Fritsch PULVERISETTE 7 premium line Operating Instructions Manual
Operating instructions
PLANETARY MICRO MILL
PULVERISETTE 7 premium line
Valid starting with: 07.5000/00100
Read the instructions prior to performing any task!
Translation of the original operating instructions
Fritsch GmbH
Milling and Sizing
Industriestraße 8
D - 55743 Idar-Oberstein
Telephone: +49 (0)6784/ 70-0
Fax: +49 (0)6784/ 70-11
Email: info@fritsch.de
Internet: www.fritsch.de
Version 10/2013 Index 020
Certifications and CE conformity
Certifications and CE conformity
Certification
CE Conformity
Fritsch GmbH has been certified by the TÜV-Zertifizierungsgemeinschaft
e.V.
An audit certified that Fritsch GmbH conforms to the requirements of
the DIN EN ISO 9001:2008.
The enclosed Conformity Declaration lists the guidelines the FRITSCH
instrument conforms to, to be able to bear the CE mark.
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Table of contents
Table of contents
Safety information and use........................................................... 8
1
1.1 Requirements for the user..................................................... 8
1.2 Scope of application............................................................... 8
1.2.1 Operating principle............................................................. 9
1.2.2 Drive motor and speed regulation...................................... 9
1.3 Obligations of the operator................................................... 9
1.4 Information on hazards and symbols used in this manual.. 10
1.5 Information on hazards at the device.................................. 13
1.6 Device safety information.................................................... 13
1.7 Protective equipment.......................................................... 15
1.8 Hazardous points................................................................. 16
1.9 Electrical safety.................................................................... 16
1.9.1 General information......................................................... 16
1.9.2 Protection against restart................................................. 17
1.9.3 Overload protection.......................................................... 17
1.9.4 Imbalance detection......................................................... 17
2 Technical data.............................................................................. 18
2.1 Dimensions.......................................................................... 18
2.2 Weight.................................................................................. 18
2.3 Operating noise.................................................................... 18
2.4 Voltage................................................................................. 18
2.5 Current consumption........................................................... 18
2.6 Power consumption............................................................. 18
2.7 Electrical fuses..................................................................... 19
2.8 Material................................................................................ 19
2.9 Final fineness....................................................................... 19
3 Installation................................................................................... 20
3.1 Transport............................................................................. 20
3.2 Unpacking............................................................................ 20
3.3 Setting up............................................................................. 21
3.4 Ambient conditions.............................................................. 22
3.5 Electrical connection............................................................ 22
4 Initial start-up.............................................................................. 24
4.1 Switching on......................................................................... 24
4.2 Function check..................................................................... 24
4.3 Switching off........................................................................ 26
5 Using the device........................................................................... 27
5.1 Safety information............................................................... 27
5.1.1 General information......................................................... 28
5.1.2 Overpressure relief of the grinding bowls........................ 29
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Table of contents
5.1.3 Grinding bowl lid............................................................... 31
5.2 Choice of grinding bowls and grinding balls........................ 31
5.2.1 Useful capacity of the grinding bowls............................... 33
5.2.2 Size of the grinding balls................................................... 33
5.2.3 Number of balls per grinding bowl (independent of the
material quantity)............................................................. 34
5.2.4 Calculated weight of a ball................................................ 35
5.3 Impact of the ball size and the material during grinding..... 35
5.4 Filling quantities of grinding bowls...................................... 36
5.5 Filling the grinding bowl....................................................... 37
5.6 Factors with an impact on grinding..................................... 37
5.6.1 Running time (grinding duration)..................................... 37
5.6.2 Speed................................................................................ 37
5.6.3 Reverse mode................................................................... 37
5.6.4 Number and size of the balls............................................ 38
5.6.5 Weight of the balls (type of material)............................... 38
5.7 Dry grinding.......................................................................... 38
5.8 Wet grinding (grinding in a suspension).............................. 38
5.8.1 The effect of high temperature........................................ 39
5.8.2 Safety measures against an excessively high pressure..... 40
5.9 Handling the grinding bowl.................................................. 41
5.9.1 Design............................................................................... 41
5.9.2 Opening the grinding bowl after a grinding operation..... 41
5.9.3 Closing the grinding bowl.................................................. 42
5.9.4 Inserting the grinding bowl in the grinding bowl holder.. 45
5.9.5 Removing the grinding bowl............................................. 46
5.10 Mass balance..................................................................... 48
5.11 Grinding duration............................................................... 49
5.12 Conducting a grinding operation....................................... 49
5.12.1 Program sequence after switching on............................ 50
5.12.2 Starting grinding at high speed....................................... 53
5.12.3 Overload......................................................................... 54
5.12.4 "Program" menu item..................................................... 54
5.12.5 Saving the current data................................................... 55
5.12.6 Loading the program....................................................... 55
5.12.7 Setting the time control.................................................. 56
5.12.8 Imbalance check............................................................. 57
5.12.9 Switching off................................................................... 59
5.12.10 Cooling the grinding bowl............................................. 59
6 Accessories................................................................................... 60
6.1 Standard gassing lid for grinding with inert gas................... 60
6.1.1 Scope of delivery............................................................... 60
6.1.2 Fitting the gassing lid on the grinding bowl...................... 61
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Table of contents
6.1.3 Hose adapter for grinding bowl gassing............................ 63
6.1.4 Removing the gassing lid in individual steps..................... 64
6.2 Gassing lid with stainless steel, swagelok hose couplings... 66
6.2.1 Scope of delivery / lid design............................................ 67
6.2.2 Fitting the gassing lid on the grinding bowl...................... 67
6.2.3 Hose adapter for grinding bowl gassing............................ 69
6.2.4 Removing the gassing lid in individual steps..................... 70
6.3 EASY GTM Gas Pressure and Temperature Measuring
System..................................................................................
6.3.1 Case contents and system design..................................... 72
6.3.2 Inserting / changing the battery....................................... 73
6.3.3 Configuration of transmitter ID and data transmission
frequency.......................................................................... 75
6.3.4 Installation of the transmission unit on the EASY GTM
bowl.................................................................................. 76
6.3.5 Installation of the receiver board in the P-7 premium
line.................................................................................... 78
6.3.6 Activating EASY GTM......................................................... 79
6.3.7 Entering the temperature limit......................................... 81
6.3.8 Entering the pressure limit............................................... 82
6.3.9 Selecting the operating mode........................................... 83
6.3.10 Deactivating EASY GTM................................................... 83
6.3.11 Cleaning the EASY GTM system...................................... 84
6.3.12 Battery arrangement...................................................... 86
6.4 Special emptying device for grinding bowls......................... 86
6.4.1 Design............................................................................... 87
6.4.2 Handling............................................................................ 87
6.4.3 Cleaning the special emptying device............................... 90
6.5 Compl. counterweight......................................................... 90
6.5.1 Design............................................................................... 91
6.5.2 Handling............................................................................ 91
6.6 Planetary mills - "MillControl" software.............................. 93
7 General and optional settings .................................................... 94
7.1 Standard Operation Procedure............................................ 94
7.1.1 Activating SOP mode......................................................... 95
7.1.2 Deactivating SOP mode..................................................... 95
7.1.3 Deleting SOP mode........................................................... 96
7.2 RFID...................................................................................... 97
7.3 Language change................................................................. 98
7.4 Screen brightness................................................................. 99
7.5 Information........................................................................ 100
7.6 Interfaces........................................................................... 101
7.7 Firmware update................................................................ 102
72
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Table of contents
8 Cleaning...................................................................................... 104
8.1 Grinding elements.............................................................. 104
8.2 Mill..................................................................................... 104
8.2.1 Removing the grinding chamber cover........................... 105
9 Maintenance.............................................................................. 106
Guarantee terms........................................................................ 107
10
11 Exclusion of liability................................................................... 109
12 Safety logbook........................................................................... 111
13 Index........................................................................................... 113
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Safety information and use
1 Safety information and use
Requirements for the user
1.1
This operating manual is intended for persons assigned with operating
and monitoring the Fritsch of the PULVERISETTE 7 premium line. The
operating manual and especially its safety instructions are to be
observed by all persons working on or with this device. In addition, the
applicable rules and regulations for accident prevention at the installation site are to be observed. Always keep the operating manual at the
installation site of the of the PULVERISETTE 7 premium line.
People with health problems or under the influence of medication,
drugs, alcohol or exhaustion must not operate this device.
The of the PULVERISETTE 7 premium line may only be operated by
authorised persons and serviced or repaired by trained specialists. All
commissioning, maintenance and repair work may only be carried out by
technically qualified personnel. Qualified personnel are persons who,
because of their education, experience and training as well as their
knowledge of relevant standards, regulations, accident prevention guidelines and operating conditions, are authorised by those responsible for
the safety of the machine to carry out the required work and are able to
recognize and avoid possible hazards as defined for skilled workers in IEC
364.
In order to prevent hazards to users, follow the instructions in this
manual.
Malfunctions that impair the safety of persons, the of the PULVERISETTE
7 premium line or other material property must be rectified immediately. The following information serves both the personal safety of operating personnel as well as the safety of the products described and any
devices connected to them: All maintenance and repair work may only
be performed by technically qualified personnel.
This operating manual is not a complete technical description. Only the
details required for operation and maintaining usability are described.
Fritsch has prepared and reviewed this operating manual with the
greatest care. However, no guarantee is made for its completeness or
accuracy.
Subject to technical modifications.
1.2 Scope of application
The planetary micro mill, "PULVERISETTE 7 premium line", can be applied
universally for the fast dry or wet grinding of inorganic and organic samples for analysis, quality inspection or material testing.
During the synthesis, the planetary micro mill is for mixing and homogenising dry samples, emulsions or suspensions.
The planetary micro mill "PULVERISETTE 7 premium line" described here
is an equipment item for use in industrial environments.
The device may be used for these purposes only.
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1.2.1 Operating principle
Safety information and use
a Rotation of the grinding bowl
b Centrifugal force
c Rotation of the support disc
The source material is crushed and ground by grinding balls in a grinding
bowl. The centrifugal forces from the rotation of the grinding bowls
around their own axis and from the rotating support disc have an effect
on the contents of the grinding bowl, consisting of material to be ground
and grinding balls.
The grinding bowl and the support disc have opposite directions of rotation, in order that the centrifugal forces alternate in the same direction
and in the opposite direction.
The result is that the grinding balls run down the inside of the bowl's wall
with a friction effect and the grinding balls hit the opposite wall of the
grinding bowl with an impact effect.
1.2.2
Drive motor and speed regulation
1.3 Obligations of the operator
A maintenance-free electric motor operated via frequency converter is
used as the drive.
Before using the of the PULVERISETTE 7 premium line, this manual is to
be carefully read and understood. The use of the of the PULVERISETTE 7
premium line requires technical knowledge; only commercial use is permitted.
The operating personnel must be familiar with the content of the operating manual. For this reason, it is very important that these persons
actually receive the present operating manual. Ensure that the operating
manual is always near the device.
The of the PULVERISETTE 7 premium line may exclusively be used within
the scope of applications set down in this manual and within the framework of guidelines put forth in this manual. In case of non-compliance or
improper use, the customer assumes full liability for the functional capability of the PULVERISETTE 7 and for any damage or injury arising from
failure to fulfil this obligation.
By using the of the PULVERISETTE 7 premium line the customer agrees
with this and recognizes that defects, malfunctions or errors cannot be
completely excluded. To prevent risk of damage to persons or property
or of other direct or indirect damage, resulting from this or other causes,
the customer must implement sufficient and comprehensive safety
measures for working with the of the PULVERISETTE 7 premium line.
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Safety information and use
Neither compliance with this manual nor the conditions and methods
used during installation, operation, use and maintenance of the of the
PULVERISETTE 7 premium line can be monitored by Fritsch GmbH.
Improper execution of the installation can result in property damage and
thus endanger persons. Therefore, we assume absolutely no responsibility or liability for loss, damage or costs that result from errors at installation, improper operation or improper use or improper maintenance or
are in any way connected to these.
The applicable accident prevention guidelines must be complied with.
Generally applicable legal and other obligatory regulations regarding
environmental protection must be observed.
Information on hazards and symbols used in this manual
1.4
Safety information
Safety information in this manual is designated by symbols. Safety information is introduced by keywords that express the extent of the hazard.
DANGER!
This symbol and keyword combination points out a directly
hazardous situation that can result in death or serious
injury if not avoided.
WARNING!
This symbol and keyword combination points out a possibly
hazardous situation that can result in death or serious
injury if not avoided.
CAUTION!
This symbol and keyword combination points out a possibly
hazardous situation that can result in slight or minor injury
if not avoided.
NOTICE!
This symbol and keyword combination points out a possibly
hazardous situation that can result in property damage if
not avoided.
Special safety information
To call attention to specific hazards, the following symbols are used in
the safety information:
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Safety information and use
DANGER!
This symbol and keyword combination points out a directly
hazardous situation due to electrical current. Ignoring information with this designation will result in serious or fatal
injury.
DANGER!
This symbol and keyword combination designates contents
and instructions for proper use of the machine in explosive
areas or with explosive substances. Ignoring information
with this designation will result in serious or fatal injury.
DANGER!
This symbol and keyword combination designates contents
and instructions for proper use of the machine with combustible substances. Ignoring information with this designation will result in serious or fatal injury.
Safety information in the procedure
instructions
WARNING!
This symbol and keyword combination points out a directly
hazardous situation due to movable parts. Ignoring information with this designation can result in hand injuries.
WARNING!
This symbol and keyword combination points out a directly
hazardous situation due to hot surfaces. Ignoring information with this designation can result in serious burn injuries
due to skin contact with hot surfaces.
Safety information can refer to specific, individual procedure instructions. Such safety information is embedded in the procedure instructions
so that the text can be read without interruption as the procedure is
being carried out. The keywords described above are used.
- 11 -
Safety information and use
Tips and recommendations
Example:
1. Loosen screw.
2.
CAUTION!
Risk of entrapment at the lid.
Close the lid carefully.
3. Tighten screw.
This symbol emphasises useful tips and recommendations
as wells as information for efficient operation without mal‐
function.
Further designations
To emphasise procedure instructions, results, lists, references and other
elements, the following designations are used in this manual:
Designation Explanation
Step-by-step procedure instructions
1., 2., 3. ...
ð
[Button] Operating elements (e.g. push button, switch),
‘Display’ Screen elements (e.g. buttons, function key
Results of steps in the procedure
References to sections in this manual and relevant documentation
Lists without a specific order
display elements (
assignment)
e.g. signal lamps)
- 12 -
1.5 Information on hazards at the device
There is a laser radiation hazard warning on the back of the device.
It is explained below.
Do not remove the information and warning signs.
Caution! Hot surface
Caution! Crushing hazard
Safety information and use
1.6 Device safety information
n Only use genuine accessories and genuine spare parts. Failure to
observe this instruction can compromise the safety of the machine.
n Accident-proof conduct is to be strictly followed during all work.
- 13 -
Safety information and use
DANGER!
Explosion hazard!
– Wear safety goggles. The high temperature or chemical
reactions during the grinding process may result in
overpressure in the grinding bowl. Splashing hazard!
Ä
Explosion hazard! Do not fail to observe
Ä
information’ on page 27 and
against an excessively high pressure’ on page 40.
– Never use brute force to open the grinding bowl. Open
the grinding bowl only if you are sure that the internal
pressure has been released completely. Observe the
opening instructions in
after a grinding operation’ on page 41 and
measures against an excessively high pressure’
on page 40.
– The device may only be operated indoors. The sur-
rounding air must not contain any electrically conductive dust.
– When grinding oxidisable substances (e.g. metal or
coal), there is a risk of spontaneous combustion (dust
explosion) if the proportion of fine particles exceeds a
certain percentage. Chemical reactions are also possible during wet grinding. When grinding these kinds of
substances, special safety measures (e.g. wet grinding)
must be taken and the work must be supervised by a
specialist.
– The device is not explosion-protected and is not suit-
able for grinding explosive materials.
Ä
‘Safety measures
‘Opening the grinding bowl
‘Safety
Ä
‘Safety
DANGER!
– Do not reuse damaged accessories.
If the planetary micro mill or its components are dam-
–
aged or if its operation is not as described in the operating manual, the device may not be put into service. In
such a case, consult your Fritsch GmbH representative
or distributor.
WARNING!
The maximum accepted concentration (MAC) levels of the
valid safety regulations must be observed. If necessary,
ventilation must be provided or the machine must be operated under an extractor hood.
- 14 -
Safety information and use
CAUTION!
– Wear hearing protection! Above a sound level of
90dB(A)
Wear safety gloves! The grinding bowls may get very
–
Ä
hot. See
effect of high temperature’ on page 39 and
the grinding bowl’ on page 59.
– Do not grind with the device for several hours in suc-
cession without cooling phases. Risk of overheating!
– The device may not be run without supervision. In cer-
tain operating states, the vibrations may result in a
shifting effect on the surface.
n Do not remove the information signs.
n Unauthorised alteration of the device will void Fritsch's declaration
of conformity to European directives and void the guarantee.
n If, after reading the operating manual, there are still questions or
problems, please do not hesitate to contact our specialists.
‘Hazardous points’ on page 16, Ä ‘The
Ä
‘Cooling
1.7 Protective equipment
Protective equipment is to be used as intended and may not
be disabled or removed.
All protective equipment is to be regularly checked for
integrity and proper functioning.
DANGER!
– The valves on the grinding bowls may not be repaired.
n Each time before using the planetary micro mill, check that the pro-
Ä
tective equipment is not damaged or contaminated (see
Ä
ardous points’ on page 16,
Ä
‘Safety information’ on page 27).
n Do not make any changes to the protective equipment, apart from
the maintenance tasks listed in the operating manual.
n The device's grinding chamber cover can only be opened and closed
by a motor and therefore not without a connection to the power
Ä
supply. See
n It can only be opened when the mill comes to a stop.
n The grinding chamber cover must always be closed during grinding.
n When the grinding chamber cover is open, the mill's mechanical unit
is locked mechanically to prevent it from starting.
‘Protection against restart’ on page 17.
‘Electrical safety’ on page 16 and
‘Haz‐
- 15 -
Safety information and use
1.8 Hazardous points
n Crushing hazard when opening and closing the grinding chamber
cover (the closing force can be adjusted, consult Fritsch GmbH).
n Crushing hazard when adjusting the control display.
n Crushing hazard when using the locking lever.
1.9 Electrical safety
1.9.1 General information
CAUTION!
Fire hazard at the grinding bowl after grinding and during
Ä
the grinding pauses. See
material during grinding’ on page 35,
temperature’ on page 39 and
on page 59.
DANGER!
The grinding bowl may open extremely suddenly if the
internal pressure is too high. Never use brute force to open
the bowl. Do not fail to observe
perature’ on page 39 and
excessively high pressure’ on page 40.
n The main switch separates the device from the power supply with
two poles.
n Turn off the main switch if the planetary micro mill is "out of service"
for prolonged periods (e.g. overnight).
‘Impact of the ball size and the
Ä
‘The effect of high
Ä
‘Cooling the grinding bowl’
Ä
‘The effect of high tem‐
Ä
‘Safety measures against an
- 16 -
1.9.2 Protection against restart
Safety information and use
In the case of a power failure during operation or after turning the
device off at the main switch, the grinding chamber cover is locked.
When the power supply is restored, the grinding chamber is not opened
until the software detects that the drive is stationary. For safety reasons,
however, the planetary micro mill does not restart.
1.9.3
Overload protection
1.9.4 Imbalance detection
n In the event of an overload, the device reduces the speed in a con-
trolled manner. This special operating state is indicated on the display.
n The device shuts down if the drive motor becomes too hot.
n The device shuts down if the drive is blocked.
Ä
The device shuts down if there is excessive imbalance. See
device’ on page 27.
‘Using the
- 17 -
Technical data
2 Technical data
Dimensions
2.1
2.2 Weight
2.3 Operating noise
360 mm x 400 mm x 580 mm
(height x width x depth)
Net: approx. 44 kg
Gross: approx. 61 kg
The sound level is approx. 74 dB (A). This value fluctuates significantly,
depending on the speed and material to be ground and on the type of
grinding bowl and grinding balls.
The device is rated with IP 20.
2.4 Voltage
2.5 Current consumption
2.6
Power consumption
The device can be operated in two voltage ranges:
n Wide range input 100-240 V ± 10 %.
Transient overvoltage according to overvoltage category II permitted.
If the device is to be operated with two different voltages,
e.g. 115 V or 230 V, it must be disconnected from the power
supply at least 60 seconds before switching over the
voltage.
The maximum current consumption is approx. 10 A (115 V)
or 5 A (230 V).
The maximum power consumption is approx. 1100 W.
- 18 -
2.7 Electrical fuses
2.8 Material
2.9 Final fineness
Technical data
n Fuses on the back of device: 2x10 A T
n Maximum feed amount in the case of hard material approx. 5 mm
n Maximum feed amount 2 x 35 ml
n Dry grinding up to d
n Wet grinding up to d
< 20 µm (depending on the material)
50
< 0.1 µm (depending on the material)
50
- 19 -
Installation
3 Installation
Transport
3.1
The device is delivered on a transport pallet with a wooden cover. We
recommend using a forklift or pallet truck for transporting the packed
device.
DANGER!
Do not step under the transport pallet during transport.
WARNING!
Improper lifting can lead to personal injury or property
damage. The machine is only to be lifted with suitable
equipment and by qualified personnel.
3.2
The guarantee excludes all claims for damage due to improper transport.
Unpacking
n Open the straps of the packaging.
n Remove the lid from the crate or open the crate upwards.
n Remove the accessory cardboard pieces and additional padding.
n Lift the upper part of the packaging off the transport pallet.
n The device can now be lifted off the pallet and out of the foam pad-
ding.
CAUTION!
Crushing hazard!
Always lift with 2 persons.
Hold the bottom edge of the housing when lifting.
n Compare the contents of the delivery with your order.
- 20 -
3.3 Setting up
Installation
Grinding bowls made of hardened steel may have recesses
on the surface caused during production. They do not have
an impact on grinding or the grinding results and usually
disappear after the first grinding operation.
These recesses on the surface, if present, are within the
range of the permissible production tolerances. Complaints
relating to such grinding bowls therefore cannot be
accepted.
n Set up the planetary micro mill indoors, on a flat and firm surface.
NOTICE!
Never operate of the PULVERISETTE 7 premium line while it
is standing on the transport pallet!
n Make sure that:
all switches / control elements are easy to access;
–
– the ventilation slots are not covered;
– the interfaces (USB / Ethernet) are easy to access.
CAUTION!
Risk of overheating!
The cover on the housing openings may reduce the supply
of air, thus causing the device to overheat.
n Please store the transport packaging in order that it can be reused in
case you need to return the product. Fritsch GmbH denies all liability
for any damage due to improper packaging (non-genuine packaging).
- 21 -
Installation
3.4 Ambient conditions
WARNING!
Mains voltage!
– The device may only be operated indoors.
The surrounding air may not carry any electrically con-
–
ductive dust.
– Maximum relative humidity 80% for temperatures up
to 31°C, linearly decreasing down to 50% relative
humidity at 40°C.
n The room temperature has to stay between 5 - 40°C.
n Altitudes up to 2000 m
n Degree of pollution 2 according to IEC 664.
3.5 Electrical connection
DANGER!
Provide short-circuit protection!
Risk of damage due to short-circuits.
– Make sure that the socket is connected to a mains line
protected with a residual current circuit breaker.
Before establishing the connection, compare the voltage and current
values stated on the type plate with the values of the power supply
system to be used.
DANGER!
Mains voltage!
Changes to the connection line may only be made by a
qualified person.
CAUTION!
Ignoring the values on the type plate may result in damage
to the electrical and mechanical components.
- 22 -
Installation
NOTICE!
Fritsch mills are speed controlled. The devices are equipped
for this with frequency converters. In order to comply with
the EMC directive, many measures must be taken to prevent operational transient emissions.
The possible leakage currents resulting from filtering measures can trigger a conventional residual current circuit
breaker in the mains line. This is no defect!
To prevent this, special residual current circuit breakers,
which are adapted for operation with frequency converters,
are commercially available.
Operation without a residual current switch is possible, but
must be done in accordance with the relevant regulations.
- 23 -
Initial start-up
4 Initial start-up
4.1 Switching on
Ä
Switch on the device only after all work as described in
on page 20 has been carried out.
1. Connect the device to the power supply using the cable provided
(device cable with IEC 320/C13 plug).
2. Turn the device on at the main switch.
3. The display lights up.
‘Installation’
4.2
Function check
1. Grinding station 1 is moved into the loading position.
2. The grinding chamber cover opens.
3. Check if grinding station 1 is empty (no bowl inserted).
4. Press BUTTON "2" on the display.
5. Grinding station 2 is moved into the loading position.
6. Check if grinding station 2 is empty.
7. Press the "<" button for confirmation and to access the main
menu.
8. Press the "Menu" button.
- 24 -
Initial start-up
9. You can make various settings in the next menu. Select the
"Parameters" menu item.
10. A sub-menu appears in which you can enter the speed using the
input keys. Set the speed to 100.
11. Press the "<" button to save your entry and return to the main
menu.
12. Press the "Start" button to close the grinding chamber cover and
start the safety check.
13. Various sensors check the bowls and the closing mechanism. That
will take a few moments.
- 25 -
Initial start-up
Switching off
4.3
14. The sensors detect that the grinding bowls are not present.
15. Press the ">" button to open the grinding chamber cover and
grinding station 1 is moved into the loading position.
16. The device functions are OK.
If the device is put out of service for a lengthy period, close the grinding
chamber cover using the "Close" button and turn the device off at the
main switch.
- 26 -
5 Using the device
Safety information
5.1
Using the device
DANGER!
The PULVERISETTE 7 premium line planetary mill from
Fritsch enables speeds of up to 1100 rpm. The application
of high energy may result in very high temperatures and
high pressures in the grinding bowl.
Failure to observe the following safety instructions could
result in the explosion of grinding bowls and parts flying
around, causing injuries and damage to the building or
device.
We cannot accept any liability for the occurrence and consequences of injuries or damage to the building or device
resulting from a reaction of the sample material in the
grinding bowl that cannot be anticipated or controlled.
Bear in mind that it is essential that test grinding operations
with unknown parameters are always carried out in a safe
room that reliably prevents damage by exploding grinding
elements.
WARNING!
Make sure before starting the machine that the grinding
bowls have been tensioned correctly and that there are no
loose parts inside the device. There is a risk of loose
grinding bowls or parts being flung out. Failure to observe
this will void the guarantee and release us from liability for
any resulting damage to the device or personal injury.
NOTICE!
During grinding, the temperatures in the grinding bowl may
get very high.
In encased grinding bowls, the inserts are glued into the
casing with a two-component construction adhesive.
The adhesive is resistant to temperatures up to approx. 140
°C. Above 140 °C, the adhesive will liquefy and accumulate
below the insert in the casing. When the adhesive cools
down, it solidifies and pushes the casing up. That can cause
irreparable damage to the insert. The grinding bowl will
definitely be rendered unusable.
Above temperatures of 200 °C, the adhesive will be
destroyed. The same applies for encased grinding bowl lids.
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Using the device
NOTICE!
The planetary drive is provided by the main disc via a
toothed belt drive. Constant high loads stress the toothed
belt severely, and may even damage it. High loads may be:
heavy loads, high speeds, high temperatures, long operating times or combinations of these.
NOTICE!
The grinding duration in the reversing mode must not
exceed 5 minutes. A longer grinding duration in the
reversing mode may damage the PULVERISETTE 7 premium
line.
NOTICE!
If the permissible maximum temperature in the bowl is
exceeded during grinding, then the device must not be
switched off with the lid closed. That could lead to heat
accumulation in the machine, which could cause damage to
the device.
Provide sufficient cooling by letting the mill continue to run
at a speed of 100 rpm for approx. 20 - 30 min. or by shutting off the mill with the lid open.
5.1.1 General information
The grinding bowls have been tested and approved for a static internal
pressure of up to 20 bar.
If the pressure increases gradually, safety elements in the lid prevent the
build-up of an unacceptable overpressure.
Fast and dynamic pressure surges (e.g. an explosion or very fast chemical
reactions, etc.) up to 30 bar will not cause any damage. A higher pressure will result in irreparable damage to the grinding bowl and possibly
also damage the machine.
In such a case, the grinding bowls and the machine are not covered by
the Fritsch guarantee.
To clean the grinding bowl and its components, follow the operating
instructions precisely ( Ä ‘Cleaning’ on page 104).
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5.1.2 Overpressure relief of the grinding bowls
The grinding bowl seals have a sealing effect but are also for overpressure relief. If the pressure increases gradually during grinding, the special
seals open at a certain pressure and release the overpressure in a
defined manner.
DANGER!
This overpressure release does not work in the event of
sudden pressure surges (e.g. explosions).
A half-round notch with a diameter of 2 mm is punched onto the outer
diameter of the flat seal. The grinding bowl's pressure release works with
flat seals made of fluororubber above a static internal grinding bowl
pressure of about 10 bar. Flat seals made of silicone open above a static
internal grinding bowl pressure of about 18 bar.
DANGER!
If flat seals are used without this defined notch, very high
pressures will develop in the grinding bowl that could cause
it to burst (resulting in damage and injuries).
Using the device
The application of high energy during grinding results in high temperatures in the grinding bowl. An 80 ml grinding bowl filled with 60 ml water
results in the development of the following pressures and temperatures:
Temperature of grinding bowl
wall [°C]
101 1
109 2
127 4
141 6
152 8
159 10
166 12
171 14
177 17
180 19
183 21
Pressure in the grinding bowl
[bar]
If water is used as an additive, the overpressure release with fluororubber flat seals is triggered at 159 °C, and with silicone flat seals at 180
°C an. Any effects by the ground material are not taken into account.
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Using the device
Be extremely careful if solvents are used. 60 ml isopropanol in an 80 ml
grinding bowl results in the development of the following pressure and
temperature:
Temperature of grinding bowl
wall [°C]
Pressure in the grinding bowl
[bar]
50 1
73 2
86 5
109 8
124 10.5
132 13
139 14
148 19
149 20
The overpressure limit for fluororubber flat seals is reached at 120 °C
and for silicone seals at 149 °C.
Here is an example of the pressure and temperature development
during an actual grinding operation:
Grinding balls: 120 g 0.4-0.7 mm ZrO
Grinding bowl: 80 ml ZrO
2
2
Material to be ground: 10 g aluminium oxide with feed size d50=20 µm
Addition: 30 ml water
Speed: 1100 rpm
Time [min] Bowl 1 [°C] Bowl 2 [°C]
10 124 119
15 140 136
Other configurations or material to be ground may result in high temperatures being reached much sooner.
Because the gases and solids are mixed completely in the
grinding bowl, pure gas is never discharged. Material to be
ground is also discharged. To clean the mills, see
Ä
‘Cleaning’ on page 104.
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