with its use. It is the responsibility of the user of this International Standard to establish appropriate safety
and health practices and to determine the applicability of regulatory limitations prior to use.
1 Scope
This International Standard specifies a laboratory method for the determination of the distillation characteristics of
light and middle distillates derived from petroleum with initial boiling points above 0 �C and end-points below
approximately 400 �C, utilizing either manual or automated equipment, with the manual procedure being the
referee method in cases of dispute, unless otherwise agreed.
NOTE The method is applicable to petroleum products incorporating a minor constitution of components from non-
petroleum origin, but the precision data may not apply in all cases.
The distillation (volatility) characteristics of hydrocarbons have an important effect on their safety and performance,
especially in the case of fuels and solvents. The boiling range gives important information on composition and
behaviour during storage and use, and the rate of evaporation is an important factor in the application of many
solvents. Limiting values to specified distillation characteristics are applied to most distillate petroleum product
specifications in order to control end-use performance and to regulate the formation of vapours which may form
explosive mixtures with air, or otherwise escape into the atmosphere as emissions (VOC).
2 Normative references
The following normative documents contain provisions which, through reference in this text, constitute provisions of
this International Standard. For dated references, subsequent amendments to, or revisions of, any of these
publications do not apply. However, parties to agreements based on this International Standard are encouraged to
investigate the possibility of applying the most recent editions of the normative documents indicated below. For
undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC
maintain registers of currently valid International Standards.
ISO 918:1983, Volatile organic liquids for industrial use — Determination of distillation characteristics.
ISO 3170:1988, Petroleum liquids — Manual sampling.
ISO 3171:1988, Petroleum liquids — Automatic pipeline sampling.
ISO 4259:1992, Petroleum products — Determination and application of precision data in relation to methods of
test.
ISO 4788:1980, Laboratory glassware — Graduated measuring cylinders.
ISO 3405:2000(E)
3 Terms and definitions
For the purposes of this International Standard, the following terms and definitions apply.
3.1
decomposition point
thermometer reading (corrected) which coincides with the first indications of thermal decomposition of the liquid in
the flask
NOTE Characteristic indications of thermal decomposition are an evolution of fumes and erratic thermometer readings
which usually show a decided decrease after any attempt has been made to adjust the heat.
3.2
dry point
thermometer reading (corrected) that is observed at the instant the last drop of liquid evaporates from the lowest
point in the flask; any drops or film of liquid on the side of the flask or on the thermometer are disregarded
NOTE The end-point (final boiling point), rather than the dry point is intended for general use. The dry point can be reported
in connection with special purpose naphthas, such as those used in the paint industry. Also, it is substituted for the end-point
(final boiling point) whenever the sample is of such a nature that the precision of the end-point cannot consistently meet the
requirements given in clause 12.
3.3
end-point
final boiling point
maximum thermometer reading (corrected) obtained during the test
NOTE This usually occurs after evaporation of all liquid from the bottom of the flask.
3.4
initial boiling point
thermometer reading (corrected) that is observed at the instant that the first drop of condensate falls from the lower
end of the condenser tube
3.5
percent evaporated
sum of the percent recovered and the percent loss
3.6
percent loss
100 minus the total recovery
NOTE Sometimes called “front-end loss”; this is the amount of uncondensed material lost in the initial stages of the
distillation.
3.7
corrected loss
percent loss corrected for barometric pressure
3.8
percent recovered
volume of condensate observed in the receiving graduated cylinder at any point in the distillation, expressed as a
percentage of the charge volume, in connection with a simultaneous temperature reading
3.9
percent recovery
maximum percent recovered, as observed in accordance with 9.10
2 © ISO 2000 – All rights reserved

ISO 3405:2000(E)
3.10
percent residue
volume of residue measured in accordance with 9.11, and expressed as a percentage of the charge volume
3.11
percent total recovery
combined percent recovery and residue in the flask, as determined in accordance with 10.1
3.12
thermometer reading
temperature recorded by the sensor of the saturated vapour measured in the neck of the flask below the vapour
tube, under the specified conditions of this test
3.13
temperature reading
thermometer or temperature-measurement device reading (3.12) which is corrected to 101,3 kPa barometric
pressure
3.14
emergent stem effect
offset in temperature reading caused by the use of a total immersion mercury-in-glass thermometer in the partial
immersion mode
NOTE The emergent part of the mercury column is at a lower temperature than the immersed portion, resulting in a lower
temperature reading than that obtained when the thermometer was completely immersed for calibration.
3.15
temperature lag
offset in temperature reading between a mercury-in-glass thermometer and an electronic temperature-
measurement device, caused by the different response time of the systems involved
4Principle
The sample is assigned into one of five groups based on its composition and expected volatility characteristics,
each group defining the apparatus arrangement, condenser temperature and operational variables. A 100 ml test
portion is distilled under the specified conditions appropriate to the group into which the sample falls, and
systematic observations of thermometer readings and volumes of condensate recovered are made. The volume of
the residue in the flask is measured, and the loss on distillation recorded. The thermometer readings are corrected
for barometric pressure, and the data are then used for calculations appropriate to the nature of the sample and the
specification requirements.
5 Apparatus
5.1 General
Typical assemblies of the manual apparatus are shown in Figures 1 and 2.
5.2 Distillation flasks
The distillation flasks shall have a capacity of 100 ml or 125 ml and be constructed of heat-resistant glass,
according to the dimensions and tolerances shown in Figures 3 and 4.
NOTE For tests specifying the dry point, especially selected flasks with bottoms and walls of uniform thickness are
desirable.
ISO 3405:2000(E)
5.3 Condenser tube and cooling bath
Typical types of condenser and cooling bath are illustrated in Figures 1 and 2.
NOTE Other types of apparatus may be used, provided that the test results obtained by their use are such as to correlate
with the results obtained with those illustrated, and to satisfy the precision criteria given in clause 12.
5.3.1 The condenser shall be made of seamless non-corrosive metal tubing, 560 mm � 5 mm in length, with an
outside diameter of 14 mm and a wall thickness of 0,8 mm to 0,9 mm.
NOTE Brass or stainless steel are suitable materials.
5.3.2 The condenser shall be set so that 393 mm � 3 mm of the tube is in contact with the cooling medium, with
50 mm � 3 mm outside the cooling bath at the upper end, and 114 mm � 3 mm outside at the lower end. The
portion of tube projecting at the upper end shall be set at an angle of 75� to the vertical. The portion of the tube
inside the cooling bath shall be either straight or bent in any suitable continuous smooth curve. The average
gradient shall be 15�� 1� with respect to the horizontal, and no 100 mm section shall have a gradient outside a 15�
� 3� range. The projecting lower portion of the condenser tube shall be curved downward for a length of 76 mm and
the lower end cut off at an acute angle. Provisions shall be made to enable the flow of distillate to run down the
side of the receiving graduated cylinder. Figure 5 gives an illustration of the lower end of the condenser tube.
NOTE The flow of distillate down the side of the graduated cylinder may be accomplished either by using a drip-deflector
which is inserted in the receiver, or by having the downward length of the condenser tube curve slightly backwards so as to
ensure contact with the wall of the graduated cylinder at a point 25 mm to 32 mm below the top of the graduated cylinder when it
is in position to receive distillate.
Key
1 Cooling bath
2 Air vents
3 Burner
4 Shield
5 Heat-resistant boards
6 Distillation flask
7 Thermometer
8 Bath cover
9 Blotting paper
10 Support
11 Graduated cylinder
12 Gas line
Figure 1 — Apparatus assembly using a gas burner
4 © ISO 2000 – All rights reserved

ISO 3405:2000(E)
Key
1 Graduated cylinder
2 Blotting paper
3 Thermometer
4 Distillation flask
5 Flask-support board
6 Electric heating element
7 Flask-support platform
8 Flask-adjusting knob
9 Indicating dial
10 Switch
11 Open bottom shield
12 Cooling bath
13 Condenser tube
14 Shield
Figure 2 — Apparatus assembly using an electric heater
ISO 3405:2000(E)
Dimensions in millimetres
Key
1 Reinforcing bead
2Wall1,8 � 0,2
3 Fire polished 100 � 3
4Wall1,15� 0,15
5Wall1,5 � 0,5
Figure 3 — 100 ml flask
6 © ISO 2000 – All rights reserved

ISO 3405:2000(E)
Dimensions in millimetres
Key
1 Reinforcing bead 4Wall1,15� 0,15
2Wall1,8 � 0,2 5 Wall 1,5 � 0,5
3 Fire polished 100 � 3
Figure 4 — 125 ml flasks – Alternative neck designs
Dimensions in millimetres
Key
1 Total length 114 � 2
2 Linear part
Approx. 38
Figure 5 — Lower end of condenser tube
ISO 3405:2000(E)
5.3.3 The volume and design of the cooling bath will depend on the cooling medium employed. The cooling
capacity of the bath shall be adequate to maintain the required temperature for the desired condenser
performance. A single cooling bath may be used for several condenser tubes.
5.4 Metal shield or enclosure for flask (manual apparatus only)
Shields shall be provided to protect the operator from damage to the unit during operation, and to protect the
distillation flask from draughts. They shall allow easy access to the distillation during operation, and be provided
with at least one window to observe the dry point at the end of the distillation.
NOTE 1 A typical shield for a unit fitted with a gas burner would be 400 mm high, 280 mm long and 200 mm wide, made of
sheet metal approximately 0,8 mm in thickness (see Figure 1).
NOTE 2 A typical shield for a unit fitted with an electric heater would be 440 mm high, 200 mm long and 200 mm wide, made
of sheet metal approximately 0,8 mm in thickness (see Figure 2).
5.5 Heat source
5.5.1 Gas burner (see Figure 1), capable of bringing over the first drop from a cold start within the time specified,
and continuing the distillation at the specified rate. A sensitive regulating valve and gas pressure governor to give
complete control of heating shall be provided.
5.5.2 Electric heater (see Figure 2), of low heat retention and adjustable from 0 W to 1 000 W.
5.6 Flask-support
5.6.1 Type 1 for use with gas burner (see Figure 1). Either a ring support of the ordinary laboratory type,
100 mm or larger in diameter, supported on a stand inside the shield, or a platform adjustable from the outside of
the shield shall be used.
Two hard boards, made of ceramic or other heat-resistant material not containing asbestos, 3 mm to 4 mm in
thickness, shall rest upon the ring or the platform, whichever is used. The board immediately above the ring or
platform shall have a central opening 76 mm to 100 mm in diameter, and outside line dimensions slightly smaller
than the inside boundaries of the shield.
The second, or flask-support board, shall be slightly smaller in outside dimensions than the first board and shall
have a central opening conforming to the dimensions given in Table 2. It shall be 3 mm to 4 mm in thickness at the
central hole rim. The flask-support board may be moved slightly in accordance with the directions for positioning
the distillation flask so that direct heat is applied to the flask only through the opening in this board. The position of
the flask is set by adjusting the length of the side-arm inserted into the condenser.
5.6.2 Type 2 for use with an electric heater (see Figure 2). The flask-support is a platform on top of the electric
heater and adjustable from the outside of the shield. The two hard boards described in 5.6.1 are mounted on this
support. Provision shall be made for moving the upper (flask-support) board slightly in the horizontal plane to
ensure that direct heat is applied only through the specified opening in this board. The flask-support assembly shall
be able to move vertically to ensure contact of the flask-support board with the bottom of the distillation flask during
the distillation, and to allow for easy mounting and removal of the distillation flask from the unit.
5.7 Graduated cylinders
5.7.1 Receiving cylinder, of 100 ml capacity, generally in accordance with ISO 4788. It shall be graduated at
intervals of 1 ml and have a graduation at the 100 ml mark. The shape of the base shall be such that the receiver
does not topple when placed empty on a surface inclined at an angle of 13� to the horizontal. Construction details
and tolerances for the graduated cylinder are shown in Figure 6.
For automated apparatus, the cylinder shall conform to the physical specifications described in this subclause, with
the exception of all graduations but that at 100 ml. Graduated cylinders for use in automated units may also have a
metal base.
8 © ISO 2000 – All rights reserved

ISO 3405:2000(E)
Dimensions in millimetres
Key
1 Fire polished
2 Wall thickness
3 Scale length
Figure 6 — 100 ml graduated cylinder (tolerance� 1,0 ml)
5.7.1.1 If required, the graduated cylinder shall be immersed up to above the 100 ml graduation line in a cooling
liquid contained in a cooling bath, such as a tall-form beaker of clear glass or transparent plastic, or placed in a
thermostatically controlled air-circulation chamber.
5.7.2 Residue cylinder, of 5 ml capacity, generally in accordance with ISO 4788.
5.8 Temperature measurement system
5.8.1 Thermometers, if used, shall be of the mercury-in-glass type, nitrogen filled, graduated on the stem and
enamel backed, and shall conform to the specifications given in annex A.
CAUTIONARY NOTE — Under certain test conditions, the bulb of the thermometer can be 28 ����C above the
temperature indicated, and at an indicated temperature of 371 ��C, the temperature of the bulb is
��
approaching a critical range in the glass. It is thus strongly recommended that distillation temperature
readings above 371 ����C are avoided, but in those cases where thermometers have been exposed to
observed temperature readings above 371 ��C, they shall not be re-used without checking their ice point to
��
verify calibration.
5.8.2 Electronic temperature-measurement devices, if used, shall exhibit the same temperature lag, emergent
stem effect and accuracy as the equivalent mercury-in-glass thermometer.
ISO 3405:2000(E)
5.8.2.1 To simulate the temperature lag of a mercury-in-glass thermometer, the circuitry and/or the algorithms
used for the electronic system shall take this fact into account.
5.8.2.2 Alternatively, place the sensor in a casing with the tip covered, so that the assembly, because of its
adjusted thermal mass and conductivity, has a temperature lag time similar to that of mercury-in-glass
thermometers.
5.8.2.3 In case of dispute, unless otherwise agreed, the referee test shall be carried out using the specified
mercury-in-glass thermometers.
5.8.2.4 A means of determining the difference in lag time between an electronic measurement system and
mercury-in-glass thermometers is given in annex B.
5.9 Centring device
The temperature sensor shall be fitted through a snug-fitting device designed for mechanically centring the sensor
in the neck of the distillation flask without vapour leakage. The use of a cork or silicone rubber stopper with a hole
drilled through the centre is not acceptable for this purpose. Examples of acceptable centring devices are shown in
Figures 7 and 8.
NOTE 1 When running tests by the manual method, products with a low initial boiling point may have one or more
temperature readings obscured by the centring device.
NOTE 2 Other centring devices not shown in Figures 7 and 8 are also acceptable provided that they position and hold the
temperature sensor in the middle of the neck of the distillation flask.
5.10 Barometer
The barometer shall be capable of measuring atmospheric pressure with an accuracy of 0,1 kPa or better, at the
same elevation relative to sea level as the apparatus in the laboratory. Do not take readings from aneroid
barometers that are precorrected to give sea level pressures.
NOTE The barometer should ideally be located in the room in which the distillation is carried out.
Key
1 Screwcap
2 O-ring
3 Knurled knob
4 Cone male NS 19/26
Figure 7 — PTFE centring device for ground-glass joint
10 © ISO 2000 – All rights reserved

ISO 3405:2000(E)
Key
1 Single O-ring
Viton or perfluoro elastomer
2 Cone-shaped for perfect
centring in neck of
distillation flask
3 Compression nut (PTFE)
4 Drilled out to fit Pt 100 probe
5 PTFE body
6 Compression without O-ring
7 Double O-rings
Viton or perfluoro elastomer
8 Compression O-ring
9 Compression nut
10 Thermometer or Pt 100
probe
11 Threads
12 Neck of distilling flask
13 Internal diameter of flask to
be precision bore
Figure 8 — Illustrative centring device designs for straight-bore neck
6 Samples and sampling
6.1 Determine the nature of the product to be sampled, and place it in the appropriate group according to Table 1,
which also gives general guidance on sampling conditions.
6.2 Unless otherwise specified, sampling shall be carried out by the procedures described in ISO 3170 or
ISO 3171, bearing in mind the special conditions described in Table 1. Maintain samples prior to testing at the
specified temperatures given in Table 1, away from sources of direct heat or sunlight.
6.2.1 Group 0. Collect the sample in a container previously cooled to below 5 �C. Clean the container, preferably
by immersing it in the liquid, where possible, and discarding the first sample. Where immersion is not possible, the
sample shall be drawn off into the previously cooled container in such a manner that agitation is kept at a minimum.
Close the container immediately with a tight-fitting stopper, and place the sample in an ice bath or refrigerator to
maintain the sample below the specified temperature.
6.2.2 Groups 1 and 2. Collect the sample in a container previously cooled to below 10 �C. Condition the
container and sample in the manner described in 6.2.1. Maintain the sample below 10 �C prior to testing, and
preferably store at or below this temperature. Where maintenance and/or storage at below 10 �C is not possible or
practicable, a temperature up to 20 �C is acceptable provided that the sample is always conditioned to a
temperature below 10 �C before the container is opened.
6.2.3 Groups 3 and 4. Maintain the sample at ambient temperature. If the sample is not fluid at ambient
temperature, maintain it at a temperature of 9 �Cto 21 �C above its pour point. Shake the sample vigorously prior
to subsampling to ensure homogeneity, and disregard the temperature range shown in Table 2 for the receiving
cylinder. Prior to analysis, heat the receiving cylinder to approximately the same temperature as the sample, and
pour the heated test portion precisely to the 100 ml mark. Transfer the test portion as rapidly and completely as
possible to the distillation flask.
CAUTION — A tightly-sealed, full, cold container of sample is likely to break if heated.
ISO 3405:2000(E)
Table 1 — Sample groups and sampling conditions
Group number 0 1 2 3 4
Typical sample type Natural gasoline Gasoline Gasoline Wide-cut Kerosine/gas oil
aviation fuel
W 65,5
Reid vapour pressure, kPa < 65,5 < 65,5 < 65,5
Distillation
u 100
Initial boiling point (IBP), �C– – – > 100
u 250 u 250
Final boiling point (FBP), �C– > 250 > 250
Temperature of sample bottle, �C<5 <10 – ––
a a
Temperature of sample at u 5 u 10 u 10
Ambient Ambient
sampling, �C
a a
Temperature of stored sample, <5 <20 < 20
Ambient Ambient
�C
If sample is wet Resample or dry Resample or Resample or Dry Dry
dry dry
(Reference) (6.3.1) (6.3.1) (6.3.1) (6.3.2) (6.3.2)
a
Samples shall always be stored at 9 �Cto 21 �C above their pour point if not fluid at ambient temperature.
6.3 Samples of materials that visibly contain water are not suitable for testing.
6.3.1 Groups 0, 1 and 2. If the sample is not dry, obtain another sample for testing that is free from suspended
water. If such a sample cannot be obtained, add a sufficient amount of anhydrous sodium sulfate or other suitable
drying agent to the sample maintained at 0 �Cto 10 �C, and physically remove the water by shaking. Once the
sample shows no visible signs of water, use a decanted portion of the sample, maintained at 0 �Cto 10 �C, for the
analysis. Record that the sample has been dried by desiccant.
NOTE Data from a round-robin exercise show that suspended water in hazy samples in group 1 and group 2 can be
removed by the above procedure without statistically affecting the results of the test.
6.3.2 Groups 3 and 4. In cases where a water-free sample is not practical, remove the suspended water by
shaking the sample with anhydrous sodium sulfate or another suitable drying agent, and separate it from the drying
agent by decantation.
7 Preparation of apparatus
7.1 Refer to Table 2 and prepare the apparatus by choosing the appropriate distillation flask, temperature-
measurement system and flask-support board as directed for the indicated group. If gas heating is used, use a
Type 1 flask-support (5.6.1); if electric heating is used, use a Type 2 flask-support (5.6.2). Bring the temperature of
the graduated cylinder, the flask, the temperature sensor and the cooling bath to the indicated temperature.
7.2 Make any necessary provisions so that the temperature of the cooling bath and graduated cylinder will be
maintained at their specified temperatures. The graduated cylinder shall be positioned in a bath such that either the
liquid level is at least as high as the 100 ml mark, or the entire graduated cylinder is surrounded by an air-
circulation chamber.
7.2.1 Groups 0, 1, 2 and 3. Suitable media for low temperature baths include chopped ice and water, refrigerated
brine and refrigerated ethylene glycol.
7.2.2 Group 4. Suitable media for ambient and higher bath temperatures are cold water, hot water and heated
ethylene glycol.
12 © ISO 2000 – All rights reserved

ISO 3405:2000(E)
7.3 Remove any residual liquid in the condenser tube by swabbing with a piece of soft, lint-free cloth attached to a
cord or wire.
7.4 For samples in groups 0, 1, 2 and 3, fit a low-range temperature sensor, provided with a snug-fitting cork or
silicone rubber stopper, tightly into the neck of the sample container, and bring the temperature of the sample to
that specified in Table 2.
Table 2 — Preparation of apparatus
Group number 0 1 2 3 4
Temperature-measurement system Low-range Low-range Low-range Low-range High-range
(see 5.8)
Diameter of hole in flask-support board, mm 32 38 38 50 50
Temperature at start of test, �C
u ambient
–flaskandthermometer 0 to 5 13to18 13to18 13to18
u ambient u ambient u ambient
– flask-support board and shield u ambient –
– graduated cylinder and 100 ml charge 0 to 5 13 to 18 13 to 18 13 to 18 13 to ambient
Flask size, ml (see 5.2) 100 125 125 125 125
7.5 When the temperature of the sample is confirmed, measure the test portion precisely to the 100 ml mark of the
receiving graduated cylinder, and then transfer it as completely as practical to the distillation flask, taking care that
none of the liquid flows into the vapour tube.
NOTE Any material which evaporates during the transfer will contribute to the loss; any material which remains in the
graduated cylinder will contribute to the observed recovery volume at the time of the initial boiling point.
7.5.1 If irregular boiling (bumping) is expected, add a small volume of clean and dry boiling chips to the test
portion.
NOTE Although theoretically the volume of deposit on the chips is part of the residue, this figure is negligible and can be
disregarded.
7.6 Fit the appropriate temperature sensor through a centring device (5.9). In the case of a mercury-in-glass
thermometer, the bulb is centred in the neck and the lower end of the capillary is level with the highest point on the
bottom of the inner wall of the vapour tube (see Figure 9). In the case of a thermocouple/resistance thermometer,
follow the manufacturer’s instructions as to placement so that the sensing position will be just below the level of the
side arm of the distillation flask.
7.6.1 Use a small quantity of vacuum grease on the mating surface of the polytetrafluoroethylene (PTFE) centring
device to facilitate dismantling after use.
7.7 Fit the flask vapour tube, provided with a snug-fitting, well-rolled cork or silicone rubber stopper, tightly into the
condenser tube. Adjust the distillation flask in a vertical position so that the vapour tube extends into the condenser
tube for a distance of 25 mm to 50 mm. Raise and adjust the flask-support board to fit snugly against the bottom of
the flask.
7.8 Place the graduated cylinder that was used to measure the test portion, without drying, into the bath under the
lower end of the condenser tube so that the end of the condenser tube is centred in the graduated cylinder and
extends therein for a distance of at least 25 mm, but not below the 100 ml mark. For manual distillations, cover the
graduated cylinder closely with a piece of blotting paper or similar material, that has been cut to fit the condenser
tube snugly.
ISO 3405:2000(E)
Figure 9 — Position of thermometer in distillation flask
7.9 Record the room temperature and prevailing barometric pressure. Proceed at once with the distillation, as
described in clause 9.
8 Apparatus verification
8.1 Level follower
For automated apparatus, the level follower/recording mechanism of the apparatus shall have a resolution of 0,1 ml
with a maximum error of 0,3 ml between the 5 ml and 100 ml points. The calibration of the assembly shall be
verified according to the manufacturer’s instructions at intervals of not more than 6 months.
NOTE The typical verification procedure involves verifying the output with the receiver containing 5 ml and 100 ml of
material respectively.
8.2 Electronic temperature-measurement devices
Temperature-measurement devices using other than the specified mercury-in-glass thermometers shall exhibit the
same temperature lag, emergent stem effect and accuracy as the equivalent mercury-in-glass thermometer.
Verification of the calibration of these temperature sensors shall be carried out at intervals of not more than
6 months. The electronic circuit for resistance thermometers shall be verified against a standard precision
resistance. When performing this verification, ensure that any algorithms used to correct the temperature for lag
and emergent stem effect are not applied (see the manufacturer’s instructions). The response of the temperature-
measurement system itself shall also be verified by one of the procedures described in 8.2.1 or 8.2.2.
8.2.1 Distill reagent grade toluene in accordance with ISO 918 and compare the 50 % (V/V) recovered
temperature with that shown by the above-mentioned mercury-in-glass thermometer when carrying out a manual
test under the same conditions. Use reagent grade toluene for this test unless it can be shown that the grade
proposed is of sufficient purity to permit its use without lessening the accuracy of the determination.
NOTE 1 For the purposes of this International Standard, the term “% (V/V)” is used to represent the volume fraction of a
material.
Toluene is used as a verification fluid for bias; it will yield almost no information on how well an electronic
measurement system simulates the temperature lag of a mercury-in-glass thermometer. Annex B describes a
method to determine this difference in lag time.
14 © ISO 2000 – All rights reserved

ISO 3405:2000(E)
NOTE 2 Toluene is shown in reference manuals as boiling at 110,6 �C under the conditions of ISO 918, which uses a partial
immersion thermometer. Because this International Standard uses thermometers calibrated for total immersion, the results will
be lower, and different for each. The approximate figures are 109,3 �C for the low-range thermometer, and 109,9 �Cfor the
high-range thermometer.
8.2.2 Distill a certified reference fluid of a specific product group, under the manual
...