MILESTONE
H E L P I N G
C H E M I S T S
Microsampling Inserts
Operator Manual
MA047
M I L E S T O N E
USER MANUAL
MILESTONE MICROSAMPLING INSERT USER MANUAL
Thank you for choosing this accessory for the Milestone microwave system.
We are sure that you will be completely satisfied with the performance of this new accessory entering your
laboratory.
We invite you to read carefully this user manual and to keep it in reach for convenient and fast
consulting. The person who will be using this accessory should have received an appropriate
training from a Milestone trained technician.
For any possible clarification or any request for assistance please contact either our Representative in your
country:
Milestone Srl
Via Fatebenefratelli, 1/5
I-24010 Sorisole (BG) Italy
Phone +39-035-573857
Fax +39-035-575498
Web site [Link]
Email analytical@[Link]
Or Milestone distributor in your country at:
MICROSAMPLING INSERTS User Manual Rev. 3/2009 – Page 1
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USER MANUAL
INDEX
HOW TO OPERATE WITH THE MICROSAMPLING INSERTS
SAMPLE WEIGHING, REAGENTS ADDITION AND VESSEL CAPPING
SETUP OF THE REFERENCE VESSEL, USED FOR TEMPERATURE CONTROL
COOLING DOWN AND UNCAPPING THE VESSELS Page 3-12
MICROSAMPLING INSERT PROCEDURE Page 13
Total pages 13
Caution!
Please read the operator manual before using the instrument!
SYMBOLS USED IN THIS MANUAL
An instruction accompanied by this symbol provides a cautionary statement: WARNING.
Failure to follow the instruction may endanger the user or cause damage to the instrument.
Please read carefully this instruction.
MICROSAMPLING INSERTS User Manual Rev. 3/2009 – Page 2
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USER MANUAL
HOW TO OPERATE WITH THE MICROSAMPLING INSERTS
The below procedure relates to the use of microsampling
TFM or Quartz inserts (P/N 34247 3ml or P/N 34477 6ml).
Picture shows the Sample holder P/N 34475, Teflon inserts
of 6ml P/N 33607 and PH00007 TFM Cover.
The weight of the Teflon insert is about 7 g, therefore
most analytical balances may be used for the purpose.
Place a Teflon insert directly on the balance plate.
Then tare the Teflon insert and directly weigh the sample
by placing it inside the insert.
Try to reduce as much as possible sample transfer, to
avoid contamination.
Add suitable reagents to the sample. When part of the
sample is left on the inner wall of the Teflon inserts, try to
wet it by adding acids drop by drop.
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Gently swirl the solution, to homogenize the sample with the
acid.
Introduce the Teflon insert into the Sample holder and its
TFM cover (PH00007).
Place the Teflon cover on the Sample holder vessel. Note the
slot on the side where the temperature sensor is to be
inserted.
Introduce the Teflon vessel into the HTC protection shield.
WARNING
The wall surfaces of the HTC protection shield, as well as the outer wall of the Teflon
vessel, must be dry and clean. Damages may occur otherwise.
Add suitable reagents to the Teflon vessel. Optimize outside
to inside reagent ratio. Sample and reagents in the insert
must not heat faster than the outer solution to avoid sample
boiling over.
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WARNING
It is recommended to use at least 12 mL of solution inside the vessel, to allow the
temperature sensor to be in contact with the liquid.
Introduce the sample holder into the Teflon vessel.
Place now the reference cover onto the vessel, as shown by
the next picture – carefully slide it down in the slot along the
side of the sample holder.
WARNING
When closing and opening the reference cover, be sure to lift the cover straight up to
avoid cracking the thermowell. Careful inspection of the thermowell should be carried
out before each use. Cracked thermowells must not be used!
The special HTC adapter plate goes onto the reference TFM
Teflon cover.
The indentation of the HTC adapter plate has to match the
indentation of the TFM Teflon cover; you will notice also that
the HTC screw will match the grove machined in the bottom
part of the TFM Teflon cover.
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Now put the special HTC safety spring onto the HTC adapter
plate.
The reference HTC spring differs from the others; it has a
smaller diameter to allow the introduction of the thermocouple
into the vessel.
Introduce the reference vessel just assembled into the reference
polypropylene segment.
Tighten the reference vessel in the same way as the other
vessels.
Introduce now the thermocouple into the reference vessel,
simply sliding-in the sensor through the hole in the HTC screw of
the reference segment.
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Detail of the upper part of the reference vessel.
The hole for the thermocouple is aligned with the thermowell,
allowing the temperature sensor to be fully introduced in the
vessel. Fully introduce the temperature sensor into the
thermowell, until the snap connector is fixed.
Introduce the segmented rotor top plate; the plate is fixed by
the connectors to each individual polypropylene segment.
Lift up one side of the top plate to facilitate the introduction of
the reference segment; then relocate back the top plate in its
position.
Details of the upper part of the reference segment complete with
rotor top plate.
Notice the temperature sensor snap, which must be free to
turn.
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Unplug now the jumper of the ATC-400 Automatic
Temperature Control device of the ETHOS.
A beep sound will be heard.
Plug-in now the temperature sensor.
Bend the temperature sensor as shown by the next picture.
This positioning of the rotor and of the sensor is now correct.
Close the door of the ETHOS and start a digestion program
(refer to the Milestone Application note for microsampling
inserts).
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COOLING DOWN AND UNCAPPING THE VESSELS
After the heating cycle has been completed, allow a 5-minute cooling time of the vessels into the microwave
cavity.
Then open the door of the ETHOS and carefully the
thermocouple from the reference vessel.
WARNING
Due to a substantial expansion of the plastics
used at high temperature, the removal of the
thermocouple should be done only when the
inner temperature of the vessel is
approximately 180°C.
Once the microwave program is completed, high temperature and pressure are reached inside the vessels,
according with the sample preparation procedure applied.
It is therefore necessary to cool down the rotor before opening the vessels.
The rotor may be air cooled inside the ETHOS and in such case the cooling time is around 25 minutes
(approximately 6-8°C/minute).
Alternatively, the segments may be removed from the ETHOS microwave cavity and immersed in a water
bath.
In such case the cooling time is around 10-15 minutes
(approximately 10-15°C/minute).
Once reached a temperature close to room temperature
the vessels can be opened.
Take the torque wrench and set the indicator to the
“open” position, as shown in the next picture.
Locate the work station under a fume hood, and
carefully loosen the screw in the upper part of each
individual segment, by using the torque wrench.
Open the vessels very slowly, since a certain pressure
may still be present, depending on the sample type,
even if the temperature is as low as room temperature.
Open the vessel opposite to your position.
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Remove the vessel from the polypropylene segment.
Carefully lift up the vessel cover, together with the TFM
Teflon indicator ring.
Remove the Sample holder from the TFM vessel as shown.
Pour the solution in a laboratory volumetric flask, washing
repeatedly the Teflon insert with distilled water.
Repeat the same operation with all vessels in the rotor,
including the reference vessel.
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TFM/Quartz Microsampling Insert Procedure
SUMMARY
This method provides for acid digestion of organic sample in a closed vessel
device using temperature controlled microwave heating for determination of
metal by spectroscopic methods.
MICROWAVE EQUIPMENT
Milestone ETHOS Labstation with temperature control, medium or high pressure rotor TFM/Quartz
microsampling insert
(Sample Holder P/N34475, Teflon insert P/N 33607 or Quartz insert P/N 34247).
SUGGESTED SAMPLE AMOUNT
<100mg*
REAGENTS
Internal reagent (into the microsampling insert 3 ml) : 1-2 ml of HNO3 65%
External reagent (into the TFM vessel 100 ml): 11 ml of H20, 1 ml of H202 30%
PROCEDURE
1. Place a TFM/Quartz microsampling insert on the balance plate, tare it and weigh sample.
2. Add the acids; if part of the sample stays on the inner wall of the insert, wet it by adding acids drop
by drop, then gently swirl the solution to homogenize the sample with the acids (see internal
reagent listed above).
3. Introduce the inserts into the Sample holder.
4. Place the TFM cover onto the Sample holder.
5. Introduce the TFM vessel into the HTC safety shield.
6. Add suitable reagents into the TFM vessel (see external reagent listed above).
7. Introduce the sample holder into the Teflon vessel.
8. Close the vessel and introduce it into the rotor segment, then tighten by using the torque wrench.
9. Insert the segment into the microwave cavity and connect the temperature sensor.
10. Run the microwave program to completion.
11. Cool the rotor by air or by water until the solution reaches room temperature.
12. Open the vessel and transfer the solutions from the inserts into marked flasks.
MICROWAVE PROGRAM
Step Time Temperature Microwave power
1 15 minutes 180°C Up to 1000
Watt**
2 10 minutes 180°C Up to 1000
Watt**
MICROSAMPLING INSERTS User Manual Rev. 3/2009 – Page 11
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TEMPERATURE PROFILE
NOTES
* The sample must be completely wet.
**Use up to 500 Watt for operations with 3 or less vessels simultaneously.
This procedure is only a guideline and it may need to be modified or changed to obtain the
required results on your sample.
Always use hand, eye and body protection when operating with the microwave system.
MICROSAMPLING INSERTS User Manual Rev. 3/2009 – Page 12
MILESTONE
Milestone Srl - via Fatebenefratelli 1/5 - 24010 Sorisole (BG) - Italy
Phone +39 035 573857 - Fax +39 035 575498
H E L P I N G
e-mail: analytical@[Link] - web: [Link]
C H E M I S T S
