Operating Manual

translation of the original

pulverisette 7
Fritsch GmbH
Laborgerätebau
Industriestrasse 8
D - 55743 Idar-Oberstein

Phone: +49 (0)6784/ 70-0

Fax +49 (0)6784/ 70-11
E-Mail: [email protected]
URL: http://www.fritsch.de

Fritsch GmbH, Laborgerätebau has been certified by the TÜV-

Zertifizierungsgemeinschaft e.V. Certificate registration number
71 100 4 008

It was verified through an audit that Fritsch GmbH satisfies the

requirements of DIN EN ISO 9001:2000.

The enclosed conformity statement states the directives

satisfied by the planetary micro mill "PULVERISETTE 7 premium
line" in order to bear the CE mark.

Instrument number 07.5000.00

Applies as of serial number 0100

Edition 06/2007 Index 003 Created Checked and Released

Table of contents................................................................................................................Page
1 General / introduction .......................................................................................................1
1.1 Notes about the operating manual ..............................................................................................1
1.2 Explanation of the symbols used on the device and in the operating manual ............................2
1.3 Brief description of the machine ..................................................................................................3
1.3.1 Fields of application......................................................................................................................3
1.3.2 Method of operation......................................................................................................................3
1.3.3 Driving motor and speed control...................................................................................................3
1.4 Technical data .............................................................................................................................4
1.4.1 Dimensions...................................................................................................................................4
1.4.2 Weight ..........................................................................................................................................4
1.4.3 Operating noise ............................................................................................................................4
1.4.4 Voltage .........................................................................................................................................4
1.4.5 Current consumption ....................................................................................................................4
1.4.6 Power consumption ......................................................................................................................4
1.4.7 Electrical fuses .............................................................................................................................4
1.4.8 Material.........................................................................................................................................4
1.4.9 Final fineness ...............................................................................................................................4

2 Operating safety ................................................................................................................ 5

2.1 General safety instructions ..........................................................................................................5
2.2 Operators.....................................................................................................................................7
2.3 Protective devices........................................................................................................................7
2.4 Danger points ..............................................................................................................................7
2.5 Electrical safety............................................................................................................................8
2.5.1 General.........................................................................................................................................8
2.5.2 Protection against restarting.........................................................................................................8
2.5.3 Overload protection ......................................................................................................................8
2.5.4 Imbalance detection .....................................................................................................................8

3 Installation.......................................................................................................................... 9
3.1 Transport .....................................................................................................................................9
3.2 Unpacking and setting up ............................................................................................................9
3.3 Ambient conditions ....................................................................................................................10
3.4 Electrical connection..................................................................................................................10
3.5 Switching on the first time / function test ...................................................................................10
4 Working with the planetary micro mill...........................................................................13
4.1 Selecting grinding bowls and grinding balls ..............................................................................14
4.1.1 Grinding bowl capacity................................................................................................................15
4.1.2 Grinding ball size ........................................................................................................................15
4.1.3 Number of balls per grinding bowl ..............................................................................................15
4.1.4 Calculated ball weight.................................................................................................................16
4.2 Effects of the ball size and material during grinding..................................................................17
4.3 Grinding bowl filling quantities ...................................................................................................17
4.4 Filling the grinding bowl .............................................................................................................18
4.5 Factors influencing the grinding ................................................................................................18
4.5.1 Duration (grinding time) ..............................................................................................................18
4.5.2 Speed .........................................................................................................................................18
4.5.3 Reversing operation (regular reversal of the direction of rotation after every grinding cycle) ....18
4.5.4 Number and size of the balls ......................................................................................................18
4.5.5 Mass of the balls (material type).................................................................................................18
4.6 Dry grinding ...............................................................................................................................18
 4.7 Wet grinding (grinding in suspension) .......................................................................................19
4.7.1 Effects of high temperature ........................................................................................................19
4.7.2 Safety measures against high pressure .....................................................................................20
4.7.3 Opening the grinding bowl in normal cases: ...............................................................................20
4.7.4 Opening the grinding bowl in event of a fault:.............................................................................20
4.8 Grinding bowl handling ..............................................................................................................22
4.8.1 Opening the grinding bowl ..........................................................................................................22
4.8.2 Closing the grinding bowl............................................................................................................22
4.9 Inserting grinding bowls into the grinding bowl mount ..............................................................23
4.9.1 Inserting grinding bowls ..............................................................................................................23
4.9.2 Removing grinding bowls............................................................................................................24
4.10 Mass balance.............................................................................................................................25
4.11 Grinding time .............................................................................................................................25
4.12 Performing a grinding ................................................................................................................25
4.12.1 Program sequence after switching on ........................................................................................26
4.12.2 Starting the grinding at high speed .............................................................................................29
4.12.3 Overloading ................................................................................................................................30
4.12.4 "Program" menu item .................................................................................................................30
4.12.5 Saving the current data ..............................................................................................................31
4.12.6 Loading a program .....................................................................................................................31
4.12.7 Setting the time control...............................................................................................................32
4.12.8 Imbalance monitoring .................................................................................................................33
4.12.9 Switching off ...............................................................................................................................33
4.12.10 Cooling the grinding bowls..........................................................................................................33

5 General and optional settings ........................................................................................34

5.1 SOP mode (Standard Operating Procedure) ............................................................................34
5.1.1 Activating the SOP mode ...........................................................................................................34
5.1.2 Disabling the SOP mode ............................................................................................................35
5.1.3 Completely deactivating the SOP mode .....................................................................................35
5.2 RFID ..........................................................................................................................................36
5.3 EasyGTM...................................................................................................................................36
5.3.1 Activating....................................................................................................................................36
5.3.2 Deactivating................................................................................................................................37
5.4 Language setting .......................................................................................................................37
5.5 Screen brightness......................................................................................................................38
5.6 Information.................................................................................................................................38
5.7 Interfaces ...................................................................................................................................39
6 Cleaning............................................................................................................................ 40
6.1 Grinding parts ............................................................................................................................40
6.2 Mill..............................................................................................................................................40
7 Maintenance ..................................................................................................................... 42
7.1 Removal of the O-ring ...............................................................................................................42
8 Warranty ........................................................................................................................... 43
9 Index ................................................................................................................................. 44
1 General / introduction
1.1 Notes about the operating manual
• The copyright to these technical documents is held by Fritsch
GmbH, Manufacturers of Laboratory Instruments.
• These operating instructions are not to be reprinted or copied
without the express approval of Fritsch GmbH.
• Study the operating manual carefully.
• All operators must be familiar with the contents of the
operating manual.
• Please follow the notes for your safety.
• The instrument was designed from a perspective of user
safety; however, some residual dangers could not be
eliminated. To prevent endangering of the users, the
instructions in this operating manual must be followed. Caution!
• The symbols in the right hand margin highlight the risks Follow the
described in the text. operating manual
Some symbols may also be found on the instrument and warn
against possible inherent hazards.
Warning symbols are surrounded by a triangle.
• This operating manual does not constitute a complete
technical description. It describes only the details required for
safe operation and maintenance for usage under normal
conditions.

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1.2 Explanation of the symbols used on the
device and in the operating manual

Attention!
Warning against danger spot
Observe operating manual

Attention! Mains voltage

Attention! Danger of explosion

Attention! Hot surface

Attention! Inflammable substances

Wear protective gloves!

Wear ear protection!

Wear safety goggles!

Do not stand under suspended load!

Attention! Danger of crushing or pinching

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1.3 Brief description of the machine
1.3.1 Fields of application
The planetary micro mill "PULVERISETTE 7 premium line" is
universally applicable for quick dry or wet grinding of inorganic
and organic samples for analysis, quality control and materials
testing.
In synthesis, the planetary micro mill can be used for mixing and
homogenisation of dry samples, emulsions and pastes.

1.3.2 Method of operation

The grinding material is pounded and ground by grinding balls in
a grinding bowl. Centrifugal forces from the rotation of the
grinding bowl around its own axis and the rotating supporting disc
act on the grinding bowl filling consisting of the grinding material
and grinding balls.
The grinding bowl and supporting disc rotate in opposite
directions so that the centrifugal forces alternately act in the
same and opposite directions.
This results in the grinding balls running along the inner wall of
the grinding bowl as a frictional effect and the balls impacting
against the opposite wall of the grinding bowl as an impact effect.

1.3.3 Driving
motor and speed control
The machine is driven by a maintenance-free electric motor that
is operated with a frequency converter.

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1.4 Technical data
1.4.1 Dimensions
360 x 400 x 580 mm
(height x width x depth)

1.4.2 Weight
Net: approx. 44 kg
Gross: approx. 61 kg

1.4.3 Operating noise

The noise level is approx. 74dB (A). The value fluctuates greatly
depending on the speed, the grinding material and the type of
grinding bowl and balls.

1.4.4 Voltage
The machine can be operated in two voltage ranges:
• Input value range 100-240 V ± 10%.
Transient excess voltage permissible as per excess voltage
category II.
Caution:
If the instrument is to be operated with two different voltages,
such as 115 V or 230 V, it must be disconnected from the mains
current at least 60 seconds before switching of the voltage.

1.4.5 Current consumption

The maximum current consumption is approx. 8.8 A (115 V) or
3.7 A (230 V).

1.4.6 Power consumption

The maximum power consumption is approx. 1300 W.

1.4.7 Electrical fuses

• Fuse insert at the rear of the machine: 2x10 A T

1.4.8 Material
• Maximum input size for hard material approx. 5 mm
• Maximum input quantity 2 x 35 ml

1.4.9 Final fineness

• Dry grinding
down to d50 < 20 µm (depending on material)
• Wet grinding
down to d50 < 0.1 µm (depending on material)

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2 Operating safety
2.1 General safety instructions
• Read the operating manual carefully before using the
planetary micro mill “pulverisette 7” for the first time. Never
allow anyone to use the instrument who has not already read
and understood the operating manual. To this end, it must be
ensured that the operating manual is situated with the
instrument, among other measures.
• Only use the planetary micro mill for the purpose described in
the operating manual (section 1.3.1).
• Every time before using the planetary micro mill, inspect that
the safety equipment is undamaged and clean (see section
2.3, 2.4, 2.5, 4.7.2, 4.7.3).
• Do not make any changes to the safety equipment, with the
exception of the maintenance measures described in the
operating manual. The valves on the grinding bowls may not
be repaired.
• Do not disable safety devices.
• Only use original accessories and original spare parts. Failure
to adhere to this may jeopardise the protection of the
machine.
• Do not continue using damaged accessories.
• Do not remove the instruction labels.
• Independent alterations to the device negate the conformity
with European directives declared by Fritsch and void the
warranty.
• Wear ear protection! As of noise level 90 dB(A)
• Wear protective gloves!
The grinding bowls can be very hot. See section 2.4, 4.7.1,
4.7.3, 4.12.10.
• Wear safety glasses!
An overpressure may result from the high temperature during
wet grinding. Spraying hazard! Explosion hazard! Always
follow the instructions in section 4.7.2.
• Never use force to open the grinding bowls. Only open the
grinding bowls if you are certain that the interior pressure has
been completely released. Follow the instructions for opening
in section 4.7.1, 4.7.2, 4.7.3 and 4.7.4.
• Do not grind with the machine for several hours at a time
without a pause for cooling. Danger of overheating!
• Care must be taken during all work to prevent accidents.
• The maximum workplace concentrations given in the valid
safety instructions must be observed and, if necessary,
ventilation should be provided or the machine should be
operated under a hood.
• The machine should be operated indoors only. The ambient
air should not contain any electrically conductive dust
particles.

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• When grinding oxidisable materials (e.g. metals or coal),
there is a risk of spontaneous ignition (dust explosion) if the
fine particles exceeds a certain percentage of the material.
While such materials are being ground, it is therefore
necessary to take special safety precautions (e.g. wet
grinding), and the work must be supervised by a specialist.
• The instrument is not explosion-proof and is not suitable for
grinding of explosive substances.
• Do not allow the machine to operate unattended. Due to the
vibrations, the machine may creep along its supporting
surface under certain operating conditions.
• If the planetary micro mill or parts of it are damaged or its
functioning does not correspond to the descriptions in the
operating manual, the device may not be put into operation.
In this case, contact Fritsch GmbH, the representative office
that covers your region or dealer who sold you the instrument.
• If you still have questions or problems after reading this
operating manual, please contact our technical personnel.

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2.2 Operators
• The planetary micro mill may only be operated by
authorised persons and may only be maintained and repaired
by trained experts.
• No one suffering from medical ailments or under the influence
of medications, drugs, alcohol or excess fatigue may operate
the planetary micro mill.

2.3 Protective devices

Protective devices should be used for the intended purpose
and must not be made unserviceable or removed.

All protective devices must be regularly inspected for

completeness and proper function. See section 7
Maintenance.

• The grinding chamber cover of the instrument can only be

opened or closed by motor and cannot be operated without a
mains power connection. See section 2.5.2.
• It can only be opened once the mill has come to a complete
stop.
• The grinding chamber cover must always be closed during
grinding.
• The mechanical components of the mill are locked against
starting up while the grinding chamber cover is open.

2.4 Danger points

• Danger of crushing when the grinding chamber cover is being
opened and closed (the closing force is adjustable, please
contact Fritsch GmbH).

• Danger of crushing when adjusting the operating display.

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 • Danger of crushing when operating the locking lever.

• Danger of burns from the grinding bowl after grinding and

during grinding pauses. See section 4.2, 4.7.1, 4.7.3, 4.12.10.
• Explosive opening of the grinding bowls due to excess
pressure. Never open the bowls with force. Always follow the
instructions in sections 4.7.1, 4.7.2 and 4.7.4.

2.5 Electrical safety

2.5.1 General
• The mains switch disconnects the machine from the mains
supply at both the poles.
• Switch off the mains switch when the planetary micro mill will
be out of operation for an extended period (e.g. over night).

2.5.2 Protection against restarting

In event of a mains failure during operation or after switching off
with the main switch, the grinding chamber cover will remain
locked. When the mains voltage is returned, the grinding
chamber will be opened only after recognition by the software
that the drive is not in motion. For safety reasons, however, the
planetary micro mill will not restart.

2.5.3 Overload protection

• In event of overloading, the speed of the machine is reduced.
This special operating state is indicated in the display.
• If the drive motor becomes too warm, the machine switches off.
• If the drive is obstructed, the machine switches off.

2.5.4 Imbalance detection

In event of an excessive imbalance, the machine switches off.
See section 4.12.8.

-8-
3 Installation
3.1 Transport
• Transport the machine on the transport pallet with a fork lift or
lift truck.

3.2 Unpacking and setting up

• Open the binding bands of the packaging.
• Remove the cover of the crate or open the top of the box.
• Remove the accessories box and additional padding.
• Lift the top packaging piece off the transport pallet.
• The machine can now be lifted from the pallet and out of the
foam padding.
Caution!
The machine must always be lifted by 2 people. Grip under the
edge of the housing to lift the machine.
• Compare the contents of the delivery with your order.
INFO!
Grinding bowls of hardened steel can exhibit surface indentations
caused by the manufacturing process. These do not influence the
grinding or the grinding result and generally disappear after the
first grinding. When present, these surface indentations lie within
the permissible manufacturing tolerance ranges. Accordingly,
complaints regarding such grinding bowls cannot be accepted.
• Place the planetary micro mill in an indoor room on a level,
stable surface.
Caution!
Operation of the planetary micro mill while standing on the
transport pallet is not permitted!
• Take care that:
⇒ All switches / operating elements are freely accessible
⇒ The ventilation slots are not covered
Caution!
Covering of the housing openings can result in reduced air
supply and thereby overheating of the machine.
⇒ The ports (USB / Ethernet) are freely accessible
• Please store the transport packaging so that it can be reused
in case of any return of the instrument. Fritsch GmbH is not
responsible for damages resulting from improper packaging
(no original packaging).

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3.3 Ambient conditions
• Only use indoors.
• The ambient temperature must range from 5 - 40°C.
• Height up to 2000 m above sea level
• Maximum relative humidity 80% for temperatures up to 31°C,
linearly decreasing to 50% relative humidity at 40°C.
• Pollution level 2 as per IEC 664.

3.4 Electrical connection

Before making the connection, compare the voltage and current
values shown on the type plate with the values of the mains
supply used.
Single-phase alternating voltage with protective conductor (see
section 1.4 ).

The connector cable may only be changed by a trained expert.

3.5 Switching on the first time / function test

Only switch on the machine once all work described in section 3
Installation has been performed!
Switching on
1. Connect the machine to the mains supply using the supplied
cable (device cable with IEC 320/C13 plug).
2. Switch on the machine at the main switch.
3. The display lights up.

4. Grinding station 1 is moved to the loading position.

5. The grinding chamber cover opens.
6. Check whether grinding station 1 is empty (no bowl
inserted).
7. Press BUTTON "2" on the display.

8. Grinding station 2 is moved to the loading position.

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9. Check whether grinding station 2 is empty.
10. Confirm and return to the main menu with the "<" button.
11. Press the "Menu" button.

12. In the next menu, you can configure various settings. Select
the "Parameters" menu item.

13. A submenu appears in which you can set the rotational

speed using the input buttons. Set the speed to 100.

14. Save the entry and return to the main menu with the "<"
button.
15. Press the "Start" button to close the grinding chamber cover
and start the safety check.

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16. Various sensors inspect the bowls and the closing
mechanism. This takes a few moments.

17. The sensors determine that the grinding bowls are not
present.

18. Press the ">" button to open the grinding chamber cover and
bring grinding station 1 to the loading position.
19. The functions of the machine are OK.
Switching off
If the machine will not be used for an extended period, close the
grinding chamber cover with the "Close" button and switch off the
machine at the main switch.

-12-
4 Working with the planetary micro mill
This grinding bowl & lid for the Fritsch P-7 are tested and
approved for static internal pressures up to 20 bars.
For normal use where a slow pressure increase inside the bowls
occurs, the safety devices incorporated into the grinding bowl lid
prevents pressure rising above the safety limit of 20 bar, thus
preventing inadmissible positive pressure and subsequent
damage to the milling bowl and the P-7 Ball Mill.
Where fast, dynamic pressure surges (e.g. explosions, very fast
chemical reactions, sudden liquid compression etc.) occur, these
will not cause damage providing the pressure surge does not
exceed 30 bars maximum. However sudden Pressure changes
greater than 30 Bar can lead to failure of the grinding bowl and
it’s lid, causing subsequent damages to the Ball Mill itself.

Please check before milling that no sudden rise of pressure

above 30 bar can occur during the milling process, bearing in
mind that milling with the P-7 is a very energetic process which
can cause a build up of heat and large temperature increases
causing a sudden pressure rise, this can be explosive high
pressure physical or chemical reactions which exceed the 30
Bar safe limit. (Remember a sudden temperature rise can turn 1
gram Mole of liquid into 22.4 litres of gas.)
Should a sudden pressure rise above 30 bar occur during the
milling process, the milling bowl(s) will react & show this. In this
specific case, the grinding bowls & lids, together with the
complete P-7 Ball Milling machine is no longer covered by the
Standard Fritsch warranty.
During the cleaning of the grinding bowls and grinding bowl parts
it is most important to adhere to the operating instructions to
prevent any problems during the milling process and should
include regular inspection of the Bowls, Lids, Lid locks and
seals for any cracks, chips or other damage to the milling
elements. Any tightness or difficulty in closing the lids manually,
could indicate problems with the seals, the bowls and lids not
being completely clean or damage to the lid clamps (chapter 6.1).

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4.1 Selecting grinding bowls and grinding balls
Caution!
When using grinding elements that are not original accessories of
the machine, no guarantee is provided and no complaints will be
accepted in event of damage to the machine.

The hardness and density (specific gravity) of the grinding bowls

and grinding balls used must be greater than that of the materials
being ground in order to prevent excessive wear.
Used for
Main components of the Abrasion
Material Density * grinding
material resistance
material
(Bowl and balls) in g/cm3
soft to
medium-
Agate (99.9% SiO2) 2.65 good
hard
samples
medium-
Sintered corundum (99.7% Al2O3) 3.7 somewhat good hard, fibrous
samples
fibrous,
Zirconium oxide (95% ZrO2) 5.7 very good abrasive
samples
Bowl:
(17-19% Cr + 8-10% Ni) medium-
Stainless steel 7.8 somewhat good hard, brittle
Balls: samples
(12.5-14.5% Cr + 1% Ni)
Bowl: (11-12% Cr) hard, brittle
Hardened steel 7.9 good
Balls: (1.0-1.65% Cr) samples

hard,
Tungsten carbide (93%TC+6% Co) 14.7 very good abrasive
samples
abrasive
samples,
Silicon nitride (90% Si3N4) 3.1 extremely good
iron-free
grinding

The grinding bowls and grinding balls of zirconium oxide are

resistant to acids – except for hydrofluoric acid.

Generally use grinding bowls and grinding balls of the same

material.
Exception: Tungsten carbide balls can be combined with
grinding bowls of hardened steel.

*
High density means high impact energy

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4.1.1 Grinding bowl capacity

Grinding bowl 20 ml 45 ml 80 ml

Capacity (grinding
1-9 ml 3-20 ml 10-30 ml
material)

4.1.2 Grinding ball size

Type of material to be ground Appropriate ball diameter
Hard samples with maximum input size of 15 mm / 20 mm
5 mm
Medium input size of 0.5 – 1 mm 15 mm / 10 mm
Fine material 0.1 – 0.5 mm 10 mm / 5 mm
Very fine material < 0.1 mm 3 mm and smaller
Homogenising of dry or liquid samples 10 mm / 5 mm

Caution!
Mixing of balls with different diameters is not recommended.
(When using various ball diameters, increased wear on the balls
must be expected!)

4.1.3 Number of balls per grinding bowl

A larger number of balls reduces the grinding time, and the
grinding results lie within a narrower range of grain sizes.
Ball
Grinding
dia-
bowl volume 20 45 80
meter
(ml)
(mm)

Number of balls
20 - - 5
(pcs.)

Number of balls
15 - 7 10
(pcs.)

Number of balls
10 10 18 30
(pcs.)

Number of balls
5 80 180 250
(pcs.)

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 Ball diameter 3 mm and smaller

Grinding
Material bowl volume 20 45 80
(ml)

Ball quantity
Zirconium oxide 30 70 100
(g)

Ball quantity
Hardened steel 40 90 150
(g)

Ball quantity
Tungsten carbide 80 200 300
(g)

The number of balls must be adhered to in order to avoid

unnecessary wear.

4.1.4 Calculated ball weight

Kugeldurchmesser in mm 5 10 15 20
Dichte errechnetes Gewicht
Werksoff in einer Kugel in g
g/cm³
Achat 2,65 0,17 1,39 4,68 11,1
Sinterkorund 3,8 0,25 1,99 6,72 15,92
Zirkonoxid 5,7 0,37 2,98 10,07 23,88
rostfreier Edelstahl 7,8 0,51 4,08 13,78 32,67
gehärteter Stahl 7,9 0,52 4,14 13,96 33,09
Wolframkarbid 14,7 0,96 7,70 25,98 61,58
Siliziumnitrid (Syalon) 3,1 0,20 1,62 5,48 12,99

To calculate the weight of the required balls, the "calculated ball

weight" is multiplied by the "number" of balls required.
Example: A 45 ml agate bowl should be filled with 185 agate
balls with 5 mm diameter.
Calculation: 0.17 g * 185 balls = 31.45 g
31.45 g of grinding balls can be weighed out and placed in the
grinding bowl in order to save the time it takes to count the balls.

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4.2 Effects of the ball size and material during
grinding
Large balls of 10 mm – 20 mm diameter result in a high
mechanical load on the system. The high mass of the balls in
connection with the high accelerations results in a high
mechanical load Æ impact effect.
The higher the density of the material used for grinding, the
higher the mechanical load.
The highest mechanical load is achieved with balls of tungsten
carbide with 20 mm diameter.
When using large agate balls, these are capable of destroying
themselves and the grinding bowl.
This is also the case for sintered corundum and silicon nitride
balls.
Balls with 5 mm diameter and smaller result in a high thermal
load on the system.
Due to the large surface of many small balls, the frictional effects
result in a high thermal load. After even 5 minutes of grinding,
temperatures exceeding 100°C can be observed on the surface
of the lid. You must measure it with a surface temperature
sensor. Inside the grinding bowl, the temperature is then many
times higher. The adhesive used has a sustained temperature
resistance of 200°C. If an external temperature of 100°C is not
exceeded, the adhesive will hold.

4.3 Grinding bowl filling quantities

Min. sample Max. sample
Grinding bowl
quantity quantity
20 ml 1 ml 9 ml
45 ml 3 ml 20 ml
80 ml 10 ml 30 ml

Caution!
During wet grinding with large ball diameter > 10 mm, at least
half the maximum sample quantity must be used. A suspension
with a viscosity that is too low offers no resistance to the balls
and can result in damage to the balls and grinding bowl. The
result is the same as if no grinding material were placed in the
bowl at all. The same also applies to dry grinding with less than
the minimum sample quantity.

Caution!
When using less than the minimum filling quantity, increased
wear must be expected! This can result in destruction of the
grinding parts.

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4.4 Filling the grinding bowl
Always observe the following order:
1. Place the grinding balls in the empty bowl.
2. Pour the grinding material onto the balls.
Caution!
Never operate the machine without grinding material because the
grinding balls and grinding bowl would be damaged!

4.5 Factors influencing the grinding

4.5.1 Duration (grinding time)
• Longer grinding time increases the share of fine particles.

4.5.2 Speed
• Higher speed reduces the grinding time and increases the
share of fine particles.

4.5.3 Reversing operation

(regular reversal of the direction of rotation
after every grinding cycle)
• Useful in mechanical alloying.
• Improves the homogeneity of the sample.

4.5.4 Number and size of the balls

• Pre-grind coarse, hard material with large balls Æ
Results in a small share of fine particles.
• A large number of small balls increases the share of small
particles with a correspondingly longer grinding time.

4.5.5 Mass of the balls (material type)

• A higher mass (density) of the grinding balls accelerates
the grinding. (See the table in section 4.1 Selecting
grinding bowls and grinding balls.)

4.6 Dry grinding

Below approx. 20 µm particle size, surface forces dominate and
the grinding material starts to "stick".
You can achieve additional dry comminution by adding surface-
active substances to the grinding material.
Examples (maximum quantity to be added in % by mass)
• Stearic acid 2-3%;
• Aerosil (highly dilute silicic acid) 0.5-2%;
• Quartz sand ~ 2%;
• Glass powder ~ 2%.

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4.7 Wet grinding (grinding in suspension)
In the transition to grinding in suspension, you can ideally add
liquids with high boiling point and low vapour pressure.
Caution!
The machine is not explosion-proof. When using flammable
liquids, it must be ensured that the heating in the grinding bowl
will not reach the boiling point of the solvent. Corresponding
cooling phases must be programmed in. If the vapour pressure is
too high, escaping vapours may ignite. If possible, we
recommend using either non-flammable liquids or liquids with a
high boiling point. The boiling point should be over 80°C or, for
long grinding times, over 100°C.

4.7.1 Effects of high temperature

Due to high internal temperature, the enlargement of the particle
surfaces through comminution and possible chemical reactions in
the bowl, very high pressure can arise in the grinding bowls
during wet grinding.
This pressure can be so large that the hooks holding the lid to
the bowl tear off, causing the lid to "fly off".

O-ring squeezed out

Broken hooks

Caution!
In event of long grinding times, always include cooling pauses to
reduce the internal pressure. For certain grinding materials, it is
also necessary to release the pressure after the cooling pause
since this can remain within the bowl even despite cooling. See
section 4.2, 4.7.2, 4.12.10!
The bowl can also stick in the mount if the bowl temperature is
too high. In this case, it is necessary to wait until the bowl has
cooled enough for it to be released from the mount.

-19-
4.7.2 Safety measures against high pressure
When a long wet grinding session is performed without cooling
pauses or ventilation during the pauses, very high pressure can
arise in the grinding bowl. To prevent the locking hooks from
tearing off, there is a kidney-shaped groove in the lid above the
O-ring. In event of high pressure (> 30 bar), the O-ring is forced
into this groove, the seal of the bowl is broken and the pressure
is released.
To prevent the bowl opening under high pressure (< 30 bar), the
hooks and the grove in the bowl have an undercut. This means
that the lid must move somewhat downward when opening. At an
internal pressure > 7 bar this can no longer be done with normal
hand strength. Opening at an internal pressure < 7 is not
dangerous (similar to opening a champagne bottle).
Attention!
Never use force to open bowls.
If the internal pressure in the bowl cannot be released (hole in
the bowl is blocked and the pressure is not large enough to
squeeze out the O-ring), the O-ring must be pressed against the
bowl wall using a small slotted screwdriver by pushing the tip
between the O-ring and the lid. This must be done carefully so
that the pressure can be released in measured amounts. The O-
ring can also be destroyed with a screwdriver to release the
pressure. If the locking hooks still cannot be opened by hand
after destruction of the O-ring, the bowl must be clamped into a
vice as described in section 4.7.4. The hooks can then be
opened carefully with a hammer.

4.7.3 Opening the grinding bowl in normal cases: a

1. Allow bowl to cool Æ
2. Release pressure by loosening the knurled screw (a). Æ
3. Open lid

4.7.4 Opening the grinding bowl in event of a fault:

1. Allow bowl to cool Æ
2. Release pressure with knurled screw Æ
3. No pressure escapes Æ
4. Lid cannot be opened by hand Æ
5. Pry the O-ring away from the lid with a screwdriver Æ
6. No pressure escapes Æ
7. Lid cannot be opened by hand Æ

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8. Stick the screwdriver into the O-ring to destroy the O-ring

Æ
9. Lid cannot be opened by hand Æ
10.Clamp the grinding bowl firmly in a vice between the lid and
bottom as shown in the image Æ

11.Open the locking hooks with a plastic hammer Æ

12.Slowly and carefully release the vice tension Æ

13.The pressure in the bowl has been released and the lid can
be lifted off.

-21-
4.8 Grinding bowl handling
4.8.1 Opening the grinding bowl
First please open the knurled screw (a) and wait until the
pressure inside the grinding bowl is completely relieved.
Then please press the locking hooks at the upper side
completely inwards. The small levers on the locking hooks press
the lid upward out of the seal. The lid can now be lifted off. a

4.8.2 Closing the grinding bowl

Press the locking hooks on the upper end entirely inward, and
place the lid on the bowl. The lid now lies on the small levers of
the locking hooks on the rim of the bowl. Turn the lid on the bowl
until the small levers of the locking hooks snap into the
indentations of the bowl rim.
Release the locking hooks and press together on the lower end
until the locking hooks snap into place and stand perfectly
vertically. Alternatively, the lid can also be pressed against the
bowl with both hands. The hooks then snap into place on their
own due to spring pressure. Please turn the knurled screw (a)
(with valve plug) off securely. The bowl is now sealed and can be
inserted into the machine.

Caution!
After the locking hooks snap into place, the lid may no longer be
turned with respect to the bowl. The position of the hooks and the
grooves in the bowl beneath the hooks must match.

-22-
4.9 Inserting grinding bowls into the grinding
bowl mount
Perform the following checks before inserting the grinding
bowls:
• Outside of the grinding bowl is clean Æ Remove any coarse dirt.
• Inside of the grinding bowl mount is clean Æ Remove any coarse dirt.
• Grinding bowl properly sealed (see section 4.8.2 )
4.9.1 Inserting grinding bowls
• Hold the grinding bowl at the grip and insert into it into the
grinding bowl mount.

• Turn the grinding bowl until the grinding bowl noticeably

snaps into place and moves several millimetres down into the
grinding bowl mount.

• Press down the locking element on the bowl mount. Æ The

grinding bowl moves farther down in the mounting mechanism.

• With vertical pressure on the grinding bowl, lock it into the

mount. The grinding bowl is properly locked in place if the
locking element on the mounting mechanism has moved back
up into its original position.

• As long as the locking element is not in its original position,

the rotation of the entire mechanical mill component is
blocked.

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4.9.2 Removing grinding bowls
• Push down the locking element on the bowl mount.

• The grinding bowl is unlocked and moves several millimetres

upward.

• The grinding bowl can now be removed (upward) from its

mount. (The grinding bowl should preferably be lifted with the
grip provided for this).

• Once the grinding bowl has been removed, the locking

element returns to its original position.

• Since a locking element that is not in its original position

blocks the mechanical mill components, the loading position
can only be changed once the locking element has properly
returned to its original position.

After several minutes of grinding and during the cooling phases,

inspect the proper condition of the grinding bowls (see section on
grinding bowls)

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4.10 Mass balance
Planetary ball mills are subject to a certain amount of
imbalance as a result of their method of operation. To keep this
imbalance low, it is necessary to balance out all rotating masses
in the system as completely as possible.
To ensure optimal mass balance (minimal imbalance) of the
machine, identical grinding bowls and identical grinding bowl
fillings must always be used at both grinding stations.
The machine can certainly be operated with different loads (such
as different grinding bowl fillings); however, this results in
performance losses and, if the imbalance is too great, switching
off of the machine. The request "Please check the imbalance"
appears on the display. See section 4.12.8 Imbalance
monitoring.

4.11 Grinding time

Depending on the application, the grinding time should be
adapted to the heating of the bowls. When grinding at high
speeds, a grinding time of 1 hour should not be exceeded; then
allow for 0.5 to 1 hour of cooling.

The extent to which the heating of the grinding material itself

must be observed naturally depends on the specific sample
being ground. It should be noted that Æ longer durations should
also be accompanied by long pauses for cooling!

If bowls are removed during a grinding pause, the proper seat of

the bowls must be inspected before reactivation.

4.12 Performing a grinding

Caution:
The following must be observed during grinding of materials
for which no values are available based on experience with
the premium line:
Initially, a grinding time of 5 minutes should be set, and after this
time, a surface thermometer should be used to measure the
temperature on the lid. If this is below 80°C, grinding can
continue for another 5 minutes until a temperature of 90°C is
reached. If this temperature is reached, insert a cooling pause of
approx. 15-30 minutes. At the end of the cooling pause, the
knurled screw should be opened to check whether pressure has
built up within the bowl. If no high pressure is present, the
grinding and pause times can be programmed so that the
temperature does not exceed 90°C.
If a high internal pressure is evident due to prolonged exhaust
noises and the escape of grinding material suspension, special
care is required for continued grinding. The pressure should
always be released again after the cooling pauses (at least 30
minutes to allow the suspension to settle) to prevent the pressure
from becoming too great. At some point, pressure will cease to
build up.

-25-
4.12.1 Program sequence after switching on
1. Switch on the machine at the main switch.
2. The display lights up.

3. During the start and initialisation phase, the INFO button can
be pressed; an info display appears with the contact address.
The display can be exited with the continue button.

4. Grinding station 1 is moved to the loading position.

The grinding chamber cover opens automatically.
5. Place the grinding bowl containing the sample (section 4.4)
and properly sealed (section 4.8.2) into the grinding bowl
mount (section 4.9.1).
6. Bring grinding station 2 to the loading position with the 2
button (a). (With the 1 button, grinding station 1 can be
brought back to the loading position).

-26-
7. Place the grinding bowl containing the sample (section 4.4)
and properly sealed (section 4.8.2) into the grinding bowl
mount (section 4.9.1).
8. The grinding chamber can be closed with the Close button
(c).
9. Press the Continue button (b) to enter the main menu.

10.To enter the process parameters, either press the display (d)
of the data (button function) or use the MENU button (e) Æ
PARAMETER button (f) to open the parameter entry function.

11.The field coloured black is active. When you start entering a

number, the previous value is deleted, or you can delete the
current parameter with the C button.
The maximum possible entries are:
• Speed = 1100 rpm,
• Time = 999 min, Pause = 99 min,
• Cycles = 99.
12.After the parameters have been input, return to the main
menu with the "<" button.

-27-
13.Press the Start button Æ The grinding chamber is closed and
the safety check is started.

14.Various sensors inspect the bowls and the closing mechanism

of the machine. This takes a few moments. The Stop button
interrupts the process.

15.If the inspection is successful, this is confirmed and the

grinding process is started immediately afterward.

16.If the sensors detect insufficient safety, the start process is

interrupted and the cause is displayed. The ">" button opens
the grinding chamber and grinding station 1 is moved to the
loading position. For measures to correct faults, see section
Checklist for fault correction. If the fault is corrected, the
grinding can be continued as described under item 9.

-28-
4.12.2 Starting the grinding at high speed
If the speed exceeds 600 rpm, the correct ball size must be
selected.
Caution!
The high grinding energy can destroy the balls if they are
selected incorrectly!

The maximum speed is reduced based on the selection of the

ball size.

A reduced speed is signalled by blinking of the set value for a

short time.
The Stop button ends the grinding process.
The Info button displays some system information as well as the
type of grinding elements.

Guide values for speed restriction

Ball diameter Speeds (rpm) Speeds (rpm)

(mm) for agate for all other materials
<5 1100 1100
5 900 1000
10 750 850
> 10 600 700

-29-
4.12.3 Overloading
In event of overloading of the planetary micro mill, the speed is
reduced. The reduced speed blinks in the display.

4.12.4 "Program" menu item

The grinding sequences can be programmed, saved and loaded
here.
1. Press the "Menu" button in the main menu.

2. Then press the "Program" button Æ A new window is opened.

Speed
Time
Pause
Cycles

3. The "Current" column shows the current parameters from

previous entries.
4. The "Program" column shows the data that was previously
saved under the 1 button.

-30-
4.12.5 Saving the current data
1. First select the program slot that is open or that should be
overwritten.

2. Then save the current parameters in the desired program slot

with the Save button.

3. After successful saving, the new parameters are now

displayed in the "Program" column.

4.12.6 Loading a program

1. Select one of the programs 1...8; the various parameter data
are displayed in the Program column.

2. Transfer the program data with the "Load" button.

3. Press the "<" button to return to the main menu.

-31-
4.12.7 Setting the time control
1.

2.

3. Select time basis for the timer.

4. Confirm entry with "<".

5. Enter time delay. With entry of a time delay, the grinding
process is only started after this amount of time has elapsed.
This function is actively displayed in the main menu.

6. Confirm entries with "<".

Timer active

7. The time delay is reset to 0000 after grinding.

-32-
4.12.8 Imbalance monitoring
A different weight distribution between the two bowls always
leads to different levels of vibrations; this also depends on the
speed.
To keep this imbalance within certain limits, the shut-off threshold
can be set.

Touch the setting bar or move it back and forth under light
pressure.
Caution!
At small setting values, the measurement system is more
sensitive; at high values it is less sensitive.
Confirm entries with "<"

4.12.9 Switching off

1. Press "STOP" on the display.
2. When the drive comes to a stop, grinding station 1 is moved
to the loading position and the grinding chamber cover opens
automatically.
3. If the machine will not be used for an extended period, close
the grinding chamber cover and switch off the main switch.

4.12.10 Cooling the grinding bowls

The grinding bowls can be cooled
1. with open grinding chamber cover and running fan (fan runs
for 1 minute after grinding);
2. or during programmed pause times with closed (locked)
grinding chamber cover and running fan.

-33-
5 General and optional settings
5.1 SOP mode (Standard Operating Procedure)
It is possible to protect the machine using the SOP mode. If this
mode is activated by the administrator, only saved programs can
be loaded for operation; changing of the parameters is no longer
possible. Parts of the menu structure can no longer be accessed.

5.1.1 Activating the SOP mode

1234

1. Enter a number from 1-9999.

2. Then press "Save".
3. Return to the main menu with the "<" button.
4. The SOP mode is displayed in the main menu.

SOP active

-34-
5.1.2 Disabling the SOP mode
To remove the restrictions on parameter changes, enter the
pin code and conclude the entry with the "ENTER" button. Return
to the main menu with the "<" button.
If the device is switched off, the SOP mode becomes active
again.

1234
Current

Entry

5.1.3 Completely deactivating the SOP mode

1. Disable the mode (section 5.1.2)
2. Enter pin code 0000 and press "Save"
3. Return to the main menu with the "<" button.

-35-
5.2 RFID
In the event of damage to a bowl, it is possible to deactivate
the bowl recognition.

Because the RFID recognition is a safety function that may not

be easily deactivated, this is protected by a pin code.
You can only obtain the pin code by contacting Fritsch GmbH.

5.3 EasyGTM
5.3.1 Activating

Confirm the entry and return to the

main menu with the "<" button.

-36-
 5.3.2 Deactivating

Confirm the entry and return to the

main menu with the "<" button.

5.4 Language setting

After selecting the national language, all further text displays are
shown in the selected language.
Confirm the entry and return to the main menu with the "<"
button.

-37-
5.5 Screen brightness

The brightness of the screen can be individually adjusted. To do

this, touch the setting bar or move it back and forth under light
pressure.
Save the entry and return to the main menu with the "<" button.

5.6 Information
System information can be accessed with the "INFO" button.

The following are displayed here:

• The operating hours
• The firmware version
• The bowl materials (if they
were detected during a START
process)
• Return to the main menu
with the "<" button.

-38-
5.7 Interfaces
By default, the machine is equipped with a USB port.
Optionally, an Ethernet port or Bluetooth interface can also be
delivered in the future.
The interface selection must be switched accordingly.
Specific installation instructions are included with the delivery for
each of the optional interfaces.

Save the entry and return to the main menu with the "<" button.

-39-
6 Cleaning
6.1 Grinding parts
Clean the grinding bowl and grinding balls after every use:
For example, brush clean under running water with typical
cleansers.
Fill the grinding bowl about half full with some sand and water
and "grind clean" for 2 to 3 minutes in the laboratory planetary
mill.
Cleaning in an ultrasound bath is permissible.
During sterilisation in a dry cabinet, only heat the grinding parts
up to 120°C.

Important!!!
Do not heat grinding parts of agate, sintered corundum,
zirconium oxide and silicon nitride over 110°C, and cool
them carefully and slowly.
The grinding parts may not under any circumstances be
heated in a microwave (heating too quickly).
They may not under any circumstances be subjected to
temperature shocks, otherwise there is a risk that the parts
may be destroyed Æ They break apart explosively.

6.2 Mill
The micro mill can be wiped off with a damp cloth while switched
off.
Before the start of cleaning work, pull the power plug and
secure the device against accidental reactivation!

The grinding chamber can be cleaned thoroughly with a damp

cloth through removal of the grinding chamber cover.
Removal of the grinding chamber cover:
1. Remove the 4 screws on the side of the housing using a
screwdriver.

-40-
2. Then carefully tip the grinding chamber cover to the right.

3. The 3 connector plugs must now be disconnected.

4. Once this is done, the cover can be lifted up entirely and the
grinding chamber can be cleaned.
5. Follow the above steps in reverse to reinstall the grinding
chamber cover.

Do not allow any liquids to flow into the device.

-41-
7 Maintenance
Before the start of maintenance work, pull the power plug
and secure the device against accidental reactivation!
Warn about maintenance work with a sign.

Regular cleaning is the most important part of maintaining the

planetary micro mill.

7.1 Removal of the O-ring

1. Insert a small slotted screw driver from above into the opening
provided on the grinding bowl.

2. Pry the O-ring to the outside with the slotted screwdriver.

3. Insert a second small slotted screw driver under the O-ring

and pull it out of the groove.

4. Press the clamping lever to release the O-ring.

-42-
8 Warranty
The warranty card enclosed with the machine upon delivery
must be completely filled out and returned to the delivering
factory so that the warranty can enter into effect.
Online registration is also possible. More information can be
found on your warranty card or on our website
http://www.fritsch.de
The company Fritsch GmbH in Idar-Oberstein and your
"Technical Application Laboratory" or the corresponding national
representatives would be happy to provide you with advice and
assistance.
Please include the serial number given on the type plate along
with any questions.

Please note that the original Fritsch packaging must be used in

the event that the machine is returned. Fritsch GmbH is not
responsible for damages resulting from improper packaging (non-
Fritsch packaging).

-43-
9 Index

A O

Accessories ............................................... 5 Operation ...................................................7

Operators...................................................7
Overload protection ...................................8
C Overloading .............................................30

Cleaning .................................................. 40
Conformity statement ................................ 2 P
Cooling the grinding bowls ...................... 33
Protective devices......................................7
D
R
Duration................................................... 25
Restarting ..................................................8
F
S
Factors influencing the grinding .............. 18
Function test............................................ 10 Suspension ..............................................19
Switching on ............................................10
G
T
Grinding................................................... 18
Grinding time ........................................... 25 Technical data ...........................................4

I W

Imbalance.................................................. 8 Warranty ..............................................5, 43

Warranty claim...........................................5
Wet grinding.............................................19

- 44 -