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NIST announces their first Hydrogen-in-Titanium pin SRM

In the fall of 2015, NIST announced their success in working with our company to produce the first high-quality pin standards with precisely-dosed levels of hydrogen in titanium at a very low uncertainty level that will benefit the industry.

Here is the article making the announcement:


The quarterly Magazine of NIST's Material Measurement Laboratory -FALL 2015

Article: "Newly Commercialized Process Makes Better Material for Hydrogen in Titanium SRMs"

Recently, NIST issued SRM 2453a Hydrogen in Titanium in pin form in support of titanium manufacturers and their customers in the aerospace, defense, and power generation industries. The material for SRM 2453a was created using a newly commercialized process based on one developed at NIST about 10 years ago. MM researchers Richard Lindstrom and Rick Paul developed a procedure for controlled dosing of known amounts of hydrogen chemically bound into the titanium alloy matrix to ensure long term stability. They used the process to prepare materials for three new SRMs, tailoring the amounts of hydrogen to match specification limits on the maximum amounts of hydrogen allowed in titanium alloys for aerospace and power generation applications. As planning began for replacements of SRMs 2452, 2453, and 2454, technical project leader John Sieber presented the project at a meeting of ASTM International CommitteeE01 on Analytical Chemistry of Metals, Ores and Related Materials. Subsequently, a small businessowner who was developing a commercial version of the NIST process in an effort to launch a company to develop and sell certified reference materials, contacted Dr. Sieber. NIST contracted with the company and, within a year, the resulting batch of titanium pins became available as NIST SRM 2453a.

The contract with the small business called for titanium alloy with a known mass fraction of total hydrogen with very low heterogeneity across the batch, plus a uniform size and mass per piece of titanium. Wire titanium alloy was chopped into pins of highly uniform mass and dimensions to make the SRM easier to use with ASTME1447 Standard Test Method for Determination of Hydrogen in Titanium and Titanium Alloys by Inert Gas Fusion Thermal Conductivity/Infrared Detection Method. The contractor was required to prove by analysis that the pins contained the required amount of hydrogen with the required low composition variance. Hydrogen analyses were performed after calibration of method E1447using a special gas–dosing approach, which served two purposes. First, the calibration parameters were traceable to the mole through the use of known volumes of ultrahigh-purity hydrogen gas. Second, the quantitative results were expected to provide data of sufficient quality for material variance characterization, for demonstration of short-term hydrogen stability, and for combination with results from NIST prompt gamma-ray activation analyses for certification of the mass fraction of total hydrogen.

A little more than one year after delivery of the titanium pins, NIST issued SRM 2453a. The overall uncertainty of the certified value for H in SRM2453a is half the uncertainty of the value for SRM2453. This improvement will enable commercial reference materials producers and manufacturing laboratories to obtain lower uncertainties of their certified values and certified product results, respectively. The titanium-pin producing small business is continuing efforts to manufacture and to market a new line of CRMs.

Contact: John Sieber, john.sieber@nist.gov

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