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Multiwave 7000: Simplified Method Development For Microwave Acid Digestion

The document describes the new Multiwave 7000 microwave digestion system from Anton Paar. It highlights key features such as its small footprint, proven plug-on cap technology for pressure-sealed vials, and streamlined workflow. The document also provides tips for method development, including how to approach unknown samples, considerations for reactivity, and adapting generic methods.

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tony
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299 views21 pages

Multiwave 7000: Simplified Method Development For Microwave Acid Digestion

The document describes the new Multiwave 7000 microwave digestion system from Anton Paar. It highlights key features such as its small footprint, proven plug-on cap technology for pressure-sealed vials, and streamlined workflow. The document also provides tips for method development, including how to approach unknown samples, considerations for reactivity, and adapting generic methods.

Uploaded by

tony
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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MULTIWAVE 7000

CLEAR SOLUTIONS – FOR SURE !


Simplified Method Development
for Microwave Acid Digestion

Dr. Markus Michaelis


product specialist microwave digestion at Anton Paar / Graz
1 | Forum analytica 2018
Anton Paar - Analytical Instruments for Your Laboratory

2 | Forum analytica 2018


History of Acid Digestion @ Anton Paar

1989 1995 2001 2012 2014

3 | Forum analytica 2018


New at analytica 2018: Multiwave 7000

For more details on


features visit us:

Halle A2 Stand 115

4 | Forum analytica 2018


Proven Concept in a Brand-new Instrument

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

5 | Forum analytica 2018


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

6 | Forum analytica 2018


Pressure-sealed Vials vs. Sealed Quartz Vessels

Plug-on Cap Quartz Lid

PTFE seal

pIN = pOUT pIN < pOUT


7 | Forum analytica 2018
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)

8 | Forum analytica 2018


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)

9 | Forum analytica 2018


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

10 | Forum analytica 2018


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)

11 | Forum analytica 2018


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

12 | Forum analytica 2018


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

13 | Forum analytica 2018


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)

14 | Forum analytica 2018


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 - -

15 | Forum analytica 2018


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 - -

16 | Forum analytica 2018


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)

17 | Forum analytica 2018


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'

18 | Forum analytica 2018


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

19 | Forum analytica 2018


Overloaded Vials

 If a few vials contain too


much sample...

20 | Forum analytica 2018


New at analytica 2018: Multiwave 7000

For more details on


features visit us:

Halle A2 Stand 115

21 | Forum analytica 2018

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