Retsch Cryomill User Manual
Manual
Mixer Mill CryoMill
Translation
© Retsch GmbH, 42781 Haan, Retsch-Allee 1-5, Germany 13.03.2013 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 ............................................................................................................ 6
1.1 Explanations of the safety warnings .................................................................................................. 7
1.2 General safety instructions ................................................................................................................ 8
1.3 Repairs ............................................................................................................................................... 9
2 Confirmation ......................................................................................................................................... 10
3 Technical data ....................................................................................................................................... 11
3.1 Protective equipment ....................................................................................................................... 11
3.2 Emissions......................................................................................................................................... 11
3.3 Degree of protection ........................................................................................................................ 12
3.4 Rated power .................................................................................................................................... 12
3.5 Dimensions and weight .................................................................................................................... 12
3.6 Required floor space ........................................................................................................................ 12
4 Transport, scope of delivery, installation .......................................................................................... 13
4.1 Packaging ........................................................................................................................................ 13
4.2 Transport.......................................................................................................................................... 13
4.3 Temperature fluctuations and condensed water ............................................................................. 13
4.4 Conditions for the place of installation ............................................................................................. 13
4.5 Installation of the machine ............................................................................................................... 14
4.6 Removing the transport safeguard .................................................................................................. 14
4.7 Type plate description ...................................................................................................................... 18
4.8 Electrical connection ........................................................................................................................ 19
4.9 Connecting the cooling agent feed .................................................................................................. 19
4.10 Removing the liquid nitrogen feed line ............................................................................................ 23
4.11 Cold air outlet ................................................................................................................................... 24
4.12 Mounting the exhaust hose.............................................................................................................. 24
5 Operating the machine ........................................................................................................................ 26
5.1 Use of the machine for the intended purpose.................................................................................. 26
5.2 Operating elements and displays .................................................................................................... 27
5.3 Summary table of device parts ........................................................................................................ 28
5.4 Operating elements and displays .................................................................................................... 29
5.5 Inserting the grinding jar .................................................................................................................. 31
5.5.1 Inserting and removing CryoMill special grinding jar ................................................................... 31
5.5.2 Inserting the cooling jacket sealing plug ...................................................................................... 34
5.5.3 Insert the adapter for 4/2 x 5 ml grinding jar ................................................................................ 35
5.5.4 Insert the adapter for 6 / 4 / 2 x 2-ml Eppendorf reaction vial ..................................................... 36
5.6 Explanations of the grinding cycles ................................................................................................. 37
5.6.1 Grinding without cooling .............................................................................................................. 37
5.6.2 Grinding with cooling ................................................................................................................... 37
3
5.7 Programs ......................................................................................................................................... 38
5.7.1 Grinding without program ............................................................................................................ 38
5.7.2 Grinding with program ................................................................................................................. 39
5.7.2.1 Selection of a program ......................................................................................................... 39
5.7.2.2 Display of the program grinding parameters ....................................................................... 39
5.7.2.3 Create/change a program .................................................................................................... 39
5.7.2.4 Delete program .................................................................................................................... 40
5.8 Setting grinding cycles ..................................................................................................................... 40
5.9 Setting the precooling time .............................................................................................................. 41
5.9.1 Precooling with definable precooling time ................................................................................... 41
5.9.2 Automatic precooling ................................................................................................................... 41
5.10 Setting the grinding time .................................................................................................................. 42
5.11 Setting the duration of intermediate cooling .................................................................................... 42
5.12 Setting the grinding frequency ......................................................................................................... 43
5.13 Starting the grinding process ........................................................................................................... 43
5.14 Interrupting and continuing the grinding process ............................................................................ 44
5.14.1 Pausing grinding ...................................................................................................................... 44
5.14.2 Cancelling grinding .................................................................................................................. 44
5.15 Stopping the grinding process ......................................................................................................... 44
5.16 Operating hours display ................................................................................................................... 45
5.17 Operating software display .............................................................................................................. 46
5.18 Replacing the machine fuses........................................................................................................... 46
6 Working instructions............................................................................................................................ 48
6.1 General ............................................................................................................................................ 48
6.2 The grinding process ....................................................................................................................... 48
6.3 Quantities of sample material and feed sizes .................................................................................. 48
6.4 Working instructions ........................................................................................................................ 49
7 Safety functions and fault display ...................................................................................................... 50
7.1 Fault messages ............................................................................................................................... 50
8 Cleaning, wear and service ................................................................................................................. 51
8.1 Cleaning ........................................................................................................................................... 51
8.2 Wear ................................................................................................................................................ 51
8.3 Wearing parts .................................................................................................................................. 51
8.4 Service ............................................................................................................................................. 51
8.5 Checks ............................................................................................................................................. 52
9 Safety and occupational health instructions ..................................................................................... 52
9.1 General ............................................................................................................................................ 52
9.2 Safety instructions on the handling of liquid nitrogen ...................................................................... 54
9.3 Oxygen deficiency ........................................................................................................................... 54
4
9.3.1 Dangers ....................................................................................................................................... 54
9.3.2 Causes ......................................................................................................................................... 54
9.3.3 Recommendations ....................................................................................................................... 54
9.3.4 General conduct in the case of an accident ................................................................................ 55
9.4 Cryogenic burns ............................................................................................................................... 55
9.4.1 Dangers ....................................................................................................................................... 55
9.4.2 Causes ......................................................................................................................................... 55
9.4.2.1 Burns through splashes ....................................................................................................... 55
9.4.2.2 Burns through contact .......................................................................................................... 56
9.4.3 Recommendations ....................................................................................................................... 56
9.4.4 General rules of conduct for splashes with liquid nitrogen .......................................................... 56
9.4.4.1 To the eyes .......................................................................................................................... 56
9.4.4.2 On the skin ........................................................................................................................... 56
9.5 Danger of explosion ......................................................................................................................... 56
9.5.1 Dangers ....................................................................................................................................... 56
9.5.2 Causes ......................................................................................................................................... 56
9.5.3 Recommendations ....................................................................................................................... 57
9.5.4 General conduct in the case of an accident ................................................................................ 57
9.6 Oxygen enrichment .......................................................................................................................... 57
9.6.1 Dangers ....................................................................................................................................... 57
9.6.2 Causes ......................................................................................................................................... 57
9.6.3 Recommendations ....................................................................................................................... 57
9.7 Surrounding area of the machine .................................................................................................... 58
9.7.1 Rooms .......................................................................................................................................... 58
10 Disposal ................................................................................................................................................. 59
11 Index ...................................................................................................................................................... 60
Appendix ............................................................................................................................... following pages
5
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.
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.
6
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
Pos: 2.3 /00003 Standard Kapitel/General Modul Warnhinweise Erklärung neu @ 0\ mod_1234858329746_9.doc @ 6190 @ @ 1
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
7
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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8
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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9
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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10
Technical data
Receptacle:
1 50ml steel grinding jar
Grinding component:
1 25mm steel ball each
Feed material:
Quartz gravel particles approx. 4.0 – 6.0mm
Feed quantity:
8ml
Frequency:
30 Hz
Receptacle:
4 5ml steel grinding jar
Grinding component:
2 8mm tungsten carbide balls each
Feed material:
Quartz gravel particles approx. 1.0 – 1.5mm
Feed quantity:
1.5ml
Frequency:
30 Hz
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3 Technical data
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3.1 Protective equipment
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The grinding chamber of the CryoMill laboratory mill is surrounded by a stable
hood.
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3.2 Emissions
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It is only possible to start the device when the hood is closed.
Noise values:
The noise values are also influenced by the properties of the sample material.
No-load operation:
Emission value with regard
to workplace L
Example 1:
Emission value with regard
to workplace L
Operating conditions:
= 61,4 dB(A)
pAeq
= 75,2 dB(A)
pAeq
Example 2:
Emission value with regard
to workplace L
= 66,3 dB(A)
pAeq
Operating conditions:
11
Technical data
CAUTION
Hearing loss
A high sound level may occur depending on the type of material, the
number of balls used, the set grinding frequency and the grinding time.
– Excess noise in terms of intensity and duration can lead to
impairments or permanent damage to hearing.
• Ensure you take suitable soundproofing measures or wear
hearing protection.
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3.3 Degree of protection
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IP30
3.4 Rated power
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260 watts
3.5 Dimensions and weight
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Height : 370 to approx. 630 mm with open hood
Width: 385 mm
Depth: 570 mm
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Weight: approx. 46 kg without grinding jar
3.6 Required floor space
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Supporting surface: 500 mm x 650 mm
12
Transport, scope of delivery, installation
NOTICE
Storage of packaging
– In the event of a complaint or return, your warranty claims may be
endangered if the packaging is inadequate or the machine has not been
secured correctly.
• Please keep the packaging for the duration of the warranty period.
NOTICE
Transport
– Mechanical or electronic components may be damaged.
• The machine may not be knocked, shaken or thrown during
transport.
NOTICE
Temperature fluctuations
The machine may be subject to strong temperature fluctuations during transport
(e.g. aircraft transport)
– The resultant condensed water may damage electronic components.
• Protect the machine from condensed water.
NOTICE
Ambient temperature
– Electronic and mechanical components may be damaged and the
performance data alter to an unknown extent.
• Do not exceed or fall below the permitted temperature range of the
machine (5°C to 40°C / ambient temperature).
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4 Transport, scope of delivery, installation
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4.1 Packaging
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The packaging is designed for the transport route. It corresponds to generally
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4.2 Transport
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acceptable packaging guidelines.
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4.3 Temperature fluctuations and condensed water
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4.4 Conditions for the place of installation
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Atmospheric humidity:
Maximum relative humidity 80% at temperatures up to 31°C, decreasing linearly up
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to 50% relative humidity at 40°C
13
Transport, scope of delivery, installation
NOTICE
Atmospheric humidity
– Electronic and mechanical components may be damaged and the
performance data alter to an unknown extent.
• Do not exceed the admissible range for atmospheric humidity.
NOTICE
Property damage
A very cold vapour plume escapes from the nitrogen gas outlet.
– The vapour plume can greatly cool objects. This is why the humidity in the
air condenses.
• The area above the nitrogen gas outlet (B) up to the ceiling must be
kept free.
NOTE
Installation
– Depending on the operating status of the mill, there may be slight
vibrations.
• Place the mill on an even, flat and balanced supporting surface only.
The supporting surface must be stable and must not vibrate.
NOTICE
Installation of the machine
– It must be possible to disconnet the machine from the mains at any time.
• Install the machine such that the connection for the mains cable is
easily accessible.
NOTICE
Transport safeguard
– Components may be damaged.
• Operate the machine only without the transport safeguard or
transport the machine only with transport safeguard.
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4.5 Installation of the machine
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Installation height: maximum 2000 m above sea level
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4.6 Removing the transport safeguard
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• Place the device on a stable table.
• Pull the device carefully beyond the edge of the table in order to be able to
14
reach the screw (TA).
Transport, scope of delivery, installation
TA
TB
TL1
TL1
Fig. 1: Removing the transport bracket
• Remove the screw (TA) using an Allen key.
Fig. 2:
• Pull the device into the position shown in order to be able to remove
the screw (TB).
• Remove the second screw (TB) and remove the transport bracket
(TL1).
NOTICE
Keep the transport brackets, screws and transport lock for future transport!
15
Transport, scope of delivery, installation
R
F1 U TL2
Fig. 3: Pulling out the condensation collecting filter
• Pull the condensation collecting filter (R) completely out of the device.
• Remove the opening aids (F1) on the side on which you have removed the
transport bracket (TL1).
• Place a soft, clean mat (U) next to the device.
• Tilt the device onto the side on which the transport bracket (TL1)
has been removed.
16
Fig. 4: Tilting the device onto its side
Transport, scope of delivery, installation
TS
TC
TD
TL2
The transport lock (TS), which is labelled with an arrow, is situated on the
underneath of the device.
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Fig. 5: Removing the transport lock
• Loosen and remove the screw (TS).
• Unscrew the two screws (TC) and (TD).
• Remove the transport bracket (TL2).
Fig. 6:
• Re-insert the condensation collecting filter (R).
NOTICE
Keep the transport brackets, screws and transport lock for future transport!
17
Transport, scope of delivery, installation
1 2 3 4 5 6 7 8 9
10
11
12
14
13
GL
Fig. 7: Grip
A grip (GL) is situated underneath both sides of the device
Pos: 5.24.1 /00005 Überschriften/1.1 Ü berschriften/1.1 Überschriften BDA/11 Type nschild Beschreibung @ 3\mod_128093 3953941_9.doc @ 22302 @ 2 @ 1
• Use the grip (GL) to move the device.
4.7 Type plate description
Pos: 5.24.2 /00003 Standard Kapitel/Gen eral Modul Typenschild @ 3\mod_1280 931092443_9.doc @ 22278 @ @ 1
Fig. 8: Type plate lettering
1 Device designation
2 Year of production
3 Part number
4 Serial number
5 Manufacturer’s address
6 CE marking
7 Disposal label
8 Bar code
9 Power version
10 Mains frequency
18
Transport, scope of delivery, installation
WARNING
WARNING
Risk of a fatal electric shock
- An electric shock can cause injuries in the form of burns and cardiac
arrhythmia, respiratory arrest or cardiac arrest.
• Do not clean the blender under running water. Use only a cloth dampened
with water.
• Disconnect the power supply plug before cleaning the blender.
NOTICE
Electrical connection
– Mechanical or electronic components may be damaged.
• Please observe the information on the type plate.
11 Capacity
12 Amperage
13 Number of fuses
14 Fuse type and fuse strength
In the case of questions please provide the device designation (1) or the part
Pos: 5.25 /00005 Überschriften/1.1 Übersc hriften/1.1 Überschriften BDA/11 Elektrisc her Anschluss @ 0\mod_122656506 7445_9.doc @ 3500 @ 2 @ 1
number (3) and the serial number (4) of the device.
4.8 Electrical connection
Pos: 5.26 /00003 Standard Kapitel/Gen eral Modul Elektrischer Anschluss @ 0\ mod_1228918538521_9.doc @ 4731 @ @ 1
When connecting the power cable to the mains supply, use an external fusethat
complies with the regulations applicable to the place of installation .
• Please check the type plate for details on the necessary voltage and
frequency for the device.
• Make sure the levels agree with the existing mains power supply.
• Use the supplied connection cable to connect the device to the mains power
Pos: 5.27 /00010 Bedienungsanleitungen K apitelsammlungen/CryoMill II/0006 Tra nsport, Lieferumfang und Aufstellen /CryoMil l II Modul externe Absicherung @ 5\mod_1343829054956_9.doc @ 33059 @ @ 1
Pos: 5.28 /00004 Warnhinweise/W0002 WARNUNG Kabelbruch Stromstoß @ 2\mod_1278055276120_9.doc @ 20557 @ @ 1
supply.
The external fuse must be at least T6.3A (230V) T8A (100/120V).
Pos: 5.29 /00004 Warnhinweise/H0008 HIN WEIS Elektrischer Anschluss @ 0\ mod_1228918882424_9.doc @ 4781 @ @ 1
Pos: 5.30 /00005 Überschriften/1.1 Ü berschriften/1.1 Überschriften BDA/11 Kü hlmittelzufluss anschließen @ 0\mod_122690 8410419_9.doc @ 3576 @ @ 1
4.9 Connecting the cooling agent feed
Pos: 5.31 /00004 Warnhinweise/H0062 HIN WEIS Risiko der Eisbildung (CryoMill) @ 4\mod_1314082100670_9.doc @ 25 455 @ @ 1
19
Transport, scope of delivery, installation
CAUTION
Blocked pipe
Ice formation
– Ice or impurities can block pipes and thereby cause malfunctions.
• Keep the cooling system and supply pipe dry and free from
impurities.
• Do not insert the grinding jar if it is damp or covered with frost.
• Insert the cooling jacket seal (KA) if you will not be using the device
for a long period.
• Do not operate the device unattended.
Pos: 5.32 /00010 Bedienungsanleitungen K apitelsammlungen/CryoMill II/0006 Tra nsport, Lieferumfang und Aufstellen /002 0 CryoMill II Modul Kühlmantel Abdichtung @ 5\mod_1344926871592_9.doc @ 34 120 @ @ 1
20
Transport, scope of delivery, installation
NOTICE
Damage to the machine
Incorrect cooling agent
– The use of cooling agents other than liquid nitrogen will cause the cooling
system to lose its leak tightness.
• Only liquid nitrogen (LN2) may be used as cooling agent with this
device.
KA
Pos: 5.33 /00010 Bedienungsanleitungen K apitelsammlungen/CryoMill II/0006 Tr ansport, Lieferumfang und Aufstellen /001 8 CryoMill II Modul Schematische Darstell ung des Kühlsystems @ 5\mod_134451 1088330_9.doc @ 33941 @ @ 1
Fig. 9: Cooling jacket seal
Fig. 10: Connecting the cooling agent supply
21
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