determination of uranium in urine using eichrom resins
DESCRIPTION
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 - PowerPoint PPT PresentationTRANSCRIPT
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EIChrom User Group Meeting 15/11/99
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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
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2RTCEIChrom User Group Meeting 15/11/99
Evaluation of some methods
Reason for the study
Inconsistency in results from certain methods
Attribute possible causes
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3RTCEIChrom User Group Meeting 15/11/99
Problem areas? A satisfactory analytical
result requires
Combination of
Analyst Method Equipment
Instrumentation Laboratory environment Materials and chemicals
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4RTCEIChrom User Group Meeting 15/11/99
Analyst
Trained limited experience
Limited time to test effectiveness
Manual procedures
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5RTCEIChrom User Group Meeting 15/11/99
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
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6RTCEIChrom User Group Meeting 15/11/99
Equipment
Materials EIChrom resin TRU
Batch to batch variation
Storage
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7RTCEIChrom User Group Meeting 15/11/99
Study protocol Part 1
PhD student - initial work
Familiarisation with techniques using Synthetic urine Genuine urine Co-precipitation Electro deposition
Actual methods
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8RTCEIChrom User Group Meeting 15/11/99
Study protocolPart 2
Evaluation of data
PhD student finished her work and left
Final tests on hydrolysis to be carried out
Conclusions to be made
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9RTCEIChrom User Group Meeting 15/11/99
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
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10RTCEIChrom User Group Meeting 15/11/99
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
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11RTCEIChrom User Group Meeting 15/11/99
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
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12RTCEIChrom User Group Meeting 15/11/99
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
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13RTCEIChrom User Group Meeting 15/11/99
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,
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14RTCEIChrom User Group Meeting 15/11/99
Results – DifferentBatches of Resin
TR6D 88%
TR6D 91%
TR6D 62%
TR7A 88%
TR7A 55%
TR8C 70%
TR8C 23%*
TR8C 86%
*blocked col.
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15RTCEIChrom User Group Meeting 15/11/99
Results using different methods
B1 45%
B2 36%
B3 32%
C1 93%
C2 88%
C3 99%
D1 76%
D2 76%
D3 74%
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16RTCEIChrom User Group Meeting 15/11/99
Results- Different methods (real urine)
A1 78%
A2 71%
A3 76%
B1 28%
B2 30%
B3 28%
C1 67%
C2 Lost in anal.
C3 68%
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17RTCEIChrom User Group Meeting 15/11/99
Conclusions – to date
Consistency for Method A and analyst satisfactory
Different batches of resin No real evidence of
effect
Different methods A, C and D reasonable B poor
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18RTCEIChrom User Group Meeting 15/11/99
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 ?
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19RTCEIChrom User Group Meeting 15/11/99
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!!
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20RTCEIChrom User Group Meeting 15/11/99
Hydrolysis proceduresevaluated using:-
Mock Urine Method B CeF3 micro pptn U-233 spike
Very large prayer mat.
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21RTCEIChrom User Group Meeting 15/11/99
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
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22RTCEIChrom User Group Meeting 15/11/99
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
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23RTCEIChrom User Group Meeting 15/11/99
Results of hydrolysischanges to Method B
Ferrous sulphate
1 6hrs 81%
2 6hrs 82%
3 15hrs 78%
4 15hrs 79%Ferrous sulphamate
5 6hrs 72%
6 6hrs 70%
7 15hrs 80%
8 15hrs 70%
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24RTCEIChrom User Group Meeting 15/11/99
Conclusions of hydrolysis changes
No significant differences
Method B appears to give good results
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25RTCEIChrom User Group Meeting 15/11/99
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!
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26RTCEIChrom User Group Meeting 15/11/99
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?