Method of treating metal analysis sample and device thereof

• US 20030010633A1
• Filed: 07/24/2002
• Published: 01/16/2003
• Est. Priority Date: 10/12/2000
• Status: Active Grant

• Current Assignee: JFE Steel Corporation (JFE Holdings Incorporated), Kenji Abiko, Japan Analyst Corp. (LECO Corporation), Ulvac-PHI, Inc. (Ulvac Incorporated)
• Original Assignee: JFE Steel Corporation (JFE Holdings Incorporated)
• Inventors: Abiko, Kenji, Shimura, Makoto, Iwai, Hideo, Yasuhara, Hisao, Niida, Takashi
• Granted Patent: US 6,726,739 B2
• Time in Patent Office: Days
• US Class Current: 204/400
• CPC Class Codes: G01N 1/32 Polishing; Etching
• CPC Class Codes: G01N 33/2022 Non-metallic constituents

Abstract

The present invention provides a pre-treatment apparatus for an analytical metal sample, the apparatus including (1) a treatment chamber having a sample charging port which can be opened and closed and provided at the top of the chamber, a sample discharging port which can be opened and closed and provided at the bottom of the chamber, and a gas inlet and gas outlet, (2) a sample carrying bar joined to a sample holder also used as a sputtering electrode, and provided to pass through at least one side wall of the treatment chamber so as to be substantially horizontally movable and axially rotatable, and (3) a sputtering counter electrode at least having portions arranged opposite to each other in a region not inhibiting the charge and discharge of an analytical metal sample so that the sample holder can be arranged in the counter electrode. The present invention also provides a pre-treatment method capable of simply cleaning the surface of the analytical metal sample by using the pre-treatment apparatus and preventing re-contamination of the cleaned sample by exposure to the air or the like. Furthermore, the present invention provides an analysis apparatus provided with the pre-treatment apparatus to permit high-accuracy quantitative determination of trace elements of metals.

Claims

1. A pre-treatment apparatus for an analytical metal sample, the apparatus comprising:

(1) a treatment chamber having a sample charging port which can be opened and closed and provided at the top of the chamber, a sample discharging port which can be opened and closed and provided at the bottom of the chamber, and a gas inlet and gas outlet;

(2) a sample carrying bar joined to a sample holder also used as a sputtering electrode, and provided to pass through at least one side wall of the treatment chamber so as to be substantially horizontally movable and axially rotatable; and

(3) a sputtering counter electrode at least having portions arranged opposite to each other in a region not inhibiting the charge and discharge of an analytical metal sample so that the sample holder can be arranged in the counter electrode.

2. A pre-treatment apparatus according to claim 1, wherein the sample contact area of the sample holder is 10% or less of the surface area of the analytical metal sample.

3. A pre-treatment apparatus according to claim 1, wherein the counter electrode at least having portions arranged opposite to each other has a cylindrical shape.

4. An elementary analysis apparatus for a metal, comprising a sample inlet port connected to a portion below the sample discharging port of the pre-treatment apparatus according to any one of claims 1 to 3.

5. A pre-treatment method for elementary analysis of a metal using the pre-treatment apparatus according to any one of claim 1 to 3, the method comprising the steps of:

(1) charging an analytical metal sample in the sample holder through the sample charging port;

(2) evacuating the treatment chamber to form a reduced pressure atmosphere, and then controlling the inside of the treatment chamber to a predetermined pressure of 100 Pa to 1000 Pa by using an inert gas;

(3) moving the analytical metal sample on the sample holder by the sample carrying bar to a position in the sputtering counter electrode at least having portions opposite to each other;

(4) applying a voltage between the sample-side electrode and the sputtering counter electrode to clean the surface of the analytical metal sample by sputtering;

(5) moving the sample holder to a position above the sample discharging port by the sample carrying bar;

(6) rotating the sample carrying bar to move the analytical metal sample to an elementary analysis apparatus through the open sample discharging port.