Appli cat i on Br i e f 4 3 1 9 5
Routine Analysis of 6N High Purity Copper
using the Thermo Scientific ELEMENT GD
Glow Discharge Mass Spectrometer
Joachim Hinrichs, Thermo Fisher Scientific, Bremen, Germany
Key Words
6N, Copper, GD-MS, High Purity, Routine
Goal
To demonstrate the capability of the ELEMENT GD MS for the routine
analysis of ultra-trace impurities in high purity copper with minimum
sample preparation.
Analytical Challenge
Trace elemental analysis of high purity 5N or 6N
metals is challenging due to both the complete
elemental coverage required in the assay and the
ultra low target levels.
For example, the sum of all impurities in a 6N Cu
(99.9999% purity) is only 1 ppm. For such high purity
materials, a routine, full mass scan quantification of all
elements at single digit ng.g-1 levels is required.
In this application brief the Thermo Scientific™
ELEMENT™ GD high resolution glow discharge sectorfield mass spectrometer is assessed for the
impurity analysis of high purity copper.
Method
In industrial manufacturing environments, the
ELEMENT GD MS is used for routine production quality
control in a 2 or 3 shift rotation. Sample throughput is
therefore critical to ensure a timely feedback based on
analytical results. Sample surfaces were prepared by wet
grinding with SiC paper (grit 120). Milling would be an
appropriate alternative for sample preparation.
The instrumental parameters listed in Table 1 were
defined to meet the needs of a routine production lab.
Table 1: Instrumental parameters
Parameter
Value
Matrix sensitivity
2 · 1010 cps total Cu (MR)
Analysis time
5 min pre-sputter
5 min acquisition
Discharge current
Discharge voltage
45 mA
~750 V
Anode parts
High purity graphite
Results
• Sample throughput at such low quantification levels is
relatively high with 5 samples per hour.
Interference
63
Cu40Ar,
65
Cu38Ar
Table 2: Results obtained from repeat analysis of a 6N Cu sample
at multiple spots
Element
Typical LoD
[µg.g-1]
Obtained LoD
[µg.g-1]
Ag
<0.01
0.005
As
<0.01
0.001
Bi
<0.01
0.0003
Fe
<0.01
0.001
Pb
<0.01
0.0004
S
<0.1
0.03
Sb
<0.01
0.001
Se
<0.01
0.002
Te
<0.01
0.001
~0.01 µg·g-1 103Rh
Figure 1: High mass resolution (R>10000) spectrum showing
baseline separation between the CuAr interferences and the
monoisotopic rhodium. Note the logarithmic intensity scale.
Conclusion
• A well characterized in-house control sample with
elemental concentrations in the µg.g-1 level can be used
to monitor daily performance.
• Typically a one-point calibration using a reference
material (e.g. ERM-EB385) is sufficient for accurate
trace element quantification due to the intrinsic linearity
of the complete system.
The ELEMENT GD MS provides a routine, reliable and
straightforward solution for ultra-trace analysis of high
purity copper. Under routine operation, detection limits of
<0.01 µg.g-1 in 5N or 6N copper samples are easily
achieved. A fast sample turn-around of 5 samples per
hour guarantees rapid feedback to production with the
capacity of analyzing ~120 samples per day. Automatic
resolution switching (within 1 s) enables the routine use of
optimum mass resolution for the elimination of matrix
induced interferences.
• When suitable reference materials are not available,
semi-quantitative analyses provide accuracies to within
± 30 % using the Standard RSF calibration strategy.
• The ELEMENT GD MS analytical process is simple
enough that routine analyses are performed by shift
operators.
• Residual precious metals are of additional interest in
Cu refining processes; the most challenging of which is
rhodium, as it suffers from polyatomic interferences.
As can be seen in Figure 1, these can be easily resolved
by the ELEMENT GD MS. Since the resolution
switching is fast (< 1 s) and automatic, elements that
require the highest resolution, such as Rh, can be
routinely analyzed at the ng.g-1 level.
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Appli cat i on Br i e f 4 3 1 9 5
• The results in Table 2 demonstrate excellent detection
limits for all trace elements analyzed.