The Separation of Beryllium from Spectral Interfering Elements in Inductively Coupled Plasma - PowerPoint PPT Presentation

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The Separation of Beryllium from Spectral Interfering Elements in Inductively Coupled Plasma

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intense method is very sensitive for the determination of beryllium ... Dipex offered the most promising beryllium retention characteristics ... – PowerPoint PPT presentation

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Title: The Separation of Beryllium from Spectral Interfering Elements in Inductively Coupled Plasma


1
The Separation of Beryllium from Spectral
Interfering Elements in Inductively Coupled
Plasma Atomic Emission Spectroscopic Analysis
  • Daniel R. McAlister and E. Philip Horwitz
  • PG Research Foundation, Inc.
  • 8205 S Cass Avenue, Suite 109
  • Darien, IL 60561

2
Problems with Current Method
Interfering elements in the AES spectrum of
Beryllium
Beryllium lines very intense ? method is very
sensitive for the determination of beryllium
Interfering lines from other elements could lead
to false positives.
3
Uptake of Selected Elements on Dipex Resin
Several EXC materials evaluated Dipex offered
the most promising beryllium retention
characteristics
4
Uptake of Selected Elements on Dipex Resin
Single column should remove all ICP-AES
interferences Load pH 2-4 Rinse 0.2 M HNO3 Strip
Be with 4 M HNO3 Potential for 2-10 x
concentration of Be depending on sample size
5
Uptake of Selected Elements on Dipex Resin
Resin selective for Be over other alkaline earth
metal ions Ca and Mg common matrix impurities
6
Uptake of Selected Elements on Dipex Resin
Fe(III) strongly retained Al(III) and Pb(II) have
similar retention to Be(II) Cu(II) more weakly
retained Large amounts of Fe(III) could
interfere with Be(II) uptake
7
Uptake of Selected Elements on Dipex Resin
Resin selectively retains Be(II) over most other
divalent metal ions Be(II) can be separated from
samples containing large quantities of divalent
metal ion impurities
8
Proposed Method for Beryllium Purification
Prepare samples as before (Digest with
H2SO4/H2O2, dilute with HNO3)
Neutralize samples to pH 1-2 with sodium
aceate Buffers to maximum pH of 4.5
Monitor pH with methyl violet or crystal violet
or pH strip
pH Range over which separation is effective
9
Elution of Be and Selected Elements on Dipex Resin
10
Elution of Be and Selected Elements on Dipex Resin
11
Elution of Be and Selected Elements on Dipex Resin
12
Simulated Sample Results Successfully separated
Be from samples digested with H2SO4/H2O2 Several
different digested methods employed in Be
analyses (HCl, H2SO4, HNO3, HF, H2O2,
HClO4) High levels of impurities
13
Digestion Methods using HF
14
Separation of Be from Large Amounts of
Interferences
15
Separation of Be from Large Amounts of
Interferences
16
Uptake of Selected Metal Ions on LN2 and LN3
Resins
U(VI), Th(IV), Ti(IV) retained from all
HNO3 LN2 Strongly retains Fe(III) LN3 Be not
retained from pH lt 2 Choice of LN2/LN3 depends on
desired operating conditions and amount of Fe in
samples
17
Elution of Be on LN2 and LN3 Guard Columns
18
Effect of Large Quantities of Uranium
LN2 and LN3 Resins effectively increase the
capacity for Uranium
With LN2, the GC remains connected through the
load, rinse and strip
With LN3, the GC can be removed following the
rinse
19
Conclusions
Efficient, Reliable method for purifying Be from
all ICP-AES spectral interfering elements has
been found using a single column
Method is compatible with current monitoring and
sample digestion methods
Method is robust and performs over a wide pH
range
Inserting a LN2 or LN3 Resin guard column
increases U capacity without changing the
chemistry or significantly decreasing Be yields.
Working to develop methods to isolate Be from
high levels of other impurities
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