SLOVENSKI STANDARD
SIST EN 1797:2002
01-november-2002
1DGRPHãþD
SIST EN 1797-1:1999
Kriogene posode - Združljivost plin/material
Cryogenic vessels - Gas/material compatibility
Kryo-Behälter - Verträglichkeit von Gas/Werkstoffen
Récipients cryogéniques - Compatibilité entre gaz et matériaux
Ta slovenski standard je istoveten z:
EN 1797:2001
ICS:
23.020.40
SIST EN 1797:2002
en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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EUROPEAN STANDARD
EN 1797
NORME EUROPÉENNE
EUROPÄISCHE NORM
July 2001
ICS 23.020.40
Supersedes EN 1797-1:1998
English version
Cryogenic vessels - Gas/material compatibility
Récipients cryogéniques - Compatibilité entre gaz et
matériaux
Kryo-Behälter - Verträglichkeit von Gas/Werkstoffen
This European Standard was approved by CEN on 9 June 2001.
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
© 2001 CEN
B-1050 Brussels
All rights of exploitation in any form and by any means reserved
worldwide for CEN national Members.
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Ref. No. EN 1797:2001 E
EN 1797:2001 (E)
Contents
page
Foreword......................................................................................................................................................................3
1
Scope ..............................................................................................................................................................4
2
Normative references ....................................................................................................................................4
3
Compatibility of materials with gases other than oxygen .........................................................................4
4
4.1
4.2
4.3
4.4
4.4.1
4.4.2
General requirements for oxygen service...................................................................................................5
Evaluation of materials for oxygen service.................................................................................................5
Evaluation of metallic materials ...................................................................................................................5
Evaluation of non metallic materials ...........................................................................................................6
Test methods and acceptance criteria ........................................................................................................6
Ignition tests...................................................................................................................................................6
Mechanical impact test in liquid oxygen (LOX) ..........................................................................................7
Annex A (normative) Spontaneous ignition test (Bomb test).................................................................................8
Annex B (normative) Pressure surge test ..............................................................................................................13
Annex C (informative) Ignition test - Advantages and disadvantages of the two alternative methods ..........16
Annex ZA (informative) Clauses of this European Standard addressing essential requirements or
other provisions of EU directives...............................................................................................................17
Bibliography ..............................................................................................................................................................18
2
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EN 1797:2001 (E)
Foreword
This European Standard has been prepared by Technical Committee CEN/TC 268, "Cryogenic vessels", the
secretariat of which is held by AFNOR.
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 January 2002, and conflicting national standards shall be withdrawn at the latest
by January 2002.
This document replaces EN 1797-1:1998.
For relationship with EU Directives, see informative annex ZA, which is an integral part of this document.
This document has been prepared under a mandate given to CEN by the European Commission and the European
Free Trade Association, and supports essential requirements of EU Directives.
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.
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EN 1797:2001 (E)
1
Scope
This European Standard specifies requirements for gas/materials compatibility for cryogenic vessels (such as
chemical resistance) but it does not cover mechanical properties (e.g. for low temperature application).
It gives guidance for compatibility with gases other than oxygen and it gives detailed requirements for oxygen and
oxygen enriched atmosphere compatibility and defines the testing methods for establishing oxygen compatibility of
materials (metallic and non-metallic) to be used for cryogenic vessels and associated equipment.
It mainly deals with materials that are normally or could be in contact with liquid/gaseous oxygen e.g., materials for
cryogenic vessels used for the storage and/or transport of liquid oxygen.
It also deals with the materials which can be in contact with oxygen enriched environment e.g. insulating materials
used for nitrogen, neon, hydrogen and helium cryogenic vessels in case of air condensation.
2
Normative references
This European Standard incorporates by dated or undated references 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 publication 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).
EN 849: 1996, Transportable gas cylinder – Cylinder valves - Specification and type testing.
EN 12300, Cryogenic vessels - Cleanliness for cryogenic service.
EN ISO 11114-1, Transportable gas cylinders - Compatibility of cylinder and valve materials with gas contents Part 1 : Metallic materials (ISO 11114-1:1997).
prEN ISO 11114-2:1997, Transportable gas cylinders - Compatibility of cylinder and valve materials with gas
contents - Part 2 : Non-metallic materials (ISO/DIS 11114-2).
3
Compatibility of materials with gases other than oxygen
The cryogenic vessels are used in a range of temperature from very low temperature to ambient temperature. The
problems of compatibility with gases other than oxygen such as corrosion, hydrogen embrittlement normally occur
at ambient temperature and become negligible at cryogenic temperature.
So, in case of gases other than oxygen, EN ISO 11114-1 and prEN ISO 11114-2:1997 may be used as a guide for
cryogenic vessels.
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EN 1797:2001 (E)
4
4.1
General requirements for oxygen service
Evaluation of materials for oxygen service
The selection of a material for use with oxygen and/or in an oxygen enriched atmosphere is primarily a matter of
understanding the circumstances that cause oxygen to react with the material. Most materials in contact with
oxygen will not ignite without a source of ignition energy. When an energy input rate, as converted to heat, is
greater than the rate of heat dissipation, and the resulting heat increase is continued for sufficient time, ignition and
combustion will occur. Thus, two things shall be considered
the material's minimum ignition temperature ;
the energy sources that will produce a sufficient increase in the temperature of the material.
These should be viewed in the context of the entire system design so that the specific factors listed below will
assume the proper relative significance.
The specific factors are :
the properties of the materials, including the factors affecting ease of ignition and the conditions affecting
potential resulting damage (heat of reaction) ;
the operating conditions : pressure, temperature, gas velocity, oxygen concentrations and oxygen state
(gaseous or liquid), surface contamination in accordance with EN 12300 ;
the potential sources of ignition (friction, heat of compression, heat from mass impact, heat from particle
impact, static electricity, electrical arc, resonance, internal flexing etc.) ;
the reaction effect (consequence on the surroundings etc.) ;
additional factors (performance requirements, prior experience, availability and cost).
CAUTION This European Standard specifies the minimum acceptance requirements for materials in oxygen and enriched air
service. In the cases of severe conditions and when the operating pressure is above 40 bar, additional tests to those specified
should be considered.
The use of materials in cryogenic vessels which do not pass the tests outlined in 4.4.1 and/or 4.4.2 shall be
supported by a favourable risk assessment and/or documented evidence of previous long term satisfactory service
in use.
4.2
Evaluation of metallic materials
Metallic materials normally used for the construction of cryogenic vessels i.e. low alloy steels, nickel steels,
stainless steels, copper and copper alloys, aluminium and aluminium alloys do not normally present any
incompatibility when in contact with oxygen.
The cases in which some ignitions or violent reactions may occur are when very thin materials are used with high
surface/volume ratio, and when high ignition energy is available e.g. pump failure. Thin materials e.g. thinner than
0,1 mm shall be tested in accordance with 4.4.2 in conditions as close as possible to the real operational conditions
(e.g. for multi-layer insulations use similar number of layers and configuration). Materials to be used in applications
where the ignition energy is potentially high should be subjected to special consideration.
For cryogenic vessels intended for oxygen service the test shall be performed with oxygen. For cryogenic vessels
intended for nitrogen, hydrogen or helium service, when materials are located in an area where contact with
condensed enriched air is a risk, the test described in 4.4.2 shall be performed with cryogenic O /N mixtures
² ²
containing at least 50 % oxygen.
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EN 1797:2001 (E)
4.3
Evaluation of non metallic materials
Non metallic materials include, for example, plastics, elastomers, lubricants, ceramics, glasses and glues. Some of
these materials present a high risk of ignition when in contact with oxygen and should be avoided or carefully
selected and used in limited quantity.
Some fully oxidised materials such as ceramics and glass present no risk of ignition provided they are not
contaminated.
Any non metallic materials, other than fully oxidised materials, in contact with liquid oxygen shall be tested in
accordance with 4.4.1 and 4.4.2. Consideration shall be given to testing materials used in those parts of the system
where liquid oxygen accumulation may incidentally occur (e.g. in the insulation).
For cryogenic vessels intended for oxygen service the test shall be performed with oxygen. For cryogenic vessels
intended for nitrogen, hydrogen or helium service, when materials are located in an area where contact with
condensed enriched air is a risk, the test described in 4.4.2 shall be performed with cryogenic O /N mixtures
² ²
containing at least 50 % oxygen.
Any non metallic materials, other than fully oxidised materials, in contact with gaseous oxygen shall be tested in
accordance with 4.4.1. Consideration shall be given to testing materials used in those parts of the system where
gaseous oxygen accumulation may incidentally occur (e.g. in the insulation).
4.4
Test methods and acceptance criteria
Each material to be tested shall be clearly identified, normally by the commercial name and the manufacturer's
name.
4.4.1
Ignition tests
Two alternative test methods are described in 4.4.1.1 or 4.4.1.2. The advantages and disadvantages of each are
given in annex C.
Materials not satisfying the requirements of 4.4.1.1 or 4.4.1.2 can still be used providing they successfully pass, in
their actual operating configuration, the "Oxygen pressure surge test" described in 5.3.8 of EN 849:1996 (e.g. for a
valve sealing material, the entire valve or a representative assembly shall be tested).
4.4.1.1
4.4.1.1.1
Spontaneous ignition test ("Bomb test")
Test procedure
The test procedure is given in annex A.
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EN 1797:2001 (E)
4.4.1.1.2
Acceptance criteria
The spontaneous ignition temperature determined in accordance with 4.4.1.1.1 shall be not less than the values
given in Table 1.
Table 1 — Minimum spontaneous ignition temperature
Maximum working
pressure
Bar (gauge)
Minimum Spontaneous
Ignition Temperature
(SIT) °C
3
200
10
230
20
250
40
300
100
350
150
375
207
400
Above 207 up to 345
400
Remark
Complementary test may
be advisable (see 4.1)
NOTE Intermediate values can be determined by linear interpolation.
4.4.1.2
Pressure surge test
4.4.1.2.1
Test procedure
The test procedure is given in annex B.
4.4.1.2.2
Acceptance criteria
No reaction shall be observed during 5 consecutive pressure surge impacts at the intended maximum working
pressure.
4.4.2
4.4.2.1
Mechanical impact test in liquid oxygen (LOX)
Test procedure
The mechanical impact test shall be performed at atmospheric pressure in liquid oxygen generally as described in
the bibliography. This is an example of preferred test equipment but the details are not mandatory. The test shall be
conducted :
on material with the surface condition that is intended for use ;
on material in a physical form delivered for use (i.e. solid, powder etc.) ;
at an impact energy per unit contact area of 79 J/cm².
4.4.2.2
Acceptance criteria
No reaction shall be detected within a series of 20 tests.
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EN 1797:2001 (E)
Annex A
(normative)
Spontaneous ignition test (Bomb test)
A.1 General
This annex defines a test method to determine the spontaneous ignition temperature of non-metallic materials in
pressurised gaseous oxygen.
Spontaneous ignition temperature is a criterion for the comparison and the classification of materials, and can be
used as an aid in the choice of materials used in the presence of pressurised gaseous oxygen.
A.2 Principle
A small quantity of the test material is slowly heated in oxygen under pressure. The continuous recording of
pressure and temperature is used to determine spontaneous ignition, which is seen as a sudden increase in
temperature and pressure.
A.3 Preparation of test pieces
Test pieces shall be prepared by procedures that prevent contamination.
Test pieces can be in liquid or solid form. In the case of solids, the materials shall be cut into a minimum of 6
pieces. The total mass of the pieces used in each test shall be at least 60 mg.
A.4 Test equipment
Figure A.1 shows the basic principle of the test equipment. When others methods of heating are used the heating
rate of the specimen should be less than 20°C/min. If inductively heated furnace are used, the temperature rate
can be up to 110°C/min.
A thermocouple inside a glove finger positioned as close as possible to the test piece is used to monitor on a
recorder temperature variation with an accuracy of ± 2° C.
The internal pressure shall be monitored and recorded with an accuracy of ± 2 bar.
The equipment, and in particular, the autoclave, shall be designed to resist violent internal reactions (explosions).
A.5 Oxygen purity
The gas used shall contain not less than 99,5% oxygen. The hydrocarbon content shall be less than 10 ppm by
volume.
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EN 1797:2001 (E)
A.6 Test procedure
The test piece contained in the sample holder is put into the bomb. The bomb is then sealed and purged to remove
any air and any possible residual combustion products from previous tests. Oxygen is then introduced at a
minimum pressure which will produce at least 120 bar at ignition.
Whilst continuously recording the temperature and pressure, the temperature is raised, at a rate of up to 20°C/min
by adjustment of the heating power, to the spontaneous ignition temperature or to a maximum temperature of
500°C.
The spontaneous ignition temperature is indicated on the recording by the sudden increase in both parameters
caused by the internal reaction.
A.7 Results
The record of the test is used as shown in Figure A.2 to determine the three parameters,
Ti
is the spontaneous ignition temperature ;
T
is the increase in temperature at moment of ignition ;
P
increase in pressure at moment of ignition.
T i , T and P , where
Materials are classified in accordance with their spontaneous ignition temperature.
Temperature and pressure increase,
T and P , characterise the violence of the reaction.
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EN 1797:2001 (E)
Key
1 Test sample
2 Oxygen : 120 bar at minimum ignition conditions
3 Pressure transducer
4 Temperature
5 Heater 20 °C/min max. 500 °C
Figure A.1 — Bomb for spontaneous ignition test
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Key
1 Temperature T (°C)
2 Time (minutes)
3 Pressure P (bar)
4 Temperature and pressure variations against time
5 Pressure at SIT
6 Peak (pressure)
7 Peak (temperature)
8 Spontaneous ignition temperature
Figure A.2 — Spontaneous ignition test - Temperature and pressure versus time
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EN 1797:2001 (E)
A.8 Test report
Test results are recorded on a report sheet, an example of which is given below :
Test No.
SPONTANEOUS IGNITION
Date
1 - TEST PERFORMED FOR
____________________________________
2 - TESTED MATERIAL
____________________________________
Function
____________________________________
Conditions of use
Temperature in °C
____
Pressure in
bar _______
Assumed composition
____________________________________
Condition, shape, appearance
____________________________________
Manufacturer
____________________________________
Supplier
____________________________________
Trade name
____________________________________
3 - RESULTS
Weight of test piece in grams :
Pressure in bar
At SIT
Peak
Temperature in °C
P
At SIT
Peak
T
Remarks :
4 - SPONTANEOUS IGNITION TEMPERATURE (°C)
5 - COMMENTS
Authorised signature
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EN 1797:2001 (E)
Annex B
(normative)
Pressure surge test
B.1 General
This annex defines a test method to establish the maximum working pressure by examining the reactivity of nonmetallic materials (solids, pastes or liquids) when exposed to a pressure surge of oxygen, air or of a gas mixture
containing oxygen.
This test simulates processes that may occur in service on non-metallic materials, e.g. in shut-off installations when
operated too fast, or on rupture of equipment or pipes etc.
This method may be applied to intended working pressures equal to or greater than 10 bar.
B.2 Principle
A small quantity of the test material is exposed to a gaseous oxygen pressure surge being generated by operating
a quick opening valve between a tube containing the test material and a vessel containing high pressurised
oxygen.
The pressure in the tube is raised from initial pressure
pi to final pressure p f as near as adiabatically as possible
given by the adjustable pressure of an oxygen accumulator.
A possible reaction of the test material with oxygen is indicated by a steep temperature rise, superimposed on the
temperature rise obtained by adiabatic compression.
In this method the maximum working pressure is defined as the maximum final pressure
p f at which no reaction of
a sample with oxygen can be observed.
B.3 Preparation of test samples
Solid materials are finely divided into a minimum of 6 pieces, liquids are coated on fibrous ceramic materials.
A total weight of 0,2 g to 0,5 g shall be used for each test.
B.4 Test equipment
Figure B.1 shows the basic principles of the test equipment.
The test sample is placed into a heatable steel tube (see Figure B.1, 9) 15 cm3 in volume. This reaction vessel is
connected to an oxygen-accumulator (see Figure B.1, 5) via a 750 mm-long pipe (see Figure B.1, 7 ; internal
diameter 14 mm) and a pneumatically operated quick opening valve (see Figure B.1, 4) guaranteeing a pressure
rising time of
0
20 5 ms.
Two heaters (see Figure B.1, 3 and 8) are used for heating the oxygen-accumulator and the reaction vessel up to
(60 3 )°C.
After a pressure surge the reaction vessel shall be relieved to atmospheric pressure by aid of a vent valve (see
Figure B.1, 6).
The temperature of the sample in the reaction vessel and the temperature of the oxygen inside the accumulator are
measured by use of
thermocouples
Figure B.1,
labelled
The projekti
pressured.o.o.
is measured by pressure
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EN 1797:2001 (E)
transducers (see Figure B.1, labelled P). Both pressure and temperature are recorded with an accuracy of 2 bar
and 2 °C respectively.
The equipment, and in particular, the reaction vessel shall be designed to resist violent internal reactions.
B.5 Oxygen purity
The gas used shall contain not less than 99,5 % oxygen. The hydrocarbon content shall be less than 10 ppm by
volume.
B.6 Test procedure
At the beginning of the test the intended working pressure,
p f , is chosen and adjusted on the oxygen-accumulator.
The reaction vessel containing the sample is attached to the connecting pipe.
Reaction vessel and connecting pipe are filled with oxygen at ambient pressure
pi (generally 1 bar).
After the sample has reached its testing temperature of (60 3) °C, preheated oxygen of (60 3) °C is led into the
reaction vessel via the quick opening valve at a pressure rising time of
0
20 5 ms.
pi ) is as near as possible adiabatically compressed
to the final pressure p f (intended maximum working pressure). p f is applied for 15 s. Afterwards the test tube is
In this way, oxygen in the low pressure part (starting pressure
relieved to atmospheric pressure.
The temperature of the sample and the pressure are continuously recorded. A possible reaction of the sample with
oxygen can be recognised by a steep temperature rise of at least 20°C superimposed on the temperature normally
reached without reaction (blank test).
In case of a reaction, the test tube is decompressed at once and the test is repeated at a smaller pressure
pf .
Pressure steps of 10 bar are always chosen.
If there is no reaction of the sample with oxygen the test is repeated up to a maximum of five consecutive tests on
the same test sample.
B.7 Results
The test result is the maximum final pressure
p f at which in five consecutive tests no reaction can be observed.
This pressure is the maximum working pressure of the non-metallic material tested.
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EN 1797:2001 (E)
Key
1 Oxygen supply
2 Inlet valve
7 Connecting pipe
8 Heater
3 Heater
4 Quick opening valve
9 Reaction vessel
10 Internal diameter DN 14
5 Oxygen-accumulator
6 Vent valve
P Pressure transducer
T Thermocouple
Figure B.1 — Pressure surge test
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EN 1797:2001 (E)
Annex C
(informative)
Ignition test - Advantages and disadvantages of the two alternative methods
This European Standard reflects the fact, that, in practice, sufficient operational safety is obtained by applying
either of the methods described in 4.4.1.
The bomb test of 4.4.1.1 is particularly representative in all cases where risks of sudden gaseous oxygen
compression are unlikely. In addition, the bomb test is suitable for working out a scale characterising the oxygen
behaviour of materials. If the behaviour of a material is satisfactory in a given application, all materials classified at
a higher or equal level within the scale will be able to be used for this application, without requiring additional
testing.
The pressure surge test of 4.4.1.2 is a severe one, because the pressure thresholds for the majority of materials
are more demanding than those obtained by the bomb test. In particular, at the highest pressures, the maximum
acceptable working pressures are lower than those resulting from the bomb test. Consequently the pressure surge
test is only justified where the likehood of sudden compression is high.
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EN 1797:2001 (E)
Annex ZA
(informative)
Clauses of this European Standard addressing essential safety
requirements of Directive 97/23/EC
This European Standard has been prepared under a mandate given to CEN by the European Commission and the
European Free Trade Association and supports essential safety requirements of Pressure Equipment Directive
97/23/EC (PED).
WARNING : Other requirements and other EU Directives may be applicable to the product(s) falling within the
scope of this standard.
The clauses of this standard given in Table ZA.1 support essential safety requirements of PED.
Table ZA.1 — Comparison between PED and this European Standard
Harmonised clauses of EN 1797
Content
PED
all
resistance to intended use
Annex 1 § 2.2.1
Compliance with the clauses of this standard provides one means of conforming with the specific safety
requirements of the Directive concerned and associated EFTA regulations.
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EN 1797:2001 (E)
Bibliography
ASTM D 25-12:1982, Test method for compatibility of materials with liquid oxygen (impact sensitivity threshold and
Pass-Fail Techniques).
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