Chemical Metrology for Metals, Ores, and Related Materials

Summary

A wide range of industrial sectors and their customers and suppliers are involved directly with NIST in the prioritization and development of certified reference materials, and in the development and validation of standard test methods for raw materials, intermediates, and finished products.

Description

High purity crystal of titanium metal.

Credit: Lane Sander

In the arena of industrial commodities, the primary challenges are to provide measurement tools and reference materials that allow U.S. industry to establish comparability of measurement results to results obtained by customers, competitors, and regulators for the basic chemical properties of products, intermediates, and by-products on a worldwide basis. All members of a given industrial supply chain benefit from critically evaluated standard test methods validated using trusted reference materials. Due to the wide range of materials and the rapid changes of product compositions, NIST efforts are targeted at key, high-value commodities with the greatest range of metrological impact. The private sector can leverage NIST reference materials by creating their own reference materials targeted at products having more specialized compositions and applications. The goals of this program are to: 

• Increase the availability of reference materials (both NIST and private sector) for basic industrial commodities including metals, ores, and related materials       
• Collaborate with the private sector through standards development organizations and industry associations
• Make use of multiple methods of analysis at NIST and collaborating laboratories 
• Contribute to development of new and improved standard methods of test
• Support other U.S. government agencies' measurement needs.

Major Accomplishments

In the past several years, the following SRMs have been developed or renewed in collaboration with industry: 

• Completed new and renewal SRMs for steel, silicon metal, zirconium, and copper mine tailings,         

• Participated in development of international standard test methods listed below,  

• Upgraded existing SRM certificates to comply with ISO Guide 31 for more than 20 ferrous alloys, nonferrous alloys, and geological materials, 

• Initiated SRM development projects for free-cutting brass, lead-free solder, molybdenum concentrates, silicon carbide, copper ore, refined copper, and feldspar. 

Standard Methods of Test

The following industry standard methods of test were developed and approved with significant contributions by NIST.

• ASTM International E135-08b Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials         
• ASTM International E539-07 Standard Test Method for X-Ray Fluorescence Spectrometric Analysis of 6Al-4V Titanium Alloy         
• ASTM International E1361-02(2007) Standard Guide for Correction of Interelement Effects in X-Ray Spectrometric Analysis         
• ASTM International E2465-06 Standard Test Method for Analysis of Ni-Base Alloys by X-Ray Fluorescence Spectrometry    
• ASTM International E2626-08 Standard Guide for Spectrometric Analysis of Reactive and Refractory Metals

Additional Technical Details 

This program is comprised of a number of collaborations between NIST and industry sectors. Design of materials for new SRMs is accomplished in cooperation with materials and analysis experts from industry. Specifications for composition, homogeneity, and quantity are based on current and projected industry needs. Value assignment projects are designed to include high-performance analytical methods at NIST, state-of-the-art laboratory methods in industry, and classical chemistry methods where available and appropriate.

Associated Product(s) 

Click on the SRM number below to be transferred to a website from which you can access the material's Certificate of Analysis. For additional materials, please refer to the online SRM catalog categories. 

• SRM 57b Silicon Metal. Values assigned for elements in manufacturing specifications for silicon metal 

• SRM 331a Copper Ores Mill Tails. Values assigned for copper, noble metals, and trace elements on the EPA Toxic Release Inventory 

• SRM 360c Zirconium Alloy (Sn-Fe-Cr). Values assigned for tin and trace elements listed in nuclear industry manufacturing specifications 

• SRMs 1761a and 1763b Low Alloy Steel. Values assigned for elements listed in manufacturing specifications for steel 

• SRM 2451 Fine Carbon (Activated). Values assigned for mercury, gold, cyanide 

ASSOCIATED PUBLICATIONS

1. Vicenzi, E. P., Lam, T., Weaver, J. L., Herzing, A. A., Mccloy, J. S., Sjolom, R., and Pearce, C. I., "Major to trace element imaging and analysis of iron age glasses using stage scanning in the analytical dual beam microscope (tandem)," Heritage Science, 10, (2022). 

2. Sieber, J., Marlow, A., Paul, R., Barber, C., Wood, L., Yu, L., Rieke, A., Carl, R., Kutnerian, A., McCandless, J., and Wallace, C., "Quantitative analysis of zirconium alloys using borate fusion and wavelength dispersive X-ray fluorescence spectrometry," X-Ray Spectrometry, 50, 210-223 (2021). 

3. Jahrman, E. P., Holden, W. M., Govind, N., Kas, J. J., Rana, J., Piper, L. F. J., Siu, C., Whittingham, M. S., Fister, T. T., and Seidler, G. T., "Valence-to-core X-ray emission spectroscopy of vanadium oxide and lithiated vanadyl phosphate materials," Journal of Materials Chemistry A, 8, 16332-16344 (2020). 

4. Weaver, J. S., Kreitman, M., Heigel, J. C., and Donmez, M. A., "Mechanical Property Characterization of Single Scan Laser Tracks of Nickel Superalloy 625 by Nanoindentation," Tms 2019 148Th Annual Meeting & Exhibition Supplemental Proceedings, 269-278 (2019). 

5. Jahrman, E. P., Seidler, G. T., and Sieber, J. R., "Determination of Hexavalent Chromium Fractions in Plastics Using Laboratory-Based, High-Resolution X-ray Emission Spectroscopy," Analytical Chemistry, 90, 6587-6593 (2018). 

6. Weaver, J. S., Li, N., Mara, N. A., Jones, D. R., Cho, H., Bronkhorst, C. A., Fensin, S. J., and Gray, G. T., "Slip transmission of high angle grain boundaries in body-centered cubic metals: Micropillar compression of pure Ta single and bi-crystals," Acta Materialia, 156, 356-368 (2018). 

7. Weaver, J. S., Jones, D. R., Li, N., Mara, N., Fensin, S., and Gray, G. T., "Quantifying heterogeneous deformation in grain boundary regions on shock loaded tantalum using spherical and sharp tip nanoindentation," Materials Science and Engineering A-Structural Materials Properties Microstructure and Processing, 737, 373-382 (2018). 

8. Wang, H. W., Wesolowski, D. J., Proffen, T. E., Vlcek, L., Wang, W., Allard, L. F., Kolesnikov, A. I., Feygenson, M., Anovitz, L. M., and Paul, R. L., "Structure and Stability of SnO2 Nanocrystals and Surface-Bound Water Species," Journal of the American Chemical Society, 135, 6885-6895 (2013). 

9. Sieber, J. R., Mackey, E. A., Marlow, A. F., Paul, R., and Martin, R., "Validation of an alkali reaction, borate fusion, X-ray fluorescence method for silicon metal," Powder Diffraction, 22, 146-151 (2007). 

10. Chen-Mayer, H. H., Mildner, D. F. R., Lamaze, G. P., and Lindstrom, R. M., "Imaging of neutron incoherent scattering from hydrogen in metals," Journal of Applied Physics, 91, 3669-3674 (2002). 

11. Paul, R. L., "Measurement of phosphorus in metals by RNAA," Journal of Radioanalytical and Nuclear Chemistry, 245, 11-15 (2000). 

12. Paul, R. L. and Lindstrom, R. M., "Determination of hydrogen in metals, semiconductors, and other materials by cold neutron prompt gamma-ray activation analysis," Hydrogen in Semiconductors and Metals, 513, 185-190 (1998).