sma70 - the analysis of iron and steel...spectro’s proprietary cmos+t technology. from trace...

Introduction

The all new SPECTROLAB S represents the

next generation of stationary metal analyzer

equipped with advanced semiconductor

detector technology combined with

additional time resolved measurement

capabilities (CMOS+T). This innovative

step improves the analytical performance

and also offers the ability of TRS (time

resolved spectroscopy) and SSE (single

spark evaluation). These two options were

the remaining two advantages of PMT (photo

multiplier tube) detectors. Modifications

regarding read out and excitation system in

combination with improved CMOS detector

capabilities have overcome these final

technical / analytical limitations.

AN APPLICATION REPORT FROMSPECTRO ANALYTICAL INSTRUMENTS

SMA-70

SPECTROLAB S LAS01

The Analysis of Iron and Steel

SPECTROLAB S – The Analysis of Iron and Steel2

The all new SPECTROLAB S now combines best analytical performance, stability, flexibility,

speed (measurement time of less than 20 seconds for low-alloy steel including the analysis of

Nitrogen) and extended maintenance intervals (spark stand cleaning intervals improved by a

factor of 8, in manual mode).

Apart from all these technical improvements, the instrument has a reduced footprint of 27%,

compared to its predecessor.

This new analyzer allows the accurate analysis of all main components and trace elements in

steel, iron and all possible alloys. The identification of unknown / unspecified elements via the

new spectra scan option is also possible.

InstrumentationSPECTROLAB S Features

Optical Systems

Optic I:

• Wavelength range 120 nm – 240 nm

• Focal length 750 mm, Holographic grating with 3600 gr. / mm

• CMOS detectors

Optic II:

• Wavelength range 210 nm – 770 nm

• Focal length 750 mm, Holographic grating 2400 gr. / mm

• CMOS detectors

The applicable and configured wavelength range is based on the customer’s application

requirements. Both optics are temperature stabilized and pressure compensated.

SPECTROLAB S – The Analysis of Iron and Steel 3

CMOS+T

The SPECTROLAB S has the world’s first CMOS-based (complementary metal oxide

semiconductor) detector system that’s perfected for high-end metal analysis — thanks to

SPECTRO’s proprietary CMOS+T technology. From trace elements to multimatrix applications, it

provides extremely fast, highly accurate, exceptionally flexible analysis.

Plasma Generator

The benefit of this full digitalization with high fidelity is the guarantee that the spark pulse

created is the spark pulse desired, every time.

Precision is improved and so is the similarity of the generated spark signals (unit uniformity).

With our off-line digital control, we ensure that each plasma generator delivers identical spark

signals, with a negligible deviation between any two plasma generators.

Every plasma generator has a programmable output power waveform for application specific

optimization.

Online drift correction and background correction

• Permanent control of the peak position of each line and readjustment if needed (iCAL 2.0)

• Recalculation of the background signal wherever it is possible

Optimized Measurement Times

• Dynamic pre-burn time, reflecting the sample quality

• Minimized delay between measurement sequences

• Optimized number of excitation parameters including frequencies of up to 1000 Hz


Time Resolved Spectroscopy

A time delayed integration to reduce the background and ionic radiation observation:

• Improved detection limits

• Reduction of line interferences caused by interfering ion lines

Single Spark Evaluation (SSE):

• Tool for fast detection of, inclusion complexity dependent, soluble and insoluble components

• Detection of inclusions

• Recognition of correlation between elements in inclusions

Intelligent Calibration Logic (iCAL 2.0)

• Profile position control and standardization with only one sample

Accuracy of Analysis

It is the aim of modern OES spectrometers to greatly reduce the influence of the structure

and composition (matrix) effects. The SPECTROLAB S combines traditional technologies like

HEPS-High Energy Pre Spark to reach the stationary phase by “remelting” a small portion of the

sample, resulting in a reduced structure effect.


Element C Si Mn P S Cr Mo Ni

Calibration range (%)

0.0001 - 5 0.0002 - 20 0.0002 - 23 0.0002 - 2.4 0.0001 - 0.450 0.0001 - 33 0.00003 - 10 0.0001 - 46

Detection Limit (ppm)

1 2 2 2 1 1 0.3 1

Element Al Co Cu Nb Ti V W Pb


0.0001 - 3.1 0.0002 - 18 0.00008 - 8.1 0.0002 - 3 0.0001 - 3.6 0.0001 - 10 0.0005 - 21 0.0002 - 0.35


1 2 0.8 2 1 1 5 2

Element Sn Mg As Zr Bi Ca Ce Sb


0.0001 - 0.4 0.00005 - 0.26 0.0003 - 0.23 0.0002 - 0.23 0.0002 - 0.040.00005 -

0.0130.0002 - 0.17 0.0005 - 0.24


1 0.5 3 2 2 0.5 2 5

Element Se Te Ta B Zn La Ag Nd


0.0005 - 0.31 0.0002 - 0.08 0.0008 - 0.76 0.00005 - 0.110.00005 -

0.0450.0002 - 0.03

0.00004 - 0.005

0.0005 - 0.013


5 2 8 0.5 0.5 2 0.4 5

Element N O


0.0004 - 1.1 0.002 - 0.025


4 20

Table 1: Calculation of detection limit (DL) according to DIN 32645:2008-11 with a confidence limit of 99.7% (3 sigma), recorded on a production series device.


Table 2: RN19/... Low-alloy steel

Element C Si Mn P S Cr Mo Ni Al Co Cu

1 0.811 1.16 1.55 0.120 0.113 2.92 0.926 2.96 0.795 0.754 0.57

2 0.811 1.15 1.56 0.119 0.112 2.93 0.928 2.96 0.800 0.757 0.565

3 0.811 1.14 1.57 0.120 0.115 2.91 0.932 2.95 0.799 0.756 0.567

4 0.809 1.13 1.56 0.119 0.113 2.91 0.932 2.95 0.807 0.756 0.561

5 0.810 1.14 1.56 0.120 0.118 2.91 0.932 2.96 0.793 0.755 0.567

6 0.815 1.14 1.56 0.119 0.115 2.91 0.925 2.95 0.802 0.756 0.567

7 0.802 1.14 1.56 0.118 0.113 2.93 0.929 2.96 0.802 0.753 0.567

0.81 1.14 1.56 0.119 0.114 2.92 0.929 2.95 0.800 0.755 0.566

SD 0.0039 0.0094 0.0069 0.00073 0.002 0.0083 0.0029 0.0058 0.0047 0.0013 0.0028

RSD (%rel.) 0.486 0.828 0.441 0.615 1.78 0.284 0.311 0.196 0.583 0.176 0.495

Element Nb Ti V W Pb Sn As Zr Bi Ca Ce

1 0.52 0.151 0.672 0.784 0.0170 0.130 0.0934 0.155 0.0089 0.001500 0.0025

2 0.521 0.153 0.670 0.779 0.0171 0.129 0.0928 0.146 0.0084 0.000050 0.0023

3 0.522 0.153 0.675 0.789 0.0168 0.128 0.0927 0.140 0.0088


Table 3: S08-SUS5/... Cast iron

Element C Si Mn P S Cr Mo Ni Al Co

1 3.71 2.09 0.624 0.0349 0.0066 0.0085 0.0013 0.9680 0.0354 0.0034

2 3.7 2.09 0.627 0.0347 0.0069 0.0085 0.0012 0.9690 0.0359 0.0034

3 3.73 2.07 0.627 0.0339 0.0069 0.0085 0.0013 0.9700 0.0355 0.0034

4 3.72 2.11 0.633 0.0338 0.0069 0.0085 0.0012 0.9690 0.0355 0.0033

5 3.72 2.09 0.627 0.0348 0.0069 0.0085 0.0012 0.9720 0.0354 0.0034

6 3.72 2.08 0.626 0.0339 0.0063 0.0084 0.0012 0.9670 0.0356 0.0033

7 3.71 2.09 0.628 0.0346 0.0069 0.0088 0.0013 0.9710 0.0355 0.0035

3.72 2.09 0.627 0.0344 0.0068 0.0085 0.0012 0.97 0.0355 0.0034

SD 0.0115 0.0132 0.0028 0.00049 0.00024 0.00013 0.00003 0.0015 0.00018 0.00006

RSD (%rel.) 0.311 0.631 0.439 1.44 3.49 1.49 0.159 0.52

Element Cu Nb Ti V W Pb Sn Mg As Zr

1 0.0035 0.0031 0.00075 0.4760 0.0023 0.00034 0.0695 0.0903 0.0042 0.0014

2 0.0034 0.0031 0.00073 0.4720 0.0025 0.00029 0.0698 0.0893 0.0043 0.0014

3 0.0033 0.0031 0.00072 0.4690 0.0024 0.00026 0.0687 0.0923 0.0042 0.0014

4 0.0036 0.0030 0.00074 0.4660 0.0021 0.00037 0.0694 0.0889 0.0043 0.0014

5 0.0034 0.0031 0.00075 0.4690 0.0023 0.00039 0.0704 0.0906 0.0045 0.0014

6 0.0034 0.0031 0.00068 0.4710 0.0024 0.00034 0.0693 0.0918 0.0042 0.0014

7 0.0034 0.0031 0.00072 0.4700 0.0024 0.00035 0.0688 0.0939 0.0042 0.0013

0.0034 0.0031 0.00074 0.47 0.0023 0.00033 0.0694 0.091 0.0043 0.0014

SD 0.00007 0.00004 0.00002 0.0032 0.00012 0.00004 0.00057 0.0018 0.0001 0.00003

RSD (%rel.) 0.676 0.822 1.95 1.82

Element Bi Ce Sb Te B Zn La N Nd Fe

1 0.0049 0.0286 0.0493 0.0016


Table 4: E/... Cr-Cr/Ni steel

Element C Si Mn P S Cr Mo Ni Al

1 0.0615 0.681 1.49 0.0083 0.0037 14.79 1.22 25.45 0.204

2 0.0611 0.684 1.49 0.0083 0.0034 14.84 1.22 25.35 0.207

3 0.0603 0.672 1.48 0.0084 0.0033 14.86 1.21 25.46 0.206

4 0.0604 0.682 1.47 0.0085 0.0033 14.87 1.22 25.38 0.205

5 0.0614 0.683 1.48 0.0085 0.0036 14.81 1.22 25.45 0.207

6 0.0608 0.683 1.48 0.0085 0.0033 14.82 1.23 25.43 0.207

7 0.0614 0.676 1.48 0.0082 0.0035 14.85 1.22 25.43 0.207

0.061 0.68 1.48 0.0084 0.0034 14.83 1.22 25.42 0.206

SD 0.0005 0.0045 0.0071 0.0001 0.00016 0.0288 0.0054 0.041 0.00095

RSD (%rel.) 0.811 0.656 0.481 1.14 0.194 0.44 0.161 0.463

Element Co Cu Nb Ti V W Sn As Zr

1 0.0709 0.0171 0.0487 2.07 0.270 0.0438 0.0013 0.0018 0.0023

2 0.0709 0.0172 0.0473 2.06 0.270 0.0423 0.0014 0.0014 0.0023

3 0.0712 0.0168 0.048 2.04 0.272 0.0436 0.0014 0.0015 0.0024

4 0.0710 0.0168 0.0488 2.05 0.274 0.0425 0.0014 0.0015 0.0023

5 0.0711 0.0168 0.0486 2.07 0.274 0.0419 0.0013 0.0020 0.0023

6 0.0711 0.0168 0.0482 2.05 0.274 0.0431 0.0013 0.0016 0.0023

7 0.0708 0.0167 0.05 2.06 0.273 0.0465 0.0014 0.0018 0.0023

0.071 0.0169 0.0485 2.06 0.272 0.0434 0.0014 0.0016 0.0023

SD 0.00014 0.00019 0.00084 0.0129 0.0016 0.0015 0.00005 0.00021 0.00003

RSD (%rel.) 0.195 1.1 1.72 0.626 0.596 3.54 3.4 1.24

Element Ca Ce Se Ta B La N O Fe

1 0.00024 0.00033 0.0044 0.0043 0.0064 0.0014 0.0019 0.0041 53.5

2 0.00029 0.00050 0.0046 0.0050 0.0064 0.0013 0.0016 0.0044 53.6

3 0.00016 0.00052 0.0048 0.0042 0.0064 0.0015 0.0018 0.0039 53.5

4 0.00022 0.00055 0.0045 0.0055 0.0064 0.0014 0.0017 0.0039 53.5

5 0.00014 0.00066 0.0045 0.0047 0.0065 0.0014 0.0014 0.0045 53.6

6 0.00015 0.00051 0.0046 0.0051 0.0064 0.0014 0.0015 0.0043 53.6

7 0.00021 0.00036 0.0044 0.0044 0.0063 0.0013 0.0016 0.0039 53.5

0.0002 0.00049 0.0045 0.0048 0.0064 0.0014 0.00017 0.0042 53.5

SD 0.00006 0.00011 0.00012 0.00046 0.00007 0.00006 0.00017 0.00025 0.0244

RSD (%rel.) 2.7 0.0456


Table 5: RH18/... Highspeed steel


1 1.20 0.362 0.240 0.0217 0.0136 4.01 3.57 0.331 0.0248

2 1.22 0.366 0.241 0.0219 0.0131 4.02 3.56 0.330 0.0244

3 1.21 0.363 0.241 0.0216 0.0138 3.99 3.55 0.332 0.0250

4 1.21 0.363 0.239 0.0221 0.0138 4.01 3.57 0.335 0.0243

5 1.23 0.366 0.241 0.0220 0.0139 4.03 3.58 0.329 0.0239

6 1.21 0.362 0.239 0.0222 0.0139 3.99 3.53 0.332 0.0247

7 1.21 0.361 0.240 0.0221 0.0137 4.02 3.54 0.330 0.0245

1.21 0.363 0.24 0.0219 0.0137 4.01 3.56 0.331 0.0245

SD 0.0095 0.002 0.001 0.00022 0.00028 0.0146 0.0184 0.002 0.00035

RSD (%rel.) 0.78 0.558 0.423 1 2.02 0.364 0.516 0.595 1.44

Element Co Cu Ti V W Sn As N Fe

1 9.76 0.129 0.0038 3.10 9.21 0.0119 0.0178 0.0364 68.0

2 9.75 0.129 0.0038 3.14 9.30 0.0120 0.0179 0.0375 67.8

3 9.72 0.130 0.0039 3.10 9.26 0.0119 0.0179 0.0373 68.0

4 9.71 0.130 0.0039 3.11 9.27 0.0121 0.0179 0.0375 67.9

5 9.78 0.129 0.0038 3.14 9.32 0.0121 0.0181 0.0377 67.7

6 9.78 0.130 0.0038 3.06 9.25 0.0123 0.0180 0.0371 68.0

7 9.76 0.130 0.0037 3.03 9.25 0.0122 0.0179 0.0355 68.0

9.75 0.13 0.0038 3.1 9.26 0.0121 0.0179 0.037 67.9

SD 0.0273 0.0006 0.00006 0.0431 0.0349 0.00017 0.0001 0.0008 0.11

RSD (%rel.) 0.28 0.461 1.39 0.377 1.38 0.549 2.16 0.162


Table 6: BAS493/... Manganese steel


1 0.826 0.847 11.11 0.125 0.0109 0.273 0.962 3.11 0.0358

2 0.824 0.845 11.12 0.124 0.0112 0.274 0.958 3.11 0.0361

3 0.825 0.849 11.18 0.125 0.0110 0.278 0.965 3.11 0.0357

4 0.841 0.857 11.19 0.127 0.0113 0.277 0.964 3.11 0.0354

5 0.834 0.843 11.13 0.124 0.0111 0.274 0.965 3.15 0.0365

6 0.832 0.857 11.19 0.123 0.0118 0.277 0.960 3.12 0.0371

7 0.824 0.852 11.11 0.122 0.0114 0.274 0.960 3.12 0.0361

0.829 0.85 11.15 0.124 0.0112 0.275 0.962 3.12 0.0361

SD 0.0063 0.0056 0.0378 0.0014 0.00031 0.002 0.0028 0.0156 0.00055

RSD (%rel.) 0.76 0.662 0.339 1.15 2.76 0.74 0.296 0.5 1.54

Element Co Cu Nb Ti V Sn N Fe

1 0.0106 0.0190 0.0048 0.0028 0.0280 0.0013 0.0232 82.6

2 0.0106 0.0190 0.0047 0.0027 0.0278 0.0015 0.0244 82.6

3 0.0110 0.0192 0.0047 0.0027 0.0282 0.0013 0.0238 82.5

4 0.0108 0.0191 0.0048 0.0026 0.0276 0.0014 0.0245 82.5

5 0.0108 0.0190 0.0047 0.0028 0.0280 0.0014 0.0233 82.5

6 0.0104 0.0190 0.0047 0.0027 0.0275 0.0014 0.0249 82.5

7 0.0111 0.0191 0.0049 0.0027 0.0279 0.0013 0.0233 82.6

0.0107 0.0191 0.0048 0.0027 0.0278 0.0014 0.0239 82.6

SD 0.00023 0.00007 0.00009 0.00005 0.00023 0.00008 0.00067 0.0652

RSD (%rel.) 2.12 0.362 1.89 1.81 0.84 2.79 0.079


Table 7: CRRM5/... Ni resist

Element C Si Mn P S Cr Mo

1 3.43 0.230 0.317 0.0281 0.0177 30.14 0.615

2 3.44 0.228 0.315 0.0279 0.0180 30.24 0.613

3 3.45 0.229 0.318 0.0277 0.0176 30.49 0.610

4 3.44 0.227 0.316 0.0283 0.0179 30.25 0.616

5 3.46 0.229 0.317 0.0282 0.0179 30.49 0.615

6 3.47 0.226 0.316 0.0284 0.0178 30.22 0.617

7 3.44 0.230 0.316 0.0279 0.0177 30.28 0.615

3.44 0.228 0.316 0.0281 0.0178 30.3 0.614

SD 0.02 0.0017 0.00091 0.00025 0.00014 0.137 0.0025

RSD (%rel.) 0.58 0.729 0.288 0.89 0.79 0.451 0.407

Element Ni Al Co Cu Ti V Fe

1 0.385 0.150 0.0051 0.231 0.0093 0.111 64.3

2 0.382 0.154 0.0047 0.228 0.0092 0.111 64.3

3 0.381 0.147 0.0045 0.226 0.0092 0.110 64.0

4 0.388 0.151 0.0054 0.229 0.0093 0.112 64.2

5 0.385 0.149 0.0049 0.228 0.0093 0.110 64.0

6 0.386 0.151 0.0051 0.230 0.0093 0.111 64.2

7 0.384 0.153 0.0049 0.233 0.0092 0.112 64.2

0.384 0.151 0.0049 0.229 0.0093 0.111 64.2

SD 0.0021 0.0022 0.0003 0.0023 0.00006 0.00063 0.142

RSD (%rel.) 0.559 1.45 0.983 0.626 0.57 0.221


Table 8: NIRM8/... Cr-hard cast

Element C Si Mn P S Cr

1 1.42 5.54 1.64 0.0771 0.0156 2.53

2 1.41 5.57 1.64 0.0782 0.0153 2.54

3 1.41 5.52 1.65 0.0786 0.0156 2.55

4 1.43 5.58 1.64 0.0788 0.0149 2.53

5 1.41 5.56 1.65 0.0771 0.0148 2.56

6 1.41 5.61 1.65 0.0797 0.0152 2.55

7 1.41 5.56 1.64 0.0782 0.0154 2.54

1.42 5.57 1.65 0.0782 0.0153 2.54

SD 0.0068 0.0285 0.0065 0.00092 0.00032 0.012

RSD (%rel.) 0.481 0.512 0.398 1.18 2.07 0.472

Element Mo Ni Cu Mg Ce Fe

1 0.751 35.23 0.224 0.037 0.0129 52.5

2 0.764 35.16 0.224 0.0368 0.0128 52.5

3 0.752 35.35 0.222 0.0369 0.0128 52.4

4 0.762 35.12 0.224 0.0359 0.0119 52.6

5 0.751 35.38 0.223 0.0351 0.0121 52.3

6 0.766 35.14 0.223 0.0366 0.0121 52.5

7 0.756 35.19 0.224 0.0371 0.0125 52.5

0.757 35.22 0.223 0.0365 0.0124 52.5

SD 0.0065 0.102 0.00082 0.00071 0.00041 0.0893

RSD (%rel.) 0.854 0.29 0.368 1.96 0.17


Summary

This report shows the capabilities of the new SPECTROLAB S for the analysis of iron and steel.

GERMANYSPECTRO Analytical Instruments GmbHBoschstrasse 10D-47533 KleveTel: +49.2821.892.0Fax: [email protected]

U.S.A.SPECTRO Analytical Instruments Inc.91 McKee DriveMahwah, NJ 07430Tel: +1.800.548.5809 +1.201.642.3000Fax: [email protected]

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www.spectro.com

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SPECTRO operates worldwide and is present in more than 50 countries. For SPECTRO near you, please visit www.spectro.com/worldwide© 2019 AMETEK Inc., all rights reserved, subject to technical modifications • F-19 • 80902327• Rev. 0 • Photos: SPECTRO, Adobe StockRegistered trademarks of SPECTRO Analytical Instruments GmbH • : USA (3,645,267); EU (005673694); “SPECTRO”: EU (009693763); SPECTROLAB: EU (1069339); Germany (39604365); USA (4,103,747); China (1069339); Japan (1069339); South Korea (1069339)

sma70 - the analysis of iron and steel...spectro’s proprietary cmos+t technology. from trace...

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