Petroleum products - Determination of distillation characteristics at atmospheric pressure (ISO 3405:2000)

Migrated from Progress Sheet (TC Comment) (2000-07-10): Decision of BT to submit this ISO document to UAP procedure. ++ Standard under revision in ISO ++ UAP procedure changed to parallel vote on revision, resolution BT C 123/1995?

Mineralölerzeugnisse - Bestimmung des Destillationsverlaufes bei Atmosphärendruck (ISO 3405:2000)

Produits pétroliers - Détermination des caractéristiques de distillation à pression atmosphérique (ISO 3405:2000)

La présente Norme internationale spécifie une méthode de laboratoire pour la détermination des caractéristiques de distillation des distillats pétroliers légers et moyens ayant un point initial de distillation supérieur à 0 °C et un point final inférieur à environ 400 °C, utilisant un équipement manuel ou automatisé, la méthode manuelle étant la procédure de référence, sauf accord contraire.NOTE : La méthode est applicable aux produits pétroliers contenant de petites quantités de composés non pétroliers.Toutefois, il est possible que dans certains cas les valeurs de fidélité ne s'appliquent pas.Les caractéristiques de distillation (volatilité) des hydrocarbures sont importantes en matière de sécurité et de performances, en particulier dans le cas des carburants et des solvants. L'intervalle de distillation donne des renseignements importants sur la composition et le comportement pendant le stockage et l'utilisation, et la vitesse d'évaporation est une caractéristique essentielle dans l'utilisation de nombreux solvants. La plupart des spécifications applicables aux distillats pétroliers fixent des valeurs limites pour certaines caractéristiques de distillation, afin de mieux maîtriser les performances en utilisation et pour contrôler la formation de vapeurs qui pourraient devenir explosives en présence d'air ou s'échapper dans l'atmosphère (COV).

Naftni proizvodi - Določevanje destilacijskih značilnosti pri tlačni atmosferi (ISO 3405:2000)

General Information

Status
Withdrawn
Publication Date
29-Feb-2000
Withdrawal Date
14-Jan-2011
Current Stage
9960 - Withdrawal effective - Withdrawal
Due Date
15-Jan-2011
Completion Date
15-Jan-2011

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SLOVENSKI STANDARD
SIST EN ISO 3405:2000
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
SIST EN ISO 3405:2000 en

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 3405:2000
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SIST EN ISO 3405:2000
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.
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SIST EN ISO 3405:2000
Page 2
EN ISO 3405:2000
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).

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SIST EN ISO 3405:2000
Page 3
EN ISO 3405:2000
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
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SIST EN ISO 3405:2000
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SIST EN ISO 3405:2000
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
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SIST EN ISO 3405:2000
ISO 3405:2000(E)
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ii © ISO 2000 – All rights reserved
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SIST EN ISO 3405:2000
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 2000 – All rights reserved iii
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SIST EN ISO 3405:2000
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
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SIST EN ISO 3405:2000
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 2000 – All rights reserved 1
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SIST EN ISO 3405:2000
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
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SIST EN ISO 3405:2000
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 2000 – All rights reserved 3
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SIST EN ISO 3405:2000
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
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SIST EN ISO 3405:2000
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 2000 – All rights reserved 5
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SIST EN ISO 3405:2000
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
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SIST EN ISO 3405:2000
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 2000 – All rights reserved 7
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SIST EN ISO 3405:2000
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
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SIST EN ISO 3405:2000
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 c
...

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