Procedure – Powder/Chip Samples

Prepare the instrument as outlined in the operator's instruction manual.

Login a minimum of three Blank reps.

Press the Analyze button on the instrument screen. After a short delay, the loading head slide-block will open. Insert a *** Nickel Capsule (leave capsule open) into the open port at top of loading head.

Note: samples using automation should be placed in the appropriate autoloader position before starting the analysis sequence. Once the sequence has started, the automatic analysis will start and end automatically.

User-Friendly Brand Software Cornerstone

LECO's exclusive brand software enables the user to have complete access to analysis Cornerstone control, method settings, diagnostics, reporting, and more in a highly organized and immersive environment. Designed through a collaboration of customer feedback and innovative engineering,Cornerstone allows the user to conduct all of their day-to-day operations within a single Analysis screen designed for speed and ease-of-use. Our innovative grouping of sample data into sets and replicates simplifies the data output and automatically calculates relevant statistics, alleviating the need for additional data processing.

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Sample Preparation

Sampling and sample preparation of refractory metals such as titanium and zirconium is somewhat different from that of steel. Unlike steel samples, hydrogen is not as mobile in this group of materials; therefore, storage in liquid nitrogen or dry ice is not required. However, it is important to keep the sample cool when cutting or sectioning. Sample preparation for oxygen and nitrogen determination has beendifferent from that of hydrogen determination.

Sample Preparation

Typically, titanium and zirconium samples are chemically etched to remove surface contamination when oxygen and nitrogen are determined. However, etching can introduce hydrogen into the sample.

ASTM method E 1409 "Determination of Oxygen and Nitrogen in Titanium and Titanium Alloys by the Inert

Gas Fusion Technique", as updated in 1996, permits either etching or abrading (filing) of the test specimen.

ASTM E 1447 "Determination of Hydrogen in Titanium and Titanium Alloys by the Inert Gas Fusion Thermal

Conductivity/Infrared Detection Method" permits surface preparation by abrading (if necessary to remove

contamination). Differences in sample preparation present somewhat of a dilemma regarding simultaneous

determination of O, N, and H in titanium. However, abrading samples with a file to remove surface

contamination will yield accurate O, N, and H results. The ONH836 utilizes a high-power electrode furnace to quickly and efficiently release the target gases from within the sample, which allows for a very rapid simultaneous determination of oxygen, nitrogen, and hydrogen.

736 Series: Oxygen/Nitrogen by Inert Gas Fusion

The 736 family of Elemental Analyzers is designed for routine measurement of oxygen and nitrogen content of

inorganic materials, ferrous and nonferrous alloys, andrefractory materials using the inert gas fusion technique.

These instruments feature our Cornerstone brand ® software, a custom interface designed specifically for

touch-screen operation. Developed by combining longterm research with customer feedback, this easy-to-use

software gives you complete access to instrument control, analysis settings, diagnostics, reporting, and more—without sacrificing valuable bench space.

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Oxygen, Nitrogen, and Hydrogen in Refractory Metals

Summary

One of the most critical chemical specifications of titanium alloys is the hydrogen content. Too high of a

hydrogen content can cause hydrides to precipitate, which can lead to embrittlement and subsequent

cracking when the alloy is stressed. Hydrogen pickup typically occurs during downstream processing steps

such as heat treating, pickling, and cleaning.

The LECO ONH836 is a simultaneous oxygen, nitrogen, and hydrogen determinator that utilizes an electrode furnace, inert carrier gas, and both infrared and thermal conductivity detection to meet the analytical needs of the refractory metal industry. 

This application note was written specifically for use with the LECO ONH836 series determinator.