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Pyrosulfate fusion vs. TEVA / TRU forcing the issue. Shane Knockemus U.S. EPA / NAREL Montgomery, AL November 11, 2002. Advantages of fusion Achieves total sample dissolution (including refractory material) of nearly any type of sample. Rapid and vigorous. Not many reagents consumed.

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Pyrosulfate fusion vs teva tru forcing the issue l.jpg

Pyrosulfate fusion vs. TEVA / TRUforcing the issue

Shane Knockemus

U.S. EPA / NAREL

Montgomery, AL

November 11, 2002


Advantages disadvantage goal l.jpg

Advantages of fusion

Achieves total sample dissolution (including refractory material) of nearly any type of sample.

Rapid and vigorous.

Not many reagents consumed.

Insures homogeneity between tracer and sample.

Disadvantage of fusion

Introduces large amount of sulfate ions into sample matrix, which may effect some separation processes.

Advantages / disadvantage / goal

Goal: To achieve a reliable separation process for

Am, Pu, Th, and U when analyzing a sample put into

solution by pyrosulfate fusion.


Potassium fluoride pyrosulfate fusion l.jpg
Potassium fluoride / pyrosulfate fusion

  • 0.5-1.0 gram soil in Pt dish

  • 1 g KF, 1.3 g KHF2…….FUSE

  • 3 mL 18 M H2SO4, 2 g Na2SO4…….FUSE



Experiment 1 flowchart l.jpg
Experiment 1 flowchart

cake

HNO3 / Al(NO3)3

TEVA / TRU




Experiment 2 flowchart l.jpg
Experiment 2 flowchart

cake

16 M HNO3

HNO3 / Al(NO3)3

TEVA / TRU




Influence of matrix constituents on teva l.jpg
Influence of Matrix Constituents on TEVA

Find a way to eliminate

the SO4-2 introduced

during the fusion before

the sample is loaded

onto TEVA / TRU.


Experiment 3 flowchart l.jpg
Experiment 3 flowchart

cake

TEVA / TRU

HCl

Calcium phosphate pptn

HNO3 / Al(NO3)3




Experiment 4 flowchart l.jpg
Experiment 4 flowchart

cake

TEVA / TRU

HCl

BaSO4 pptn

HNO3 / Al(NO3)3

Titanous hydroxide pptn

K+EDTA




Experiment 4 results l.jpg
Experiment 4 Results

**Uranium recovery was 0% because there was no valence adjustment prior to BaSO4 coprecipitation


Experiment 5 l.jpg
Experiment 5

  • This experiment was carried out the same as experiment 4, but instead of a titanous hydroxide precipitation, a calcium phosphate precipitation was used.

  • Prior to the BaSO4 precipitation U+6 was reduced to U+4 with hydrazine and TiCl3




Experiment 6 flowchart l.jpg
Experiment 6 flowchart

cake

HCl / HF

TEVA / TRU

diphonix

destroy resin

HNO3 / Al(NO3)3


Usefulness of diphonix l.jpg
Usefulness of diphonix

  • Diphonix will help separate the sample from certain matrix constituents introduced to the sample as part of the digestion process.

  • Sample loaded in 1 M HCl / 0.5 M HF. Actinides stick, while troublesome ions not be sorbed by the resin.


Loading of sample on diphonix l.jpg
Loading of sample on diphonix

  • 0.3 g of diphonix resin packed into column

  • Resin charged with 5 mL 1 M HCl

  • Cake dissolved in 30 mL 1 M HCl / 0.5 M HF

  • Sample loaded onto column

  • Column rinsed with 5 mL 1 M HCl

  • Resin destroyed by charring with H2SO4 and HNO3, followed by oxidation of organics with HClO4




Evaluation of data for exp 6 l.jpg
Evaluation of data for exp. 6

MAPEP did not have certified values for Th nuclides