JP4094558B2 - Thermal analyzer with automatic transfer mechanism - Google Patents
Thermal analyzer with automatic transfer mechanism Download PDFInfo
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- JP4094558B2 JP4094558B2 JP2004012347A JP2004012347A JP4094558B2 JP 4094558 B2 JP4094558 B2 JP 4094558B2 JP 2004012347 A JP2004012347 A JP 2004012347A JP 2004012347 A JP2004012347 A JP 2004012347A JP 4094558 B2 JP4094558 B2 JP 4094558B2
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- 230000007246 mechanism Effects 0.000 title claims description 7
- 239000000523 sample Substances 0.000 claims description 115
- 239000013558 reference substance Substances 0.000 claims description 68
- 238000005259 measurement Methods 0.000 claims description 62
- 239000012925 reference material Substances 0.000 claims description 49
- 238000001514 detection method Methods 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 4
- 230000007723 transport mechanism Effects 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 2
- 238000002076 thermal analysis method Methods 0.000 claims 1
- 230000032258 transport Effects 0.000 description 19
- 239000012611 container material Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 3
- 238000000113 differential scanning calorimetry Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 1
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Description
試料や参照物質の自動搬送機構を備えた、示差走査熱量測定（DSC測定）や、示差熱・熱重量同時測定（TG/DTA測定）等の熱分析装置に関する。 The present invention relates to a thermal analyzer such as differential scanning calorimetry (DSC measurement) and differential thermal / thermogravimetric measurement (TG / DTA measurement) equipped with an automatic transport mechanism for samples and reference materials.
従来のこの種の装置としては、特許3140099に見られるような、トレーに載置された試料を加熱炉内の試料ホルダーに自動搬送する機構を備え、多数の試料の測定を自動で行えるようにしたものがある。
示差走査熱量測定（DSC測定）や、示差熱・熱重量同時測定（TG/DTA測定）を行う場合、試料に加え参照物質が必要となる。従来のこの種の自動搬送機構を備えたDSC測定装置やTG/DTA測定装置においては、参照物質もトレー上に載置し試料と同様に自動搬送が可能であり、測定前の条件設定において各試料ごとにどの参照物質を使用するか指定するようになっていた。
When performing differential scanning calorimetry (DSC measurement) or differential thermal / thermogravimetric measurement (TG / DTA measurement), a reference substance is required in addition to the sample. In conventional DSC measurement devices and TG / DTA measurement devices equipped with this type of automatic transfer mechanism, the reference substance can be placed on the tray and automatically transferred in the same way as the sample. It was designed to specify which reference material to use for each sample.
DSC測定においては試料と参照物質間の示差熱量を測定し、TG/DTA測定においては試料と参照物質間の示差熱、示差重量を測定する。そのため、参照物質としては、DSCの場合には試料と同じ熱容量を持つもの、TG/DTAの場合には試料と同じ質量または同じ熱容量を持つものを使用したときに精度の高い測定データが得られる。もし試料と大きく異なる熱容量や質量を持つ参照物質を使用した場合には、測定データのベースラインのゆらぎやノイズの増加を生じさせ、測定データの精度を低下させてしてしまう。従って、熱容量や質量の異なる複数の試料の測定を行う場合には、各々の試料に合わせた熱容量や質量の複数の参照物質を用意し、各々の試料ごとに最適なものを使用することが理想である。試料ごとに異なる参照物質を使用して測定する場合、従来の自動搬送機構付きDSCまたはTG/DTA装置においては測定前の条件設定において各試料それぞれについてトレー上に載置された参照物質のうちどれを使用するかを入力するようになっていた。しかしながら、たくさんの試料それぞれについて参照物質を入力しなければならないのは手間が掛かり、各試料の試料情報の入力や温度プログラムの入力などただでさえ煩雑な測定前の条件設定がより煩雑になっていた。そのため、試料の数が多い場合でも参照物質はひとつしか用意せず、その参照物質をすべての試料の測定に使用するということがしばしば行われており、測定データの精度低下を生じさせていた。 In DSC measurement, the differential calorific value between the sample and reference material is measured, and in TG / DTA measurement, the differential heat and differential weight between the sample and reference material are measured. Therefore, as a reference material, high-accuracy measurement data can be obtained when using a reference material that has the same heat capacity as the sample in the case of DSC, or a material that has the same mass or the same heat capacity as the sample in the case of TG / DTA. . If a reference material having a heat capacity or mass that is significantly different from that of the sample is used, the baseline of the measurement data will fluctuate and noise will increase, reducing the accuracy of the measurement data. Therefore, when measuring multiple samples with different heat capacities and masses, it is ideal to prepare multiple reference materials with different heat capacities and masses for each sample and use the optimal one for each sample. It is. When measuring using different reference materials for each sample, in the conventional DSC or TG / DTA device with automatic transfer mechanism, which of the reference materials is placed on the tray for each sample in the condition setting before measurement. Was supposed to enter what to use. However, it is troublesome to input reference materials for each of many samples, and it is more complicated to set the conditions before measurement, such as inputting sample information for each sample and entering a temperature program. It was. For this reason, even when the number of samples is large, only one reference material is prepared, and the reference material is often used for measurement of all samples, resulting in a decrease in accuracy of measurement data.
本発明における自動搬送器講付き熱分析装置は、
トレー上に載置された試料の容器の材質や質量等の測定上の特性とトレー上の容器位置とを示す試料情報を保持する試料情報保持器と、
トレー上に載置された参照物質の容器の種類や質量等の測定上の特性とトレー上の容器位置とを示す参照物質情報を保持する参照物質情報保持器と、
参照物質情報保持器に接続され、試料情報が入力されると参照物質情報保持器が保持する参照物質情報の中からその試料情報に最も適した参照物質情報を検索する参照物質検索器と、
試料情報保持器と参照物質情報検索器に接続され、測定を行う試料の試料情報を試料情報保持器から取得し、その試料情報を参照物質情報検索器に出力してその試料に最も適した参照物質情報を取得し、取得した試料情報と参照物質情報に示される試料と参照物質の測定を行う測定制御器とを備え、
トレー上に載置されている参照物質の中から、次に測定が行われる試料に最も適した参照物質を自動で検索する機能を備える。
The thermal analyzer with an automatic carrier in the present invention is
A sample information holder for holding sample information indicating measurement characteristics such as material and mass of the container of the sample placed on the tray and the position of the container on the tray;
A reference substance information holder for holding reference substance information indicating the measurement characteristics such as the type and mass of the reference substance container placed on the tray and the container position on the tray;
A reference substance searcher that is connected to a reference substance information holder and searches for reference substance information most suitable for the sample information from the reference substance information held by the reference substance information holder when sample information is input;
Connected to the sample information holder and the reference substance information searcher, obtains sample information of the sample to be measured from the sample information holder, outputs the sample information to the reference substance information searcher, and references the most suitable for the sample A measurement controller for acquiring substance information, measuring the sample and reference substance indicated in the acquired sample information and reference substance information,
A function is provided for automatically searching for the reference material most suitable for the sample to be measured next from the reference materials placed on the tray.
以上のように、本発明によれば、多数の試料について個々に参照物質を指定する手間が無くなり、自動で最適な参照物質を使用されるようになるため、測定前の条件設定の省力化が図れるとともに、設定の手間を嫌ってひとつの参照物質を使い回すようなことがなくなり、測定精度の向上を図ることができた。 As described above, according to the present invention, it is not necessary to individually specify the reference material for a large number of samples, and the optimum reference material is automatically used. As a result, it was possible to improve the measurement accuracy by avoiding the use of a single reference substance because the setting work was disliked.
本発明の実施の形態を図面に基づいて説明する。 Embodiments of the present invention will be described with reference to the drawings.
図1は自動搬送機構を備えたDSCまたはTG/DTA測定装置の構成を示す。 FIG. 1 shows the configuration of a DSC or TG / DTA measuring device equipped with an automatic transport mechanism.
図1中１は試料容器2および参照物質容器３を載置するトレーである。トレー1上には試料容器および参照物質容器を載置する場所にくぼみが設けられており、それぞれの載置場所を識別するための位置番号が割り当てられ、表示されている。 In FIG. 1, reference numeral 1 denotes a tray on which the sample container 2 and the reference substance container 3 are placed. On the tray 1, a recess is provided at a place where the sample container and the reference substance container are placed, and a position number for identifying each placement place is assigned and displayed.
４はDSCまたはTG/DTA測定装置の検出部である。 Reference numeral 4 denotes a detection unit of the DSC or TG / DTA measuring device.
５は搬送器であり、トレー１から検出部４への試料容器および参照物質容器の搬送と、検出部４からトレー１への試料および参照物質の搬送を行う。 Reference numeral 5 denotes a transporter that transports the sample container and the reference material container from the tray 1 to the detection unit 4 and transports the sample and the reference material from the detection unit 4 to the tray 1.
搬送制御器6は、測定制御器7から搬送の指示を受け取り、搬送器5を制御して試料容器および参照物質容器の搬送を制御する。 The transport controller 6 receives a transport instruction from the measurement controller 7 and controls the transporter 5 to control transport of the sample container and the reference substance container.
測定制御器7は搬送制御器に対し、搬送する試料容器および参照物質容器のトレー1上の位置番号と、搬送を行う方向（トレー1から検出部4への搬送か、検出部4からトレー1への搬送か）を出力する。 The measurement controller 7 sends to the transport controller the position number of the sample container and reference material container to be transported on the tray 1 and the direction of transport (from the tray 1 to the detection unit 4 or from the detection unit 4 to the tray 1). Is transported).
試料情報8および参照物質情報10は、トレー上に載置されている試料および参照物質の情報であり、参照物質検索器12が参照物質の検索を行うときに使用される。その内容を図2に示す。 The sample information 8 and the reference material information 10 are information on the sample and the reference material placed on the tray, and are used when the reference material searcher 12 searches for the reference material. The contents are shown in FIG.
位置番号は、当該試料または参照物質のトレー1上の位置番号である。容器は、当該試料または参照物質が封入されている容器の材質を表す。質量は、当該試料または参照物質の質量を表す。比熱は、当該試料または参照物質の比熱を表し、DSC測定装置の場合のみに使用される項目である。当該試料または参照物質の熱容量を次式により算出するために使用される。 The position number is a position number on the tray 1 of the sample or reference substance. The container represents the material of the container in which the sample or reference substance is enclosed. The mass represents the mass of the sample or reference substance. Specific heat represents the specific heat of the sample or reference substance, and is an item used only in the case of a DSC measurement device. It is used to calculate the heat capacity of the sample or reference material according to the following equation.
熱容量 ＝ 比熱容量×質量 （１）
試料情報8および参照物質情報10は入力装置12を介してオペレータにより入力され、試料情報保持器9および参照物質情報保持器11に保持されている。
Heat capacity = specific heat capacity x mass (1)
The sample information 8 and the reference substance information 10 are input by the operator via the input device 12, and are held in the sample information holder 9 and the reference substance information holder 11.
なお、試料の自動秤量機能を備える熱分析装置の場合、試料および参照物質の自動秤量を行った結果が試料情報および参照物質情報の質量として自動的に入力されるように構成することも可能である。 In the case of a thermal analyzer equipped with an automatic sample weighing function, the result of automatic weighing of the sample and reference substance can be automatically input as the mass of the sample information and reference substance information. is there.
参照物質検索器12は、測定制御器7と参照物質情報保持器11に接続され、測定制御器7から測定しようとするひとつの試料情報を受け取り、その試料の参照物質として最も適するものを参照物質情報保持器11の参照物質情報10の中から検索し、見つかった参照物質情報を測定制御器7に出力する。 The reference substance search unit 12 is connected to the measurement controller 7 and the reference substance information holding unit 11, receives one piece of sample information to be measured from the measurement controller 7, and selects the most suitable reference substance for the sample as the reference substance. The reference material information 10 in the information holder 11 is searched and the found reference material information is output to the measurement controller 7.
参照物質検索器12による参照物質情報10の検索は、図３に示したフローチャートのように行われる。すなわち、
（ステップ3-1）測定制御器7から参照物質検索器12に試料情報を入力する。
（ステップ3-2）入力した試料情報の容器材質と同じ容器材質を持つ参照物質情報を参照物質情報保持器11の中から抽出し、抽出した参照物質情報のリストを作成する。
（ステップ3-3）入力した試料情報と同じ容器材質を持つ参照物質情報が参照物質情報保持器11中にひとつも無かった場合は、試料情報と同じ容器材質の参照物質情報が無かったことを示すエラーステータスを測定制御器に出力し検索を終了する。
（ステップ3-4）作成した参照物質情報リストの中から、DSCの場合であれば入力した試料情報と最も近い熱容量を持つもの、TG/DTAの場合であれば入力した試料情報と最も近い質量を持つものを検索する。
（ステップ3-5）見つかった参照物質情報を測定制御器7に出力する。
測定制御器7は、以下の手順を踏んで、搬送制御器6と検出部4を制御して測定を実行する。
The search of the reference substance information 10 by the reference substance searcher 12 is performed as in the flowchart shown in FIG. That is,
(Step 3-1) The sample information is input from the measurement controller 7 to the reference substance searcher 12.
(Step 3-2) The reference material information having the same container material as the container material of the input sample information is extracted from the reference material information holder 11, and a list of the extracted reference material information is created.
(Step 3-3) If there is no reference substance information in the reference substance information holder 11 having the same container material as the input sample information, it means that there is no reference substance information of the same container material as the sample information. The error status shown is output to the measurement controller and the search is terminated.
(Step 3-4) From the created reference substance information list, the DSC has the closest heat capacity to the entered sample information, and the TG / DTA has the closest mass to the entered sample information. Search for things with.
(Step 3-5) The found reference substance information is output to the measurement controller 7.
The measurement controller 7 performs the measurement by controlling the transport controller 6 and the detection unit 4 according to the following procedure.
測定制御器７は、入力装置13を介してオペレータから測定開始の指示を受けとると、まず試料情報保持器9から次の測定対象となる試料情報をひとつ取得する。取得した試料情報を参照物質検索器に出力し、その試料に最も適した参照物質情報を取得する。 When receiving a measurement start instruction from the operator via the input device 13, the measurement controller 7 first acquires one piece of sample information to be measured next from the sample information holder 9. The acquired sample information is output to the reference substance searcher, and the reference substance information most suitable for the sample is acquired.
次に測定制御器7は、搬送制御器6へ、取得した試料情報の位置番号と、参照物質情報の位置番号と、それらをトレーから検出部へ搬送する指示を出力する。もし参照物質検索器が試料情報と同じ容器材質の参照物質情報が無かったことを示すエラーステータスを返してきた場合、測定制御器7は取得した試料情報を破棄してその試料の測定をスキップし、次の測定対象の試料情報の取得へ進む。 Next, the measurement controller 7 outputs to the transport controller 6 the position number of the acquired sample information, the position number of the reference substance information, and an instruction to transport them from the tray to the detection unit. If the reference substance searcher returns an error status indicating that there is no reference substance information for the same container material as the sample information, the measurement controller 7 discards the acquired sample information and skips the measurement of that sample. Then, the process proceeds to acquisition of sample information of the next measurement target.
試料と参照物質の検出部への搬送が終了すると、測定制御器は検出部4に測定開始指示を出力し、測定を開始する。 When the transport of the sample and the reference substance to the detection unit is completed, the measurement controller outputs a measurement start instruction to the detection unit 4 and starts measurement.
測定が終了すると、測定制御器7は搬送制御器6に検出部4の試料と参照物質をトレー1上の元の位置に搬送する指示を出力する。 When the measurement is completed, the measurement controller 7 outputs an instruction to the transport controller 6 to transport the sample of the detection unit 4 and the reference material to the original positions on the tray 1.
測定制御器７は上記の動作を試料情報保持器9の試料情報8すべてについて繰り返し行う。
次に、本発明の熱分析装置の全動作を図４に示すフローチャートに沿って説明する。
（ステップ4-1）測定する試料を容器に封入し、該封入した容器を少なくともひとつトレー１上に載置する。
（ステップ4-2）載置した試料の試料情報を入力装置13を介して入力する。
（ステップ4-3）特性の異なる参照物質をそれぞれ別の容器に封入し、該封入した複数の容器をトレー1上に設けられた各くぼみにそれぞれ載置する。
（ステップ4-4）載置した参照物質容器あるいは参照物質容器内の参照物質情報を入力装置13を介して入力する。
（ステップ4-5）オペレータは入力装置13を介して測定制御器に測定開始指示を与える。
（ステップ4-6）測定制御器7は試料情報保持器9が保持している試料情報をひとつ入力し、入力した試料情報を参照物質検索器8に出力する。
（ステップ4-7）参照物質検索器8は、入力した試料情報に最も適する参照物質情報を検索し、見つかった参照物質情報を測定制御器7に出力する。
（ステップ4-8）測定制御器7は、入力した試料情報と参照物質情報の位置番号を搬送制御器6に出力し、搬送制御器6は、試料搬送器を制御して入力した位置番号の試料と参照物質を検出部4に搬送する。
（ステップ4-9）測定制御器7は検出部4に動作開始指示を与え、試料の測定を行う。
（ステップ4-10）試料の測定が終了すると、測定制御器7は搬送制御器6に試料と参照物質をトレーに搬送する指示を与え、測定が終わった試料と参照物質がトレーに戻される。
（ステップ4-11）試料情報保持器に保持されている試料情報すべてについて、ステップ6から11のループを繰り返し行う。
The measurement controller 7 repeats the above operation for all the sample information 8 of the sample information holder 9.
Next, the entire operation of the thermal analyzer of the present invention will be described with reference to the flowchart shown in FIG.
(Step 4-1) A sample to be measured is sealed in a container, and at least one sealed container is placed on the tray 1.
(Step 4-2) The sample information of the placed sample is input via the input device 13.
(Step 4-3) Reference materials having different characteristics are sealed in separate containers, and the plurality of sealed containers are placed in the respective recesses provided on the tray 1.
(Step 4-4) The reference substance container placed or the reference substance information in the reference substance container is input via the input device 13.
(Step 4-5) The operator gives a measurement start instruction to the measurement controller via the input device 13.
(Step 4-6) The measurement controller 7 inputs one piece of sample information held by the sample information holder 9, and outputs the inputted sample information to the reference substance searcher 8.
(Step 4-7) The reference substance search unit 8 searches for reference substance information most suitable for the input sample information, and outputs the found reference substance information to the measurement controller 7.
(Step 4-8) The measurement controller 7 outputs the input sample information and the position number of the reference material information to the transport controller 6, and the transport controller 6 controls the sample transporter to The sample and reference material are transported to the detection unit 4.
(Step 4-9) The measurement controller 7 gives an operation start instruction to the detector 4 and measures the sample.
(Step 4-10) When the measurement of the sample is completed, the measurement controller 7 instructs the transport controller 6 to transport the sample and the reference material to the tray, and the sample and the reference material that have been measured are returned to the tray.
(Step 4-11) The loop from Step 6 to 11 is repeated for all the sample information held in the sample information holder.
１ トレー
２ 試料
３ 参照物質
４ 検出部
５ 搬送器
６ 搬送制御器
７ 測定制御器
８ 試料情報
９ 試料情報保持器
10 参照物質情報
11 参照物質情報保持器
12 参照物質検索器
13 入力装置
DESCRIPTION OF SYMBOLS 1 Tray 2 Sample 3 Reference material 4 Detection part 5 Transporter 6 Transport controller 7 Measurement controller 8 Sample information 9 Sample information holder
10 Reference material information
11 Reference substance information holder
12 Reference substance searcher
13 Input device
Claims (3)
試料を収納した複数の試料容器と、参照物質を収納した複数の参照物質容器を載置するためのトレーと、
前記トレーと前記検出部間で前記試料容器および前記参照物質容器の搬送を行う搬送器と、
前記搬送器に接続され、トレー上の指定された位置の試料容器および参照物質容器の搬送が行われるように搬送器を制御する搬送制御器と、
前記トレー上に載置された試料および試料容器の測定上の特性と該試料容器の前記トレー上の位置とを示す試料情報を保持する試料情報保持器と、
前記トレー上に載置された参照物質および参照物質容器の測定上の特性と該参照物質容器のトレー上の位置とを示す参照物質情報を保持する参照物質情報保持器と、
前記参照物質情報保持器に接続され、測定を行う試料の試料情報が入力されると前記参照物質情報保持器が保持する参照物質情報の中から前記測定を行う試料の試料情報に最も適した参照物質情報を検索する参照物質検索器と、
前記検出部、前記搬送制御器、前記試料情報保持器及び前記参照物質情報検索器に接続され、前記測定を行う試料の試料情報を試料情報保持器から取得し、その試料情報を参照物質情報検索器に出力してその試料情報に最も適した参照物質情報を取得し、前記搬送制御器を制御して取得した試料情報と参照物質情報に示される試料と参照物質を前記検出部に配置し、測定を行う測定制御器とを備えることにより、
前記トレー上に載置されている参照物質の中から、前記測定を行う試料に最も適した参照物質を自動で搬送する機能を備えたことを特徴とする自動搬送機構付き熱分析装置。 A detector for performing thermal analysis measurement;
A plurality of sample containers containing a sample, a tray for placing a plurality of reference substance containers containing a reference substance, and
A transporter for transporting the sample container and the reference material container between the tray and the detection unit;
A transport controller connected to the transporter for controlling the transporter so that the sample container and the reference substance container at a specified position on the tray are transported;
A sample information holder for holding sample information indicating the measurement characteristics of the sample and sample container placed on the tray and the position of the sample container on the tray;
A reference substance information holder for holding reference substance information indicating the measurement characteristics of the reference substance and the reference substance container placed on the tray and the position of the reference substance container on the tray;
The reference most suitable for the sample information of the sample to be measured among the reference substance information held by the reference material information holder when the sample information of the sample to be measured is input and connected to the reference substance information holder A reference substance searcher for searching for substance information;
Connected to the detection unit, the transport controller, the sample information holder, and the reference substance information searcher, acquires sample information of the sample to be measured from the sample information holder, and retrieves the sample information from the reference substance information search The reference material information most suitable for the sample information is output to the container, and the sample and reference material indicated by the sample information and the reference material information acquired by controlling the transport controller are arranged in the detection unit, By providing a measurement controller that performs measurement,
A thermal analyzer with an automatic transport mechanism, comprising a function of automatically transporting a reference material most suitable for the sample to be measured from the reference materials placed on the tray.
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