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Volumes
Minimum volume :
• 10 mL (without inserts)
• 5 mL (with QS-50 quartz inserts)
• 1 mL (with 3-positions rack inserts)
Temperature
Maximum working temperature: 230°C
Pressure
Maximum working pressure: 100 bar
Acid solutions
The possibility of use different types of acid solutions is strictly related to the material of the vessels and
accessories.
TFM vessels and TFM inserts: HNO3 , HCl, HF, HBF4, H2SO4, H3PO4, HClO4, H2O2
Glass and quartz inserts: HNO3 , HCl, HBF4, H2SO4, H3PO4, HClO4, H2O2
SK-15 Segments
Each closed, microwave sample preparation vessel is actually a system of components. They function in
tandem to provide :
1. A closed, clean environment for containing the sample during processing, thereby preventing
contamination;
2. A closed container that prevents loss of volatile species, even when processing materials at
temperatures far above the normal boiling point of the mixture;
3. A closed container that minimizes the use of expensive acids/solvents;
4. A system that can safely release (vent) over-pressure in the vessels, then reseal the vessel and
continue the microwave process until completion.
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Milestone Srl MA176-002 –SK15– User Manual
Components
Each SK-15 segment assembly is a system of components that consists of :
1) A rotor segment with a compressor screw that ensures the right positioning of the vessel and the
approppriate pressure applied on the safety spring;
2) A vessel that contains the sample;
3) A vessel cover that seals the vessels and acts as an overpressure reseal valve;
4) A safety spring that allows a safe and controlled release of gases from the vessels, in case of
overpressure and a perfect reseal;
5) A safety shield that surrounds the vessel and prevents deformations at high temperatures and
pressures.
Labeling
Milestone recommends to store the components of each individual vessel assembly as a set.
Vessels and covers, in particular, should share a common history and Milestone suggests not to mix new
vessels with old ones, but to keep them in separate batches.
This will facilitate maximum useful lifetime, maximize performance for routine operations at the limits of
vessels specifications and easy identification, isolation and replacement of worn components when they
begin to affect sample preparation performance.
Milestone suggests labeling each complete vessel assembly. A diamond-tipped scribe is recommended to
mark the bottom of the TFM vessel and the top of the TFM cover.
Usage Log
A log system is an important tool to help in determining the expected lifetime of the assemblies in particular
application and can provide a rationale for budgeting for future consumables purchases. A usage log can
also help in tracking variable sample results by providing a complete elemental history for the vessel.
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Milestone Srl MA176-002 –SK15– User Manual
Reference vessel(s)
The reference vessel is a specialized vessel that facilitates reaction parameter monitoring (temperature
and/or pressure) and allows feedback process control.
To allow feedback process control, a reference vessel must be prepared to contain chemistry identical to any
other sample vessel being processed during the same run.
What differentiates the reference vessel from the other vessels (standard vessels) is basically the cover.
There are two different reference covers available for SK-15 rotor : ATC reference cover for temperature
monitoring and APC reference cover for pressure monitoring.
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Milestone Srl MA176-002 –SK15– User Manual
The springs MUST be completely dry from any acid and water drops.
NEVER clean the springs with water, acids or solvents
Milestone recommend to replace safety springs after 500 runs or one year of work.
The pressure sensor enables the control of a microwave program by measuring the reaction pressure in the
reference vessel.
The pressure sensor installed outside the sample chamber is connected by a pressure tube to the pressure
vessel.
The pressure tube is designed for routine operations up to 50 bar for maximum 20 minutes. At higher
pressure it has shown an increased stress.
When programs above 50bar are used, an accurate monitoring of the program run is necessary.
In SK-15 rotor the internal pressure can be measured, represented and controlled during a run by the
special pressure cover.
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Milestone Srl MA176-002 –SK15– User Manual
Milestone recommends to handle the components of the APC reference vessel assembly
(cover + vessel) as a set.
Setting APC tube is necessary to remove the vessel positioned on the right side of the reference
(Fig.B).
Fig. A Fig. B
The TWIST function of microwave unit must be activated when APC (pressure) sensor is
used together with ATC sensor, otherwise both sensors will be damaged.
Before every start, check that the pressure tube and the temperature sensor can freely
move, without getting stuck and twisted against each other. This is also true for a start
after a rotation interruption.
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Milestone Srl MA176-002 –SK15– User Manual
To clean the line, fill the reference vessel with 20 mL of water, secure the reference vessel in its
corresponding segment and execute a brief program that brings the water to high temperature, so
that the generated steam will flush the line.
Time Temperature
00:10:00 150°C
00:05:00 150°C
This may indicate leakage of reaction vapors, under temperature and pressure, around the hex nut
plug.
The plug should be tightened using the slip wrench and, if the discoloration continues, the line
should be replaced.
In extreme cases, the cover will need to be replaced.
Operating tips
The following is an overview of all operating steps (sample weighing, acid addition, vessel closure/opening)
with some important tips and suggestions to work at best with your SK-15 high pressure rotor.
Sample Weighing
As per rotor specifications, the maximum sample amount is 1 g considering a dried organic material.
Anyway, the sample amount can be different according to the sample reactivity.
Water samples
- 45 mL
(i.e.EPA 3015)
During the weighing in the PTFE vessels, some powdered samples can show “electrostatic” issues,
making the weighing procedure more difficult and causing instability of the balance.
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Milestone Srl MA176-002 –SK15– User Manual
Anti-electrostatic gun
Acid additions and digestion temperature
Milestone recommends that all additions of acid mixtures or hazardous solvents to the
vessels should take place inside an appropriately vented fume-hood.
In order to obtain a good digestion result, the sample must be completely wet by the acid and the
acid volume must be enough in order to complete the digestion.
As we have seen previously, the minimum volume for SK-15 is 10 mL in order to allow the end of
the thermowell to be sufficiently submerged by the solution.
Vessels closure
- Proper Torqueing
The closure of the vessel assembly is one of the most important steps, because it is directly related
to the pressure capacity of the vessel itself.
The handle of the torque wrench should be grasped with one hand
(near to the end) and the other hand should grip the segment body.
Long rather than short movements of the wrench are best. Several
long, smooth, continuous arcs of the wrench should be used to secure
the vessel assembly until the wrench clicks.
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Milestone Srl MA176-002 –SK15– User Manual
This issue can be easily solved spraying PTFE lubricant directly on the
pressure screw.
Milestone suggests to repeat this operation every six months.
SK-15 vessels, as well as any other kind of microwave vessels, should never be opened before they
have been sufficiently cooled down. In this way you will not only eject hot acid vapors from the
vessels, but it will also reduce the useful life of the vessel components.
The rotor or segments should be secured in the workstation and under a fume-hood.
When opening vessels, very short movements of the torque wrench are best. With each short turn
of the pressure screw, one listens and looks for release of process vapors. With each release of
vapors, you should pause briefly until the release stops and only then should the pressure screws be
given an additional turn.
This is repeated until no additional pressure releases are noted.
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All external surfaces of vessel components should be cleaned and dried before they are reassembled and
used for the next microwave sample preparation process. It is particularly important to eliminate any
moisture or process residues from between component surfaces (between the vessel and safety shield,
between the vessel cover and safety spring, etc.). Such trapped moisture or residues will accelerate the
degradation of components during subsequent heating cycles.
Surface Cleaning
1. Single Rinse – In some applications, particularly where the concentration of the analyte of interest is
sufficiently high, vessel cleaning may involve nothing more than simply rinsing the vessels with
deionized water after each use. This may be appropriate when little or no analyte is retained on the
surface or when the analyte concentration is very high (percent level).
If large organic molecules are the analytes of interest, such as when microwave acid extractions are
being performed, then rinsing with clean solvent may be all that is necessary as large molecules do not
easily diffuse into the vessel material.
2. Closed Vessel Acid Reflux –The reflux cleaning technique consists of processing a blank in the closed
vessels. In this procedure, the acids or solvents used to process samples are run in the vessels under
the same time, power and temperature conditions used to digest them (usually 180 °C – 200 °C). The
blank is then discarded and the vessels rinsed and dried before.
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Milestone Srl MA176-002 –SK15– User Manual
The above procedures are used specifically for closed vessel cleaning techniques. It is never
appropriate to heat an open vessel containing acids in the Milestone Microwave Labstation.
Heating acids in open vessels does not provide the elevated temperatures that can be obtained
in closed vessels. Furthermore, operators will be exposed to acid vapors and instrument
longevity may be affected.
1. PFA or TFM vessels and covers (excluding the reference cover) are submerged in a container of
high purity acid, typically 1:1 nitric acid and water, and heated on a hot plate to between 80°C - 90°C
for an hour, or more. The vessels and covers are then rinsed with high purity deionized water and
allowed to air dry before they are used to process samples.
2. A further step is to submerge vessels and covers (excluding the reference cover) in a container of a
second-high purity acid, typically 1:1 hydrochloric acid and water, and heated on a hot plate to
between 80 °C – 90 °C for an hour, or more. The vessels and covers are then rinsed with high purity
deionized water and allowed to air dry before they are used to process samples.
3. Some may need to use even a third step in the cleaning process. After the hot acid cleaning steps, the
vessels and covers are submerged in high purity deionized water, and heated on a hot plate to between
80 °C – 90 °C for an hour, or more. The vessels and covers are then allowed to air dry before they are
used to process samples.
There is no definite period of time that can be recommended for the cleaning process. Only experience and
the demands of the particular application will determine the time required to thoroughly leach contaminants
that have diffused into the bulk of the vessel material. Some users complete one, two or three of the
cleaning steps outlined above. The period for each step may extend anywhere from 1 to 24 hours.
TFM vessels and covers, due to their extensive use, could accumulate NOx that could affect the microwave
performance (TFM starts absorbing MW).
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Milestone Srl MA176-002 –SK15– User Manual
This mainly occurs in case of digestion temperatures over 200°C and is accelerated by even high
temperatures and high pressure.
- Rinse the pre-cleaned vessels with deionized water thoroughly and place them at least for 4 hours in
a drying oven (ventilated, if possible) at 140°C.
- PTFE vessel should be placed with the opening facing up.
- PTFE cover should be placed with the bottom side facing up.
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