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Determination of Uranium in Urine using EIChrom Resins

Determination of Uranium in Urine using EIChrom Resins. Helen E Carter Loughborough University UK Arthur E Lally OBE RTC Ltd UK Michaela Langer EIChrom Europe France Peter Warwick Loughborough University UK. Evaluation of some methods. Reason for the study

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Determination of Uranium in Urine using EIChrom Resins

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  1. Determination of Uranium in Urine using EIChrom Resins Helen E Carter Loughborough University UK Arthur E Lally OBE RTC Ltd UK Michaela Langer EIChrom Europe France Peter Warwick Loughborough University UK EIChrom User Group Meeting 15/11/99

  2. Evaluation of some methods • Reason for the study • Inconsistency in results from certain methods • Attribute possible causes EIChrom User Group Meeting 15/11/99

  3. Problem areas? • A satisfactory analytical result requires • Combination of • Analyst • Method • Equipment • Instrumentation • Laboratory environment • Materials and chemicals EIChrom User Group Meeting 15/11/99

  4. Analyst • Trained • limited experience • Limited time to test effectiveness • Manual procedures EIChrom User Group Meeting 15/11/99

  5. Analytical Methodology • For this study all were similar • Method A no apparent problems • Method B inconsistencies in results • Method C less of a problem than B • Method D small inconsistencies EIChrom User Group Meeting 15/11/99

  6. Equipment • Materials EIChrom resin TRU • Batch to batch variation • Storage EIChrom User Group Meeting 15/11/99

  7. Study protocol Part 1 • PhD student - initial work • Familiarisation with techniques using • Synthetic urine • Genuine urine • Co-precipitation • Electro deposition • Actual methods EIChrom User Group Meeting 15/11/99

  8. Study protocol Part 2 • Evaluation of data • PhD student finished her work and left • Final tests on hydrolysis to be carried out • Conclusions to be made EIChrom User Group Meeting 15/11/99

  9. Outline - Method A • Mineralisation with HNO3 • Copptn on Ca phosphate • Muffle at 900Oc 8 hrs • Dissolution HNO3+ Al nitrate • Reduction with Fe(II) sulphate • TRU resin column • Elution with Amm. Oxalate • Source preparation • Reduction with TiCl3 • Micro pptn on CeF3 EIChrom User Group Meeting 15/11/99

  10. Outline – Method B • Mineralise with HNO3/H2O2 • Muffle at 500oc 6 hrs • Hydrolyse 1.4 M HNO3 • Copptn Ca phosphate • Ferrous sulphate/ Al2(NO3)3 • TRU resin • U elution • Micro pptn with LaF3 EIChrom User Group Meeting 15/11/99

  11. Outline- Method C • Similar to method B but • Muffle 12hrs at 500oC • Separation on AGMP1 resin • Pu on column • U in load + 8M HNO3 wash • U fraction on to TRU resin • As for method B EIChrom User Group Meeting 15/11/99

  12. Outline- Method D • Mineralisation and evaporation on hotplate • Hotplate to 500oC 5hrs • Dissolution / hydrolysis in 2M HNO3 • Co pptn Ca phosphate • Dissolution HCl • Co pptn Fe phosphate • As per method C EIChrom User Group Meeting 15/11/99

  13. Results - same batch of resin • Method A, Mock Urine • Batch TR8B resin • CeF3 pptn • % recovery • 84, 75, 77, 94, 88, 92, • 89, 95, 92, 87, 93, 77, EIChrom User Group Meeting 15/11/99

  14. Results – DifferentBatches of Resin EIChrom User Group Meeting 15/11/99

  15. Results using different methods EIChrom User Group Meeting 15/11/99

  16. Results- Different methods (real urine) EIChrom User Group Meeting 15/11/99

  17. Conclusions – to date • Consistency for Method A and analyst • satisfactory • Different batches ofresin • No real evidence of effect • Different methods • A, C and D reasonable • B poor EIChrom User Group Meeting 15/11/99

  18. What is going on? Analyst or method ! • Method A always OK • Method B always poor • Give the analyst a chance! • What else could be wrong? • HYDROLYSIS ? EIChrom User Group Meeting 15/11/99

  19. HydrolysisAlways been a problem • Actinides U and Pu love pyrophosphates better than any ion-exchange resin • (yes even EIChrom!) • Experiment with hydrolysis procedures • New analyst on job • Old analyst in years!! EIChrom User Group Meeting 15/11/99

  20. Hydrolysis proceduresevaluated using:- • Mock Urine • Method B • CeF3 micro pptn • U-233 spike • Very large prayer mat. EIChrom User Group Meeting 15/11/99

  21. Method B amendments 1 • Samples 1 and 2 • Standard 500oC 6hrs • Standard 1.4M nitric hydrolysis and Fe(II) SO4 • Samples 3 and 4 • As above but 500oC 18hrs EIChrom User Group Meeting 15/11/99

  22. Method Bamendments 2 • Samples 5 and 6 • Standard 500oC 6hrs • Standard 1.4M nitric but- with ferrous sulphamate and Fe(II) SO4 • Samples 7 and 8 • As above but 500oC 18hrs EIChrom User Group Meeting 15/11/99

  23. Results of hydrolysischanges to Method B EIChrom User Group Meeting 15/11/99

  24. Conclusions of hydrolysis changes • No significant differences • Method B appears to give good results EIChrom User Group Meeting 15/11/99

  25. Overall Conclusions • The resin appears to make no difference with regards to • Age • Batch • Packing • Methods all appear OK at times • What about the operator? • Think about method, operator and equipment combination! EIChrom User Group Meeting 15/11/99

  26. Summary of all experiments • No effect of resin • All methods satisfactory • Human factor • Bored staff? • Staff in wrong method? • Automation • Who wants an old chemist? EIChrom User Group Meeting 15/11/99

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