MA209-001 SK-15eT User Manual

MILESTONE
H E L P I N G
C H E M I S T S
SK-15 eT
User Manual
MA209
Milestone Srl MA209-001 – SK-15 eT – User Manual
Thank you for selecting our microwave system.

We are sure that you will be completely satisfied with the performance of this
new unit 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 unit 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:
or Milestone at the following address:
Milestone Srl
Via Fatebenefratelli, 1/5
24010 Sorisole (BG) Italy
Tel +39 035 573857
Fax +39 035 575498
Website www.milestonesrl.com
E-mail analytical@milestonesrl.com
Pubblication date (gg/mm/aaaa) 06/02/2019

1
1 SAFETY RULES ................................................... 6

1.1 GENERAL INFORMATION ................................... 6
1.2 SAFETY IN OPERATIONS ................................... 6
1.3 ANY UNIT MANIPULATION ALLOWED ............... 7
1.4 MAINTENANCE AND PARTS REPLACEMENT....... 7
1.5 CUSTOMER SUPPORT ......................................... 7
1.6 OTHER HINTS .................................................... 7
1.6.1 Working with accessories ....................................................... 7
2 DESCRIPTION OF THE SYSTEM.......................... 8

2.1 OVERVIEW ......................................................... 8
2.1.1 Technical Specifications ......................................................... 8
2.2 SK-15 TECHNOLOGY .......................................... 9

2.2.1 Components ......................................................................... 9
2.2.2 "Vent and reseal" system ..................................................... 11
2.3 TEMPERATURE CONTROL ................................ 11

3 OPERATIONS ................................................... 13
3.1 OPERATIONS WITH MILESTONE SEGMENTED
ROTORS ................................................................... 13
3.1.1 Sample weighing, reagents addition and vessel capping ........ 13
3.1.2 Cooling down and uncapping the vessels .............................. 17
3.1.3 Summary of the working parameters for SK-15 ..................... 19
4 CARE AND MAINTENANCE INSTRUCTIONS ..... 20
2
4.1 GENERAL CLEANING ........................................ 20

4.2 CARE AND MAINTENANCE OF IR (EASYTEMP)
SENSOR ................................................................... 20
4.2.1 Cleaning of IR (easyTEMP) sensors ...................................... 20
4.2.2 EasyTEMP Calibration Test instructions ................................. 21
4.2.3 eT Calibration Test procedure .............................................. 22
4.2.4 eT protection cover (SL0239C) ............................................. 23
4.3 TFM COVER ...................................................... 23

4.4 PROTECTION SHIELD ...................................... 23
4.5 SAFETY SPRING ............................................... 23
4.6 PRESSURE SCREW ........................................... 24
4.7 ROTOR BODY ................................................... 24
4.8 CLEANING OF TFM VESSELS ............................ 24
4.8.1 Cleaning procedure ............................................................. 24
4.8.2 “US EPA” recommended cleaning procedure ......................... 25
4.8.3 Microwave absorption .......................................................... 25
5 GUIDELINES FOR MICROWAVE ACID

DIGESTION .............................................................. 26
5.1 INTRODUCTION TO THE MOST COMMONLY
USED REAGENTS IN MICROWAVE DIGESTION ....... 26
5.2 NITRIC ACID .................................................... 26
5.3 HYDROGEN PEROXIDE .................................... 27
5.4 HYDROCHLORIC ACID ..................................... 27
3
5.5 HYDROFLUORIC ACID ..................................... 28

5.5.1 Acid digestion ..................................................................... 28
5.5.2 Evaporation/Concentration ................................................... 28
5.5.3 Complexation ...................................................................... 28
5.6 AQUA REGIA .................................................... 29

5.7 PERCHLORIC ACID .......................................... 30
6 REGULAR TESTS
ACCESSORIES/VESSELS/ROTORS........................... 31
7 SK-15 ET ROTOR TIPS AND TECHNIQUES ....... 32
7.1 GENERAL WORKING SPECIFICATIONS ........... 32
7.1.1 Sample amount ................................................................... 32
7.1.2 Volumes ............................................................................. 32
7.1.3 Temperature ....................................................................... 32
7.1.4 Pressure ............................................................................. 32
7.1.5 Acid solutions...................................................................... 32
7.2 SK-15 ET SEGMENTS ........................................ 32

7.3 COMPONENTS .................................................. 33
7.3.1 Labeling.............................................................................. 33
7.3.2 Usage Log .......................................................................... 34
7.3.3 Examining the Spring – what to look for ............................... 34
7.4 APC REFERENCE VESSEL COVER ...................... 34

7.4.1 APC reference vessel and cover as a set ............................... 35
7.4.2 APC tube positioning ........................................................... 35
7.4.3 Cleaning the pressure line.................................................... 35
7.4.4 Checking the pressure line for leaks ..................................... 36
4
7.5 OPERATING TIPS ............................................. 36

7.5.1 Sample Weighing ................................................................ 36
7.5.2 Acid additions and digestion temperature ............................. 37
7.5.3 Small volume processing...................................................... 37
7.5.4 Vessels closure.................................................................... 37
7.5.5 Vessels opening (slow and gentle, avoid vapours) ................. 38
7.6 MAINTENANCE AND CARE ............................... 39

7.6.1 Active cooling after every run............................................... 39
7.6.2 Clean and dry between runs ................................................ 39
7.6.3 Cleaning Safety springs ....................................................... 39
7.6.4 Cleaning vessels and covers ................................................. 39
7.6.5 Surface Cleaning ................................................................. 40
7.6.6 Alternative Cleaning Procedures ........................................... 40
7.6.7 Cleaning vessels and covers from NOx contamination ............ 41
7.6.8 Microwave absorption test ................................................... 41
7.6.9 NOx decontamination procedure .......................................... 42
5
1 SAFETY RULES
1.1 General Information
Please read carefully this operator manual before starting the system and follow its prescriptions
with the utmost care.
In case the system was delivered with additional accessories, also read carefully the instruction
manuals of such accessories.
Follow particularly the recommended instructions for Service and Maintenance.
This Operator Manual is part of the delivery, hence shall be always kept together with the
instrument on its working place.
It is imperative that every person operating this system has read and fully understood this manual.
The non-observance of the instructions contained herein or improper use may involve
damages/injuries not covered by product liability!
The national ruling and international safety norms in working environment shall in any case be observed
under user’s responsibility.
It is also user’s responsibility to keep constantly updated all safety norms ruling in the country or
operation.
Information= indicates important information/recommendation for the user.
Attention = means that the warning non-observance may cause damages to unit or properties.
Warning = means that the warning non-observance may cause injuries, even severe, to people.
1.2 Safety in operations

The unit shall be operated only according to its intended purpose.
The unit shall only be operated within the power limits set by technical specifications.
The unit shall be operated exclusively by specially trained people.
All electrical parts shall always be protected from wet and humidity.
The unit shall be kept clean.
Basic rules of chemistry will always apply. The basic rules of chemistry are valid also for chemicals
handling. Working with chemicals, always take into account all safety measures usually required
(e.g. lab coat, protective gloves, protective glasses/mask, exhausts hood, etc.)
6
1.3 Any unit manipulation allowed

Constructive changes/modifications of the unit and its accessories are forbidden.
1.4 Maintenance and parts replacement

In order to guarantee the good functioning of the unit and user’s safety, all replacement parts
shall be exclusively original supplied by the manufacturer. The original parts are produced with
particular attention to quality and manufactory production.
1.5 Customer support

The warranty certificate and qc report are included in the documents supplied with the unit.
In case of unit reparation, please send us a service report with complete problem or damage
description.
For any question or spare parts order, please contact our representative in your country or directly
Milestone.
1.6 Other hints

Please take into account all the safety measures when filling in the vessels before the run or
when opening the vessel, once completed the run.
Don’t label the vessels. Discoloration may occur on protection shield with the consequent
damage.
1.6.1 Working with accessories

The complete vessel system must be treated with the utmost care and regularly tested. In case
of damage, the corresponding components must be replaced. Please pay particular attention to
the chapter “Care and maintenance instructions”.
7
2 DESCRIPTION OF THE SYSTEM

2.1 Overview
SK-15 High pressure rotor
The SK-15 (high pressure segmented rotor) contains 15 vessels for acid digestion of easy to medium-difficult
samples, such as soils, sludges, sediments, wastewater, food and feed, metals, alloys, etc. and of difficult
samples, such as coals, coke, ashes, rocks, plastics, lubrificants, pharmaceuticals, ceramics, etc.
The SK-15 includes one reference segment, used for internal temperature control, and 14 standard
segments.
Internal Pressure control can be provided optionally by an appropriate reference cover.
2.1.1 Technical Specifications
Max Max working Max holding

Rotor Min volume Max volume temperature pressure time at
220°C
SK-15 5 ml 100 ml 300°C 100 bar 30 min
When exceeding the limit value, take into accounts that some parts could be stressed or damaged.
If you set the maximum routine conditions, a regular test of the vessel system is necessary. All
maximum values can be reached only by using material in perfect conditions. This includes as
well system maintenance, as usual in an analytical lab.
8
2.2 SK-15 Technology

Milestone microwave rotor (MDR) technology provides analysts with unsurpassed performance capabilities
and the highest standard of safety in closed vessel. The vessels used in MDR rotors have no molded or
machined threads to be chemically attacked and weakened by hot vapours during vessel venting and
opening. This unique feature is an important factor in the durability and safety of Milestone vessels.
All vessels in MDR rotors are protected by a re-closing (vent and reseal) relief valve mechanism.
Vessels fitted into a MDR rotor body are sealed and have a relief valve functioning using a calibrated torque
wrench. The torque wrench ensures vessels are sealed for maximum operating pressure and will safely vent
when gases in excess are generated
2.2.1 Components
The rotor segment consists of a mould of high-density polypropylene charged with 30% of glass fiber.
The compact mould has the required strength to withstand the elevated pressure generated inside the
vessel during extraction.
The moulded rotor segment tolerates this pressure without any deformation and therefore with high safety.
Special plastic compression screws are located on the top of the segment.
Suitable pressure is applied to the safety spring holding the cover to the top of the vessel by tightening the
screws to the appropriate degree (10Nm).
The safety spring is the “heart” of the MDR technology. Due to its deformation, in case of overpressure
inside the vessel, it allows a safe and controlled release of gases inside the cavity and a perfect reseal when
the pressure returns under the operating limit.
9
The safety spring (upper part)
The safety spring (bottom)

The cover has a flat bottom rim and perfectly fits the top rim of the vessel.
Warning
To avoid the wrong positioning of the safety spring on the top of the cover, the bottom of it is
marked with the word “down”.
The “down” side of the spring must be turned towards the cover.
Warning
Milestone recommend to replace safety springs after 500 runs or one year of work.
Warning
The springs MUST be completely dry from any acids and water drops.
Drops of liquids in contact with the internal metal spring, could generate a hotspot with
consequently damages of the whole spring.
Discolored, cracked, deformed, corroded of springs must be replaced
NEVER clean the springs with water, acids or solvents
corrosion
Sealing between cover and vessel takes place on a very large surface area without any intermediate seal
ring, which could deteriorate in contact with hot vapors.
10
Vessels and covers are made of TFM Teflon, chemically modified PTFE, which has a very dense structure
with smooth surface and low permeability to gases and vapours. TFM Teflon is chemically inert to most
organic solvents and combinations of them. It is a thermal insulator with a very high stability to temperature
extremes.
TFM Teflon is microwave transparent.
Safety shields are made of high resistant PEEK (Polyether ether ketone) and prevents lateral deformation of
the vessels.
2.2.2 "Vent and reseal" system

The drawing below clearly show the instantaneous release of overpressure due to the deformation of the
safety spring. The figure at left represents a vessel in normal working conditions. When pressure increases
over the maximum spring working pressure (figure in the center), the entire cover is allowed to lift up
because of the elastic deformation of the safety spring. The overpressure is instantaneously released thanks
to the large surface area. The larger the surface area the shorter the time required to release the pressure.
Once the pressure inside the vessel has returned within the vessel limit, the cover reseals the vessel,
permitting the operator to continue with the digestion without any loss (figure at right).
This is the unique operating principle of the microwave rotor technology of Milestone.
2.3 Temperature control

SK eT rotor is totally controlled by easyTEMP infrared sensor.
The sensor is positioned on the back side of the

bottom cavity in correspondence of the rotor ring.
11
The easyTEMP contactless sensor directly controls

the temperature in all vessels through TFM vessels
bottom.
Warning
Please, refer to Ethos UP/Ethos EASY User manual for detailed info on the sensors.
eT protection cover
In order to protect the eT sensor lenses, a
protection cover (SL0239C) is placed on sensor
window. The conditions of the protection cover
must be periodically checked and, in case, it must
be replaced.
Warning
Please, refer to eT Calibration Test instructions for more details.
12
3 OPERATIONS
3.1 Operations with MILESTONE segmented rotors
When working with Milestone rotors, observe all safety indications and specifications. The user must be
familiar with the operations with vessel systems. In addition, follow the operating instructions reported in
the microwave system user manual.
3.1.1 Sample weighing, reagents addition and vessel capping
Introduce the rotor bottom plate into the microwave cavity

of the Milestone unit.
Milestone suggests to leave the rotor body always inside the
microwave cavity.
Place a Teflon vessel directly on the balance plate.

The weight of the Teflon vessel is about 115 g, therefore
most of the analytical balances may used for the purpose.
Tare the vessel and directly weigh the sample by placing it

inside the vessel.
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 vessel, try to
wet it by adding acids drop by drop.
Introduce the Teflon vessel into the PEEK protection shield.
13
The shields must be oriented with the bevel down
Warning
The wall surface of PEEK protection shield, as well as the outer wall of the Teflon vessel, must
be dry and clean. Damages may occur otherwise.
Gently swirl the solution to homogeneize the sample with the

acid.
Place the Teflon cover on the Teflon vessel.
Place the safety spring onto the Teflon cover.
Warning
The safety spring must be dry and clean.
Be careful to avoid to wet the inner parts of safety spring; if this should happen be sure to dry it
very well ! Damages may occur otherwise.
14
Introduce the vessel into the polypropylene rotor segment.
Take the torque wrench and set the indicator to the “close”
position, as shown in the picture.
Put the polypropilene segment with the vessel onto the

workstation.
It’s possible to use the “manual” adapter (P/N 934063C) to

initially close the vessel screw.
Vessel must be anyway closed with the torque wrench!
Tighten the safety screw using the torque wrench.

Make long rotations instead of short ones and do proceed
slowly until you hear a clicking sound informing that the
vessel is properly close.
15
Warning
Stop turning the torque wrench when a click is heard. The torque wrench may overload the safety
spring if further tightening is applied, compromising its correct work.
Place the segment into the rotor bottom plate.
Select the positions directly from the rotor page. The plate moves to
the selected position in order to facilitate the introduction of the
vessel.
Alternatively, switch on the "exhaust" (see picture) in order to start
the continuous rotation of the rotor plate.
Warning
Never force the rotation of rotor by hand. This could
damage the central PEEK adapter
Repeat the same procedure for all the remaining standard vessels.
16
Warning
Never use vessel / vessels standing in a fix position. Always use the rotating rotor plate (rotor body).
Introduce the top rotor plate; the plate is fixed by the

connectors to each individual polypropylene segment.
Select a method from the software library (the method

should be marked with “eT”).
Start the digestion method, and introduce the number of

vessels that you have loaded on the rotor plate and wait the
end of the program.
Press start and wait the end of the digestion program. It’s
possible to monitor the internal temperature of each vessels
from the sample list / rotor window (see the Ethos UP user
manual for more details).
Wait for the end of the digestion program.
Warning
Open the vessels only when the internal
temperature is 80°C
3.1.2 Cooling down and uncapping the vessels

After the heating cycle has been completed, leave the vessels into the microwave cavity for the cooling time.
Set the cooling time (ventilation) in the terminal of the system, see Software manual.
Once the microwave program is completed, high temperature and pressure are reached inside the vessels,
according to the sample preparation procedure applied.
17
It is therefore necessary to cool down the rotor before opening the vessels. The rotor may be air cooled
inside the ETHOS unit and in such case the cooling time is around 15 minutes. Once reached a temperature
less than 80°C the vessels can be opened.
Remove the vessels one by one, rotating the motor through the software
Remove the vessels one by one, rotating the motor through

the software.
Take the torque wrench and set the indicator to the “open”
position, as shown in the next picture.
Place 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.
Remove the vessel from the polypropylene segment.

Slide the vessel from the protection shield and remove the
safety spring.
Carefully lift up the vessel cover and rinse the lower part of
the TFM Teflon cover with distilled water, collecting the same
inside the vessel.
18
Pour the solution in a laboratory volumetric flask, washing

repeatedly the TFM Teflon vessel with distilled water. Repeat
the same operation with all vessels in the rotor, including the
reference vessel.
Your sample is now ready to be analyzed.
3.1.3 Summary of the working parameters for SK-15

Max Max working Max holding
Rotor Min volume Max volume temperature pressure time at
220°C
SK-15 5 ml 100 ml 300°C 100 bar 30 min
These are only guidelines; contact your local Milestone distributor to get an appropriate method for your
samples.
19
4 CARE AND MAINTENANCE

INSTRUCTIONS
The vessel must not be labeled. The label color contaminates the protection shield and
diffuses into the vessel.
• All components should be completely dried, after cleaning and before the use.
• Regular test of the vessel system.
• The vessel systems are designed for applications under high stress. Therefore vessels and covers
are subjected to increase wear out. The vessel can deform, so that at the end the vessel sealing
with the cover is no longer guaranteed. Thus regularly check the parts and replace the ones
damaged.
• In case of irregular rotor movement, check the bullets on the bottom side of the rotor body. If they
can’t be easily moved in the guide, dust or dirt may be present between the bullets and can be
removed by using alcohol. The bullets can be sprayed with some lubricant and releasing agent on
the PTFE base
4.1 General cleaning

• All rotors should be regularly checked and cleaned. Don’t use any organic solvent (e.g. acetone) to
clean or dry any part of the rotor, with the exception of the TFM Teflon vessels and covers.
• Water or acid residues should be thoroughly dried before use in the microwave, because they are
heated in the microwave and can lead to damages. This concerns particularly water or acid residues
between the PTFE inner vessel and the protection shield. For any question, contact Milestone or our
representative in your country.
• In case acids, especially high boiling acids (e.g. sulfuric acid), reach the rotor bottom side, the whole
rotor must be washed with plenty of water and then completely dried (no water residue should be
present at the moment of microwave irradiation).
4.2 Care and maintenance of IR (easyTEMP) sensor

The IR (easyTEMP) sensor calibration must be weekly tested following the instructions in
chapter “EasyTEMP Calibration Test instructions” (see the following chapter).
In case the test is not passed, the IR sensor must be cleaned. Then the calibration test must
be repeated.
To ensure a correct measuring by the IR sensor, the sensor lenses must be periodically cleaned from
impurities.
In case of contamination or unusual/abnormal program, the IR sensor must be cleaned after each run.
In case chemicals reach the sample chamber, the IR sensor must be properly cleaned and its functionality
must be tested in accordance with test prescription.
The IR sensor lens can be chemically attacked by HF vapours. The consequence of sensor lens corrosion is
lower measuring values.
4.2.1 Cleaning of IR (easyTEMP) sensors

The recommended cleaning procedure of easyTEMP sensor housing and lenses is the following:
20
1. The eT sensor for SK eT rotor is located on the back side of the cavity bottom.
2. Remove the eT sensor protection cover (SL0239C). For this operation, a small screwdriver can be
used, paying attention not to scratch the cavity coating.
3. Remove dust or possible solid residues from the IR housing. It can be easily done using a gas duster
(1) or compressed air (2), if available.
1 2
4. Clean IR lenses with a cotton bud moistened with water. Cotton buds package (p/n 70484 – 100
pcs) is included in the microwave system.
4.2.2 EasyTEMP Calibration Test instructions

SK eT rotor is monitored by an infrared (easyTEMP) sensor which is positioned on the cavity bottom in
accordance to the rotor ring.
eT sensor calibration test is based on the boiling point of water in an open vessel (atmospheric pressure). At
this working condition, the boiling point of water is unique and it can be used as reference for sensor
calibration check.
21
The boiling point of water depends on the elevation above the sea level. At sea level the boiling
point of water is 100 °C; at 1200 m it lowers down to 96°C. For the calibration test, this
variable data must be considered.
4.2.3 eT Calibration Test procedure

For the calibration test, a single SK-15 vessel
is used.
Fill the vessel with 30 mL of DI water.
Insert the vessel into the safety shield and

place it into the segment.
The vessel must be used without cover.
Place the rotor body into microwave cavity.
Place the segment into the rotor (Pos.1).
Close microwave door.
Enter the software library and select “eT-

Test” method from “Cleaning” application
folder.
eT-Test method.
22
Start the MW program.
When the temperature stops increasing,

despite continuous microwave emission, the
boiling point of the solution is reached.
The acceptability range of eT-Test is ±10°C from the expected boiling point (generally, 100°C).
If test result is out of the acceptability range, please check the vessel conditions for contaminations and
repeat the test using a different vessel.
If test repeatedly fails, please, contact the Service department.
4.2.4 eT protection cover (SL0239C)

eT protection cover conditions must be periodically checked and, in case, it
must be replaced.
To check the conditions of eT protection cover, repeat the eT calibration
test (explained above), placing the cover on eT sensor.
If both tests, with and without cover, are passed, the cover is in good
conditions and it can be used.
In case the test with cover fails, the protection cover must be replaced
with a new one.
4.3 TFM cover

The cover can be cleaned with clear water. If a cover is leaky, e.g. due to deformation, it must be replaced.
4.4 Protection shield

The protection shield can be cleaned with clear water and must be dried before the use.
4.5 Safety spring

The safety spring can be cleaned with a moist paper cloth and must be well dried before the use.
Warning
Be careful to avoid to wet the inner parts of safety spring; if this should happen be sure to dry it
very well ! Damages may occur otherwise.
23
Warning
4.6 Pressure screw

The pressure screw of the segment may encounter difficulties when closing with the torque wrench. This can
be due to increasing of friction between the threads.
This issue can be solved spraying PTFE lubricant directly on the pressure screw (see the photo below) once
every 6 months.
4.7 Rotor Body

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.
4.8 Cleaning of TFM vessels

Graphite or grease residues on all TFM vessels can be cleaned with organic solvents (e.g. alcohol). It is
recommended to clean the surface with a paper cloth. The vessels can be cleaned in a laboratory
dishwasher.
An almost complete decontamination can be reached by a cleaning procedure with HNO3 65 %. A maximum
cleaning temperature of 180°C is enough for this purpose. The steaming out of vessels with Milestone
TraceCLEAN is easier and more efficient.
4.8.1 Cleaning procedure

1. Add 5 mL of HNO3 and 5 mL of H2O in each vessel;
2. Start the following microwave program
20 min 180°C 1800 W
10 min 180°C 1800 W
3. Cool down and open the vessels;
4. Rinse the vessels with bi-distilled water
24
4.8.2 “US EPA” recommended cleaning procedure

The cleaning procedure briefly described here is part of the US EPA approved method 3052 for the
microwave acid digestion of environmental samples.
1. Store TFM Teflon parts in 1:1 sub-boiled HCl overnight at 80-120°C;
2. rinse with bi-distilled water;
3. store in 1:1 sub-boiled HNO3 overnight at 80-125°C;
4. rinse with bi-distilled water;
5. store in bi-distilled water;
6. allow parts to dry in a particle and fume-free environment.
4.8.3 Microwave absorption

TFM vessel and cover, due to their extensive use, accumulate e.g. NOx, that the microwave properties are
considerably changed. This mainly occurs in case of digestion temperatures over 200°C and is accelerated
by even high temperatures and high pressure.
If TFM vessel and cover absorb excessively the microwaves, please operate as follow:
Rinse the pre-cleaned vessels with deionized water thoroughly and place them at least for 4 hours in a
drying oven (if possible ventilated) at 140°C.
PTFE vessel should be placed with the opening facing up.
PTFE cover should be placed with the bottom side facing up.
25
5 GUIDELINES FOR MICROWAVE

ACID DIGESTION
5.1 Introduction to the most commonly used reagents in
microwave digestion
The acids used in microwave digestion may be classified in two main groups:
• non-oxidizing acids, such as hydrochloric acid, hydrofluoric acid, phosphoric acid, diluted sulfuric acid and
diluted perchloric acid;
• oxidizing acids, such as nitric acid, hot concentrated perchloric acid, concentrated sulfuric acid and
hydrogen peroxide.
5.2 Nitric acid

Nitric acid has the following properties:
• boiling point is 120°C at 65% concentration;
• poor oxidizing strength at concentrations less than 2M; oxidizing strength increases with concentration
and reaction temperature;
• the most common acid for oxidation of organic matrices with this typical reaction: (CH2)X + 2HNO3 ->
CO2(g) + 2NO + 2H2O;
• it dissolves most metals forming soluble nitrates, exceptions are Au and Pt (non oxidized) and Al, B, Cr, Ti
and Zr (passivated);
• these metals require acid mixtures or diluted nitric acid;
• often mixed with H2O2, HCl and H2SO4;
• available in high purity for trace level analysis.
26
The above graphic represents the temperature and pressure profile of nitric acid up on microwave heating.
Notice that pressure has been controlled at 25bar, resulting in a temperature of 225°C.
5.3 Hydrogen peroxide

Hydrogen peroxide is an oxidizing agent (2H2O2 -> 2H2O + O2); added to nitric acid it reduces the nitrous
vapors and it accelerates the digestion of organic samples by raising the temperature.
A typical mixture ratio is HNO3:H2O2= 4:1 (volume/volume).
5.4 Hydrochloric acid

Hydrochloric acid has the following properties:
• boiling point of azeotropic mixture with H2O with 20,4% HCl is 110°C;
• available with 38% concentration;
• it dissolves salts of weak acids (carbonates, phosphates) and most metals are soluble with the exception
of AgCl, HgCl and TiCl;
• excess of HCl improves the solubility of AgCl, converted into AgCl2-;
• strong complex nature;
• widely used for iron-based alloys because of its ability to hold large amounts of chloro-complex in
solution;
• other complexes formed are Ag (I), Au (II), Hg (II), Ga (III), Tl (III), Sn (IV), Fe (II) and Fe (III);
• it does not dissolve oxides of Al, Be, Cr, Ti, Zr, Sn and Sb; sulphates of Ba and Pb, group II fluorides,
SiO2, TiO2 and ZrO2.
The graphic above represents the temperature and pressure profile of hydrochloric acid up on microwave
heating.
27
5.5 Hydrofluoric acid

Hydrofluoric acid has the following properties:
5.5.1 Acid digestion

• Boiling point is 108°C at 40% concentration;
• non-oxidizing, strong complex nature;
• used in digestion of minerals, ores, soils, rocks and even vegetables containing silicates;
• major use is the decomposition of silicates according with this reaction: SiO2 + 6HF -> H2SiF6 + 2H2O;
• often used in combination with HNO3 or HClO4.
5.5.2 Evaporation/Concentration
• Following dissolution, many analyses require removal of HF to prevent equipment damage or to
resolubilize insoluble fluorides;
• many analytes such as As, B, Se, Sb, Hg and Cr may volatilize.
5.5.3 Complexation
• Alternative approach to remove HF from the solution, by addition of Boric acid;
• the following reactions take place: H3BO3 + 3HF -> HBF3(OH) + 2H2O and HBF3(OH) + HF -> HBF3 +
H2O;
• 10-50 times excess Boric acid enhances reaction rate.
The above graphic represents the temperature and pressure profile of hydrofluoric acid up on microwave
heating.
28
Sulfuric acid
Sulfuric acid has the following properties:
• boiling point is 340°C at 98% concentration, exceeding the maximum working temperature of TFM Teflon
vessels;
• careful reaction monitoring is required to prevent vessel damages;
• it destroys organics by dehydrating action;
• many sulfates are insoluble (Ba, Sr, Pb).
The above graphic represents the temperature and pressure profile of sulfuric acid up on microwave
heating.
Notice that temperature has been controlled at 300°C (for 1 minute only), without any pressure increase.
It is clear that the use of concentrated sulfuric acid in the MDR rotors poses significant problems because of
its high boiling point.
300°C are critical for TFM Teflon vessels and simply too high for PFA Teflon vessels (they melt down at such
temperature).
It is therefore advisable to use sulfuric acid only with a strict temperature control.
5.6 Aqua regia

Aqua regia properties are the following:
• made up by hydrochloric acid and nitric acid in a 3:1 (volume/volume) mixture;
• it produces NOCl (nitrosyl chloride), which decomposes in NO and Cl2 up on heating;
• it dissolves precious metals;
• it must be freshly prepared and used immediately, otherwise it evolves chlorine gas overpressurizing and
venting the vessel
29
The above graphic represents the temperature and pressure profile of aqua regia up on microwave heating.
5.7 Perchloric acid

Perchloric acid has the following properties:
• boiling point is 203°C at 72% concentration;
• hot and concentrated is the strongest oxidizing acid;
• rapid, sometimes explosive, reaction with organic matrices;
• often mixed with nitric acid for a controllable digestion of organic matrices;
• all perchlorate are soluble with the exception of KClO4;
• perchloric acid decomposes at 245°C in a closed microwave vessel, developing gaseous by-products and
a tremendous excess pressure.
Warning
Special care has to be taken when the use of perchloric acid is required.
Do not use perchloric acid with organic samples.
It may be possible to use perchloric acid with inorganic samples when the temperature does not
exceed 200°C and when the amount of perchloric acid is below 20% (volume/volume) of the
total solution volume.
30
6 REGULAR TESTS
ACCESSORIES/VESSELS/ROTORS
Customer address
Company:
Department:
Contact:
Address:
Post Code, place:
Tel./FAX:
E-mail:
VESSEL SYSTEMS CONDITIONS
Vessel type Art.-Nr. Status
ROTOR BODY CONDITIONS
Rotor type Art.-Nr. Status
PRESSURE VALVE/APCU ETC.
Art Art.-Nr. Status
UNIT/ACCESSORIES GENERAL CONDITIONS
31
7 SK-15 ET ROTOR TIPS AND

TECHNIQUES
7.1 General working specifications
7.1.1 Sample amount
Maximum sample amount: 1 g (of organic dried
matter)
7.1.2 Volumes
Minimum volume:
• 5 mL (without inserts)
• 3 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)
7.1.3 Temperature
Maximum working temperature: 240°C
Maximum holding time at maximum working temperature: 30 minutes
7.1.4 Pressure
Maximum working pressure: 100 bar
7.1.5 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
7.2 SK-15 eT 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;
32
4. A system that can safely release (vent) over-pressure in the vessels, then reseal the vessel and
continue the microwave process until completion.
7.3 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
appropriate 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.
7.3.1 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.
33
Etching the sides of vessels is not recommended.

Vessels must not be ink-labeled. The label color contaminates the protection shields and diffuses
into the vessels.
7.3.2 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.
7.3.3 Examining the Spring – what to look for

Before each use of the reference vessel cover, the operator should
examine the springs 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 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.
7.4 APC Reference vessel cover

The pressure sensor enables to measure the pressure (bar) inside the reference vessel.
The pressure sensor installed outside the sample chamber is connected by a pressure tube to the reference
vessel.
The pressure tube is designed for routine operations up to 50 bar for up to 20 minutes. At higher pressures
it showed an increased stress.
The internal pressure can be measured during the run by the special pressure cover.
34
7.4.1 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.
7.4.2 APC tube positioning

The APC tube could be set directed to the central opening of the top rotor plate, 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.
The TWIST function of microwave unit must be activated when APC (pressure) sensor is used,
otherwise sensor will be damaged.
Before every start, check that the pressure tube can freely move.
7.4.3 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
00:15:00 150°C
00:05:00 150°C
35
7.4.4 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.
7.5 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.
7.5.1 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, API, Pharmaceuticals, etc… (some cases up to 0,5 g)
Oils, high fat content cheese, API,

Highly reactive samples Up to 0,25 g
Pharmaceuticals, 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.
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
36
7.5.2 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.
7.5.3 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.
7.5.4 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.
37
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.
7.5.5 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 vapours 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.
Slowly open the vessels and gently release the acid

vapors using the appropriate torque wrench.
During vessel opening, it may occur that some
condensate drops, remained on the vessel cover
surface, come 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).
38
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.
7.6 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.
7.6.1 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.
7.6.2 Clean and dry between runs

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.
7.6.3 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.
7.6.4 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
39
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.
7.6.5 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
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.
7.6.6 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.
40
1. PFA or TFM vessels and covers 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 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.
7.6.7 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).
This mainly occurs in case of digestion temperatures over 200°C and is accelerated by even high
temperatures and high pressure.
7.6.8 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. The parts to be
tested must be washed and dried.
41
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.
7.6.9 NOx decontamination procedure

If TFM vessels and covers 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.
42
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@milestonesrl.com - web: www.milestonesrl.com
C H E M I S T S

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MILESTONE

Thank you for selecting our microwave system.

or Milestone at the following address:

Pubblication date (gg/mm/aaaa) 06/02/2019

1 SAFETY RULES ................................................... 6

2 DESCRIPTION OF THE SYSTEM.......................... 8

2.2 SK-15 TECHNOLOGY .......................................... 9

2.3 TEMPERATURE CONTROL ................................ 11

4 CARE AND MAINTENANCE INSTRUCTIONS ..... 20

4.1 GENERAL CLEANING ........................................ 20

4.3 TFM COVER ...................................................... 23

5 GUIDELINES FOR MICROWAVE ACID

5.5 HYDROFLUORIC ACID ..................................... 28

5.6 AQUA REGIA .................................................... 29

7.2 SK-15 ET SEGMENTS ........................................ 32

7.4 APC REFERENCE VESSEL COVER ...................... 34

7.5 OPERATING TIPS ............................................. 36

7.6 MAINTENANCE AND CARE ............................... 39

Information= indicates important information/recommendation for the user.

1.2 Safety in operations

1.3 Any unit manipulation allowed

1.4 Maintenance and parts replacement

1.5 Customer support

1.6 Other hints

1.6.1 Working with accessories

2 DESCRIPTION OF THE SYSTEM

SK-15 High pressure rotor

2.1.1 Technical Specifications

Max Max working Max holding

SK-15 5 ml 100 ml 300°C 100 bar 30 min

2.2 SK-15 Technology

The safety spring (upper part)

The safety spring (bottom)

2.2.2 "Vent and reseal" system

2.3 Temperature control

The sensor is positioned on the back side of the

The easyTEMP contactless sensor directly controls

3.1.1 Sample weighing, reagents addition and vessel capping

Introduce the rotor bottom plate into the microwave cavity

Place a Teflon vessel directly on the balance plate.

Tare the vessel and directly weigh the sample by placing it

Add suitable reagents to the sample. When part of the

Introduce the Teflon vessel into the PEEK protection shield.

The shields must be oriented with the bevel down

Gently swirl the solution to homogeneize the sample with the

Place the Teflon cover on the Teflon vessel.

Place the safety spring onto the Teflon cover.

Introduce the vessel into the polypropylene rotor segment.

Put the polypropilene segment with the vessel onto the

It’s possible to use the “manual” adapter (P/N 934063C) to

Tighten the safety screw using the torque wrench.

Place the segment into the rotor bottom plate.

Introduce the top rotor plate; the plate is fixed by the

Select a method from the software library (the method

Start the digestion method, and introduce the number of

3.1.2 Cooling down and uncapping the vessels

Remove the vessels one by one, rotating the motor through

Place the work station under a fume hood, and carefully

Remove the vessel from the polypropylene segment.

Pour the solution in a laboratory volumetric flask, washing

Your sample is now ready to be analyzed.

3.1.3 Summary of the working parameters for SK-15

SK-15 5 ml 100 ml 300°C 100 bar 30 min