Application

Note: 41260
Analysis of Iron and Steel with desktop
Optical Emission Spectrometer
ARL QuantoDesk CCD-based Metals Analyzer

To these can be added some more specific

Key Words characteristics, including image analysis in discrete
elements (pixels) with exact field registration.
• ARL QuantoDesk
• CCD
• Iron & Steel
• Optical Emission

Introduction
The Thermo Scientific ARL QuantoDesk is a compact
desktop spectrometer for metals analysis based on CCD
(Charge Coupled Device) technology. A single CCD
replaces the photomultiplier detectors used in traditional
arc/spark spectrometers and gives the instrument immense
flexibility. The argon flushed sample stand and spark
source are comparable to those of larger instruments and
enable the ARL QuantoDesk to be as capable as a
conventional laboratory spectrometer.
The ARL QuantoDesk offers the solution to perform a
rapid check close to the furnace where its performance
meets the analytical needs of Quality Control departments.
Its simple architecture allows for high accuracy, stability
and reliability, making it the solution for numerous
industrial applications in rugged environments.
Charge Coupled Device (CCD)
In its broadest definition, a charge-coupled device (CCD)
image sensor is an analogue integrated circuit that
converts an optical image into an electronic output. As
with many semiconductor components, the evolution of
CCD’s from a laboratory concept has been extremely
rapid, boosted by their potential for a wide range of
applications in both consumer products and sophisticated
professional equipment.
Today, our company uses this advanced technology in
its spectrometers. The ARL QuantoDesk’s CCD has the
equivalent of 8,044 detectors of 7 by 7 µm. Because of
this, all the wavelengths (from 170 to 410 nm) necessary
for multi-element, multi-base analysis are available
without the need for additional hardware. Their
integrated nature provides their best-known features,
namely unlimited lifetime and miniaturization.
Each spectrum is stored, and a retrospective analysis
for “extra” elements is possible without the need to spark
the sample another time.
Factory calibration (CARL)
Thermo Scientific optical emission spectrometers can be
factory calibrated for iron and steel utilizing CARL, a very
sophisticated multi-variable regression tool that corrects
for matrix effects as well as spectral interferences. CARL
provides an immediate “turnkey” system which gives the
user the highest accuracy possible. The calibrations are
available for the different qualities given below. For each
quality, we use certified material as standard samples and
setting-up samples are delivered with the instrument to
maintain the accuracy of the calibration.
The calibrations available are for:
• Low alloy steel
• Cast iron
• Cr steel
• Cr-Ni steel
• Mn steel
• High speed steel
• Ni resist
• High alloy cast iron
Sample preparation Table 2: Accuracy example on a low cast iron sample
The sample is usually prepared with a grinding machine.
BS 1C
EL CERTIFIED CONF. INTERVAL MEASURED DIFFERENCE
Sample analysis time VALUE % % VALUE % %

C 2.359 0.019 2.376 0.017

MATERIAL TIME PER RUN
S 0.060 0.0039 0.054 0.0061
Low Alloy Steel 24 s
Mn 1.79 0.011 1.77 0.023
Chrome-Nickel Steel 24 s
Ni 1.99 0.011 2.01 0.016
Cast Iron 31 s
Cr 0.52 0.02 0.51 0.016
Mo 0.433 0.009 0.426 0.007
Accuracy V 0.116 0.005 0.121 0.005
Precision is only a small part of providing accurate analyses. Ti 0.083 0.0032 0.089 0.0057
The most important factor is the accuracy and quality of Co 0.244 0.0086 0.266 0.0225
the calibration standards. Spectral interferences are Al 0.033 0.0023 0.033 0.0001
significantly reduced by the high flexibility of the
ARL QuantoDesk. The example below illustrates the Table 3 : Accuracy example on a stainless steel sample
excellent linearity and the reduced absorption effects
achieved on element carbon in low alloy steel. IARM 18B
EL CERTIFIED CONF. INTERVAL MEASURED DIFFERENCE
VALUE % % VALUE % %
C 0.085 0.0028 0.082 0.0031
Si 3.70 0.04 3.61 0.086
P 0.032 0.0028 0.037 0.0051
Mn 8.58 0.085 8.59 0.014
Ni 8.50 0.06 8.30 0.20
Cr 16.4 0.1 16.5 0.14
Cu 0.362 0.0073 0.360 0.0024
Co 0.124 0.007 0.1327 0.0087

Memory effects
Memory effects are determined by running an alloyed
sample (Ni: 20,7 %, Cr: 25,75 %) and then measuring a
pure sample, until the correct concentrations are
measured. No memory effect is observed: the correct
concentration is obtained at the second run already,
confirming the suitability of the ARL QuantoDesk for
multiple matrices and multiple qualities purposes.
Tables 1 to 3 show that the analysis of CRM’s (Certified
Reference Material) provides results within the uncertainty Performance guarantee
interval (3s) of the certified values in most cases. Our company guarantees the precision shown in Table 4
using homogeneous samples and recommended sample
Table 1: Accuracy example on a low alloy steel sample preparation. The list will be updated as improvements are
CKD187A announced. Please contact your nearest Thermo Fisher
EL CERTIFIED CONF. INTERVAL MEASURED DIFFERENCE Scientific office or consult our website at
VALUE % % VALUE % %
www.thermo.com/oes for the most recent values.
Al 0.019 0.002 0.0239 0.005
C 0.119 0.004 0.126 0.007
The precision is calculated from the formula:
Cr 3.51 0.04 3.526 0.02 where:
Cu 0.036 0.003 0.0281 0.008 i=n
X i the individual readings
Mn 0.525 0.007 0.5334 0.008 (X i - X i )2
X i the arithmetic means of
Mo 0.565 0.008 0.533 0.032 i=1 the individual readings
SD (1s) = +
n-1
Ni 0.085 0.004 0.0904 0.005 n the number of determinations
P 0.035 0.0015 0.0366 0.0016
S 0.0018 0.001 <3*DL
Si 0.567 0.023 0.5447 0.022
V 0.558 0.008 0.551 0.008
W 0.67 0.02 0.6645 0.006
Table 4: ARL QuantoDesk typical detection limits (3 sigma) and precision values (1 sigma) for iron base
ELEMENT Al C Ca Ce Co Cr Cu La Mg Mn Mo

Guaranteed DL [ppm] 30 20 1 50 15 25 15 10 6 20 50
Level % SD SD SD SD SD SD SD SD SD SD SD
0.001 0.00005
0.002 0.0001 0.0002
0.005 0.002 0.00025 0.0007 0.001 0.0005 0.001 0.0003 0.001
0.01 0.001 0.002 0.0005 0.0035 0.001 0.001 0.001 0.0015 0.0005 0.001 0.0045
0.02 0.0015 0.002 0.0035 0.001 0.001 0.001 0.0015 0.001 0.001 0.0045
0.05 0.0015 0.002 0.004 0.0035 0.001 0.0015 0.0015 0.002 0.005
0.1 0.002 0.002 0.005 0.0015 0.002 0.0035 0.002 0.0055
0.2 0.0025 0.003 0.008 0.002 0.0025 0.0025 0.007
0.5 0.003 0.007 0.003 0.005 0.0035 0.01
1 0.015 0.005 0.009 0.0055 0.02
2 0.025 0.01 0.02 0.01 0.03
3 0.03 0.02 0.025 0.02 0.04
4 0.04 0.035 0.035 0.025 0.05
5 0.05 0.035 0.065
10 0.06 0.09
20 0.07

ELEMENT Nb Ni P S Si Sn Ti V W Zn Zr

Guaranteed DL [ppm] 30 25 15 40 30 30 5 10 250 3 20

Level % SD SD SD SD SD SD SD SD SD SD SD
0.001 0.0004
0.002 0.0003 0.00055 0.0004
0.005 0.0015 0.001 0.0003 0.00055 0.0005 0.001
0.01 0.0015 0.0015 0.0025 0.002 0.0025 0.002 0.0003 0.0006 0.0005 0.001
0.02 0.002 0.0015 0.003 0.002 0.0025 0.0025 0.0004 0.0007 0.0005 0.0015
0.05 0.004 0.002 0.003 0.0025 0.003 0.003 0.0005 0.001 0.015 0.0025
0.1 0.0045 0.002 0.005 0.003 0.0035 0.0035 0.001 0.0015 0.015 0.004
0.2 0.005 0.0025 0.005 0.005 0.007 0.002 0.0025 0.02
0.5 0.01 0.004 0.008 0.007 0.003 0.0035 0.025
1 0.015 0.006 0.015 0.01 0.0035 0.0055
2 0.025 0.01 0.02 0.008
3 0.04 0.025 0.02
4 0.05 0.03 0.05
5 0.055
10 0.085
20 0.2
30 0.25

This data applies when homogeneous samples are prepared by recommended sample preparation methods.
The precision given is typical performance. Guaranteed values will be 1.5 times higher.
SD = Standard Deviation. DL = Detection Limit.
Stability Conclusion In addition to these
Stability of the instrument is of the utmost importance The ARL QuantoDesk is a compact, desktop spectrometer offices, Thermo Fisher
when performing routine analysis. Mid-term stability for metals analysis, based on CCD technology, which Scientific maintains
measured in a laboratory environment over 24 hours provides flexibility for the analysis. It can be installed and a network of represen-
shows that the standard deviation achieved is at the level be operational on the same day it is delivered. Simple to tative organizations
of the precision value. handle, the ARL QuantoDesk provides quick, precise and throughout the world.
The example below shows the long-term stability of reliable analysis.
nickel and sulfur in a stainless steel sample recorded over Its accuracy, associated with its excellent stability and
a period of 8 days without any intermediate drift correction. reliability allows to have results you can rely on 24 hours
No standardization was required, as the measured a day, 365 days a year without spending a lot of time in
concentrations stayed almost within the control limits. long lasting and expensive drift corrections.
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