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FRITSCH
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Instruction manual
Laboratory Vibrating Cup Mill
„ pulverisette 9 “
Edition 11/1995 Index 001
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Fritsch GmbH Manufacturers of Laboratory Instruments Industriestrasse 8 D - 55743 Idar-Oberstein
Phone: *6784/ 70-0 Fax: *6784/ 70-11 E-Mail: [email protected]: http://www.fritsch.de
Instrument number Model I 09.0030.00 / 09.0050.00 Model II 09.2030.00 / 09.2020.00
applies as of serial number 458
Fritsch GmbH, Laborgerätebau has been certificated by the TÜV-Zertifizierungsgemeinschaft e.V. on June 24, 1994.
An audit certificated the accordance of the Fritsch GmbH to the DIN EN ISO 9001.
The enclosed declaration of conformity calls the directives which the „pulverisette 9“ corresponds to. This permitts us to mark the instrument with the CE-Sign.
pulverisette 9
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Table of contents page1 Safety Symbols, Application and Use ........................................11.1 Indication of general dangers: ................................................................... 12 Safety Instructions .......................................................................23 Unpacking .....................................................................................34 Operating Instructions .................................................................45 Method of Operation.....................................................................46 Operating Safety ...........................................................................57 Erecting the Laboratory Vibrating Cup Mill................................68 Electrical Connection ...................................................................68.1 Checking for correspondence of voltage and current ............................... 68.2 Motor protecting switch.............................................................................. 69 Removing the Shipping Brace.....................................................710 Setting the Clamping Device .......................................................711 Grinding Sets: ...............................................................................811.1 Utilizing the grinding sets:.......................................................................... 812 Reducing the Size of Grinding Material ......................................912.1 Filling the milling vessels ........................................................................... 912.2 Grinding ..................................................................................................... 912.3 Final fineness and grinding time.............................................................. 1013 Cleaning.......................................................................................1014 Warranty ......................................................................................1015 Maintenance and Servicing .......................................................1115.1 Using the grinding set.............................................................................. 1215.2 Setting the contact pressure.................................................................... 1215.3 Checks after each grinding process: ....................................................... 1215.4 Weekly checks and maintenance............................................................ 1315.5 Semi-annual checks and maintenance ................................................... 1311.6 Emergency release of protection switch interlock ................................................ 13
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1 Safety Symbols, Application and Use 1.1 Indication of general dangers:
Combustiblematerials
Materials hazardousto health
Caution Warning symbol of hazards
Danger,electricvoltage
Wear eye protection
Attention: high temperature
possibly the grinding set can get very hot during the grinding process!
high temperature can disturb the grinding set!
Use of Laboratory Vibrating Cup Mill: These operating instructions describe the applications and use of the Laboratory Vibrating Cup Mill.
No other use is permitted!
Make no modifications to the Laboratory Vibrating Cup Mill with-out first consulting FRITSCH and receiving written approval.If modifications are made without approval, the CE conformity confirmed by FRITSCH ceases to apply.
Caution when handling combustible or toxic materials!
Compliance with the relevant safety regulations (MAC values) is mandatory if material to be ground is hazardous to health or dan-gerous. Where applicable, place Laboratory Vibrating Cup Mill in a well-ventilated safety zone.
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2 Safety Instructions Do not remove information signs! Maintenance must be performed by properly briefed personnel! Put covers back on following maintenance! Do not permanently deactivate safety devices! Check safety device regularly!
Only properly instructed personnel are to work on machine! Do not open Laboratory Vibrating Cup Mill until it has come to a
complete stop!
Do not start Laboratory Vibrating Cup Mill until grinding set (grind-ing vessel) mounted and fixed in place!
Do not put hands into mill while it is running! Do not work without safety glasses!
Vibrating cup mill must be set up indoors. Erect on a solid floor. Ambient temperature 0 to 40°C .
Noise level: 81 dB.
Dimensions: 940 x 760 x 650 mm (H x W x D). Weight (net): approx. 310 kg
Danger due to electric voltage: Located on the mill are controlgears with a voltage in the low volt-
age range of 230 or 400 Vrms.
Risk of pinching/crushing exists with hood! Risk of pinching/crushing exists with fastening clip!
Read and comply with the operating instructions!
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3 Unpacking Caution: Vibrating Cup Mill weighs 310 kg. Compare your order with the contents of the crate!
Pull out the staples with a pry bar (or pliers). Lift off the top of the crate. The vibrating cup mill is fastened on the pallet with 4 square tim-bers.You can pull out the nails fastening the square timbers with a pry bar (or pliers). The pallet is so stable that you could even leave the vibrating cup mill on it during operation.
Use a pallet truck to move the pallet:
Use a crane or fork lift to lift the vibrating cup mill off the pallet.
Attach sturdy lifting tackle to the 4 eyebolts screwed into the sides.
If you have to use cable, make certain that they are se-curely fastened to eyebolts, crane hook or forks of fork lift.
Pull the free ends through the eyebolts at the sides of the vibrat-ing cup mill and tie a knot.
The control box to operate the vibrating cup mill is enclosed, not attached. To attach the vibrating cup mill, bolt the side bracket on the right-hand side with the 4 bolts enclosed. Plug the cable con-nector for the vibrating cup mill into the plug-and-socket connec-tion on the right-hand side.
Do not switch on the vibrating cup mill until the shipping brace has been removed.
Do not switch on the vibrating cup mill until the grinding vessel has been installed.
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4 Operating Instructions The laboratory Vibrating Cup Mill "pulverisette 9" is employed for rapid intermittent dry or wet fine grinding of brittle to very hard material samples, e.g. from the fields mining (coal, ore, minerals), metallurgy (slag, cast samples), the ceramics industry, the ce-ment and building materials industry, agriculture and forestry. The quantity of material to be crushed depends on the model of grinding set used; the maximums are 50, 100 and 250 ml. The initial sample size also depends on the model and size of the grinding set and is max. 7 and 12 mm.
5 Method of Operation The "pulverisette 9" operates on the vibration-grinding principle, i.e. The grinding set is placed on a vibrating disk and the grinding elements in it (disk and rings) are accelerated by centrifugal force and grind the sample due to both impact and friction. The grinding sets (made of hardened steel, tungsten carbide or agate) are sealed with an inlaid gasket, eliminating losses during wet or dry grinding. With model I, the powerful drive motor has two different rotational speeds (750 and 1,000 RPM), making it possible to adapt the grinding effect to practical requirements. The high speed is auto-matically blocked when the agate grinding set is used, as this is sensitive to impact. Model II achieves a rotational speed of 1,500 RPM and is particu-larly suitable for utilization with sets made of tungsten carbide or hardened steel in the 100 or 250 ml sizes. In many cases with this model, grinding yield the same results in a relatively short time. Utilization of this model is particularly suitable if an ex-tremely hard material is to be ground in a very short time. The agate grinding set is not to be used on model II.
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6 Operating Safety The Laboratory Vibrating Cup Mill has an extensive safety sys-tem:
1. During operation, a protection switch with safety interlockmonitors the start-up of the Laboratory Vibrating Cup Mill after the mill is switched off and the cover is open.
The mill is locked during operation. The Laboratory Vibrating Cup Mill won't start when the
hood is open. The hood cannot be opened until the mill is at a standstill
and the "Hood" button has been pressed. The cup mill cannot be opened once it is deenergized (it
can be opened only via emergency release of interlock). 2. The Laboratory Vibrating Cup Mill features the correct motor
protecting switch for the mains voltage (listed on nameplate). 3. In the event of an overload or a faulty motor, the protecting
switch automatically interrupts the supply of electricity. The mill can be switched back on once the malfunction has been eliminated and the motor protecting switch has cooled down.
4. Press the Start button to switch on the Laboratory Vibrating Cup Mill.
Do not switch on until the shipping block is removed. Do not switch on until grinding set is installed.
5. Press the Stop button to switch off the Laboratory Vibrating Cup Mill.
6. In the event of a power failure during operation the Laborato-ry Vibrating Cup Mill comes to a stop in about 3 seconds.
7. When the power returns, the Laboratory Vibrating Cup Mill does not start.
Vibrating cup mill is secured against restart. Press the Start button: The Laboratory Vibrating Cup Mill
starts.
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If the Laboratory Vibrating Cup Mill is "out of order" for a pro-tracted
Night cut-off: Separate Laboratory Vibrating Cup Mill from mains.
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7 Erecting the Laboratory Vibrating Cup MillPlace the Laboratory Vibrating Cup Mill on a flat, stable base. No fastening is required. You can also leave the Laboratory Vibrating Cup Mill on the stable shipping pallet when you start the mill.
8 Electrical Connection 8.1 Checking for correspondence of voltage and
currentBefore connecting the Laboratory Vibrating Cup Mill, make cer-tain that the voltage and current values specified on the name-plate correspond to the those of your local electrical supply:
Model P9/I 3~ 230 V ± 10%; 50 to 60 Hz with protective conductor
950 watt power consumption under high stress(markedly lower in normal use), fuse 16 A
3~ 400 V ± 10%; 50 to 60 Hz with PEN conductor and pro-tective conductor 950 watt power consumption under high stress(markedly lower in normal use), fuse 16 A
Model P9/II 3~ 230 V ± 10%; 50 to 60 Hz with protective conductor
2900 watt power consumption under high load (markedly lower in normal use), 230 / 400 volts,fuse 16 A
3~ 400 V ± 10%; 50 to 60 Hz with PEN conductor and pro-tective conductor 2900 watt power consumption under high stress(markedly lower in normal use), fuse 16 A
Pole-changing model I drive motors are permanently set to the specified voltages at the factory and cannot be changed subse-quently.
8.2 Motor protecting switch The motor protecting switch in the breaker enclosure interrupts the flow of power when the motor is overloaded, bringing the mill to a standstill. In the case of model I, the motor protecting switch is ready for operation a short time thereafter and the mill can be switched back on when the malfunction is remedied. To restart model II after the malfunction is remedied, you will have to remove the front panel of the break enclosure and press the blue "RESET" button (contactor). You can restart the mill af-ter you close the front panel.
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9 Removing the Shipping Brace To remove the shipping brace: 1. Open the hood:
Turn the master switch on. Press the button "Open the
hood".2. Open the grinding vessel clamp-
ing device and remove the piece of wood clamped in it.
3. Remove the two M 10 locking screws on the vibrating plate.
10 Setting the Clamping Device Adapt the clamping device to your grinding set: 1. Insert the clamping set:
Insert the grinding device (grinding set) into the receiver on the vibrating plate such that the two surfaces milled on the sides fit into the circular seg-ments, locking the clamping lever.
Attention: The entire contact surface of grinding set must touch the receiver ring. 2. Setting the contact pressure: The contact pressure is adjusted with the aid of spacer rings.Loosely place the fasten-ing clip with rubber buffer loosely on the set. Place the clamping head such that the inside ring fits into the semicircular recess of the fastening clip.The clamping lever is then almost vertical. If the clamping lever is slanted more than about 15° towards the clip, unscrew the rubber buffer (16) and place further spacer rings under the rubber buffer before bolting it back on. Push the clamping lever down hard until it snaps down by itself in the lower area - when you have pressed the clamping head over the bent lever closure. If it is extremely difficult to push the clamping lever down and you cannot hear it snap in, remove one or two of the spacer rings un-der the rubber buffer.
safety screws
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11 Grinding Sets: You can employ the following grinding vessels:
Useful contents of grinding vessel
50 ml 100 ml 250 ml
Grinding element 1 washer 1 washer, 1 ring 1 washer, 2 rings Order numbers Hardened steel 48.1050.00 48.1100.00 48.1250.00Reducing Ring 48.0020.09 48.0010.09 ----Tungsten carbide 48.2050.00 48.2100.00 48.2250.00Agate (steel mount) 48.3050.00 48.3100.00 - ----
11.1 Utilizing the grinding sets: 1. Laboratory Vibrating Cup Mill "pulverisette 9", model I (750/1,000 RPM) Grinding vessel 50, 100 and 250 ml Hardened steel 50, 100 and 250 ml Tungsten carbide 50 and 100 ml Agate with automatically reduced speed of 750 RPM
2. Laboratory Vibrating Cup Mill "pulverisette 9", model II (1,500 RPM) Grinding vessel 100 and 250 ml Hardened steel 100 ml Tungsten carbide
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12 Reducing the Size of Grinding Material 12.1 Filling the milling vessels
1. Place the grinding elements in the grinding vessel such that their rounded edge is at the bottom.
2. Fill the material to be crus-hed uniformly between the grinding rings (note the maxi mum useful volumes 50, 100 and 250 ml).
3. Clean the sealing surface and put the cover on so that it seals well.
12.2 Grinding Caution: High temperature: Grinding set becomes very hot during grinding! Do not exceed the maximum grinding time, 15 minutes! Before continuing a grinding process:
Let grinding set and crushed material cool to room tempera-ture!
Never switch on the Laboratory Vibrating Cup Mill unless grinding set has been inserted.
Never switch on Laboratory Vibrating Cup Mill while grinding sets are empty (contain no crushed material):
More wear develops and the grinding elements are da-maged.
Kits made of agate must be filled with material to at least about 40% the useful volume.
Place the filled grinding set into the plate receiver and clamp the clamping lever so tightly that the rubber buffer presses hard against the cover of the vessel (see Section 6, "Setting the Clamping Device"). Afterwards, close the Laboratory Vibrating Cup Mill. Use the timer to set the time module and the desired processing time.On the basis your results, determine the speed and the process-ing time to be selected. The average grinding time is between 1 and 5 minutes.With the model I Laboratory Vibrating Cup Mill you can select the speed of the mill by pressing the relevant buttons: Press button II (1,000 RPM) for faster milling. If you press the speed "Button I" (750 RPM), the material to be
crushed and the set are handled more gently. The high speed is automatically blocked to the agate grinding
set.
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The model II Laboratory Vibrating Cup Mill achieves a speed of 1,500 RPM. It is particularly suitable for the use of grinding sets made of tung-sten carbide (100 ml) and hardened steel (100 ml or 250 ml). The agate set is not to be used with the model II mill.
12.3 Final fineness and grinding time The attainable final fineness depends primarily on the grinding time. Under favourable preconditions (good crushability of the material) it may be in a tight bandwidth under about 40 μm. The required grinding time depends on the crushability of the sample and the desired final fineness. It is influenced by the
size of the grinding vessel - and thus also by the number of grinding elements, type of material, grinding vessel and speed of the Laboratory Vibrating Cup Mill.
Certain materials tend to "bond" during the grinding, i.e. the ma-terial is baked onto the outside wall and the grinding elements if the grinding process has already progressed relatively far. Wet grinding is advisable in this case. On average, a higher high fine-ness is achieved during wet milling.
13 Cleaning To clean the grinding vessels, hold vessels under running water and use a brush and conventional, mild detergent. Depending on how dirty the set is, you can also "grind the set un-til clean" with a small amount of sand (50 ml) in a brief grinding process.Following a wet cleaning, always dry the set before putting it away.
14 Warranty The warranty card accompanying this mill when delivered must be filled out completely and returned to the delivering factory in order for it to take effect. The company FRITSCH GmbH, Idar-Oberstein, Germany, its ap-plication technology laboratory or our representatives in your country will be glad to provide advice and assistance. Please in-dicate the serial number stamped on the nameplate if you have any questions.
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15 Maintenance and Servicing Cleaning the Laboratory Vibrating Cup Mill carefully is a precon-dition for its safe use. Aside from following the instructions for care and maintenance described here, make certain that the electrical supply conductor and equipment operate correctly - especial that the safety ele-ments are installed appropriately and operated correctly. All articulated joints must be serviced at certain intervals, de-pending on the length of time in use. The maintenance intervals mentioned here apply for a period of use of about 2 hours daily. Do not neglect testing and maintenance: This leads to consider-able damage to the mill and may result in cancellation of claims under the warranty. Cons. No.Qnty. Article No. Designation 1 2 91.617.09 Socket hex dowel screw 2 2 91.795.09 Washer 13 DIN 125 3 2 91.992.09 Lock washer Nordlock M10 4 2 92.418.09 Hex nut M10 DIN 439 5 2 82.802.00 Bushing D = 12 / 25 6 1 92.505.00 Cyl. button GN 519-29-M12 7 1 09.120.09 Clamping lever 8 1 93.416.00 Rubber buffer D = 25 x 25 9 1 92.116.09 Headless pin M6x25 DIN 553 10 1 09.102.29 Clamping head 11 1 09.124.09 Hinged pin 12 2 92.431.09 Locking ring 13 1 82.613.09 Inner ring 14 1 09.127.09 Setbolt 15 1 09.103.29 Clamp clip 16 1 93.415.00 Rubber buffer D = 50 x 18 17 1 09.101.29 Fastening clip 18 (4)* 09.122.09 Equalizing ring 1 mm 19 (3)* 09.123.09 Equalizing ring 2 mm 20 1 91.791.09 Hex nut M12 B ISO 4035 21 6 91.301.09 Fillister head bolt M5x12 - 12.9 DIN 912 22 2 09.136.09 Locking element
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15.1 Using the grinding set The grinding set must be used with those surfaces which have been milled on the sides inserted into the circular sections (part 22). The circular sections are bolted to the vibrating plate. When old grinding sets are used, you must unbolt the circular sections.Attention!! The entire contact surface of the grinding set must be seated on the receiver ring.
15.2 Setting the contact pressure The contact pressure is adjusted with the aid of the equalizing rings (parts 18 and 19). Insert the grinding set "correctly" (see Section 11.1) and place the fastening clip (part 17) with the rub-ber buffer 50 x 18 (part 16) loose on the set. Place the clamping head (part 10) with the inner ring (part 13) into the milled semicircular recess in the fastening clip. The clamping lever (part 7) must be pointed almost straight up (max. 15° in the direction of the fastening clip). If the clamping lever is slanted more than 15° in the direction of the fastening clip, you must unbolt the 50 x 18 rubber buffer (part 16) and place further equalizing rings (parts 18 and 19) under the rubber buffer. Press the clamping lever down hard until it snaps down by itself in the lower area - if you have pressed the clamping head over the bent lever closure. If it is extremely difficult to push the clamping lever down and you cannot hear it snap in place in the bottom area, remove one or two of the spacer rings.
15.3 Checks after each grinding process: Nuts M10 (part 4) seated tightly Locking rings (part 12) secure and tight The two rubber buffers (parts 8 and 16) seated tightly clamping lever (part 7) and locking nut (part 20) seated tightly
in clamping head (part 10) and cylinder button (part 6) seated tightly
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15.4 Weekly checks and maintenance (10 hours of operation) Tight seating of the 6 socket hex bolts (part 21) used to fasten
the disk shaped segments to prevent them from turning in the receiver for the grinding set.
Check the disk shaped segments for wear (exchange if nec-essary).
Check the rubber buffers for wear (exchange if necessary). Lightly oil all articulated joints with machine oil.
15.5 Semi-annual checks and maintenance (300 hours of operation) Check all bushings (part 5) for deformation and distortion
(change if necessary). If the bushings are completely worn out, the bore will begin to deform; the clamp clip (part 15) and the fastening clip (part 17) must be exchanged.
11.6 Emergency release of protection switch inter-lockOnce the Laboratory Vibrating Cup Mill is deenergized, the pro-tection switch can be unlocked with the triangular key provided. Afterwards the mill can be opened.
The Laboratory Vibrating Cup Mill cannot be put into service when the switch is unlocked. Unbolt the cover plate
on the left-hand side of the Laboratory Vi-brating Cup Mill.
Insert the triangular key through the opening and turn the switch clockwise.
After opening the cover, reset the interlock of the pro-tection switch.
