MULTIWAVE 7000

CLEAR SOLUTIONS – FOR SURE !

Simplified Method Development
for Microwave Acid Digestion

Dr. Markus Michaelis

product specialist microwave digestion at Anton Paar / Graz
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 Anton Paar - Analytical Instruments for Your Laboratory

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 History of Acid Digestion @ Anton Paar

1989 1995 2001 2012 2014

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 New at analytica 2018: Multiwave 7000

For more details on

features visit us:

Halle A2 Stand 115

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 Proven Concept in a Brand-new Instrument

Small footprint:
50 x 80 x 47 cm
(20 x 31 x 19 inch)

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 From HPA-S to Multiwave 7000

+ µW heating
+ Thin-walled quartz vials
+ Disposable vials
+ TFM vials
+ Plug-on caps
+ State of the art interaction
+ Streamlined workflow
+ Automated de-/pressurization
+ PTFE shielded pressure vessel
+ Water cooling – built-in!!

– Improved handling of lightweight items

– Less process time
– No need to be placed in fume hood
– Better corrosion situation
– Less nitrogen needed

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 Pressure-sealed Vials vs. Sealed Quartz Vessels

Plug-on Cap Quartz Lid

PTFE seal

pIN = pOUT pIN < pOUT

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 Racks with Pressure-sealed Vials

Sample weight per vial increases

Rack 18
Rack 24 Rack 9 Rack 6 Rack 5
(18 mL)
(8 mL) (30 mL) (55 mL) (80 mL)

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 Sealed Quartz Vessels

• Rack 6 with vessel 50 mL quartz

• Rack 18 with vessel 15 mL quartz
• Closed with quartz lids and
wrapped with PTFE film
• For aqua regia digestions
• For floating 'burning' samples
(polymers, petrochemicals)

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 How to Approach an Unknown Sample?

 Make yourself familar and find out about approx. composition

 Assess the expected reactivity, it‘s important
 Check available literature like
 Application Guide,
 Application Reports
 Chose appropriate generic method (organic, reactive,
inorganic) for a start

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 Things to Consider Before You Start

 Sample type
 Sample weight
 Type and amount of acids
 Appropriate vial/vessel size
 Appropriate program

>> Influence on 'Reactivity'

If not considered properly, safety disk may break (200 bar)

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 How to Cope with Reactivity? (1)

'Start with a low sample weight'

 Consider the overall sample weight
>> 'Start with a lower number of vials'
 Consider the 'max.' and 'recommended' sample weights
>> Check the Application Guide in the manual
 Higher sample amount may turn 'organic' into 'reactive'
 Consider overall sample weight vs. sample weight per vial
>> 18 x 1 g vs. 6 x 3 g

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 How to Cope with Reactivity? (2)

 Allow for pre-reaction (10-20 min)

 Especially with alcoholic samples
 Adjust the method to the sample type, use generic methods
(e.g. 'Reactive' or 'Reactive.HIGH')
 Do not use H2O2
 Dilution of reagents (=addition of water) will „cool“ exothermal
reactions

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 Type and Amount of Reagents

 Rule of thumb:
'1 mL HNO3 for 100 mg organic matter'
 Multiwave 7000:
'1 mL HNO3 for 100-200 mg organic matter'

>> Try different reagent mixtures in one run

e.g. polymers ± HF
>> Try different amounts of acid in one run
e.g. 500 mg sample + 2/3/4/5 mL HNO3 (± 1/2/3 mL H2O)

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 Digestion of 500 mg Milkpowder

After the run:

HNO3 2.0 1.0 2.0 3.0 3.0 1.0

H2O2 - - 0.5 - - 0.25
H2O 0.5 0.25 - 1.0 - -

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 Digestion of 500 mg Milkpowder

After dilution:

HNO3 2.0 1.0 2.0 3.0 3.0 1.0

H2O2 - - 0.5 - - 0.25
H2O 0.5 0.25 - 1.0 - -

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 Methods & Programs

 Method Library ('small for all'):

 Generic methods
 Sample-specific methods (e.g. Petro, Food, Pharma, EPA,...)
 Method vs. program
 Program consists of:
 Starting Pressure (30-70 bar)
 Steps of the T-program Adapt or modify here
 Cooling temperature (≤ 80 °C)
 p-Release rate (5-10 bar/min)

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 How to Adapt (Generic) Methods (1)

 Change hold time

 Increase hold time
with increasing 'difficulty'
 Change temperature
 Increase temperature
with increasing 'difficulty'
 Change ramp time
 Increase ramp time
with increasing 'reactivity'

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 How to Adapt (Generic) Methods (2)

 Change the chemistry

 Add more reagents (e.g. more HNO3 with organic materials)
 Add/use different acids (esp. with inorganic samples)

 Decrease cooling temperature

 When running long time & high temperature
(e.g. 280 °C for 2 h)
 When using HCl

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 Overloaded Vials

 If a few vials contain too

much sample...

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 New at analytica 2018: Multiwave 7000

For more details on

features visit us:

Halle A2 Stand 115

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