Analysis of Iron and Steel for Spark Spectrometers

Analyzing iron and steel is the main analytical use of today’s spark spectrometers. In addition to the conventional commercial applications for steel, increasing demands from the automotive industry has ushered in a rapid wave of alloy developments.

These new alloys are sought after in automotive manufacturing due to their lightweight and enhanced properties while delivering optimal performances.

The Q4 POLO is the perfect tool for the precise analysis of steel and cast iron.

With the latest optimized MultiVisionTM optics, the Q4 POLO offers exceptional analytical performance allowing the instrument to monitor the nitrogen content in low alloyed steels and iron casting processes, identify other trace elements, and, of course, provide dependable results on all relevant alloying elements.

Iron and steel samples.

Figure 1. Iron and steel samples. Image Credit: Bruker AXS Inc.

Sampling and Sample Preparation

The chemical composition at various phases of the steel refining and casting processes is monitored by establishing the composition of the steel samples extracted from the liquid steel.

The preparation of the samples is carried out by grinding or milling processes to produce a flat and homogeneous surface. Each of the samples in this article had been prepared following the sample preparation procedure using a grinding machine.

Certified Reference Material (CRM)

Certified Reference Material (CRM) refers to reference materials characterized by a metrologically authentic proce­dure for a number of specified properties: an accompanying certificate provides the value of the properties specified (whether one or many), any associated uncertainty and a statement of metrological traceability.

A recognized certifying organ­ization will grant CRMs certification by applying approved certification procedures, as set out in the most up-to-date ISO Guide 35. The organ­ization is typically associated with a federal government or at least recognized by a federal government or an authenticated accreditation entity.

A CRM is the greatest standard to which an analytical ref­erence material can be held because it can be directly traced back to the appropriate SI units and because of the con­fidence placed on the company or organization from which the material came.

Statistics

Population: The entire group that conclusions will be taken from.

Sample: A specific group used for data acquisition.

Average (X): A number denoting the central or general value in a set of data, particularly the mode, median or (most commonly) the mean, which is determined by divid­ing the sum of the values in the set by their overall number.

Standard Deviation (σ): Measures the amount of variation or dispersion of a set of values

Precision and Accuracy

The International Organization for Standardization (ISO) stipulates that ‘precision’ is the closeness of agreement between independent test results acquired under a set of agreed conditions.

Precision is contingent on the distribution of random errors and is not relative to the true or spec­ified value. On the other hand, accuracy is the closeness of agreement between a test result and the accepted reference value (SSE).

Precision and accuracy.

Figure 2. Precision and accuracy. Image Credit: Bruker AXS Inc.

Performance Disclaimer and Remarks
The published values have been acquired from quite different types of materials and should be regarded as “typical” values.
The given performances only apply for homogeneous samples, appropriately prepared, and are subject to technical modification. Calibration ranges can be extended with samples provided by the customer.

Q4 POLO – Certified Reference Material

Results

The Q4 POLO’s reproducibility and the method described are demonstrated by a sequence of repetitive measure­ments of certified reference material across various groups of alloys and element concentrations.

Table 2. CRM Low Alloy Steel - Fe110 - 181A. Source: Bruker AXS Inc.

Element [%] C Si Mn P S Cr Mo Ni Cu Al V W N
MEAN1) 0.224 0.434 0.973 0.039 0.0071 0.660 0.385 0.727 0.092 0.016 0.303 0.186 0.0057
STD2) 0.0031 0.0032 0.0074 0.0008 0.0003 0.0038 0.004 0.0011 0.0019 0.0005 0.0013 0.005 0.0006
1 0.224 0.431 0.975 0.038 0.0075 0.662 0.387 0.727 0.090 0.017 0.304 0.189 0.0051
2 0.221 0.434 0.981 0.039 0.0069 0.654 0.386 0.729 0.091 0.016 0.304 0.188 0.0054
3 0.226 0.432 0.967 0.039 0.0072 0.662 0.382 0.726 0.092 0.017 0.302 0.18 0.0053
4 0.221 0.439 0.963 0.038 0.0073 0.658 0.381 0.727 0.095 0.016 0.305 0.192 0.0064
5 0.228 0.436 0.977 0.04 0.0067 0.663 0.391 0.728 0.093 0.016 0.302 0.182 0.0064
Certified Values
Value 0.225 0.435 0.971 0.039 0.007 0.660 0.385 0.725 0.093 0.016 0.302 0.188 0.005
Error 0.008 0.013 0.022 0.002 0.001 0.011 0.009 0.011 0.003 0.001 0.006 0.005 -

 

Table 3. CRM Stainless Steel - Fe130 - 463/1. Source: Bruker AXS Inc.

Element [%] C Si Mn P S Cr Mo Ni Cu B Co N
MEAN1) 0.019 0.272 1.402 0.025 0.019 18.44 0.267 10.24 0.277 0.0021 0.116 0.062
STD2) 0.0007 0.0025 0.0063 0.0008 0.0011 0,027 0,0033 0.030 0.0014 0.0002 0.0013 0.0024
1 0.018 0.273 1.402 0.025 0.019 18.48 0.265 10.20 0.276 0.0022 0.116 0.062
2 0.019 0.276 1.408 0.024 0.018 18.46 0.264 10.23 0.278 0.0018 0.117 0.060
3 0.019 0.270 1.408 0.024 0.017 18.44 0.272 10.25 0.279 0.0019 0.117 0.059
4 0.020 0.272 1.396 0.025 0.020 18.43 0.265 10.25 0.276 0.0021 0.114 0.063
5 0.019 0.270 1.395 0.026 0.019 18.41 0.268 10.28 0.276 0.0024 0.115 0.065
Certified Values
Value 0.019 0.270 1.400 0.025 0.019 18.46 0.265 10.20 0.276 0.0022 0.116 0.063
Error 0.002 0.008 0.011 0.002 0.002 0.05 0.007 0.06 0.005 0.0003 0.005 0.001

 

Table 4. CRM Cast Iron - Fe120 - 238A. Source: Bruker AXS Inc.

Element [%] C Si Mn P S Cr Mo Ni Cu Co Mg V Zn
MEAN1) 3.5142 1.511 0.440 0.053 0.0060 0.017 0.0021 1.101 0.977 0.0065 0.040 0.112 0.024
STD2) 0.0063 0.0066 0.0009 0.0008 0.0002 0.0008 0.0005 0.0046 0.0044 0.0004 0.0013 0.0004 0.0004
1 3.520 1.509 0.441 0.054 0.0066 0.017 0.0019 1.098 0.976 0.0069 0.039 0.112 0.024
2 3.521 1.521 0.439 0.052 0.0065 0.017 0.0021 1.099 0.973 0.0062 0.040 0.111 0.024
3 3.514 1.509 0.440 0.053 0.0060 0.018 0.0024 1.101 0.98 0.0062 0.039 0.112 0.024
4 3.509 1.512 0.439 0.053 0.0064 0.018 0.0029 1.109 0.983 0.0062 0.039 0.112 0.023
5 3.507 1.503 0.439 0.054 0.0065 0.016 0.0015 1.098 0.973 0.0069 0.042 0.112 0.024
Certified Values
Value 3.5 1.5 0.43 0.054 0.006 0.018 0.002 1.1 0.97 0.006 0.039 0.11 0.024
Error 0.02 0.02 0.007 0.001 0.0006 0.001 0.001 0.02 0.01 0.001 0.02 0.005 0.001

 

1) MEAN = arithmetic average
2) STD = absolute standard deviation (1
σ)
3) %RSD = relative standard deviation in percent

Q4 POLO – Long-term Stability – Stainless Steel

Results

The stability of the Q4 POLO is determined by a sequence of repetitive measurements on a reference material, registered over several days, without the correction of any intermediate drift.

Typical Chemical Composition of X2CrNiMo17-12-2 - 1.4404 – AISI/SAE 316L

  C Si Mn P S Cr Mo Ni N
min % - - - - - 16.50 2.00 10.00 -
max % 0.030 1.00 2.00 0.045 0.030 18.50 2.50 13.00 0.10

 

Element [%] C Si Mn P S Cr Mo Ni Cu
MEAN 0.019 0.329 1.70 0.039 0.026 16.57 2.013 10.211 0.441
STD 0.0013 0.0010 0.012 0.0010 0.0005 0.0308 0.0097 0.040 0.0029
1 0.020 0.329 1.69 0.041 0.026 16.59 2.014 10.22 0.443
2 0.018 0.329 1.69 0.039 0.025 16.62 2.019 10.20 0.443
3 0.020 0.329 1.69 0.038 0.026 16.59 2.027 10.25 0.441
4 0.020 0.331 1.69 0.040 0.026 16.59 2.003 10.20 0.441
5 0.018 0.330 1.69 0.039 0.025 16.57 2.022 10.22 0.441
6 0.020 0.330 1.71 0.040 0.025 16.52 2.004 10.25 0.439
7 0.020 0.328 1.72 0.040 0.026 16.57 2.017 10.16 0.441
8 0.017 0.330 1.69 0.039 0.025 16.59 2.020 10.14 0.446
9 0.017 0.328 1.71 0.038 0.025 16.53 1.998 10.27 0.436
10 0.020 0.328 1.72 0.038 0.026 16.55 2.005 10.20 0.437

 

Element [%] Al B Co Nb Ti V W N Fe
MEAN 0.009 <0.0005 0.163 0.059 0.0066 0.037 0.049 0.047 68.28
STD 0.0002 0.0002 0.0008 0.0045 0.0004 0.0016 0.0032 0.0011 0.034
1 0.0094 <0.0005 0.162 0.055 0.0065 0.039 0.046 0.047 68.26
2 0.0094 <0.0005 0.163 0.055 0.0072 0.039 0.050 0.048 68.25
3 0.0096 <0.0005 0.163 0.062 0.0065 0.039 0.050 0.047 68.21
4 0.0096 <0.0005 0.164 0.056 0.0064 0.037 0.055 0.046 68.28
5 0.0092 <0.0005 0.164 0.055 0.0064 0.036 0.043 0.048 68.28
6 0.0092 <0.0005 0.164 0.064 0.0072 0.035 0.050 0.046 68.29
7 0.0091 <0.0005 0.163 0.065 0.0063 0.039 0.052 0.048 68.30
8 0.0092 <0.0005 0.163 0.055 0.0063 0.037 0.049 0.049 68.34
9 0.0091 <0.0005 0.162 0.055 0.0066 0.035 0.048 0.046 68.29
10 0.0096 <0.0005 0.164 0.064 0.0070 0.037 0.050 0.048 68.30

 

Summary

The compact Q4 POLO is a Spark Optical Emission Spectrometer (OES) that combines ultra-precision analysis capabilities with a lower cost of ownership in a practical, small foot­print.

It is ready for analysis from the first day, covering all relevant elements and wide concentration ranges. Meanwhile, the Q4 POLO also offers high uptime, reduced maintenance and trouble-free operation.

High precision, dependable analysis is now available for every production floor and foundry to easily and cost-effectively obtain results.

Analysis of Iron and Steel for Spark Spectrometers

Image Credit: Bruker AXS Inc.

ELEMENTAL.SUITE

ELEMENTAL.SUITE software assists routine daily tasks. Automated average and limit checks guarantee safe operation. Just one click is required to save, print and report any analyses.

Developed for maximum usability, the plug-in-based architecture of ELE­MENTAL.SUITE offers optimal flexibility for all analytical require­ments.

Analysis of Iron and Steel for Spark Spectrometers

Image Credit: Bruker AXS Inc.

This information has been sourced, reviewed and adapted from materials provided by Bruker AXS Inc.

For more information on this source, please visit Bruker AXS Inc.

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