Fritsch PULVERISETTE 7 classic line User manual

1-1
PULVERISETTE 7
FRITSCH PLANETARY MICRO MILL
Operating Manual
Translation of the original

PULVERISETTE 7

Edition 08/2002 Index 008
PULVERISETTE 7
Fritsch GmbH
Manufacturers of Laboratory Instruments
Industriestrasse 8
D - 55743 Idar-Oberstein
Phone: [phone]
Fax: [phone]
E-Mail: [e-mail]
Internet: http://www.fritsch.de
Fritsch GmbH, has been certified by the
TÜV-Zertifizierungsgemeinschaft e.V.
Certificat registration number 71 100 J 596.
It was verified through an audit that Fritsch GmbH satisfies the requirements of
DIN EN ISO 9001:2008.
The enclosed declaration of conformity calls the directives
which the „PULVERISETTE 7“ corresponds to.
This permitts us to mark the instrument with the CE-Sign.
Instrument number 07.4000.00
Applies as of serial number 487

Page 1
PULVERISETTE 7
Table of Contens Page
1General Information / Introduction....................................................3
1.1 Notes about Operating Instructions...............................................................3
1.2 Explanations of the signs at the instrument and in the
operating instructions....................................................................................4
1.3 Short Description of the Machine..................................................................5
1.3.1 Applications.........................................................................................................5
1.3.2 Method of Operation............................................................................................5
1.3.3 Drive Motor and Speed Control...........................................................................5
1.4 Technical Data..............................................................................................6
2Operating Safety.................................................................................7
2.1 General Safety Instructions...........................................................................7
2.2 Operators......................................................................................................8
2.3 Protective Devices ........................................................................................8
2.4 Danger Points ...............................................................................................9
2.5 Electrical Safety ............................................................................................9
3Installation.........................................................................................10
3.1 Unpacking...................................................................................................10
3.2 Transport.....................................................................................................10
3.3 Erection.......................................................................................................10
3.4 Ambience conditions...................................................................................11
3.5 Electrical Connection ..................................................................................11
3.6 Adaptation to Mains Supply Voltage / Changing the
Timer / Setup-Mode ....................................................................................11
3.7 Switching On for the First Time / Test for Correct
Functioning..................................................................................................12
4Working with the Planetary Micromill .............................................13
4.1 Choice of Grinding Bowls and Grinding Balls .............................................14
4.1.1 Size of the Grinding Balls..................................................................................14
4.1.2 Number of Balls per Grinding Bowl ...................................................................15
4.1.3 Calculated Ball Weight......................................................................................15
4.2 Filling the Grinding Bowl .............................................................................16
4.3 Influencing Quantities During Grinding .......................................................16
4.3.1 Dry Grinding ......................................................................................................16
4.3.2 Wet Grinding (Grinding in Suspension).............................................................17
4.4 Clamping the Grinding Bowls......................................................................17
4.5 Mass Balance..............................................................................................18
4.6 Grinding Time..............................................................................................18
4.7 Control Panel ..............................................................................................18
4.7.1 Setting the Speed..............................................................................................18
4.7.2 Setting the Running Time..................................................................................19
4.7.3 Reversing Operation..........................................................................................19
4.7.4 Repetition of the Grinding / Break Cycles..........................................................19
4.8 Performing a Grinding Operation................................................................20
4.9 Cooling the Grinding Bowls.........................................................................20
4.10 Standby.......................................................................................................20

Page 2
PULVERISETTE 7
5Cleaning ............................................................................................21
5.1 Grinding accessories...................................................................................21
5.2 Mill...............................................................................................................21
6Maintenance...................................................................................... 22
7Warranty............................................................................................23
8Troubleshooting Checklist...............................................................24
9Disclaimer .........................................................................................25

Page 3
PULVERISETTE 7
1 General Information / Introduction
1.1 Notes about Operating Instructions
The copyright to these technical documents is the property of Fritsch GmbH,
Manufacturers of Laboratory Instruments.
These operating instructions are not to be reprinted or copied without
the express approval of Fritsch GmbH.
Please study these instructions carefully before operation.
All operators must be familiar with the contents of the operating instruc-
tions.
Please observe all notes concerning your safety.
The sieve shaker was designed with the user's safety in mind, however in-
herent risks cannot be excluded. Follow the advices in these instructions to
avoid risks to users. The symbols in the right hand margin highlight the risks
described in the text.
Symbols are also to be found on the instrument warning users of possible
risks.
Warning symbols are surrounded by a triangle.
These operating instructions do not constitute a complete technical descrip-
tion. They describe only the details required for safe operation and mainte-
nance for usage under normal conditions.

Page 4
PULVERISETTE 7
1.2 Explanations of the signs at the instrument and in the
operating instructions
Attention!
warning against danger spot
observe operating instructions
Attention! mains voltage
Attention! risk of explosion
Attention! hot surface
Attention! inflammable substances
wear protective gloves!
wear ear protectors!
wear safety goggles!
Do not step below lifted load!

Page 5
PULVERISETTE 7
1.3 Short Description of the Machine
1.3.1 Applications
The "pulverisette 7" planetary micromill is universally applicable for quick dry or
wet grinding of inorganic and organic samples for analysis, quality control, ma-
terials testing and mechanical alloying.
In synthesis, the planetary micromill can be used for mixing and homogenisa-
tion of dry samples, of emulsions and of pastes.
1.3.2 Method of Operation
The material is crushed and disintegrated in a grinding bowl by grinding balls.
The grinding balls and the material in the grinding bowl are acted upon by the
centrifugal forces due to the rotation of the grinding bowl about its own axis and
due to the rotating supporting disc.
The grinding bowl and the supporting disc rotate in opposite directions, so that
the centrifugal forces alternately act in the same and opposite directions.
This results in, as a frictional effect, the grinding balls running along the inner
wall of the grinding bowl, and impact effect, the balls impacting against the op-
posite wall of the grinding bowl.
1.3.3 Drive Motor and Speed Control
The machine is driven by a maintenance-free three-phase a.c. motor, which is
operated with a frequency converter.

Page 6
PULVERISETTE 7
1.4 Technical Data
Dimensions
500 x 370 x 530 mm
(height x width x depth)
Weight
Net: 35 kg
Gross: 55 kg
Operating Noise
The noise level can be as high as approx. 90dB (A). The value fluctuates great-
ly depending on the speed, the material being ground and on the type of grind-
ing bowl and grinding balls.
Voltage
The machine can be operated in two voltage ranges:
Single-phase alternating voltage 100-120V ± 10% and
Single-phase alternating voltage 200-240V ± 10%.
(see also section 3.6)
Current Input
The maximum current input is approx. 8,8 A (115V),
3,7 A (230V).
Power consumption
The maximum power consumption is approx. 600 W.
Electrical Fuses
Fuse unit at the rear of the machine: 2 x 8 A T
Miniature fuse 2 x 0.063 A T
on printed circuit board (remove housing)
Miniature fuse 10 A T
in the frequency converter (remove housing)
Material
Maximum feed size approx. 5 mm
Maximum feed quantity 2 x 20 ml
Final fineness
Dry grinding
down to d50 < 20 µm (depending on material)
Wet grinding
down to d50 < 1 µm (depending on material)

Page 7
PULVERISETTE 7
2 Operating Safety
2.1 General Safety Instructions
Read the operating instructions carefully before use.
The instrument can only to be used for the purpose described in sec-
tion 1.3.1 Applications.
Use only original accessories and original spare parts. Failure to do so
may call into question the performance of the instrument.
The operators must be familiar with the contents of the operating in-
structions.
To this end, for example, the operating instructions must with the instrument.
Do not remove labels.
Protective devices must not be made unserviceable or removed.
Unauthorized modification of the instrument or any part thereof will re-
sult in the loss of the conformity to European directives which is as-
serted by Fritsch and the warranty.
Wear protective gloves!
Grinding bowls may be very hot after grinding.
Wear safety glasses
Wet grinding may cause high pressure in the grinding bowl- Danger of
squirting!
Wear ear protectors if the noise level is higher than 85dB(A).
Don’t run the instrument several hours without cooling phases - Dan-
ger of overheating.
Behaviour at all times must be such as to strictly preclude any accidents.
Furthermore, the MAC values at place of work specified in the perti-
nent safety regulations must be adhered to. Where applicable, ventila-
tion must be provided or the instrument must be operated under an
exhaust hood.
Use the instrument only inside. The air must not contain any electrical
conductive dust.
When oxidizable materials such as metals, organic materials, wood, coal,
plastic, etc. are ground or sieved, the risk of spontaneous ignition (dust
explosion) exists whenever the fine particles exceed a specific percent-
age. 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 unsuitable to grind or sieve
materials which are explosive, combustible or promote combustion.
Do not allow the planetary micromill to run unsupervised. Due to the vibra-
tions, under certain operating conditions, the machine may creep along the
surface on which it is located or mounted.

Page 8
PULVERISETTE 7
2.2 Operators
No one other than authorized persons should operate the instrument and it
must be serviced and repaired by trained specialists.
No one suffering from medical problems or under the influence of medica-
tions, drugs, alcohol or overtiredness should be permitted to operate the in-
strument.
2.3 Protective Devices
Protective devices should be used for the intended purpose and must not
be made unserviceable or removed.
All protective devices should be regularly checked for completeness and
to ensure that they are functioning correctly. See section 6 on Mainte-
nance.
The hood must be closed when the machine is started up.
The hood is locked:
when the machine is disconnected from the mains supply
during operation
The hood can be opened only when the drive of the mill has come to a
standstill.
Opening the hood when the machine is disconnected from the mains
supply
1. Remove the plug from the safety lock. It can be accessed via the bore in the
base of the machine.
2. Insert the attached triangular wrench through the bore, and turn clockwise.
3. The closure hatch can now be opened after the spring-loaded lock at the
front of the hood is opened.
4. The planetary micromill can now not be switched on. If it is to be switched
on, the safety lock must be activated by turning the triangular wrench anti-
clockwise, and the hood must be closed.

Page 9
PULVERISETTE 7
2.4 Danger Points
Danger of crushing when the hood is being closed.
Danger of crushing at the grinding bowl holder.
Balance the mill:
Symmetrical charging by using two bowls of the same weight.
2.5 Electrical Safety
General
The main switch disconnects the machine from the mains supply at two
poles.
Switch off the main switch if the planetary micromill is to be inoperative for an
extended period (e.g. over night).
Protection against Restarting
In the event of a mains failure during operation or after switching-off with the
main switch, the hood will remain locked. When the mains voltage is restored,
the lock of the hood will open. For safety reasons, however, the plane-
tary micromill will not start again.
Overload Protection (see Troubleshooting Checklist)
In the event of overloading, the speed of the machine will be reduced.
This is indicated by the OVERLOAD light beeing illuminated.
If the drive motor overheats, the machine will switch off.
If the drive is obstructed, the machine will switch off.
Unbalance Detection (see Troubleshooting Checklist)
In the event of an excessive unbalance, the machine will switch off.

Page 10
PULVERISETTE 7
3 Installation
3.1 Unpacking
Open the bandages with which the hood is fastened on the transport pallet.
The hood is a wooden box placed over the transport pallet.
Lift the hood off the transport pallet.
The cellular parts can be removed now or during the installation. To ease this
removal you can break the performated segments.
Check that the items supplied correspond to your order.
Grinding bowls of hardened steel may exhibit surface indentations caused by
the manufacturing process. These do not influence the grinding or the grind-
ing result and generally disappear after the first grinding.
When present, these surface indentations lie within the permissible manufac-
turing tolerance ranges. Accordingly, complaints regarding such grinding
bowls cannot be accepted.
Please store the transport packing carefully to use it again in case of an
eventual return of the instrument. Fritsch GmbH does not bear the risk of
damages depending on improper packings (non-Fritsch packings).
3.2 Transport
Transport the planetary micromill on the transport pallet with a
fork lift truck or a hand fork lift truck.
To carry the machine, grip it below the edge of the housing.
Carrying the machine will require at least two persons.
3.3 Erection
Lift the planetary micromill off the transport pallet.
Lifting the machine down will require at least two persons.
If the cellular parts have not yet been removed, this can be done now. See
section 3.1 Unpacking.
Place the planetary micromill on a level, stable surface, indoors. It is not
necessary to fasten the planetary micromill on the erection site.
The planetary micromill can also be mounted on a sturdy table.
It is inadvisable to operate the planetary micromill while it is stand-
ing on the transport pallet.
Ensure that there is good access to the planetary micromill. There
must be enough space to reach the main switch.
Do not block the exit of air from the ventilator louver at the side. There
is a danger of overheating if the louver is blocked.

Page 11
PULVERISETTE 7
3.4 Ambience conditions
Use the instrument only inside.
The ambient temperature must be between 5 and 40°C.
Height up to 2000m M.S.L.
Maximum relative humidity of air 80% temperature up to 31C, linear de-
creasing down to 50% relative humidity of air at 40C
Contamination level 2 (IEC 664)
3.5 Electrical Connection
Before making the connection, compare the voltage and current values shown
on the nameplate with the values of the mains supply to which the planetary
micromill is to be connected.
Single-phase alternating voltage with protective conductor (see section 1.4).
The connecting cable may be changed only by a trained expert.
3.6 Adaptation to Mains Supply Voltage / Changing the
Timer / Setup-Mode
The voltage range of the machine should be switched over only by specialist
staff:
1. Disconnect the machine from the mains supply.
2. At the rear of the machine, set the changeover switch to the voltage range.
3. Connect the machine to the mains supply.
4. Press and hold down the STOP button on the control panel at the front.
5. Switch on the main switch at the rear of the machine and release the STOP
button immediately afterwards.
6. The POWER SUPPLY light must flash. If it does not, repeat the
procedure.
7. With the + / - ROTATIONAL SPEED buttons, select the mains
supply voltage level (90 - 260 V).
8. The timer function can now also be altered:
With the right-hand + button in the TIMER panel, select the time
range: Hours and minutes (display: -) or
Minutes and seconds (display: 1)
9. To store the settings and end the setup mode, press the STOP button.
Pressing the + / - REPETITIONS buttons alters the machine type.
Do not change anything here: P7 should be indicated in the display. Oth-
erwise, damage will occur during operation!
CAUTION
Electrical Safeguard!
Danger of damages due to short-circuit.
Ensure that the socket is connected to a power line se-
cured with a circuit breaker.
Caution
Non-observance of the values on the type plate may dam-
age electrical as well as mechanical components.

Page 12
PULVERISETTE 7
3.7 Switching On for the First Time / Test for Correct Func-
tioning
Switch on the machine only when all the work described in section 3 on Instal-
lation has been done.
Switching On
1. Connect the machine to the mains supply.
2. Switch on the machine with the main switch at the rear.
3. The green POWER SUPPLY display will come on.
4. Open the hood.
5. Both bowl holders: clamp the wood or empty bowl with the spindle.
6. Close the hood.
7. Set the speed to 100 on the control panel.
8. Press START on the control panel.
9. The hood will be locked and the mill will run at the preselected speed.
Switching Off
Press STOP on the control panel.
After a short period (after the mill has come to a standstill), the hood is un-
locked and can be opened.

Page 13
PULVERISETTE 7
4 Working with the Planetary Micromill
Warning!!!
Before starting the machine, ensure that the grinding bowl is correctly braced
and there are no loose parts inside the device. There is a risk that loose grind-
ing bowls or parts will be thrown out. 
guarantee or claims will be accepted for damages to the device or injuries to
persons.
Caution!!!
The grinding tools are subject to normal wear. Prior to each comminution the
thickness of the grinding bowl wall is to be inspected. With severe wear the
grinding bowl is to be changed. If not, the possibility exists that the grinding ball
due to high centrifugal forces which occur during the grinding may strike
through the grinding bowl wall, damaging the mill. We don’t honour the warran-
ty or accept complaints for instrument damage or personal injuries occurring
when disregarding the above information.
NOTE
During milling, high temperatures can build up in the grinding
bowl.
In encased grinding bowls, the inserts are glued into the cas-
ing with a two-component construction adhesive.
The adhesive is temperature-resistant up to approx. 140°C.
Above 140°C, the adhesive becomes liquefied and collects
below the insert in the casing. When the adhesive cools
down, it solidifies again and presses the casing upward. As a
result, the insert could get damaged. This always makes the
grinding bowl unusable.
At temperatures above 200°C, the adhesive is ruined. The
same applies for encased grinding bowl lids.

Page 14
PULVERISETTE 7
4.1 Choice of Grinding Bowls and Grinding Balls
Caution!!!
No warranty or claims shall be accepted in case of damages caused on ac-
count of using grinding bowls and grinding balls that are not original accesso-
ries of the appliance.
In order to prevent excessive abrasion, the hardness of the grinding bowl used
and of the grinding balls must be higher than that of the material used.
Material
(bowl and balls)
density*
in g/cm3
restistance to
abrasion
Agate
(99.9% SiO2)
2.65
Good
Sintered corundum 1
(99.7% Al2O3)
3.8
Fairly good
Zirconium dioxide
(95% ZrO2)
5.7
Very good
Stainless steel
bowl:
(17-19% Cr + 8-10% Ni)
ball:
(12,5-14,5% Cr + 1% Ni)
7.8
Fairly good
Tempered steel
bowl: (11-12% Cr)
ball: (1,0-1,65% Cr)
7.9
Good
Tungsten carbide
(93%WC+6% Co)
14.7
Very good
Silicon nitride (Syalon)
(90% Si3N4)
3.1
Extremely good
The grinding bowls and grinding balls of zirconium dioxide are resistant to acids
with the exception of hydrofluoric acid.
Normally, grinding bowls and grinding balls of the same material should be
chosen.
Exeption:
Tungsten carbide balls may be combined with steel bowls.
The size of the grinding bowls and grinding balls should be determined experi-
mentally.
4.1.1 Size of the Grinding Balls
Type of feed material
Ball diameter
Hard samples feed with a piece size be-
tween 2mm and 5mm
15 mm
Fine material (0.5 mm)
10 mm / 5 mm
Homogenisation of dry or liquid samples
10 mm /
These are just clues: the size of the grinding bowls and grinding balls
should be determined experimentally if necessary.
Attentione:
Mixing balls with different diameters is not recommended.
(If different ball diameters are used there is the danger of higher abrasion
of the balls!)
*
High density means high impact energy

Page 15
PULVERISETTE 7
4.1.2 Number of Balls per Grinding Bowl
A larger number of balls reduces the grinding time, and the grinding result will
lie within a narrower grain band width.
Ball Ø
(mm)
Grinding
bowl volume
(ml)
12
45
5
Number of balls
(piece)
50
180 - 200
10
Number of balls
(piece)
6 - 8
18 - 20
15
Number of balls
(piece)
7
The number of balls should be observed to prevent attrition.
4.1.3 Calculated Ball Weight
510 15
Material
density
in g/cm³
Agate 2.65 0.17 1.39 4.68
Sintered corundum 3.8 0.25 1.99 6.72
Zirconium oxide 5.7 0.37 2.98 10.07
Stainless steel 7.8 0.51 4.08 13.78
Tempered steel 7.9 0.52 4.14 13.96
Hardmetal tungsten carbide 14.7 0.96 7.70 25.98
Silicon nitride (Syalon) 3.1 0.20 1.62 5.48
Ball diameter in mm
Calculated ball weight
in g
To calculate the weight of the required balls, the “calculated ball weight” is mul-
tiplied by the “number” of balls needed.
Example: A 45 ml agate bowl must be filled with 185 agate balls of 5 mm diam-
eter.
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;
this saves the time required for counting out the balls.

Page 16
PULVERISETTE 7
4.2 Filling the Grinding Bowl
Grinding bowl
Min. filling
max. filling
45ml
3ml
20ml
12ml
0,5ml
5ml
Using less sample material than recommended will cause
higher abrasion!
It is imperative that the following sequence be observed:
1. Place the grinding balls in the empty bowl.
2. Fill the material to be ground on the balls.
Never use the mill without sample material!
Danger of badly damage of the grinding balls and bowl!
4.3 Influencing Quantities During Grinding
Running time (grinding time)
A longer grinding time will increase the fine fraction.
Speed
A higher speed will reduce the grinding time and increase the fine fraction.
Reversing operation (regular reversal of the direction of rotation)
May improve the grinding; useful for mechanical alloying.
Number and size of the balls
Pregrinding coarse, hard material with large balls:
small fine fraction.
Use of many small balls will increase the fine fraction if the running time is in-
creased.
Mass of the balls (type of material)
A higher mass (density) of the grinding balls will accelerate the grinding.
(See the table in section 4.1.)
4.3.1 Dry Grinding
Below a particle size of approx. 20 µm, surface forces predominate and the
material will start to "stick".
Further dry grinding can be achieved if surface-active substances are added to
the material.
Examples (maximum quantity to be added in % by mass)
Stearic acid 2-3%
Aerosil (microdispersed silicic acid) 0.5-2%
Silica sand ~ 2%
Glass powder ~ 2%
filling = sample material

Page 17
PULVERISETTE 7
4.3.2 Wet Grinding (Grinding in Suspension)
When grinding in suspension, you can add auxiliary substances in liquid
form with a high boiling point and low vapour pressure.
Flammable liquids with a boiling point <100°C should not be used.
4.4 Clamping the Grinding Bowls
The following tests should be performed before the grinding bowls are clamped
in the machine:
Check the cork disc for damage.
Replace cork discs that are black and flattened.
The flat Teflon seal (for sealing between the lid and the bowl) must
not be damaged or dirty.
Replace severely deformed flat Teflon seals.
Check the rubber disc for damage.
Replace rubber discs that are flattened and project laterally beyond
the pressure piece.
The plane surfaces of the counter plate and of the clamp clip must
not be dirty.
The surfaces of the lid and of the bowl on which the flat Teflon seal
rests must be clean.
Clamping
Place the sealing ring and the lid on the bowl.
Insert the grinding bowl in the pot mounting on the cork disc. Do not tilt it.
Screw the spindle down fully until the rubber disc of the pressure piece rests
flat on the lid.
Tighten the spindle by hand.
Screw the counter plate down fully until it rests flat on the clamp clip.
Tighten the counter plate by hand.
After a few minutes of grinding, and in the cooling phases, check that the
spindle and the counter plate are secure.
Attention!
inflammable
substances