Manual
Dewar LN2 Autofill 50l
Translation
© Retsch GmbH, 42781 Haan, Retsch-Allee 1-5, Germany 08.02.2012 0002
Copyright
Copyright by
Retsch GmbH
Haan, Retsch-Allee 1-5
D-42781 Haan
Federal Republic of Germany
2
1 Notes on the Operating Manual ............................................................................................................ 5
1.1 Explanations of the safety warnings .................................................................................................. 6
1.2 General safety instructions ................................................................................................................ 7
1.3 Repairs ............................................................................................................................................... 8
2 Confirmation ........................................................................................................................................... 9
2.1 Type plate description ........................................................................................................................ 9
3 Safety and occupational health instructions ..................................................................................... 10
3.1 General ............................................................................................................................................ 11
3.2 Safety instructions on the handling of liquid nitrogen ...................................................................... 12
3.3 Oxygen deficiency ........................................................................................................................... 12
3.3.1 Dangers ....................................................................................................................................... 12
3.3.2 Causes ......................................................................................................................................... 12
3.3.3 Recommendations ....................................................................................................................... 12
3.3.4 General conduct in the case of an accident ................................................................................ 13
3.4 Cryogenic burns ............................................................................................................................... 13
3.4.1 Dangers ....................................................................................................................................... 13
3.4.2 Causes ......................................................................................................................................... 13
3.4.2.1 Burns through splashes ....................................................................................................... 13
3.4.2.2 Burns through contact .......................................................................................................... 14
3.4.3 Recommendations ....................................................................................................................... 14
3.4.4 General rules of conduct for splashes with liquid nitrogen .......................................................... 14
3.4.4.1 To the eyes .......................................................................................................................... 14
3.4.4.2 On the skin ........................................................................................................................... 14
3.5 Danger of explosion ......................................................................................................................... 14
3.5.1 Dangers ....................................................................................................................................... 14
3.5.2 Causes ......................................................................................................................................... 14
3.5.3 Recommendations ....................................................................................................................... 15
3.5.4 General conduct in the case of an accident ................................................................................ 15
3.6 Oxygen enrichment .......................................................................................................................... 15
3.6.1 Dangers ....................................................................................................................................... 15
3.6.2 Causes ......................................................................................................................................... 15
3.6.3 Recommendations ....................................................................................................................... 15
3.7 Surrounding area of the machine .................................................................................................... 16
3.7.1 Rooms .......................................................................................................................................... 16
4 Operating the machine ........................................................................................................................ 17
4.1 Views of the Instrument ................................................................................................................... 17
4.2 Overview table of the parts of the device ........................................................................................ 18
4.3 Technical Data ................................................................................................................................. 19
3
4.4 Vacuum closure and safety device .................................................................................................. 19
4.5 Level Display ................................................................................................................................... 19
4.6 Filling the vessel .............................................................................................................................. 20
4.7 Pressure build-up ............................................................................................................................. 21
4.8 Withdrawal of liquid nitrogen............................................................................................................ 21
4.9 Pressure relief .................................................................................................................................. 21
4.10 Transport.......................................................................................................................................... 21
4.11 Admitting the test pressure .............................................................................................................. 22
4.12 Checking the seat tightness............................................................................................................. 22
4.13 Checking the response pressure ..................................................................................................... 22
5 Index ...................................................................................................................................................... 23
4
Notes on the Operating Manual
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1 Notes on the Operating Manual
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This operating manual is a technical guide on how to operate the device safely and
it contains all the information required for the areas specified in the table of
contents. This technical documentation is a reference and instruction manual. The
individual chapters are complete in themselves.
Familiarity (of the respective target groups defined according to area) with the
relevant chapters is a precondition for the safe and appropriate use of the device.
This operating manual does not contain any repair instructions. If faults arise or
repairs are necessary, please contact your supplier or get in touch with Retsch
GmbH directly.
Application technology information relating to samples to be processed is not
included but can be read on the Internet on the respective device’s page at
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www.retsch.com.
Changes
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Subject to technical changes.
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Copyright
Disclosure or reproduction of this documentation, use and disclosure of its contents
are only permitted with the express permission of Retsch GmbH.
Infringements will result in damage compensation liability.
5
Notes on the Operating Manual
WARNING
Type of danger / personal injury
Source of danger
– Possible consequences if the dangers are not observed.
• Instructions on how the dangers are to be avoided.
WARNING
CAUTION
Type of danger / personal injury
Source of danger
– Possible consequences if the dangers are not observed.
• Instructions on how the dangers are to be avoided.
CAUTION
NOTICE
Nature of the property damage
Source of property damage
– Possible consequences if the instructions are not observed.
• Instructions on how the dangers are to be avoided.
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1.1 Explanations of the safety warnings
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In this Operating Manual we give you the following safety warnings
Serious injury may result from failing to heed these safety warnings. We give you
the following warnings and corresponding content.
We also use the following signal word box in the text or in the instructions on action
to be taken:
Moderate or mild injury may result from failing to heed these safety warnings.
We give you the following warnings and corresponding content.
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We also use the following signal word box in the text or in the instructions on action
to be taken:
In the event of possible property damage we inform you with the word
“Instructions” and the corresponding content.
We also use the following signal word in the text or in the instructions on action to
be taken:
NOTICE
6
Notes on the Operating Manual
CAUTION
Read the Operating Manual
Non-observance of these operating instructions
– The non-observance of these operating instructions can
result in personal injuries.
• Read the operating manual before using the device.
• We use the adjacent symbol to draw attention to the
necessity of knowing the contents of this operating
manual.
CAUTION
Changes to the machine
– Changes to the machine may lead to personal injury.
• Do not make any change to the machine and use spare parts and
accessories that have been approved by Retsch exclusively.
NOTICE
Changes to the machine
– The conformity declared by Retsch with the European Directives will lose
its validity.
– You lose all warranty claims.
• Do not make any change to the machine and use spare parts and
accessories that have been approved by Retsch exclusively.
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1.2 General safety instructions
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Target group : All persons concerned with the machine in any form
This machine is a modern, high performance product from Retsch GmbH and
complies with the state of the art. Operational safety is given if the machine is
handled for the intended purpose and attention is given to this technical
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documentation.
You, as the owner/managing operator of the machine, must ensure that the people
entrusted with working on the machine:
• have noted and understood all the regulations regarding safety,
• are familiar before starting work with all the operating instructions and
specifications for the target group relevant for them,
• have easy access always to the technical documentation for this machine,
• and that new personnel before starting work on the machine are familiarised
with the safe handling of the machine and its use for its intended purpose,
either by verbal instructions from a competent person and/or by means of
this technical documentation.
Improper operation can result in personal injuries and material damage. You are
responsible for your own safety and that of your employees.
Make sure that no unauthorised person has access to the machine.
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7
Notes on the Operating Manual
The Retsch representative in your country
Your supplier
Retsch GmbH directly
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Reperaturen
1.3 Repairs
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This operating manual does not contain any repair instructions. For your own
safety, repairs may only be carried out by Retsch GmbH or an authorized
representative or by Retsch service engineers.
In that case please inform:
Your Service Address:
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8
Confirmation
I have read and taken note of the contents of all chapters in this operating
manual as well as all safety instructions and warnings.
User
Surname, first name (block letters)
Position in the company
Signature
Service technician or operator
Surname, first name (block letters)
Position in the company
Place, date and signature
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Bestätigung
2 Confirmation
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This operating manual contains essential instructions for operating and maintaining
the device which must be strictly observed. It is essential that they be read by the
operator and by the qualified staff responsible for the device before the device is
commissioned. This operating manual must be available and accessible at the
place of use at all times.
The user of the device herewith confirms to the managing operator (owner) that
(s)he has received sufficient instructions about the operation and maintenance of
the system. The user has received the operating manual, has read and taken note
of its contents and consequently has all the information required for safe operation
and is sufficiently familiar with the device.
As the owner/managing operator you should for your own protection have your
employees confirm that they have received the instructions about the operation of
the machine.
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2.1 Type plate description
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9
Safety and occupational health instructions
CAUTION
Danger of injury to eyes and skin
Frostbites through liquid nitrogen
– Liquid nitrogen has a temperature of –196 °C and may cause
injuries similar to burns on skin or eye contact or cause frostbite.
• Always use goggles and wear protective gloves when
opening the cooling casing and the grinding jar.
CAUTION
Use of liquid nitrogen
– Retsch GmbH rules out any liability claims that may arise in the
use of liquid nitrogen or similar cooling agents.
• Please observe the safety regulations of the cooling liquid
supplier.
1 2 3 4 5 6 7
8
Fig. 1: Type plate marking
1 Instrument name
2 Year of manufacture
3 Article number
4 Serial number
5 Manufacturer’s address
6 CE marking
7 Waste disposal marking
8 Barcode
When making enquiries, please quote the name of the instrument (1) or the article
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number (3) and serial number (4) of the instrument.
3 Safety and occupational health instructions
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10
CAUTION
Handling liquid nitrogen
General hazardous situations
– The following hazardous situations may arise in the handling of liquid
nitrogen: oxygen deficiency situations, cryogenic burns, danger of
explosion, oxygen enrichment
• All users must be informed about the dangers of working with liquid
nitrogen in order to be able to work safely.
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3.1 General
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Safety and occupational health instructions
This section summarises the general occupational health and safety guidelines for
the handling of liquid nitrogen.
11
Safety and occupational health instructions
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3.2 Safety instructions on the handling of liquid nitrogen
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3.3 Oxygen deficiency
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The main components of air according to volumes are as follows:
– Oxygen O2 21 %
– Nitrogen N2 78 %
– Argon Ar 1 %
The gases contained in the atmosphere are not toxic. However, a change in
concentration (in particular changes to the oxygen concentration) may have effects
on life and burns. It is therefore essential for the air breathed in to contain sufficient
oxygen (> 19 %).
Humans cannot detect changes in the composition of air within the time that will
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3.3.1 Dangers
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actually be necessary because the components are colourless and odourless.
A danger of suffocation exists as a result of the normal evaporation of the liquid
nitrogen that pushes out the oxygen in the air. An oxygen deficiency is dangerous
and can cause death through suffocation. The reaction of the organism to oxygen
deficiency will differ greatly depending on the individual. It is not possible to provide
precise and generally applicable information on the symptoms of an oxygen
deficiency.
Example: under normal conditions (20° C; 1013 mbars) 1 l liquid nitrogen
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evaporates to produce 680 l nitrogen gas.
3.3.2 Causes
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An oxygen deficiency may arise during the following work or in the following
conditions:
– Nitrogen as liquid or gas
– Natural evaporation of liquid nitrogen
– Refilling of liquid nitrogen
– Leaks in containers for liquid or gaseous nitrogen
– Defect in the air feed or outlet
– Tipping over of the container
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This list is not complete.
3.3.3 Recommendations
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In order to prevent the danger of an oxygen deficiency, the following measures
must be taken.
The vessel:
• must be kept in a vertical position.
12
• must be provided with a suitable insulating lid.
• must be protected from direct sunlight and may not be set up near heat
sources.
Safety and occupational health instructions
• may not be transported in vehicles in filled state.
• must be protected from impact, knocks and rapid movements.
• Ventilate all installation rooms constantly and appropriately.
• Wear protective clothing (suitable gloves, goggles or face protection and
safety shoes).
• Check the oxygen content of the room constantly.
• Always carry an oxygen metre.
• Only trained personnel may work with liquid nitrogen.
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This list is not complete.
3.3.4 General conduct in the case of an accident
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In the case of an accident from oxygen deficiency the following regulations should
be observed.
• Secure the surrounding area to avoid any subsequent accidents.
• Act quickly.
• The rescuers must take measures to protect themselves (respiratory
protection device).
• Move the injured persons from the hazardous area.
• Observe the company instructions for emergencies.
• Ventilate the rooms affected sufficiently.
• Investigate the cause of the accident.
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This list is not complete.
3.4 Cryogenic burns
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Liquid nitrogen is very cold (-196° C).
The surfaces of vessels that were in contact in liquid nitrogen (in particular during
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3.4.1 Dangers
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the filling process) may cause skin burns on contact.
Cryogenic liquids may:
– bring about burns to the human body
– make specific materials (metal and plastic) that are not suitable for low
temperatures brittle
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– generate strong misting depending on atmospheric humidity
3.4.2 Causes
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There are two types of cryogenic burns:
3.4.2.1 Burns through splashes
When handling samples and in general when handling liquid nitrogen, personnel
must protect themselves from splashes. They can cause cryogenic burns with
serious consequential damage, in particular to eyes and face.
13
Safety and occupational health instructions
3.4.2.2 Burns through contact
Contact of the skin with cold material causes frostbite or cryogenic burns.
The interior of vessels or the samples may never be touched or held with bare
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3.4.3 Recommendations
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hands.
In order to prevent the danger of burning the following points must be observed:
• Never bring cryogenic liquids in contact with the skin.
• Never touch the cold non-isolated or iced walls of a vessel.
• Wear personal protective equipment (suitable gloves, goggles or face
protection and safety shoes).
• Keep the vessel upright.
• Use suitable material (e.g. metal hose or PTFE hose) to refill.
• Train personnel.
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This list is not complete.
3.4.4 General rules of conduct for splashes with liquid nitrogen
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3.4.4.1 To the eyes
• Rinse eyes with much water for 15 min.
• Follow the company instructions for emergencies.
• Consult a doctor
3.4.4.2 On the skin
• Do not rub.
• If possible remove or loosen clothing.
• Slowly and gradually warm the parts affected.
• Do not apply anything to the burnt area.
• Follow the company instructions for emergencies.
• Consult a doctor.
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Both lists are not complete.
3.5 Danger of explosion
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3.5.1 Dangers
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3.5.2 Causes
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The evaporation of liquid nitrogen may lead to an overpressure in the vessel.
An increase in the vessel may be attributable to:
14
– incorrect set-up (use of a closable lid)
– icing on the neck and on the insulating lid
Safety and occupational health instructions
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This list is not complete.
3.5.3 Recommendations
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To avoid the danger of explosion:
• Always use suitable insulating lids (pay attention to waste gas opening).
• Observe filling levels to avoid the formation of ice on the insulating lid.
• Set up the vessel in dry and roofed rooms.
• Monitor atmospheric humidity in the installation room.
• Check vessel regularly for the collection of condensed water.
• Check vessel regularly for damage to surface or material damage
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This list is not complete.
3.5.4 General conduct in the case of an accident
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In the case of an accident from oxygen deficiency the following regulations should
be observed.
• Secure the surrounding area to avoid any subsequent accidents.
• Act quickly.
• The rescuers must take measures to protect themselves (respiratory
• Move the injured persons from the hazardous area.
• Observe the company instructions for emergencies.
• Ventilate the rooms affected sufficiently.
• Investigate the cause of the accident.
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This list is not complete.
3.6 Oxygen enrichment
Pos: 5.38 /00005 Überschriften/1.1.1 Ü berschriften/111 D ewar Gefahr en @ 0\mod_ 1233906093088 _9.doc @ 5946 @ @ 1
3.6.1 Dangers
Pos: 5.39 /00010 Bedienungsanleitungen K apitelsammlung en/CryoMil l/0020 Cryo Sic herheitskapitel/Cr yo Kapitel Kr yo Sauerstoffanr eicherung Gefa hren @ 0\ mod_1233907417 378_9.doc @ 6113 @ @ 1
Pos: 5.40 /00005 Überschriften/1.1.1 Ü berschriften/111 D ewar Ursac hen @ 0\mod_ 12339061241 98_9.doc @ 5952 @ @ 1
3.6.2 Causes
Pos: 5.41 /00010 Bedienungsanleitungen K apitelsammlung en/CryoMill/0 020 Cryo Sic herheitskapitel/Cr yo Kapitel Kryo Sauerstoffanr eicherung Urs achen @ 0\ mod_123390741 7863_9.doc @ 6120 @ @ 1
Pos: 5.42 /00005 Überschriften/1.1.1 Ü berschriften/111 D ewar Empf ehlungen @ 0\m od_12339061 48542_9.doc @ 5 958 @ @ 1
3.6.3 Recommendations
Pos: 5.43 /00010 Bedienungsanleitungen K apitelsammlung en/CryoMill/0 020 Cryo Sic herheitskapitel/Cr yo Kapitel Kryo Sauerstoffanr eicherung E mpfehlungen @ 0 \mod_123390 7418394_9.d oc @ 6127 @ @ 1
Oxygen enrichment may increase the danger of explosion and fire.
Oxygen may be condensed from the air if liquid nitrogen is used and similarly be
liquefied because the boiling point of oxygen (approx. -183° C) is above that of
nitrogen (-196° C).
The following points must be considered in the case of oxygen enrichment:
protection device).
• Do not smoke.
• Where possible, keep easily inflammable materials away from the vessel.
15
Safety and occupational health instructions
• Remove all sources of fire (naked flame and light, spark producers, matches,
lighters etc.).
• Ventilate installation rooms constantly and appropriately.
• Clean floor regularly.
• Train personnel.
• Wear personal protective equipment.
• Check oxygen content constantly.
• Always carry an oxygen metre.
Pos: 5.44 /00005 Überschriften/1.1 Übersc hriften/1.1 Übersc hriften Dewar/ 11 Dewar U mgebung des Gerä tes @ 0\m od_123375219 5937_9.doc @ 5 722 @ @ 1
This list is not complete
3.7 Surrounding area of the machine
Pos: 5.45 /00005 Überschriften/1.1.1 Ü berschriften/ 111 Dewar Räu mlichkeiten @ 0\m od_123390671 2889_9.doc @ 5976 @ @ 1
3.7.1 Rooms
Pos: 5.46 /00010 Bedienungsanleitungen K apitelsammlung en/CryoMill/0 020 Cryo Sic herheitskapitel/Cr yo Kapitel Kryo U mgebung Räu mlichkeiten @ 0\mod_12 33907185424_9.d oc @ 6057 @ @ 1
The room in which the machine is located must:
• permit operation without danger to the employees
• have a constantly running and appropriate ventilation system
• have a level and non-porous floor that is also able to bear the load of the
vessel
• have safety datasheets on liquid nitrogen visible for all to see
• prevent unauthorised access
• permit the safe filling of the vessel
• permit accessibility to the vessel for inspection, cleaning and maintenance
Pos: 6.1 /00010 Bedienungsanleitungen Kapitelsammlung en/------- Seitenumbruch ----------- @ 0\mod_12223443 73758_0.doc @ 2386 @ @ 1
This list is not complete.
16
Operating the machine
V1
PSV
CSV
DM
FA
V3
V2
FA
CSV
PSV
ZF
V3
VV
DM
V1
V2
ZF
KS
KS
SA
SA
Pos: 6.2 /00005 Überschriften/1. Überschri ften/1 Bedie nung des Gerätes @ 0\mod_ 12265658802 11_9.doc @ 3519 @ @ 1
4 Operating the machine
Pos: 6.3 /00010 Bedienungsanleitungen Kapitelsammlung en/CryoMill/ 0016 LN2 Dewar 5 0l/1607 Modul D ewar 50l Beschrei bung @ 2\mod_12677 85565238_9.d oc @ 18900 @ @ 1
The APOLLO ® vessel is a vacuum super-insulated pressure vessel made of
corrosion-resistant stainless steel for storing refrigerated liquid nitrogen in
conformance to the European Pressure Equipment Directive 97/23/EG, Category I
Pos: 6.4 /00005 Überschriften/1.1 Üb erschriften/1.1 Ü berschriften BDA/ 11 Ansichten des Gerätes @ 0\ mod_122899 0581782_9.doc @ 4966 @ 2 @ 1
4.1 Views of the Instrument
Pos: 6.5 /00010 Bedienungsanleitungen Kapitelsammlung en/CryoMill/ 0016 LN2 Dewar 5 0l/1601 Modul Dewar 50l A nsichten der Ger äteteile @ 2\ mod_1267688 670954_9.doc @ 18820 @ @ 1
module A, with CE marking.
Fig. 2: Front view
Fig. 3: Rear view
Pos: 6.6 /00010 Bedienungsanleitunge n Kapitelsamml ungen/------- Seitenumbruch ----------- @ 0\mod_12223443 73758_0.doc @ 2386 @ @ 1
17
Operating the machine
Element
Description
Function
V1
Withdrawal valve
Valve for taking out liquid nitrogen
V2
Pressure build-up valve
Valve for building up working pressure quickly
V3
Waste gas valve
Valve for draining liquid nitrogen
CSV
Overflow valve
Safety valve for the feed line to the CryoMill
DM
Pressure indicator
Gas pressure display
PSV
Dewar flask pressure relief valve
KS
Quick-release clamp
Sealing and attachment of the siphon to the Dewar
flask.
VV
Vacuum closure and safety device
Sealing of high vacuum in the intermediate hollow
space
ZF
Withdrawal hose
Liquid nitrogen supply line to the CryoMill
FA
Level display
Shows the liquid nitrogen level
Pos: 6.7 /00005 Überschriften/1.1 Überschrif ten/1.1 Übers chriften BDA/1 1 Übersichtstab elle der Geräteteile @ 0\mo d_122899061 6846_9.doc @ 4 972 @ @ 1
4.2 Overview table of the parts of the device
Pos: 6.8 /00010 Bedienungsanleitungen Kapitelsammlung en/CryoMill/ 0016 LN2 Dewar 5 0l/1602 Modul D ewar 50l Ü bersichtstabelle der Geräteteile @ 2\mod_12 67691643620_ 9.doc @ 1882 7 @ @ 1
Safety valve 1.3 bar of the Dewar flask
Pos: 6.9 /00010 Bedienungsanleitunge n Kapitelsam mlungen/------- Seitenumbr uch ----------- @ 0\mod_1222344373758_ 0.doc @ 2386 @ @ 1
18
Operating the machine
Overall height:
80cm
Outside diameter:
50cm
Overall width:
76cm
Immersion depth
58.5cm
Neck diameter:
5.0cm
Weight empty:
44kg
Weight full:
85 kg
Geometrical capacity:
49.5 litres
Stat. rate of evaporation:
2% / day
Operating pressure:
max. 1.3 bar
WARNING
CAUTION
Pos: 6.10 /00005 Überschriften/1.1 Übersc hriften/1.1 Übersc hriften BDA/ 11 Technische Da ten @ 0\ mod_12223445 69224_9.doc @ 2470 @ @ 1
4.3 Technical Data
Pos: 6.11 /00010 Bedienungsanleitungen K apitelsammlung en/CryoMill/0 016 LN2 De war 50l/1611 Mod ul Dewar 50l Tech nische Date n @ 2\mod _1268230808 121_9.doc @ 1895 0 @ @ 1
Type: APOLLO® 50
Pos: 6.12 /00005 Überschriften/1.1 Übersc hriften/1.1 Übersc hriften BDA/ 11 Vakuumversc hluss und Sich erheitseinricht ung @ 2\m od_1268297292 227_9.doc @ 1 8970 @ @ 1
4.4 Vacuum closure and safety device
Pos: 6.13 /00010 Bedienungsanleitungen K apitelsammlu ngen/CryoMill/0 016 LN2 De war 50l/1613 Mod ul Dewar 50l V akuumverschluss u nd Sich erheitseinrichtung @ 2\mod_12 68297689386_ 9.doc @ 1897 7 @ @ 1
Pos: 6.14 /00005 Überschriften/1.1 Übersc hriften/1.1 Übersc hriften BDA/ 11 Füllstandsanz eige @ 2\ mod_1268300 595137_9.doc @ 18991 @ @ 1
4.5 Level Display
Pos: 6.15 /00010 Bedienungsanleitungen K apitelsammlung en/CryoMil l/0016 LN2 D ewar 50l/1614 Mo dul Dewar 50l Füllstandskurve Apollo ® 50 @ 2 \mod_1268 298441800_9.d oc @ 18984 @ @ 1
Fig. 3: Vacuum closure and safety device
The vacuum closure and the safety device protect the vacuum space from positive
pressure . Only the manufacturer’s qualified staff may conduct the re-evacuation .
The protective cap (2) retains the valve insert (1) if excessive pressure builds up in
the vacuum space.
• Do not remove the protective cap (2).
• Protect the valve from heat or cooling because embrittlement can lead to the loss
of operating vacuum.
19
Operating the machine
Fig. 4: Level Display
Determination of the level in the vessel
• Read the Dewar flask level on the scale in the level display.
• Alternatively, you can use a dipstick to determine the level and compare it
The black area on the level display scale marks 25% of the remaining contents.
Pos: 6.16 /00005 Überschriften/1.1 Übersc hriften/1.1 Übersc hriften BDA/ 11 Füllen des B ehälters @ 2 \mod_126777 4868556_9.d oc @ 18870 @ @ 1
Fig. 5: Level curve Apollo ® 50
4.6 Filling the vessel
Pos: 6.17 /00010 Bedienungsanleitung en Kapitelsam mlungen/CryoMill /0016 LN2 De war 50l/1603 Mo dul Dewar 50l B efüllen @ 2\ mod_1267698 001736_9.doc @ 1 8834 @ @ 1
• Close all valves. (V1, V2, V3)
with the level curve (see picture of Apollo® 50 level curve).
20
• Take the withdrawal hose (ZF) off the connection (SA).
• Attach the filling line to the connection (SA).
• Open the waste gas / overflow valve (V3).
• Open the withdrawal valve (V1).
• Fill the Dewar flask until liquid nitrogen comes out of the waste gas /
overflow valve (V3).
• Close the withdrawal valve (V1).
Operating the machine
CAUTION
Risks of liquid or gaseous nitrogen
Positive pressure in the vessel
– The introduction of energy during transport can cause a sudden surge in
pressure. Nitrogen is blown off then and this can cause a lack of oxygen,
cryogenic burns, oxygen enrichment and associated risks.
• Make sure the vessel is depressurised before you transport it,
• Remove the siphon and put in the transport plugs.
• Transport the vessel only in an upright position.
• Avoid impacts and vibrations.
• Secure the vessel against falling down, rolling away and damage.
DM
Pos: 6.18 /00005 Überschriften/1.1 Übersc hriften/1.1 Übersc hriften BDA/ 11 Druckaufbau @ 1\mod _1240400926229 _9.doc @ 824 0 @ @ 1
• Close the waste gas / overflow valve (V3).
4.7 Pressure build-up
Pos: 6.19 /00010 Bedienungsanleitungen K apitelsammlung en/CryoMil l/0016 LN2 D ewar 50l/1604 Mo dul Dewar 50l Druckaufbau @ 2 \mod_1267 701477789_9.d oc @ 18841 @ @ 1
• Close the withdrawal valve (V1) and the waste gas / overflow valve (V3).
• Open the pressure build-up valve (V2).
• Watch the pressure indicator (DM).
• Close the pressure build-up valve (V2) as soon as the needle reaches the
red marking or nitrogen comes out of the pressure relief valve (PSV).
Pos: 6.20 /00005 Überschriften/1.1 Übersc hriften/1.1 Übersc hriften BD A/11 Entnahm e von Flüssigstic kstoff @ 2\ mod_126777495 7314_9.doc @ 18 877 @ @ 1
Fig. 6: Pressure gauge
4.8 Withdrawal of liquid nitrogen
Pos: 6.21 /00010 Bedienungsanleitungen K apitelsammlung en/CryoMill/0 016 LN2 De war 50l/1605 Mod ul Dewar 50l Entnahme Flüssi gstickstoff @ 2 \mod_1267 709072517_9.d oc @ 18855 @ @ 1
• Attach the liquid nitrogen line to the CryoMill and to the connection (SA).
Pos: 6.22 /00005 Überschriften/1.1 Übersc hriften/1.1 Übersc hriften BDA/ 11 Druckentl astung @ 2\ mod_1267777113 490_9.doc @ 18891 @ @ 1
4.9 Pressure relief
Pos: 6.23 /00010 Bedienungsanleitungen K apitelsammlung en/CryoMil l/0016 LN2 D ewar 50l/1606 Mo dul Dewar 50l Dr uckentlastung @ 2\mod_1 267709470983_9. doc @ 18862 @ @ 1
Pos: 6.24 /00005 Überschriften/1.1 Übersc hriften/1.1 Übersc hriften BDA/ 11 Transport @ 0\mod_1 226495164391_ 9.doc @ 3398 @ 2 @ 1
4.10 Transport
Pos: 6.25 /00004 Warnhinweise/V0019 VOR SICHT Überdr uck im Behält er - Gefärdu ng durch LN2 @ 2\mod_126 7775099915_9.doc @ 18884 @ @ 1
• Open the filling and withdrawal valve (V1).
• After taking the liquid, close the filling and withdrawal valve (V1) again.
• Close the pressure build-up valve (V2).
• Open the waste gas valve (V3).
Pos: 6.26 /00005 Überschriften/1. Überschrif ten/1 Prüfa nweisungen @ 1 \mod_1245 230896441_9.d oc @ 11114 @ @ 1
Pos: 6.27 /00010 Bedienungsanleitungen K apitelsammlung en/CryoMill/0 016 LN2 De war 50l/1612 Mod ul Dewar 50l Verb oten ist die An wendung f olgender Mittel und @ 2\ mod_126823154047 3_9.doc @ 18 957 @ @ 1
It is impermissible to use the following agents and tools:
• pliers
• striking tools
21
Operating the machine
• lubricating spray
• hemp
• open flame
• steam
• leak detection spray
• suds
Pos: 6.28 /00010 Bedienungsanleitungen K apitelsammlung en/CryoMill/0 016 LN2 De war 50l/1610 Mod ul Dewar 50l Prüfu ngen des Sich erheitsve ntiles @ 2\mod_ 126780050589 5_9.doc @ 18 921 @ @ 1
Only the bubble method outlined below may be used to test that the safety valve is
securely in place and has the correct response pressure. This prevents the valve
mechanics becoming dirty and rusty . The response pressure is marked on the
safety valve.
4.11 Admitting the test pressure
Use a suitable test device to introduce the test pressure. Where the safety valves
are not to be removed, the vessel’s inherent pressure is used for the test.
Do not conduct the tests with oxygen or inflammable or corrosive gases.
4.12 Checking the seat tightness
Increase the test pressure to 90% of the response pressure. The valve must
remain leak-tight.
4.13 Checking the response pressure
Slowly increase the test pressure to 100%. The safety valve blows off. The
=== Ende der Liste für Textmarke Inhalt ===
response pressure can deviate from the nominal level by +/- 10%.
22
5 Index
A
Article number ..................................................... 10
B
Barcode............................................................... 10
Bubble method .................................................... 22
C
Causes ............................................. 12, 13, 14, 15
CE marking ......................................................... 10
Changes ............................................................... 5
Confirmation ......................................................... 9
Copyright .............................................................. 5
Cryogenic burns .................................................. 13
D
Danger of explosion ............................................ 14
Dangers ........................................... 12, 13, 14, 15
Description .......................................................... 18
L
Level display ...................................................... 20
Level Display ...................................................... 19
Levels in the vessel ............................................ 20
M
Manufacturer’s address ..................................... 10
Moderate or mild injury ........................................ 6
N
Neck diameter .................................................... 19
Nominal level ..................................................... 22
Notes on the Operating Manual ........................... 5
O
Operating pressure ............................................ 19
Operating the machine....................................... 17
Outside diameter ................................................ 19
Overall height ..................................................... 19
Dirt ...................................................................... 22
E
Explanations of the safety warnings ..................... 6
F
Filling the vessel ................................................. 20
Front view ........................................................... 17
Function .............................................................. 18
G
General ............................................................... 11
General conduct in the case of an accident . 13, 15
General rules of conduct for splashes with liquid
nitrogen ........................................................... 14
General safety instructions ................................... 7
Geometrical capacity .......................................... 19
I
Immersion depth ................................................. 19
Inherent pressure ................................................ 22
Instrument name ................................................. 10
Overall width ...................................................... 19
Overview table of the parts of the device........... 18
Oxygen deficiency .............................................. 12
Oxygen enrichment ............................................ 15
P
Positive pressure ............................................... 19
Pressure build-up ............................................... 21
Pressure gauge .................................................. 21
Pressure relief .................................................... 21
Prohibited agents ............................................... 22
Prohibited tools .................................................. 22
property damage .................................................. 6
R
Rear view ........................................................... 17
Recommendations ................................. 12, 14, 15
Re-evacuation .................................................... 19
Repairs ................................................................. 8
Response pressure ............................................ 22
23
Rooms................................................................. 16
Rust ..................................................................... 22
S
Safety and occupational health instructions ....... 10
Safety instructions on the handling of liquid
nitrogen ........................................................... 12
Safety warnings .................................................... 6
Seat tightness ..................................................... 22
Serial number ..................................................... 10
serious injury ......................................................... 6
Service Address .................................................... 8
Static rate of evaporation .................................... 19
Surrounding of the machine ............................... 16
T
Target group ......................................................... 7
Technical Data .................................................... 19
Test device ......................................................... 22
Test pressure ...................................................... 22
Transport ............................................................ 21
Type ................................................................... 19
type plate description ........................................... 9
Type plate marking ............................................ 10
V
Vacuum closure and safety device .................... 19
Vacuum closure and safety device .................... 19
Vacuum space ................................................... 19
Valve mechanics ................................................ 22
Views of the Instrument ..................................... 17
W
Waste disposal marking ..................................... 10
Weight empty ..................................................... 19
Weight full .......................................................... 19
Withdrawal of liquid nitrogen .............................. 21
Y
Year of manufacture .......................................... 10
24
25
Copyright
® Copyright by
Retsch GmbH
Haan, Retsch-Allee 1-5
D-42781 Haan
Federal Republic of Germany
28
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