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Milestone Srl MA176-002 –SK15– User Manual

SK-15 rotor Tips and Techniques


General working specifications
Sample amount
Maximum sample amount: 1 g (of organic
dried matter)

Volumes
Minimum volume :
• 10 mL (without inserts)
• 5 mL (with QS-50 quartz inserts)
• 1 mL (with 3-positions rack inserts)

Maximum working volume :


• 50 ml (without inserts)
• 15 mL (with QS-50 inserts)
• 3 mL (with 3-positions rack inserts)

Temperature
Maximum working temperature: 230°C

Maximum holding time at maximum working


temperature: 30 minutes

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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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.

Etching the sides of vessels is not recommended.


Vessels must not be ink-labeled. The label colour contaminates the protection shields and diffuses
into the vessels.

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.

ATC Reference vessel cover


ATC reference vessel cover is the essential component of SK-15 rotor.
ATC reference vessel cover has a PTFE coated, closed end ceramic thermowell that allows the introduction
of a sensing probe for direct temperature monitoring and control.

Care of ATC reference vessel cover


The reference vessel must be maintained in working order. An improperly used or improperly
maintained reference vessel may prevent the correct feedback of temperature information and
interfere with control of the reaction conditions.
Once the reference vessel cover is assembled, it should not be disassembled, except for replacing
the ceramic thermowell.

Opening ATC reference vessel


Particular attention must be payed during opening operations.
The vessel must be opened by moving the reference cover straight up vertically, otherwise the
thermowell could get damaged.

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Safe storage of the reference vessel cover


Once assembled, the reference vessel cover must be protected from mechanical stresses that could
damage the ceramic thermowell.
By far the safest way to store the reference vessel cover is to fully assemble an empty reference
vessel and secure it (without torquing) in a reference rotor segment.

Examining the Ceramic thermowell – what to look for

Before each use of the reference vessel cover, the operator


should examine the entire lenght of the thermowell, looking for
eventual cracks.

A crack will appear as a faint white line around the


circumference of the ceramic.

Particular attention should be given to the area of the ceramic


where it exits the bottom of the cover.
The ceramic should be firm and inflexible in the cover

Examining the fixing screw – what to look for


Before each use of the reference vessel cover, the operator
should examine the top of the threaded plug looking for
discoloration.

This may indicate leakage of reaction vapors, under


temperature and pressure, around the ferrule and plug.

This may also indicate a cracked thermowell.


The plug should be gently tightened and, if the
discoloration continues, the ferrule and thermowell should
be replaced. In extreme cases, the cover will need to be
replaced.
Check very well the condition of Thermowell before each run. Leakages of acid vapours
from thermowell, could generate corrosion of the metal spring on top of the reference
vessel.

Examining the Spring – what to look for


Before each use of the reference vessel cover, the operator
should examine the spring for cracks.

If any cracks appear, no matter how small, the


spring must be replaced.

The spring should also be checked for discoloration.


Operating with a compromised thermowell or threaded plug, hot
acid vapors can reach the springs causing its damage.

Marked discoloration or development of a spot on the perimeter


of the spring, it is a clear evidence of a problem associated with

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the thermowell or plug acid loss.

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.

Replacing the Thermowell of the ATC reference vessel cover

If the ceramic thermowell is damaged, it must be replaced


as well as the TFM ferrule.

The reference vessel cover must be assembled following


specific instructions and heeding appropriate cautions.

Slide-in the thermowell into the Teflon cover.


The open-end of the thermowell, should be left in the upper
part of the Teflon cover, to allow the subsequent
introduction of the probe.
Introduce the TFM Teflon sealing ferrule.

Locate the fixing screw onto the TFM Teflon


sealing ferrule.

Push the fixing screw, along with the TFM ferrule


and the ceramic thermowell, until the screw is in
contact with the TFM Teflon cover.

Close the fixing screw using the special tool.


Care should be taken not to over tighten the plug.
Finger tight is sufficient.

The screw should remain at the same level of the


surface of the TFM Teflon cover.
After a newly installed thermowell has been
used for the first time, Milestone recommends to check
the tightness of the threaded plug.

APC Reference vessel cover

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

ATC and APC separate covers


APC reference vessel cover is a different cover from the one used for temperature control.
Working with SK-15, the direct control of temperature and pressure of the same reference vessel is
not possible; two different positions are requested for monitoring and controlling of temperature and
pressure.

APC reference vessel and cover as a set


Due to its design, the APC reference cover will impress the sealing surface of the vessel used in
combination with it.
Standard vessel cover may not mate well to the sealing surface of a vessel, once that vessel has
been used with APC cover.

Milestone recommends to handle the components of the APC reference vessel assembly
(cover + vessel) as a set.

APC tube positioning


The APC tube could be set directed to the central opening of the top rotor plate (Fig. A), or on the
external side of the rotor.

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.

Care of APC reference vessel cover

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Cleaning the pressure line


It is advisable to routinely flush out the pressure line installed in the reference vessel cover. This can
be easily accomplished by heating water in the APC reference vessel.

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

Checking the pressure line for leaks


Before each use of the reference vessel cover, the operator should examine the hex nut plug of the
pressure line, looking for discoloration.

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.

Samples reactivity Samples type Sample amount

Water samples
- 45 mL
(i.e.EPA 3015)

Soils, aqueous solutions,


Non-reactive samples environmental samples, fertilizers, Up to 1 g
etc..

Samples with medium Food (dried), feed (dried), organic


Up to 1 g
reactivity tissues, etc…

Highly reactive Oils, high fat content cheese,


Up to 0,3 g
samples etc…

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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To reduce such electrostatic issues, Milestone suggests:

• to rinse PTFE vessels with high purity water

• to use an Anti-electrostatic gun or other Anti-


electrostatic devices

• to use a disposable plastic funnel to weigh sample instead


of using a spatula directly.

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.

Small volume processing

Many applications require processing of small amount of sample and/or


small volumes of reagents.
Milestone offers different types of inserts for micro-sampling and ultra-
trace applications that allow to work down to 2 ml of acid reagent and
made of different materials: TFM, glass and quartz.

Comprehensive information regarding SK-15 Ultra-trace Inserts and


their proper use are available.

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 closure of the vessel assembly is performed by the help of a


torque wrench.
The torque wrench is an essential tool for working with SK-15 rotor,
because it produces a calibrated radial force on the pressure screws
which is translated into a downward force on the vessel assemblies.

The torque wrench is calibrated at a tightening of 10 Nm.


The torque wrench is best used with segment body secured in the
workstation on a firm level surface.

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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- Lubrication of the pressure screws


After several runs the pressure screws may encounter difficulties when
closing with the torque wrench.
This can be due to an increased friction between the threads and could
affect the real closure of the segment assembly.

This issue can be easily solved spraying PTFE lubricant directly on the
pressure screw.
Milestone suggests to repeat this operation every six months.

PTFE spray lubricant can be easily find on the market.

- Lubrication of the bottom plate


Once every 6 months, clean the bottom of the turntable rotor body
with some ethanol. After cleaning, spray the PTFE lubricant directly
onto the rotor bearings.

Vessels opening (slow and gentle, avoid vapours)

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.

- Condensate drops leakage


During vessel opening, it may occur that some condensate drops,
remained on the vessel cover surface, fall out from the vessel due to
the pressure release.
Milestone ensures that this small spillage does not result in any loss of
elements (even for volatile elements).

However, this issue can be easily fixed by “tapping” a bit the


segment just before opening it. This makes the condensate
drops to fall inside the vessel.

Maintenance and Care


Each vessel assembly requires a certain level of care and attention to its components in order to maintain
sample preparation performance, maximize the useful lifetime, and to ensure continued safe operation of
the labstation. The exact lifetime of each component cannot be specified, as it is a complicated function of
the temperatures, pressures and chemistry of your specific application.

Active cooling after every run


After the completion of a microwave heating cycle, Milestone recommends active cooling of each microwave
vessel (while still in its individual rotor position or rotor segment).
Active cooling is important, because it reduces the time the vessel components are exposed to temperature
and pressure limits, which in turn minimizes the stress on the vessel components. Active cooling also allows
faster access to prepared samples.

Clean and dry between runs

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Milestone Srl MA176-002 –SK15– User Manual

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.

Cleaning Safety springs


Particular attention must be payed to keep safety springs clean and dry.
Milestone recommends to clean safety springs just using a moist paper cloth and to well dry them before
every use.
Never use solvents or acids to clean safety springs.
Never put safety springs into water. If this should happen, be sure to dry them very well, especially the
internal parts, by placing them into an electrical oven for at leat 2 hours at 100°C.

Cleaning vessels and covers


Milestone vessels and vessel covers are made of a modified
polytetrafluoroethylene blend (TFM). The characteristics of the
TFM material make it chemically inert and resistant to the
digestion process. TFM has additional unique properties of
material density and mechanical strength. Under strict quality
control standards, the vessels and covers are crudely formed from
the raw material under isostatic pressure, sintered under high
temperature, and finally machined to close tolerances.

TFM is not a crystalline material. As such, all vessels have a


certain degree of permeability.
Under the influence of heat and pressure, as such, trace
quantities of elements may migrate into the bulk of the vessel
material.
Milestone’s TFM vessels can be cleaned to any level of analytical
sensitivity. At present, Milestone sample vessels are being used to
effectively process samples for analysis at concentrations from the percent level all the way down to parts
per trillion (ppt). Specific cleaning procedures are recommended to achieve this large dynamic range.
The following are recommended cleaning procedures for PFA and TFM vessels used in Milestone microwave
labstations.

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.

Standard cleaning procedure (suggested) :


• Add 5 ml of HNO3 and 5 ml of H2O to each vessel;
• Start the following microwave program :

Time Power Temperature


00:15:00 1800W 180°C

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Milestone Srl MA176-002 –SK15– User Manual

00:10:00 1800 W 180°C

• Cool down and open the vessels;


• Rinse the vessels with bi-distilled water.

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.

Alternative Cleaning Procedures


Under the influence of heat and/or pressure, trace contaminants can diffuse past the surface and into the
bulk of the vessel material.
To achieve the lowest level blanks and, therefore, the greatest analytical sensitivity, this deeply diffused
contamination must be removed.
Deep cleaning involves heating the vessels in a volume of acid for an extended period of time.
How long the process takes will depend on the particular application and the level of contaminants to be
removed. Heat and time are required to effectively leach out any contaminants that have diffused into the
vessel walls. One or more cleaning steps may be required.

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.

An alternative and effective way for a deep cleaning of vessels is to use


an acid steam cleaning system such as the Milestone TraceCLEAN.

Thanks to the high performance of this unit, it is possible to clean all


Teflon vessels to trace metal level, in a very short time (typically about
1.5 hours).

The extended cleaning time is often the reason


that some users will maintain several sets of vessels and covers for their
laboratory. In many cases users may even dedicate sets of vessels to
specific applications or levels or sensitivity. One must always be kept in
mind that the vessels can be cleaned to any level of sensitivity required
for the application. However, the effort needed to achieve and maintain
a specific level of sensitivity will depend on the application, the
laboratory environment and skill of the operator.

Cleaning vessels and covers from NOx contamination

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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This mainly occurs in case of digestion temperatures over 200°C and is accelerated by even high
temperatures and high pressure.

Microwave absorption test


In order to check, if vessels and covers are contaminated by NOx gases, the following simple test
could be performed :
1. Place the dried rotor body into the microwave and distribute the parts to be tested.
Notice that the parts to be tested must be washed and dried, so that no acid residues may
be located on the parts.

2. Start the following microwave program, depending on the vessels number.


• 45 seconds 600 W (for 10 up to 15 vessels)
• 45 seconds 450 W (for 6 or less vessels)
3. Once concluded the run, check immediately the temperature with the hands (it would be
better with thin gloves) or possibly via the IR control. A rough evaluation of the temperature,
such as cold/slightly warm/really warm/hot is enough.

NOx decontamination procedure


If TFM vessel and cover absorb excessively the microwaves, please operate as follows:

- 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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