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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 TiOSamples

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

    For TiOsample, add 2mL of HNOand 2 mL of HF; for the other samples, add 2 mL of HNOand 1mL of HF.

    Perform digestion according to the program outlined in Table 1.

Table 1  Digestion Program for HfO2, Ta2O5 and TiOSamples

Pre-pressurization

to 4MPa

Ramp Time

10 min 

Target Temperature 240
 Hold Time 20 min
 Depressurization Temperature  60

2.2 Digestin Solution for ZrOSample

    Weigh 0.1000g of ZrOsample 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 ZrOSample

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 ZrOsamples were clear and transparent, with no precipitate.