ARL 3460 Metal Analyzer déf. 15.3.

2001 17:16 Page 3

Analysis of Iron and Steel Application

by Optical Emission
Summary
ARL 3460 Metals Analyzer

Introduction following elements: nickel, chromium, manganese,

silicon, cobalt, tungsten, molybdenum and
The ARL 3460 Metals Analyzer is custom designed to vanadium. This category covers steels which are
meet your specific requirements whether you are a destined for a wide variety of uses such as :
small cast iron foundry or a large steel plant. Thermo • Stainless steels (ferritic or austenitic 18/8,
ARL’s long experience in metals analysis comes from maraging and all types of special stainless steels)
an installed base of over 6000 spectrometers world- • Tool steels
wide. The ARL 3460 is the answer to your metallurgi- • High manganese steels
cal analysis needs; whether they be incoming material • High speed steels
control or metal QC and production analysis. • Special high alloys steels, such as Ni-hard,
Working 24 hours a day and 7 days a week, the ARL Ni-resist, etc..
3460 delivers dependable performance year after year.
ARL 3460 Metals Analyzer
Iron
Several kinds of iron exist, distinguished by their
composition and use. They belong to two main
categories:
• Pig irons (hot metal); basic product for the
manufacture of steel.
• Cast irons; used for the production of semi-
manufactured products.

From a metallographic point of view, a distinction can

be made between white cast iron with a cementite
structure, and grey cast iron which contains free
graphite, either in the form of laminae or nodules.

Alloy cast irons also exist where alloying elements

such as nickel, chromium, manganese, copper, etc.,
are added to improve hardness, corrosion resistance
or engineering properties (Ni-hard, Ni-resist, etc. …).
Steel
Typically steels are divided in two main qualities:
1. Low alloy steels (≤ 94% iron)
2. High alloy steels (with notable quantities of Cr,
Ni, Mn, Mo, Co, W, etc. …).
The ARL 3460 optical emission spectrometer can
determine up to 60 elements. The HiRep source has
the flexibility to customize the excitation parameters
providing the best analytical conditions for a wide
variety of sample types.
The source uses the HEPS (High Energy-Spark)
technique to minimize the metallurgical effects and
produce consistently accurate results.

1. Low alloy steels The printout of average concentration for the

The total element alloying is generally less than
5-7 %. The main elements are: Mn (≤ 2%),
Cr (≤ 3%), Mo (≤ 1.5%), Cu (≤ 2%), Ni (≤ 5%),
and V (≤ 1%). The so called “free-cutting steels”
with a concentration of 0.2 - 0.3% sulfur or lead,
need a special calibration.
required elements from a repeat analysis is obtained
in typically one minute.
Sample preparation
The sample is generally prepared by using a grinding
machine. Milling machines can also be recommended.

2. High alloy steels Sample analysis time

High alloy steels contain, in addition to iron and Low Alloy Low Alloy Cast Iron Free
Steels with Steels with Cutting
carbon, notable quantities of one or more of the Nitrogen & Nitrogen Steels
sol./insol. Al
27s 25s 31s 68s
ARL 3460 Metal Analyzer déf. 15.3.2001 17:16 Page 4

Calibration summary Factory calibration (CARL)

Twelve “qualities” are available for specific alloy types: Thermo ARL's optical emission spectrometers can
be factory calibrated for iron and steel utilizing
• Low Alloy Steel
CARL (Calibration Applied Research Laboratories).
• Free Cutting Steel (S and Pb ≤0.3 %)
CARL is a very sophisticated multi-variable regression
• Chrome Steel (ferritic stainless steel)
tool that corrects for matrix effects as well as spectral
• Chrome-Nickel Steel (austenitic stainless steel)
interferences. CARL can provide an immediate
• Manganese Steel (Mn ≤20 %)
"turnkey" system which gives the user the highest
• High Speed Steel (Co ≤10 %)
accuracy possible. The calibrations are available for
• Valve Steel (Ni, Mn and Cr ≤20 %)
the different qualities given left. For each quality
• Low Alloy Steel NIST (USA calibration with
Thermo ARL uses certified material as standard
NBS samples)
samples and setting-up samples are delivered with
• Cast Iron (including Ni-hard - Ni ≤7 %)
the instrument to maintain the accuracy of the
• High Alloy Cast Iron (Cr ≤32 % & Ni ≤16 %)
calibration.
• Nickel Resist (Ni ≤35 %)
• Global (including all qualities except for free
cutting steel)

Example of factory calibration

CAL-34Fe-01 CAL-34Fe-02 CAL-34Fe-03 CAL-34Fe-04 CAL-34Fe-05 CAL-34Fe-06 CAL-34Fe-09 CAL-34Fe-12

Element Low Alloy Steel Free Cutting Steel Cr Steel Cr-Ni Steel Mn Steel High Speed Steel Cast/Nodular Global
Iron Ni-Hard
Fe 99.9%-80% 99.9%-90% 90%-65% 89%-45% 91%-70% 95%-48% 97%-70% 99.8%-42%
Al 0.001-0.3 0.001-0.10 0.002-0.3 0.001-0.2 0.003-0.1 0.001-0.1 0.003-1.5
As 0.001-0.1 0.01-0.07 0.002-0.1 0.003-0.1
B 0.0002-0.01 0.0002-0.01 0.0005-0.1 0.001-0.1
Bi 0.002-0.01 0.003-0.03
C 0.003-1.3 0.003-1.3 0.03-2. 0.01-1. 0.5-1.5 0.3-1.2 1.7-4.2 0.01-4.2
Ca 0.0002-0.01 0.0005-0.015
Ce 0.002-0.08 0.002-0.015
Co 0.001-0.3 0.008-0.15 0.01-0.2 0.02-0.4 0.1-0.4 0.05-10. 0.001-0.2 0.002-12.
Cr 0.001-5. 0.001-3. 10.-25. 10.-26. 0.1-4. 2.-5. 0.008-9. 0.005-32.
Cu 0.001-0.7 0.001-0.7 0.04-1.5 0.03-4. 0.003-0.5 0.01-0.1 0.003-2.5 0.005-6.5
La 0.003-0.025 0.002-0.04
Mg 0.001-0.1 0.001-0.15
Nodular Cast only
Mn 0.001-2. 0.05-1.7 0.2-1.5 0.02-10. 8.-20. 0.08-0.5 0.002-2. 0.005-20.
Mo 0.001-1.5 0.001-1. 0.03-2.5 0.01-6. 0.02-2. 0.1-9. 0.001-1.3 0.005-9.
Nb 0.001-0.6 0.005-0.05 0.005-1.5 0.005-2.5 0.002-0.06 0.002-2.7
Ni 0.002-5. 0.002-3. 0.05-4. 3.-35. 0.03-1.5 0.03-0.45 0.003-7. 0.005-35.
P 0.001-0.1 0.001-0.1 0.003-0.03 0.002-0.04 0.01-0.06 0.01-0.05 0.002-1. 0.005-1.4
Pb 0.001-0.02 0.001-0.3 0.002-0.03 0.002-0.03
S 0.0005-0.08 0.001-0.3 0.001-0.03 0.001-0.04 0.005-0.06 0.001-0.04 0.001-0.2 0.002-0.2
Sb 0.002-0.07 0.002-0.15 0.005-0.15
Si 0.001-3. 0.002-1.4 0.2-1.2 0.05-4. 0.2-1.4 0.1-0.4 0.2-3.5 0.005-5.5
Sn 0.001-0.1 0.001-0.1 0.002-0.03 0.005-0.03 0.001-0.3 0.002-0.3
Ta 0.008-0.15 0.008-0.04 0.01-0.1
Te 0.002-0.03 0.002-0.03
Ti 0.001-0.4 0.001-0.1 0.02-0.2 0.002-2. 0.001-0.3 0.002-2.
V 0.001-1. 0.001-0.5 0.03-0.9 0.005-0.25 0.02-0.3 0.4-3. 0.001-0.4 0.002-9.5
W 0.004-0.6 0.05-0.3 0.1-0.5 0.02-4. 1.8-22. 0.003-0.1 0.01-22.
Zn 0.001-0.02 0.002-0.025 0.002-0.025
Zr 0.001-0.1 0.005-0.05 0.002-0.1

CAL-34Fe-01 CAL-34Fe-34 CAL-34Fe-312

N 0.001-0.02 0.003-0.65 0.005-0.65
ARL 3460 - TYPICAL DETECTION LIMITS (3 sigma) AND PRECISION VALUES (1 sigma) FOR IRON BASE

ELEMENT Al As B Bi C Ca Ce Co Cr Cu Mg Mn Mo N Nb
Typical
1.1 2.4 0.3 4.1 6.9 0.4 6.0 1.2 1.6 0.6 2.8 1.2 1.7 3.5 2.6
DL [ppm]
ARL 3460 Metal Analyzer déf.

Guaranteed
≤ 2.2 ≤ 6.2 ≤ 0.9 ≤ 8.3 ≤ 12 ≤ 1.5 ≤ 11 ≤ 2.0 ≤ 4.0 ≤ 1.8 ≤ 5.6 ≤ 2.0 ≤ 3.9 ≤ 6.9 ≤ 5.0
DL [ppm]
Level [%] SD SD SD SD SD SD SD SD SD SD SD SD SD SD SD
0.001 0.00006 0.00015 0.00002 0.00018 0.00023 0.00007 0.00025 0.00005 0.00015 0.00006 0.0001 0.00005 0.0002 0.0003 0.00013
15.3.2001

0.002 0.00009 0.00015 0.00004 0.00026 0.00023 0.00014 0.00025 0.00005 0.00015 0.00007 0.0001 0.00005 0.0002 0.0003 0.00016
0.005 0.00016 0.00015 0.00012 0.00042 0.00023 0.00033 0.00025 0.00005 0.00015 0.00009 0.00025 0.00005 0.0002 0.00045 0.00022
17:16

0.01 0.00025 0.00020 0.00038 0.00062 0.00023 0.00065 0.00030 0.00010 0.0002 0.00012 0.0005 0.00008 0.0003 0.0006 0.00035
0.02 0.00038 0.00025 0.0010 0.00085 0.0003 0.0013 0.00050 0.00015 0.0003 0.00018 0.0009 0.00015 0.0006 0.0008 0.0005
0.05 0.0007 0.00035 0.0006 0.0013 0.0004 0.0005 0.0003 0.0022 0.00032 0.0010 0.0013 0.0010
Page 5

0.1 0.0012 0.00050 0.0010 0.0007 0.0008 0.0006 0.0043 0.0006 0.0015 0.0018 0.0015
0.2 0.0020 0.0020 0.0015 0.0012 0.0012 0.0080 0.0011 0.0020 0.0025 0.0025
0.3 0.0030 0.0025 0.0020 0.0015 0.0020 0.0026 0.0030 0.0031 0.0048
0.5 0.0050 0.0037 0.0030 0.0020 0.0035 0.0048 0.0050 0.009
1. 0.008 0.0062 0.0060 0.0035 0.0065 0.0091 0.008 0.017
2. 0.010 0.010 0.0050 0.010 0.0135 0.010 0.030
3. 0.015 0.015 0.007 0.015 0.017 0.012
4. 0.020 0.020 0.008 0.020 0.021 0.015
5. 0.025 0.010 0.025 0.039 0.025
10. 0.05 0.015 0.065 0.040
20. 0.025
30. 0.035
40. 0.045

Remarks: 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.
For multibase instruments, some analytical performance may vary based on the analytical line selected.
Values in brackets for detection limits can be obtained by using the most sensitive lines, or a longer analysis time.
Guaranteed DLs are calculated at 95% confidence limit.
 ARL 3460 - TYPICAL DETECTION LIMITS (3 sigma) AND PRECISION VALUES (1 sigma) FOR IRON BASE

ELEMENT Ni P Pb S Sb Si Sn Ta Te Ti V W Zn Zr
Typical
1.8 2.0 3.3 1.5 8.5 3.6 1.8 16 4.3 0.7 1.4 9.0 3.0 1.7
DL [ppm]
ARL 3460 Metal Analyzer déf.

Guaranteed
≤ 5.1 ≤ 4.2 ≤ 5.7 ≤ 3.0 ≤ 23 ≤ 8.4 ≤ 3.5 ≤ 32 ≤ 22 ≤ 1.0 ≤ 2.0 ≤ 20 ≤ 5.0 ≤ 3.3
DL [ppm]
Level [%] SD SD SD SD SD SD SD SD SD SD SD SD SD SD
0.001 0.00015 0.00008 0.00017 0.00009 0.00025 0.00015 0.0001 0.0006 0.00015 0.00003 0.00007 0.00045 0.0002 0.00012
15.3.2001

0.002 0.00015 0.00009 0.00020 0.00014 0.00025 0.00015 0.0001 0.0006 0.00025 0.00005 0.00007 0.00045 0.00025 0.00012
0.005 0.00015 0.00010 0.00035 0.00028 0.00027 0.00015 0.0001 0.00075 0.0004 0.00012 0.00007 0.00050 0.0003 0.00013
17:16

0.01 0.00015 0.00013 0.0007 0.00050 0.00033 0.00020 0.00015 0.0010 0.0007 0.00022 0.0001 0.00050 0.00035 0.0003
0.02 0.00016 0.00026 0.0014 0.0009 0.00046 0.00025 0.00025 0.0015 0.0005 0.0002 0.00055 0.00038 0.0006
0.05 0.0003 0.0006 0.0035 0.0020 0.0010 0.00030 0.00040 0.0025 0.0010 0.0005 0.00065 0.00042 0.0015
Page 6

0.1 0.0005 0.0016 0.007 0.0040 0.0022 0.0007 0.00065 0.0035 0.0020 0.0008 0.00085 0.0052
0.2 0.0009 0.0033 0.014 0.0075 0.0012 0.0030 0.0015 0.0015 0.021
0.3 0.0013 0.005 0.021 0.012 0.0018 0.0050 0.0020 0.002 0.046
0.5 0.0020 0.009 0.0028 0.010 0.0030 0.003 0.10
1. 0.004 0.019 0.0053 0.020 0.006 0.005
2. 0.007 0.010 0.011 0.010
3. 0.011 0.015 0.015 0.015
4. 0.013 0.02 0.020 0.020
5. 0.016 0.025 0.025
10. 0.035 0.045
20. 0.065 0.09
30. 0.10 0.15
40. 0.13

Remarks: 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.
For multibase instruments, some analytical performance may vary based on the analytical line selected.
Values in brackets for detection limits can be obtained by using the most sensitive lines, or a longer analysis time.
Guaranteed DLs are calculated at 95% confidence limit.
ARL 3460 Metal Analyzer déf. 15.3.2001 17:16 Page 1

Accuracy
Precision is only a small part of providing accurate
analyses. The most important factor is the accuracy
and quality of the calibration standards. Next is the
development of the calibration curve relative to a
specific analytical task. Matrix matching and high
energy pre-burn reduce or eliminate matrix effects,
and spectral interferences are significantly reduced by
applying appropriate corrections.
The example shown below illustrates the significant
improvement with the CARL calibration.
Stability
Stability of the instrument is of the utmost importance
when doing routine analysis. Typical mid-term stability
measured over 24 hours shows that the standard
deviation achieved is below two times the precision
value, which is excellent.
The example below shows the long term stability of
two elements recorded over a period of more than 15
days without any intermediate drift correction. The
values almost never went outside the control limits.
Moving Average Chart: C%
0.0200

0.0180

0.0160

0.0140

0.0120

11-12-9 15-12-9 20-12-9 24-12-9 28-12-9 04-01-9

18:30:0 19:55:0 23:21:3 23:13:5 22:46:0 19:00:0
50 100 150 200 250 300

Moving Average Chart: Cr%

0.0310

0.0300

BEFORE CARL 0.0290

0.0280

0.0270

0.0260

0.0250

11-12-9 15-12-9 20-12-9 24-12-9 28-12-9 04-01-9

18:30:0 19:55:0 23:21:3 23:13:5 22:46:0 19:00:0
50 100 150 200 250 300

Performance guarantee
Thermo ARL guarantees the precision shown in the
attached tables using homogeneous samples and
recommended sample preparation

This list will be updated as improvements are announced.

AFTER CARL Please contact your nearest Thermo ARL office for
the most recent values.

Options The precision is calculated from the formula:

1. Global calibration for iron i=n

where:
Σ(Xi-Xi)2
SD(1σ)=± i=l Xi the individual readings
This calibration offers more than a sorting pro- n–1 Xi the arithmetic mean of the
gram in terms of accuracy and number of analyzed individual values
elements. The global calibration for iron can be RSD = SD n the number of determinations
considered as the basic low cost calibration of the Xi
instrument, allowing the analysis of unknown samples.
The DL (Detection Limit)) is defined as three times
2. PIM 2 the standard deviation of the background expressed
in concentration units.
This option permits the determination of
soluble/insoluble aluminum and boron in low
alloy steel. It does not need special skills from the
operator and replaces a costly wet chemistry procedure.

For both options, separate application notes are

available on request.
ARL 3460 Metal Analyzer déf. 15.3.2001 17:16 Page 2

Thermo ARL
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En Vallaire Ouest C, case postale, CH-1024 Ecublens, Switzerland
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Conclusion Tel.: ++61-(0)2-9898-1244, Fax : ++61-(0)2-9684-4244
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meet the critical needs of the metals analysis markets: Tel.: ++43-(0)1-333 50 34-0, Fax : ++43-(0)1-333 50 34-26
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