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How to digest Insoluble Oxide Samples by SMWD5000 Super Microwave Digestion System

April.22

Instrument Introduction

The SMWD5000 Super Microwave Digestion System boasts a miaximum operating temperature of 280℃, requires minimal acid usage, and offers high automation. It can be optionally equipped with a magnetic stirring system to facilitate the digestion reaction, which simplifies the digestion process.


Experiment

1. Sample and Reagent

    Samples: HfO2, Ta2O5, TiO2, ZrO2

    Solid power reagents: HNO3, HF, H2SO4, H3PO4, all of GR

2. Digestion Experiment

2.1 Digestin Solution for HfO2, Ta2O5 and TiO2 Samples

    Weigh 0.1000g of HfO2, Ta2O5 and TiO2 samples into digestion tubes.

    For TiO2 sample, add 2mL of HNO3 and 2 mL of HF; for the other samples, add 2 mL of HNO3 and 1mL of HF.

    Perform digestion according to the program outlined in Table 1.

Table 1  Digestion Program for HfO2, Ta2O5 and TiO2 Samples

Pre-pressurization

to 4MPa

Ramp Time

10 min 

Target Temperature 240℃
 Hold Time 20 min
 Depressurization Temperature  60℃

2.2 Digestin Solution for ZrO2 Sample

    Weigh 0.1000g of ZrO2 sample into a digestion tube.

    Place a high-temperature resistant magnetic stirring bar into the digestion tube (without stirring, the sample weight should be less than 0.05g, and the digestion time at 260℃ should be over 60 min to achieve a clear, precipitate-free solution).

    Add 2 mL of H2SO4, 2 mL of H3PO4, 1 mL of HF, and 2 mL of HNO3.

    Perform digestion according to the program outlined in Table 2.

Table 2                         Digestion Program for ZrO2 Sample

Pre-pressurization

to 4MPa

Ramp Time

20 min 

Target Temperature 260℃
 Hold Time 40 min
 Depressurization Temperature  60℃


3. Experimental Results

Conclusion: After digestion and dilution to volume, the solutions of HfO2, Ta2O5, TiO2 and ZrO2 samples were clear and transparent, with no precipitate.