Peroxide Fusion: Powerful and Safe Dissolution of Mining Samples for AA and ICP Analysis

Luc Brub, M. Sc. Chemist Sales and Services Manager Philippe Daigle, M. Sc. Chemist Technical Representative

CMA 2008, Bathurst

Presentation Overview


Standard dissolution methods vs peroxide fusion Chemistry of peroxide fusion Choice of crucible Application examples Peroxide fusion vs borate fusion Peroxide fusion on automated fusion machines
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Standards dissolution methods for mining samples

  

Hot plate or micro-wave acid digestion Multi-step, multi-reagent methods Manipulation of HF (threat to human health-bones) and sometimes HClO4 (explosive)

  
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Use of high pressure vessels Usually long (1h and more) Method is matrix dependant Difficulty to obtain total dissolution
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Chemistry of Peroxide Fusion

 

Chemical formula: Na2O2 Chemical structure:

Na O O Na

Melting point: 460C

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Chemistry of Peroxide Fusion



Oxidation: Na 2 O 2  E T u 460Cp Na 2O  EO Reaction in solution:

Na 2O  O  H 2O p 2 Na  ( aq )  O  2OH  ( aq)

Acidification

EO( s )  2 H p H 2O  E
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( aq )

Zr or Ni Crucibles?
Temperature must not exceed 525C

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Peroxide Fusion Application (FeSi)

1. Weigh 0.5g sample, 8 g Na2O2 and 2g of Na2CO3 on top into a zirconium crucible.

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2. Heat slowly to avoid a violent reaction and sputtering.

3. Rise the gas pressure. The melt should be red hot. 7

Peroxide Fusion Application (FeSi)

4. Once the oxidation reaction is ended, the melt cool down to ambient temperature.

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5. The zirconium crucible is then immerged into a water solution. The liquid level must cover the crucible. 8

Peroxide Fusion Application (FeSi)

6. When the decomposition reaction stop, add successively two portion of 10 ml of HCl to dissolve the hydroxides and acidify the solution. 7. Boil the solution to totally decompose the peroxide then complete to volume.

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Peroxide Fusion Applications

1. 2. 3. 4. 5. 6. 7. 8. 9.
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Chromium ores Precious metals (Pt, Pd, Rh) Niobium Tantalum Beryllium Aluminum Silicate Silica rocks Chromites Ferro-chromium and other ferroalloys Ferro-silicon, silicon, silicon carbide Magnetite, illmenite, rutile Other alloys and steels
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Advantages of Peroxide Fusion

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Peroxide vs Borate Fusion for AA/ICP Sample Preparation

Borate fusion Crucible Fusion + Dissolution time Sample matrix type
Pt-5%Au 10-12 min.
oxides (rocks, zeolithes, cement) Reduced

Peroxide fusion
Zirconium 15-30 min. as borate fusion. Easy for metallic and reduced materials. Carbides and nitrides. Max 500C Sodium peroxide Good 12
Same

samples need oxidizer. Carbides and nitrides difficult.

Temperature Fluxes used

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900-1050C Lithium borate Moderate

Retention of volatiles

Instrumentation for Peroxide Fusion

Bunsen burner Ovens Opened system automatic fusion machines

  

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Peroxide Fusion on Claisse Peroxide

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Conclusion


Peroxide fusion is a powerful technique that allows the dissolution of many difficult samples

 

Peroxide fusion is simple and safe Peroxide fusion can be performed in opened system fusion machines to increase safety, result consistency and throughput
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