Tips & Techniques, UltraWAVE, Rev12

Milestone Srl MA149-012 – UltraWAVE – User Manual
ULTRAWAVE
TIPS AND
TECHNIQUES
How to maximize the

performances of your
UltraWAVE
107
Milestone Srl
Via Fatebenefratelli, 1/5
24010 Sorisole (BG) Italy
Tel +39 035 573857 – Fax +39 035 575498
www.milestonesrl.com
The aim of this document is to provide applications and technical guidelines in order to get the
best from your UltraWAVE system, enhancing its capabilities even for the most challenging
samples.
This document provides an update of the most important parameters to select during a digestion
with the UltraWAVE; it will considers base load, high temperature applications, microwave
programs, cleaning procedures and enhanced chemical resistance capabilities.
The tips and techniques have been divided in two main categories:
• Applications
• Cleaning/maintenance
Applications
New standard base load

The suggested base load for the UltraWAVE has always been:
120 ml of H2O, 5 ml of H2O2 and 2 ml of H2SO4
The above base load is replaced by the new standard base load:
130 ml of H2O + 5 ml of HNO3 67/68%
The new base load comes from an over four years experience with the UltraWAVE and it is used
regardless the sample type, the acid chemistry and the set temperature.
Base load for reactive samples

The UltraWAVE allows to digest even very reactive samples such as large amount of organic
samples (above 0,5g), polymers, petrochemical products, oils, etc.. The digestion of these samples
generates strong fast exothermal reactions, therefore the following base load is used for reactive
samples:
150 ml of H2O + 5 ml of HNO3 67/68%
The higher water volume further enhances the capability of the UltraWAVE to control exothermal
reactions, ensuring a better digestion.
108
High temperature applications (≥260°C)

Some samples require high temperature to get complete digestion. The UltraWAVE allows to work
at very high temperatures; in particular for applications equal or above 260°C Milestone suggests
the following configuration: 8, 5 and 4 positions racks for routine applications.
The 15 and 22 positions racks are not suggested for routine digestions at high temperature.
In order to further increase the stability of the PTFE vessels/racks at high temperature, Milestone
suggests to use the below PTFE disks (p/n MCL0699A).
The two PTFE disks must be replaced after some usage, when some strong deformations are
noticed.
HF applications
The UltraWAVE can be used for digestion of inorganic samples which in some cases require to use
HF. The hydrofluoric acid, due to the reaction with Si or B, is transformed into gas and gets in
touch with the base load and the thermowell.
Milestone has developed a PTFE protection (p/n MCL0664A) for the thermowell which allows the
use of HF:
The PTFE protection has to be installed onto the thermowell whenever the application requires
large volume of HF:
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HF volume per vial

Rack Max HF volume per vial
(mandatory the use of the
(only PTFE vials) (without PTFE protection)
PTFE protection)
4 pos Up to 2 ml Above 2 ml
22 pos Up to 0,5 ml Above 0,5 ml
Microwave program guidelines

The UltraWAVE allows to digest a wide range of samples such as environmental, food, pharma,
petrochemical, polymer, etc.
Most of the samples can be used simultaneously with a standard microwave program:
Step 1 20 min 240°C

Step 2 10 min 240°C
In some cases, due to the reactivity of the samples or to the high temperature required, the
microwave program should be slightly modified. Below is reported a table that gives clear
indications of the approach to be used for the different samples. The table considers two main
parameters:
- Reactivity of the sample
- Target temperature
Samples Standard ramping

Samples type Target temperature
reactivity time
Soils, aqueous
solutions, 10 min up to 180°C
Not reactive
environmental 180-220°C or
samples
samples, fertilizers, 15 min up to 220°C
feed, etc..
Samples with Food (fatty samples), 20 min up to 220°C
medium pharma ingredients, 200-240°C or
reactivity feed 25 min up to 240°C
5 min to 100°C
Polymer,
15 min to 180°C
Highly reactive petrochemical, large
220-250°C 10 min to 220°C*
samples amount of food, oils,
*depending on the
solvents
target T
25 min up to 250°C
Geological, metals,
High temperature 250-270°C Or
ceramics, inorganics
30 min up to 270°C
110
Cleaning/ Maintenance
Maintenance of the PTFE vessel

The main PTFE vessel is subjected to very hard conditions, such as high temperature, pressure
and acid, therefore Milestone has developed a cleaning procedure to further increase the lifetime
of the main PTFE vessel.
The cleaning of the main vessel should be performed once per month and it consists of a very
easy and fast procedure:
• Clean the vessel with a paper moistened of Ethanol
• Dry it very well and put it into a conventional electrical (not microwave) oven at least 4
hours at 140°C.
Protective spray and grease suitable for Si determination

The standard maintenance of the UltraWAVE requires to clean the stainless steel reactor and cover
with a protective spray. The cleaning procedure consists in using a paper towel with silicon
grease/oil on the stainless steel parts.
The protective spray is a silicon based grease which could not be appropriate in case of Si
determination; for this reason in case of Si analysis, Milestone suggests to use a different spray
and grease:
• Oil of perfluoropolyether (PFPE) to clean the stainless steel components
• Grease of perfluoropolyether (PFPE) to grease between the TFM and stainless steel cover
Milestone provides both the Si-free oil and grease (P/N 70717). Please contact our local partner to
get additional information.
Flushing of the UltraWAVE

At the end of every working day, the cleaning of the UltraWAVE is required to remove some acid
drops that could re-condensate inside the pressure/gas line.
Beside the Maintenance described in the User Manual, Milestone suggests to daily flush the system
with Nitrogen (or Argon) gas.
In case the unit will not be used for more than a day, Milestone suggests to run a microwave
program with water; this cleaning cycle will remove the acid from the unit and from the high
pressure lines. See as well the chapter “Cleaning before long operational break”.
The below procedure shows how simple is to perform the flushing of the UltraWAVE:
111
Put the empty PTFE vessel inside the unit. Vessel must be
dried very well inside and outside
Close the reactor and the clamps. (See user manual for more
details on this operation)
Enter in the system page of the software and press “Pressure

release” button, in order to completely open the release
valve.
Slowly open the gas regulator valve on cylinder, in order to

flush the inert gas inside the unit (set about 5 bar).
Let the nitrogen (or argon) flow into the system, until the pressure reaches a value of 2 - 3 bar.
Hold the flush for 10-15 seconds, then close the pressure regulator.
After this operation, open the reactor and dry the PTFE vessel and cover.
The UltraWAVE equipped with compressor or automatic gas module option doesn’t require the
manual flushing, since it’s automatically done by the software after each digestion program.
Contact your local distributor to get additional information on these accessories.
112
Cleaning before long operational breaks

Whenever the system is not going to be used for long period (≥ 3 days), Milestone suggests to
perform a fast cleaning cycle. The below procedure allows to remove the acid from the high
pressure lines.
Place 200 ml of deionized water into the PTFE vessel (do not use the rack) and run the following
heating program.
Load pressure: 25 bar
Step Time T1 T2 P Power

1 00:10:00 200°C 60°C 100 1500W
2 00:05:00 200°C 60°C 100 1500W
At the end of the program, open the reactor and clean it. Open the reactor and remove the water,
then clean the system (with Silicon oil) following the user manual description.
ULTRAWAVE ECR (Enhance Chemical Resistance)

Milestone has recently introduced a new UltraWAVE version, called UltraWAVE ECR, that further
expands the capabilities of the standard UltraWAVE.
The standard UltraWAVE is suitable for the digestion of a wide range of samples with a very wide
range of acid mixtures.
Milestone has further improved the chemical resistance of the UltraWAVE by using a new Alloy
which is able to stand at very aggressive media, such as aqua regia and large volume of HCl.
The ECR version of the UltraWAVE consists of new pressure lines made of a different material and
it is mainly suggested for all applications that require big volumes of HCl i.e. :
• Applications that require more than 15 mL of hydrochloric acid, considering the complete
rack (i.e. more than 1 mL in each 15-positions rack or 3 mL in each 5-positions rack, etc…)
• Routine applications with high volume of hydrochloric acid.
• Applications that require the use of aqua regia (3:1 HCl:HNO3)
All the other applications can be performed into the standard UltraWAVE.
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Milestone Srl MA149-012 – UltraWAVE – User Manual

How to maximize the

New standard base load

120 ml of H2O, 5 ml of H2O2 and 2 ml of H2SO4

130 ml of H2O + 5 ml of HNO3 67/68%

Base load for reactive samples

High temperature applications (≥260°C)

HF volume per vial

22 pos Up to 0,5 ml Above 0,5 ml

Microwave program guidelines

Step 1 20 min 240°C

Samples Standard ramping

Maintenance of the PTFE vessel

Protective spray and grease suitable for Si determination

Flushing of the UltraWAVE

Enter in the system page of the software and press “Pressure

Slowly open the gas regulator valve on cylinder, in order to

Cleaning before long operational breaks

Load pressure: 25 bar

Step Time T1 T2 P Power

ULTRAWAVE ECR (Enhance Chemical Resistance)

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