JP2014070922A - Method for analysing sample using laser ablation icp analysis method - Google Patents

Method for analysing sample using laser ablation icp analysis method Download PDF

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JP2014070922A
JP2014070922A JP2012215131A JP2012215131A JP2014070922A JP 2014070922 A JP2014070922 A JP 2014070922A JP 2012215131 A JP2012215131 A JP 2012215131A JP 2012215131 A JP2012215131 A JP 2012215131A JP 2014070922 A JP2014070922 A JP 2014070922A
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JP6009303B2 (en
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Kenichi Kamimura
憲一 上村
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JX Nippon Mining and Metals Corp
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Abstract

PROBLEM TO BE SOLVED: To provide a method for analysing a sample, which can perform continuous analysis of the sample efficiently.SOLUTION: The method for analysing a sample uses a laser ablation ICP analysis method, and includes: a step 1 of taking out a holder sequentially from a sample arrangement part in which a plurality of holders each provided with a sample are arranged, and placing the holder at a predetermined position of a holder transfer part; a step 2 of measuring a position of the sample by irradiating with a laser beam the sample provided in the holder on the holder transfer part; a step 3 of transferring the holder after the position measurement to a laser ablation part; a step 4 of irradiating the sample provided in the holder with a laser beam by the laser ablation part to analyse the sample; a step 5 of transferring the holder provided with the analysed sample to a predetermined position for taking out the holder; and a step 6 of returning the holder, transferred to the predetermined position for taking out the holder, to the sample arrangement part.

Description

本発明は試料の元素分析等に用いられるレーザーアブレーションICP分析法を用いた試料の分析方法に関する。   The present invention relates to a sample analysis method using a laser ablation ICP analysis method used for elemental analysis of a sample.

一般に、試料の元素分析等に用いられる試料分析方法は、例えば、非特許文献1に開示されているような、レーザー光の照射により試料を気化又は霧化させるレーザーアブレーション部と、レーザーアブレーション部で気化又は霧化させた試料に含まれる構成元素を検出する元素検出部とを備えた試料分析装置にて行われている。   In general, a sample analysis method used for elemental analysis or the like of a sample includes, for example, a laser ablation unit that vaporizes or atomizes a sample by laser irradiation, and a laser ablation unit as disclosed in Non-Patent Document 1. This is performed by a sample analyzer including an element detection unit that detects a constituent element contained in a vaporized or atomized sample.

「レーザーアブレーション誘導結合プラズマ質量分析法」,JFE技報,No.13,2006年8月,p.106−108“Laser Ablation Inductively Coupled Plasma Mass Spectrometry”, JFE Technical Report, No. 13, August 2006, p. 106-108

しかしながら、従来のような試料分析装置を用いた分析方法で複数の試料を連続的に分析しようとすると、まず、試料を一つずつ装置の分析部に配置し、分析が終了すると試料を戻し、その後、新しく試料を分析部へ配置してから分析するという作業を繰り返している。このように、従来技術では、効率的に試料を連続分析することが困難である。そこで、本発明は試料の連続分析を効率良く行うことが可能な試料の分析方法を提供することを課題とする。   However, when trying to analyze a plurality of samples continuously by an analysis method using a conventional sample analyzer, first, the samples are placed one by one in the analysis section of the device, and when the analysis is completed, the samples are returned, Thereafter, a new sample is placed in the analysis unit and then analyzed. As described above, in the conventional technique, it is difficult to efficiently analyze the sample continuously. Therefore, an object of the present invention is to provide a sample analysis method capable of efficiently performing continuous analysis of a sample.

本発明者は上記課題を解決するために研究を重ねたところ、複数の試料をそれぞれ個別のホルダーに設けた状態で配置しておき、配置部からの取り出し、試料の位置測定、レーザー分析、配置部への取り出し、それらの間の搬送を、それぞれ独立した工程として制御することで、試料の連続分析を効率良く行うことが可能となることを見出した。   The present inventor has conducted research to solve the above-mentioned problems, and arranged a plurality of samples in a state where they are provided in individual holders, taken out from the arrangement part, sample position measurement, laser analysis, arrangement It has been found that the continuous analysis of the sample can be efficiently performed by controlling the extraction to the part and the conveyance between them as independent processes.

以上の知見を基礎として完成した本発明は一側面において、レーザーアブレーションICP分析法を用いた試料の分析方法において、試料を設けたホルダーを複数個配置する試料配置部から前記ホルダーを順に取り出し、ホルダー搬送部の所定の位置に前記ホルダーを載せる工程1と、前記ホルダー搬送部上のホルダーに設けられた試料にレーザー光を照射することで試料の位置測定を行う工程2と、前記位置測定を終えたホルダーをレーザーアブレーション部へ搬送する工程3と、前記レーザーアブレーション部で前記ホルダーに設けた試料にレーザー光を照射して分析する工程4と、分析後の試料が設けられた前記ホルダーを、取り出すための所定の位置へ搬送する工程5と、取り出すための所定の位置へ搬送された前記ホルダーを、前記試料配置部へ戻す工程6とを備えたレーザーアブレーションICP分析法を用いた試料の分析方法である。   In one aspect, the present invention completed on the basis of the above knowledge is a sample analysis method using laser ablation ICP analysis. In the sample analysis method, the holders are sequentially taken out from a sample placement portion where a plurality of holders provided with samples are placed. Step 1 of placing the holder at a predetermined position of the transport unit, Step 2 of measuring the position of the sample by irradiating the sample provided on the holder on the holder transport unit with laser light, and finishing the position measurement Step 3 for transporting the prepared holder to the laser ablation unit, Step 4 for irradiating the sample provided on the holder with the laser ablation unit for analysis, and taking out the holder provided with the sample after analysis The step 5 for transporting to a predetermined position for the removal, and the holder transported to the predetermined position for removal The laser ablation ICP analysis method and a step 6 to return to the sample placement part is a sample analysis method used.

本発明に係る試料の分析方法は一実施形態において、前記工程3と前記工程5とを同時に実施する。   In one embodiment of the sample analysis method according to the present invention, the step 3 and the step 5 are performed simultaneously.

本発明に係る試料の分析方法は別の一実施形態において、前記工程4の間に、前記工程1及び前記工程6を順に実施する。   In another embodiment of the sample analysis method according to the present invention, the step 1 and the step 6 are sequentially performed during the step 4.

本発明に係る試料の分析方法は更に別の一実施形態において、前記工程1と前記工程6とを同じ位置で実施する。   In still another embodiment of the sample analysis method according to the present invention, the step 1 and the step 6 are performed at the same position.

本発明に係る試料の分析方法は更に別の一実施形態において、前記工程1から前記工程6を、試料配置部から取り出されたホルダーを載せ、且つ、取り出すための所定の位置1、前記位置測定を行う位置2、前記レーザーアブレーション部で分析する位置3、及び、
前記分析後のホルダーを待機させる位置4の4つの位置を持ったターンテーブルによって実施する。
In still another embodiment of the sample analysis method according to the present invention, the steps 1 to 6 are carried out by placing the holder taken out from the sample placement unit and taking the predetermined position 1 for taking out, and the position measurement. Position 2 to perform, position 3 to analyze in the laser ablation section, and
This is carried out by a turntable having four positions 4 for waiting the holder after the analysis.

本発明に係る試料の分析方法は更に別の一実施形態において、前記工程4における試料の分析を2〜5分/回で実施する。   In still another embodiment of the sample analysis method according to the present invention, the sample analysis in the step 4 is performed at 2 to 5 minutes / time.

本発明に係る試料の分析方法は更に別の一実施形態において、前記試料配置部が前記試料の分析前に所定の位置に設置される。   In still another embodiment of the sample analysis method according to the present invention, the sample placement unit is installed at a predetermined position before analysis of the sample.

本発明に係る試料の分析方法は更に別の一実施形態において、前記工程1の間に、試料の識別表示のためのバーコードの、前記ホルダーへの貼り付けを行う。   In still another embodiment of the sample analysis method according to the present invention, a bar code for sample identification display is attached to the holder during the step 1.

本発明に係るレーザーアブレーションICP分析法を用いた試料の分析方法によれば、試料の連続分析を効率良く行うことができる。   According to the sample analysis method using the laser ablation ICP analysis method according to the present invention, the continuous analysis of the sample can be performed efficiently.

本発明の実施形態に係るレーザーアブレーションICP分析法を用いた試料の分析装置の模式図を示す。The schematic diagram of the analyzer of the sample using the laser ablation ICP analysis method which concerns on embodiment of this invention is shown. 本発明の実施形態に係る搬送部及び試料配置部の模式図を示す。The schematic diagram of the conveyance part which concerns on embodiment of this invention, and a sample arrangement | positioning part is shown. 本発明の実施形態に係る試料を設けたチャンバー(チャンバー上部及びチャンバー下部)の模式図を示す。The schematic diagram of the chamber (chamber upper part and chamber lower part) which provided the sample which concerns on embodiment of this invention is shown.

(分析装置の構成)
図1に、本発明の実施形態に係るレーザーアブレーションICP分析法を用いた試料の分析装置の模式図を示す。分析装置は、試料配置部、ホルダー搬送部、位置測定部、レーザーアブレーション部、元素検出部及びホルダー移動部を備えている。
(Configuration of analyzer)
FIG. 1 shows a schematic diagram of a sample analyzer using a laser ablation ICP analysis method according to an embodiment of the present invention. The analyzer includes a sample placement unit, a holder transport unit, a position measurement unit, a laser ablation unit, an element detection unit, and a holder moving unit.

本実施形態において、試料の種類に限定されるものではないが、例えば、金属中に微量に含まれる貴金属の定量分析において、分析対象となるサンプル物質と酸化鉛をアルカリ系の融解剤と混合したものと共にルツボ等で融解させて生ずる鉛ボタンに成形された試料が用いる。また、分析装置内において、試料はアルミニウム製等のホルダー内に設けられており、当該ホルダー単位で装置内を搬送され、また、分析される。ホルダーの形状は特に限定されず、円形や矩形の平板状、皿状、椀状等に形成することができる。   In the present embodiment, the type of the sample is not limited. For example, in the quantitative analysis of the noble metal contained in a trace amount in the metal, the sample material to be analyzed and lead oxide are mixed with an alkaline melting agent. A sample molded into a lead button that is produced by melting with a crucible or the like is used. Further, in the analyzer, the sample is provided in a holder made of aluminum or the like, and is transported through the apparatus and analyzed in units of the holder. The shape of the holder is not particularly limited, and the holder can be formed in a circular or rectangular flat plate shape, a dish shape, a bowl shape, or the like.

図2に、本発明の実施形態に係る搬送部及び試料配置部の模式図を示す。試料配置部は、試料を設けたホルダーが複数個配置されるトレーを多段で備えている。本実施形態では、図2に示すように、1つのトレーに試料を設けたホルダーが縦4個×横5個で合計20個配置され、さらにこのトレーが5段構成となっているため、20個×5段で合計100個設けられている。このような構成により、多数の試料を設けたホルダーを小さなスペースで配置することができる。試料配置部は、取り出し用のアームが容易に届く位置等、ホルダーの取り出しが容易な位置や、ホルダー搬送部へ搬送しやすい位置に設置することができる。   In FIG. 2, the schematic diagram of the conveyance part which concerns on embodiment of this invention, and a sample arrangement | positioning part is shown. The sample placement unit includes a plurality of trays on which a plurality of holders provided with samples are placed. In this embodiment, as shown in FIG. 2, a total of 20 holders each provided with a sample on one tray are arranged in 4 × 5 in total, and this tray has a 5-stage configuration. A total of 100 pieces are provided in 5 pieces per piece. With such a configuration, a holder provided with a large number of samples can be arranged in a small space. The sample placement section can be installed at a position where the holder can be easily taken out, such as a position where the take-out arm can easily reach, or a position where the sample placement section can be easily transported to the holder transport section.

ホルダー搬送部には、ホルダー取り出し部(本実施形態では後述のようにホルダー移動部が兼ねている)によって試料配置部から順に取り出されたホルダーが載せられる。本実施形態では、ホルダー搬送部は回転テーブルを構成しており、回転することによって順に載せられた分析前の試料が設けられたホルダーを後述の位置測定部、レーザーアブレーション部へと搬送し、さらに分析後の試料が設けられたホルダーを元の位置(ホルダー取り出し部によって取り出されたホルダーを初めに載せる位置)へ戻すことができる。このような構成により、搬送経路を短くすることができ、スペースを効率的に使用することができる。ホルダー搬送部の構成は特に限定されず、ホルダーの搬送経路が直線上に伸びるようにライン状に形成されていてもよい。   A holder taken out in order from the sample placement portion by a holder take-out portion (also serving as a holder moving portion as will be described later in this embodiment) is placed on the holder transport portion. In this embodiment, the holder transport unit constitutes a rotary table, and transports a holder provided with a sample before analysis placed in order by rotating to a position measurement unit and a laser ablation unit described below, and The holder provided with the sample after the analysis can be returned to the original position (position where the holder taken out by the holder taking-out portion is first placed). With such a configuration, the conveyance path can be shortened and the space can be used efficiently. The configuration of the holder transport unit is not particularly limited, and the holder transport unit may be formed in a line shape so that the transport path of the holder extends linearly.

ホルダー搬送部は、ホルダー取り出し部によって試料配置部から順に取り出されたホルダーが直接載せられてもよいが、本実施形態では、チャンバー下部を複数設けて、チャンバー下部に各ホルダーを載せており、ホルダー搬送部が回転することで、チャンバー下部ごとホルダーが搬送される構成となっている。   The holder transport unit may be directly placed with the holders taken out from the sample placement unit in order by the holder take-out unit. However, in this embodiment, a plurality of lower chambers are provided, and each holder is placed under the chamber. The holder is transported together with the lower part of the chamber by rotating the transport unit.

位置測定部は、ホルダー搬送部で搬送されたホルダーに設けられた試料にレーザー光を照射して、試料の高さを測定する。このように、位置測定部であらかじめ試料の高さを測定して当該測定結果を利用することで、後段のレーザーアブレーション部によるレーザー光の照射の精度が良好となる。   The position measurement unit irradiates the sample provided on the holder conveyed by the holder conveyance unit with laser light to measure the height of the sample. In this way, by measuring the height of the sample in advance using the position measurement unit and using the measurement result, the accuracy of laser light irradiation by the laser ablation unit at the subsequent stage becomes good.

レーザーアブレーション部は、レーザー光を照射する発振出力5W以上のレーザー発振源を有する。レーザーアブレーション部は、位置測定部で高さが測定された試料の表面に、当該測定結果を利用してレーザー発振源から精度良くレーザー光照射を行い、試料の一部を微粒子化させる。レーザーアブレーション部は、このように発振出力5W以上の高出力のレーザー発振源を用いるため、レーザー出力が安定となり、試料の連続分析を良好に行うことが可能となる。レーザー発振源としては、例えば、5〜13Wの出力で発振できるQスイッチ周波数1〜400kHzのNd:YVO4レーザー等のYVO4レーザーを用いることができる。 The laser ablation unit has a laser oscillation source that emits laser light and has an oscillation output of 5 W or more. The laser ablation unit irradiates the surface of the sample whose height has been measured by the position measurement unit with high accuracy from the laser oscillation source using the measurement result, and makes a part of the sample fine particles. Since the laser ablation unit uses a high-power laser oscillation source having an oscillation output of 5 W or more in this way, the laser output becomes stable and continuous analysis of the sample can be performed satisfactorily. As the laser oscillating source, for example, Nd Q-switch frequency 1~400kHz which can oscillate at the output of 5~13W: can be used YVO 4 YVO 4 laser such as a laser.

レーザーアブレーション部には、チャンバー上部が設けられている。チャンバー上部は、ホルダー搬送部で搬送されたホルダーを載せたチャンバー下部と組み合わせて試料を覆うチャンバーを構成する。図3に、試料を設けたチャンバー(チャンバー上部及びチャンバー下部)の模式図を示す。図3に示すように、チャンバー下部はホルダー搬送部にチャンバー下部固定具で固定されている。また、レーザーアブレーション部から下降するチャンバー上部と組み合わされて密閉空間を作り、これによって試料を設けたホルダーを覆うチャンバーを構成している。レーザーアブレーション部では、このようにチャンバーで試料を設けたホルダーを覆った状態でレーザー光の照射を行っている。   The upper part of the chamber is provided in the laser ablation part. The upper part of the chamber constitutes a chamber that covers the sample in combination with the lower part of the chamber on which the holder transported by the holder transport unit is placed. FIG. 3 shows a schematic diagram of a chamber (chamber upper portion and chamber lower portion) provided with a sample. As shown in FIG. 3, the lower part of the chamber is fixed to the holder transport unit with a lower chamber fixture. Moreover, it forms a sealed space in combination with the upper part of the chamber descending from the laser ablation part, thereby constituting a chamber covering the holder on which the sample is provided. In the laser ablation part, the laser beam is irradiated in such a state that the holder provided with the sample is covered in the chamber.

元素検出部は、レーザーアブレーション部のレーザー光照射によって微粒子化された試料を導入し、試料に含まれる構成元素を検出する。元素検出部における元素分析は、例えば、ICP質量分析又はICP発光分析とすることができる。   The element detection unit introduces a sample that has been microparticulated by laser light irradiation of the laser ablation unit, and detects constituent elements contained in the sample. Elemental analysis in the element detection unit can be, for example, ICP mass spectrometry or ICP emission analysis.

ホルダー移動部は、レーザーアブレーション部で試料にレーザー光を照射して分析を終えた後のホルダーをホルダー搬送部から試料配置部へ戻す。ホルダー移動部の形態は特に限定されず、例えばアーム状に形成されていてもよい。また、本実施形態では、ホルダー移動部は、試料配置部から順にホルダーを取り出してホルダー搬送部へ載せるホルダー取り出し部を兼ねている。このような構成により、搬送効率が良好となる。   The holder moving unit returns the holder after the analysis by irradiating the sample with the laser beam in the laser ablation unit from the holder transport unit to the sample placement unit. The form of the holder moving part is not particularly limited, and may be formed in an arm shape, for example. In the present embodiment, the holder moving unit also serves as a holder taking-out unit for taking out the holder in order from the sample placement unit and placing it on the holder transporting unit. With such a configuration, the conveyance efficiency is improved.

(試料分析方法)
次に、本発明に係る試料の分析方法の実施形態の例について説明する。
まず、分析対象となるサンプル物質と酸化鉛をアルカリ系の融解剤と混合したものと共にルツボ等で融解させて生ずる鉛ボタンを成形して試料を作製する。
次に、試料をホルダー内へ設け、このホルダーを試料配置部の多段に設けられたトレー上に配置する。
次に、ホルダー取り出し部(本実施形態ではホルダー移動部が兼ねている)によって1つずつ順に試料配置部のホルダーをホルダー搬送部上に取り出していく。取り出されたホルダーは、図1及び2に便宜的に記したポジション(pos.1〜4)におけるpos.1に設けられたチャンバー下部上に載置する。なお、このポジションの数は特に限定されない。
次に、ホルダー搬送部が回転することにより、pos.1のチャンバー下部上に載置されたホルダーがpos.2へ搬送される。pos.2では、位置測定部のレーザー照射による試料高さの測定が行われる。また、このとき、pos.1では、試料配置部から新たなホルダーが取り出されて載置される。
次に、ホルダー搬送部が回転することにより、pos.2のチャンバー下部上に載置されたホルダーがpos.3へ搬送される。pos.3では、レーザーアブレーション部のレーザー照射が行われる。このとき、まずpos.3のチャンバー下部が不図示の上昇手段によって上昇し、レーザーアブレーション部に設けられたチャンバー上部と組み合わせられてチャンバーとされ、ホルダーを覆う密閉空間を構成する。続いて、このチャンバー内を例えばヘリウムガス等でパージした後、発振出力5W以上のレーザー発振源によるレーザー光照射を行い、試料の一部を微粒子化させる。このとき、前段で位置測定部により測定されて得られた結果がレーザーアブレーション部の精度の良いレーザー光照射に利用される。
次に、レーザーアブレーション部のレーザー光照射によって微粒子化された試料が元素検出部へ導入され、試料に含まれる構成元素が検出される。
レーザー光照射が完了したら、ホルダーを載置したチャンバー下部を不図示の下降手段により下降させて、ホルダー搬送部のpos.3へ戻す。また、この間に、pos.1のチャンバー下部上に載置されたホルダーがpos.2へ搬送されて位置測定部のレーザー照射による試料高さの測定が行われ、さらにpos.1では、試料配置部から新たなホルダーが取り出されて載置される。
次に、ホルダー搬送部が回転することにより、pos.3のチャンバー下部上に載置されたホルダーがpos.4へ搬送される。pos.4では、特に操作は行わず、ただホルダーを待機させている。この間、pos.3ではホルダー上の試料がレーザーアブレーション部でレーザー光照射され、pos.2では位置測定部のレーザー照射による試料高さの測定が行われ、pos.1では新たなホルダーが試料配置部から取り出されている。
次に、ホルダー搬送部が回転することにより、pos.4のチャンバー下部上に載置されたホルダーがpos.1へ搬送される。pos.1へ搬送されたホルダーは、ホルダー移動部によって試料配置部へ戻され、続いて新たなホルダーが試料配置部からpos.1へ取り出される。この間、上記と同様に、pos.4ではホルダーが待機しており、pos.3ではホルダー上の試料がレーザーアブレーション部でレーザー光照射され、pos.2では位置測定部のレーザー照射による試料高さの測定が行われている。
このようにして、安定したレーザー出力による試料の分析を行うことができ、さらに試料を設けた多数のホルダーを自動で次々に効率良く分析することができる。このような構成により、本発明に係る試料の分析方法では、試料の測定を2〜5分/回という短時間で行うことができる。
また、ホルダー取り出し部によって1つずつ順に試料配置部のホルダーをホルダー搬送部上に取り出していく際に、試料の識別表示のためのバーコードのホルダーへの貼り付けを行ってもよい。
(Sample analysis method)
Next, an example of an embodiment of a sample analysis method according to the present invention will be described.
First, a lead button formed by melting a sample substance to be analyzed and lead oxide mixed with an alkaline melting agent together with a crucible or the like is formed to prepare a sample.
Next, a sample is provided in a holder, and this holder is placed on a tray provided in multiple stages of the sample placement portion.
Next, the holders of the sample placement unit are sequentially taken out onto the holder transport unit one by one by a holder taking-out unit (also serving as a holder moving unit in this embodiment). The removed holder is pos.1 at the positions (pos.1 to 4) indicated for convenience in FIGS. 1 is placed on the lower part of the chamber provided in 1. The number of positions is not particularly limited.
Next, when the holder transport section is rotated, pos. 1 is a pos. 1 holder mounted on the lower part of the chamber. 2 is conveyed. pos. In 2, the sample height is measured by laser irradiation of the position measurement unit. At this time, pos. In 1, a new holder is taken out from the sample placement section and placed.
Next, when the holder transport section is rotated, pos. 2 is a pos. 3 is conveyed. pos. In 3, the laser irradiation of the laser ablation part is performed. At this time, first, pos. The lower portion of the chamber 3 is raised by a raising means (not shown) and combined with the upper portion of the chamber provided in the laser ablation portion to form a chamber, which constitutes a sealed space that covers the holder. Subsequently, after purging the inside of the chamber with, for example, helium gas, laser light irradiation is performed by a laser oscillation source having an oscillation output of 5 W or more, and a part of the sample is atomized. At this time, the result obtained by the measurement by the position measurement unit in the previous stage is used for laser beam irradiation with high accuracy of the laser ablation unit.
Next, the sample that has been atomized by laser light irradiation in the laser ablation unit is introduced into the element detection unit, and constituent elements contained in the sample are detected.
When the laser beam irradiation is completed, the lower part of the chamber on which the holder is placed is lowered by a lowering means (not shown), and the pos. Return to 3. During this time, pos. 1 is a pos. 1 holder mounted on the lower part of the chamber. 2 and the sample height is measured by laser irradiation of the position measuring unit. In 1, a new holder is taken out from the sample placement section and placed.
Next, when the holder transport section is rotated, pos. 3 is a pos. 3 holder mounted on the lower part of the chamber. 4 is conveyed. pos. In No. 4, no particular operation is performed, and the holder is simply kept waiting. During this time, pos. 3, the sample on the holder was irradiated with laser light at the laser ablation part. 2, the sample height is measured by laser irradiation of the position measurement unit. In 1, a new holder is taken out from the sample placement section.
Next, when the holder transport section is rotated, pos. 4 is a pos. 1 is conveyed. pos. 1 is returned to the sample placement unit by the holder moving unit, and then a new holder is moved from the sample placement unit to pos. 1 is taken out. During this time, pos. 4, the holder is waiting, and pos. 3, the sample on the holder was irradiated with laser light at the laser ablation part. In 2, the sample height is measured by laser irradiation of the position measurement unit.
In this way, the sample can be analyzed with a stable laser output, and a number of holders provided with the sample can be automatically and efficiently analyzed one after another. With such a configuration, in the sample analysis method according to the present invention, the sample can be measured in a short time of 2 to 5 minutes / times.
Further, when the holders of the sample placement units are sequentially taken out onto the holder transport unit one by one by the holder take-out unit, a barcode for sample identification display may be attached to the holder.

以下に本発明を実施例でさらに詳細に説明するが、本発明はこれらに限定されるものではない。   The present invention will be described in more detail with reference to the following examples. However, the present invention is not limited to these examples.

(実施例)
上述の図1〜3に記載した本発明に試料の分析方法を用いて、合計100個の試料(鉛ボタン)を分析した。レーザーアブレーション部のレーザー発振源としては、5〜13Wの出力で発振できるQスイッチ周波数1〜400kHzのNd:YVO4レーザーを用いた。
実施例では、100個の試料を分析している間のレーザー出力は安定しており、安定した分析結果を得ることができた。また、試料の搬入、分析及び搬出までが自動化されているため、従来の装置及び方法では3〜4日程度要していた分析を1日で行うことができた。
(Example)
A total of 100 samples (lead buttons) were analyzed using the sample analysis method of the present invention described in FIGS. As a laser oscillation source of the laser ablation unit, an Nd: YVO 4 laser having a Q switch frequency of 1 to 400 kHz that can oscillate at an output of 5 to 13 W was used.
In the example, the laser output was stable while 100 samples were analyzed, and a stable analysis result could be obtained. In addition, since the sample loading, analysis, and unloading are automated, it was possible to perform the analysis in about one day, which required about 3 to 4 days with the conventional apparatus and method.

Claims (8)

レーザーアブレーションICP分析法を用いた試料の分析方法において、
試料を設けたホルダーを複数個配置する試料配置部から前記ホルダーを順に取り出し、ホルダー搬送部の所定の位置に前記ホルダーを載せる工程1と、
前記ホルダー搬送部上のホルダーに設けられた試料にレーザー光を照射することで試料の位置測定を行う工程2と、
前記位置測定を終えたホルダーをレーザーアブレーション部へ搬送する工程3と、
前記レーザーアブレーション部で前記ホルダーに設けた試料にレーザー光を照射して分析する工程4と、
分析後の試料が設けられた前記ホルダーを、取り出すための所定の位置へ搬送する工程5と、
取り出すための所定の位置へ搬送された前記ホルダーを、前記試料配置部へ戻す工程6と、
を備えたレーザーアブレーションICP分析法を用いた試料の分析方法。
In the sample analysis method using the laser ablation ICP analysis method,
Step 1 of sequentially removing the holders from a sample placement unit that places a plurality of holders provided with samples, and placing the holders at predetermined positions of a holder transport unit;
A step 2 of measuring the position of the sample by irradiating the sample provided in the holder on the holder conveying unit with a laser beam;
Step 3 for transporting the holder after the position measurement to the laser ablation unit;
A step 4 of irradiating the sample provided in the holder with the laser ablation unit for laser beam analysis;
A step 5 of transporting the holder provided with the sample after analysis to a predetermined position for taking out;
A step 6 of returning the holder transported to a predetermined position for removal to the sample placement unit;
Sample analysis method using laser ablation ICP analysis method comprising:
前記工程3と前記工程5とを同時に実施する請求項1に記載の分析方法。   The analysis method according to claim 1, wherein the step 3 and the step 5 are performed simultaneously. 前記工程4の間に、前記工程1及び前記工程6を順に実施する請求項1又は2に記載の分析方法。   The analysis method according to claim 1, wherein the step 1 and the step 6 are sequentially performed during the step 4. 前記工程1と前記工程6とを同じ位置で実施する請求項1〜3のいずれかに記載の分析方法。   The analysis method according to claim 1, wherein the step 1 and the step 6 are performed at the same position. 前記工程1から前記工程6を、
試料配置部から取り出されたホルダーを載せ、且つ、取り出すための所定の位置1、
前記位置測定を行う位置2、
前記レーザーアブレーション部で分析する位置3、及び、
前記分析後のホルダーを待機させる位置4
の4つの位置を持ったターンテーブルによって実施する請求項4に記載の分析方法。
From step 1 to step 6,
A predetermined position 1 for placing and taking out the holder taken out from the sample placement unit,
Position 2 for performing the position measurement;
Position 3 to be analyzed by the laser ablation section, and
Position 4 for waiting the holder after the analysis
The analysis method according to claim 4, wherein the analysis is performed by a turntable having the following four positions.
前記工程4における試料の分析を2〜5分/回で実施する請求項1〜5のいずれかに記載の分析方法。   The analysis method according to claim 1, wherein the analysis of the sample in the step 4 is performed at 2 to 5 minutes / time. 前記試料配置部が前記試料の分析前に所定の位置に設置される請求項1〜6のいずれかに記載の分析方法。   The analysis method according to claim 1, wherein the sample placement unit is installed at a predetermined position before analysis of the sample. 前記工程1の間に、試料の識別表示のためのバーコードの、前記ホルダーへの貼り付けを行う請求項1〜7のいずれかに記載の分析方法。   The analysis method according to claim 1, wherein a barcode for identifying and displaying a sample is attached to the holder during the step 1.
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