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C H E M I S T S
Microsampling Inserts
Operator Manual
MA047
M I L E S T O N E
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
INDEX
Total pages 13
Caution!
Please read the operator manual before using the instrument!
Place the Teflon cover on the Sample holder vessel. Note the
slot on the side where the temperature sensor is to be
inserted.
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.
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.
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.
Now put the special HTC safety spring onto the HTC adapter
plate.
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.
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).
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
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.