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.

Instrument calibration/drift correction.

a. Login a minimum of 3 Standard replicates.

b. Weigh a ~1.000 gram of a calibration/drift standard, enter the mass and standard identification into appropriate replicate fields.

c. Press the Analyze button on the instrument screen. After a short delay, the loading head slide-block will open.

d. Place the calibration/drift standard into the open port at the top of the loading head.

e. Press the Analyze button on the instrument screen again, the loading head slide-block will close and the lower electrode will open.

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氧氮氫分析儀的操作過程

氧氮氫分析儀可根據的用戶的要求定制。該分析儀配備兩個不同靈敏度的探測器，在更多的應用中保證了準確度。

操作簡單而且安全。在樣品稱重以后，樣品的重量數據通過電子界面傳導至相連的電腦中，也可以在軟件界面中手動輸入樣品的重量。

樣品被放置在水平放置的爐子中的低溫區域。分析開始以后，爐子開始向上轉動，然后樣品逐漸落入加熱區。通過添加載體氣體氮氣，氫氣被擴散出來并且隨載體被傳導至一個高靈敏度的熱傳導測量池。

通常一次測量的時間在3到15分鐘之間。在分析的過程中設備可以顯示測試信號和設備的參數，從信號的評估到結果在界面上的顯示全部自動完成；而測量數據則被傳導至LIMS（實驗室信息管理系統）中。無需過多的保養和維護，而除塵器和凈化管的維護工作也方便。

Sample Preparation

Sampling and sample preparation is an important issue because traditional methods used to obtain samples for oxygen and nitrogen determination are different from those recommended for hydrogen, especially when sampling molten metal. The main difference in steel sampling procedures for oxygen/nitrogen and hydrogen is due to the mobilityof hydrogen. Special precautions must be used when sampling for hydrogen. From molten steel and iron, a sample must be quickly quenched in cold water and chilled in a refrigerant such as liquefied nitrogen or a mixture of acetone and solid carbon dioxide in order to reduce losses of hydrogen from diffusion. Losses of oxygen and nitrogen from diffusion are not a problem. A sample that is taken for hydrogen and

chilled in a refrigerant can also be used for oxygen and nitrogen determination. However, a sample that is typically taken for oxygen and/or nitrogen determination is not suitable for hydrogen determination due to hydrogen loss (diffusion). Surface contamination must be removed by filing or light grinding, using care not to overheat the sample.

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Procedure – Powder/Chip Samples

Determine the instrument blank.

Press the Analyze button on the instrument screen again, the loading head slide-block will close and the lower electrode will open.

Clean the upper and lower electrode either manually or remove the crucible and press the analyze button to clean with an automatic cleaner if applicable.

Add approximately 0.05 g of *** Graphite Powder to a 782-720 Graphite Crucible.

Firmly place the crucible on the lower electrode tip or appropriate autoloader position.

Cornerstone氧氮氧分析軟件允許用戶在單一分析界面中完成日常的所有工作，快速而且簡單易用。廣東LECO分析儀廠家供應

Procedure – Powder/Chip Samples

Instrument calibration/drift correction.

Press the Analyze button on the instrument screen. After a short delay, the loading head slide-block will open.

Place the Nickel Capsule containing the sample into the open port at the top of the loading head.

Press the Analyze button on the instrument screen again, the loading head slide-block will close and the lower electrode will open.

Clean the upper and lower electrode either manually or remove the crucible and press the analyze button to clean with an automatic cleaner if applicable.