JPH06100557B2 - Boiling point - Google Patents
Boiling pointInfo
- Publication number
- JPH06100557B2 JPH06100557B2 JP1142587A JP14258789A JPH06100557B2 JP H06100557 B2 JPH06100557 B2 JP H06100557B2 JP 1142587 A JP1142587 A JP 1142587A JP 14258789 A JP14258789 A JP 14258789A JP H06100557 B2 JPH06100557 B2 JP H06100557B2
- Authority
- JP
- Japan
- Prior art keywords
- sample
- container
- liquid level
- fractionation
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は、石油製品等の蒸留点を測定するために用いる
沸点計に関する。The present invention relates to a boiling point meter used for measuring the distillation point of petroleum products and the like.
従来より、石油精製工業においては、ガソリン等の石油
製品の中間留出温度、終点などを沸点計により測定する
ことが行なわれている。この測定結果は、JISに規定さ
れた標準試験による測定結果に合わせて調整され、この
値に基づいて操業管理、製品管理等が行なわれるもので
ある。Conventionally, in the petroleum refining industry, the middle distillation temperature and end point of petroleum products such as gasoline have been measured with a boiling point meter. This measurement result is adjusted according to the measurement result by the standard test specified in JIS, and operation management, product management, etc. are performed based on this value.
このような沸点計として、従来第３図に示す構成のもの
が知られている。As such a boiling point meter, one having a structure shown in FIG. 3 is conventionally known.
即ち、第３図において１は試料液が導入される容器、２
は容器１内の試料を加熱するヒータ（加熱装置）、３は
容器１に連結された試料導入管、４は試料導入管３の上
端に連結された計量カップ（計量装置）、５は計量カッ
プ４に連結されたオーバーフロー管、６は試料導入管３
に介装された第１電磁バルブ、７は試料導入管３の計量
カップ４と第１電磁バルブ６との間に連結された試料流
通管、８は試料流通管７に介装された第２電磁バルブを
示す。また、９は容器１の上部に連結された試料冷却
管、10は試料冷却管９の周囲に配設された冷却水流通
管、11は試料冷却管９内に挿入され、その先端検知部が
容器１の上部に位置するように配設された温度検出器、
12は試料冷却管９の先端に連結された試料留出管、13は
試料留出管12の下端に連結された分留容器、14は分留容
器13とＵ字管14aを介して連結された液面検出管であ
る。この液面検出管14には、５％留出点、50％留出点等
の各留出点における液面を検出する検出端15aを具備す
るレベルセンサ15が配設され、試料の留出量に応じて上
昇する液面検出管14内の液面がこのレベルセンサ15によ
って検出されるようになっている。この場合、レベルセ
ンサ15の各検出端15aは検出すべき留出点に予め設定さ
れている。なお、16は分留容器13の下端に連結された試
料排出管、17は試料排出管16に介装された第３電磁バル
ブ、18はヒータ２、温度検出器11及びレベルセンサ15と
それぞれ連絡する制御部である。That is, in FIG. 3, 1 is a container into which the sample solution is introduced, 2
Is a heater (heating device) for heating the sample in the container 1, 3 is a sample introducing pipe connected to the container 1, 4 is a measuring cup (measuring device) connected to the upper end of the sample introducing pipe 3, 5 is a measuring cup An overflow pipe connected to 4, a sample introduction pipe 3
A first electromagnetic valve interposed between the measuring cup 4 of the sample introduction tube 3 and the first electromagnetic valve 6; and a second electromagnetic valve 8 interposed between the sample circulating tube 7 Indicates a solenoid valve. Further, 9 is a sample cooling pipe connected to the upper part of the container 1, 10 is a cooling water flow pipe arranged around the sample cooling pipe 9, 11 is inserted into the sample cooling pipe 9, and its tip detecting portion is A temperature detector arranged so as to be located above the container 1,
Reference numeral 12 is a sample distillation tube connected to the tip of the sample cooling tube 9, 13 is a fractionation container connected to the lower end of the sample distillation tube 12, and 14 is a fractionation container 13 and a U-shaped tube 14a. It is a liquid level detection tube. The liquid level detection tube 14 is provided with a level sensor 15 having a detection end 15a for detecting the liquid level at each distillation point such as 5% distillation point and 50% distillation point. The level sensor 15 detects the liquid level in the liquid level detection tube 14 that rises according to the amount. In this case, each detection end 15a of the level sensor 15 is preset to the distillation point to be detected. In addition, 16 is a sample discharge pipe connected to the lower end of the fractionation container 13, 17 is a third electromagnetic valve interposed in the sample discharge pipe 16, and 18 is a heater 2, a temperature detector 11, and a level sensor 15, which communicate with each other. It is a control unit that does.
上記沸点計を用いて試料の蒸留点を測定する場合、まず
第１電磁バルブ６を閉じ、第２電磁バルブ８を開けた状
態で試料導入管３に試料流通管７から試料を導入する。
これにより、一定量の試料が計量カップ４に貯えられる
と共に、余分の試料はオーバーフロー管５からオーバー
フローされる。次に、第１電磁バルブ６を開き、第２電
磁バルブ８を閉じることにより計量カップ４内の試料を
容器１内に入れた後、この試料を制御部18の制御によっ
てヒータ２により所定加熱速度で連続的に加熱し、蒸留
する。そして、試料蒸気が冷却管９に流入してこの中で
液化され、更に留出管12から分留容器13内に滴下して液
面検出管14内の液面が上昇すると、予め設定された各留
出点、例えば５％,10％,90％,95％等の中間留出点や終
点に対応する液面がレベルセンサ15で検出され、この信
号が制御部18に送られると共に、このとき温度検出器11
で検出した試料温度が制御部18に保持されることによ
り、試料の蒸留点が測定されるものである。なお、上記
動作が終了すると加熱が停止され、分留容器13及び液面
検出管14内の試料が排出された後、次の測定動作に移
る。When measuring the distillation point of a sample using the above-mentioned boiling point meter, first, the sample is introduced into the sample introduction pipe 3 from the sample flow pipe 7 with the first electromagnetic valve 6 closed and the second electromagnetic valve 8 opened.
As a result, a fixed amount of the sample is stored in the measuring cup 4, and the excess sample is overflowed from the overflow pipe 5. Next, after the first electromagnetic valve 6 is opened and the second electromagnetic valve 8 is closed to put the sample in the measuring cup 4 into the container 1, the control unit 18 controls the sample 2 to be heated at a predetermined heating rate by the heater 2. Continuously heat and distill. Then, when the sample vapor flows into the cooling pipe 9 and is liquefied therein, and further drops from the distilling pipe 12 into the fractionating container 13 and the liquid level in the liquid level detecting pipe 14 rises, it is set in advance. The liquid level corresponding to each distillation point, for example, 5%, 10%, 90%, 95%, etc. intermediate distillation points and end points is detected by the level sensor 15, and this signal is sent to the control unit 18 and When temperature detector 11
The distillation point of the sample is measured by holding the sample temperature detected in step 1 in the controller 18. When the above operation is completed, the heating is stopped, the sample in the fractionation container 13 and the liquid level detection tube 14 is discharged, and then the next measurement operation is performed.
近年、特定の留出温度における留出量を測定することが
要望されているが、従来の沸点計は特定の留出量におけ
る留出温度は測定できるが、特定の留出温度における留
出量を測定することはできず、従って測定装置として十
分満足すべき機能を有するものではなかった。In recent years, it has been desired to measure the amount of distillate at a specific distillate temperature. Conventional boiling point meters can measure the distillate temperature at a particular distillate temperature, but the amount of distillate at the particular distillate temperature can be measured. Was not able to be measured, and therefore, it did not have a sufficiently satisfactory function as a measuring device.
更に、第３図の装置による蒸留はJISに合わせて常圧蒸
留とするために蒸留経路を大気開放状態として行うもの
であり、このため試料の一部が大気開放経路を通って減
失するが、JISと対応する測定値を得るためには減失分
を測定し、実際の測定値に減失分に応じた補正を加えて
減失分加算留出点を求めなければならない。しかし、従
来の沸点計では、減失分加算留出点を求めるための減失
分の測定手段はなく、誤差を有するものであった。Further, the distillation by means of the apparatus shown in FIG. 3 is carried out with the distillation path open to the atmosphere in order to carry out atmospheric distillation in accordance with JIS. Therefore, a part of the sample is lost through the atmosphere open path. In order to obtain a measurement value corresponding to JIS, the loss amount must be measured and the actual loss value must be corrected according to the loss amount to obtain the loss-increasing distillation point. However, in the conventional boiling point meter, there is no means for measuring the loss component for obtaining the loss-addition distillation point, and there is an error.
したがって、本発明の第１の目的は、所望の留出温度に
おける留出量を測定できる沸点計を提供することにあ
る。Therefore, the first object of the present invention is to provide a boiling point meter capable of measuring the amount of distillate at a desired distilling temperature.
本発明の第２の目的は、減失分による補正を行わずに減
失分加算留出点に近似した留出点を求めることが可能な
沸点計を提供することにある。It is a second object of the present invention to provide a boiling point meter capable of obtaining a distillation point that is similar to the loss-increasing distillation point without performing correction by the loss component.
本発明の第３の目的は、ゼロ−スパンを精密に設定でき
ると共に、減失分を簡単に算出することができ、したが
って減失分加算留出点を容易に求めることが可能な沸点
計を提供することにある。A third object of the present invention is to provide a boiling point meter capable of precisely setting the zero-span and easily calculating the loss component, and thus easily obtaining the loss-increasing distillation point. To provide.
［課題を解決するための手段］ 本発明は、上記目的を達成するため、請求項１〜３の発
明を提供する。[Means for Solving the Problems] The present invention provides the inventions of claims 1 to 3 in order to achieve the above object.
（請求項１） 試料が導入される容器と、この容器内の試料を加熱する
加熱装置と、容器内に生じた試料の蒸気が導入されると
共に、この蒸気を冷却して液化する冷却管と、前記冷却
管で液化した試料が滴下される分留容器と、前記容器内
に生じた試料蒸気の温度を検出する温度検出器とを有
し、前記分留容器内に滴下された試料の液面を検出する
ことにより求めた試料の留出量と温度検出器で検出した
容器内の試料温度とから試料の蒸留点を測定する沸点計
において、分留容器内の試料の液面変動を検出する液面
検出機構を具備してなり、温度検出器で検出した容器内
の試料温度が所定の値になったときに前記液面検出機構
で分留容器内の試料液面を検出するようにしたことを特
徴とする沸点計。(Claim 1) A container into which a sample is introduced, a heating device for heating the sample in the container, and a cooling pipe for introducing the sample vapor generated in the container and cooling the vapor to liquefy it. , A fractionation container in which the sample liquefied in the cooling pipe is dropped, and a temperature detector for detecting the temperature of the sample vapor generated in the container, and the liquid of the sample dropped in the fractionation container In the boiling point meter, which measures the distillation point of the sample from the amount of sample distilled out by detecting the surface and the sample temperature in the container detected by the temperature detector, the change in the liquid level of the sample in the fractionation container is detected. A liquid level detection mechanism is provided, and when the sample temperature in the container detected by the temperature detector reaches a predetermined value, the liquid level detection mechanism detects the sample liquid level in the fractionation container. A boiling point meter characterized in that
（請求項２） 試料が導入される容器と、この容器内の試料を加熱する
加熱装置と、容器内に生じた試料の蒸気が導入されると
共に、この蒸気を冷却して液化する冷却管と、前記冷却
管で液化した試料が滴下される分留容器と、前記容器内
に生じた試料蒸気の温度を検出する温度検出器とを有
し、前記分留容器内に滴下された試料の液面を検出する
ことにより求めた試料の留出量と温度検出器で検出した
容器内の試料温度とから試料の蒸留点を測定する沸点計
において、分留容器内の試料の液面変動を検出する液面
検出機構と、この液面の変動幅を記憶する記憶手段とを
具備してなり、実際に蒸留点を測定したときの蒸留開始
時及び蒸留終了時における分留容器内の試料液面をそれ
ぞれ前記液面検出機構によって検出すると共に、これら
両液面間の液面変動幅を前記記憶手段によって記憶し、
これら両液面間の液面変動幅をゼロ−スパンとして蒸留
点を測定するようにしたことを特徴とする沸点計。(Claim 2) A container into which the sample is introduced, a heating device for heating the sample in the container, and a cooling pipe for introducing the vapor of the sample generated in the container and cooling the vapor to liquefy it. , A fractionation container in which the sample liquefied in the cooling pipe is dropped, and a temperature detector for detecting the temperature of the sample vapor generated in the container, and the liquid of the sample dropped in the fractionation container In the boiling point meter, which measures the distillation point of the sample from the amount of sample distilled out by detecting the surface and the sample temperature in the container detected by the temperature detector, the change in the liquid level of the sample in the fractionation container is detected. Liquid level detection mechanism and a storage means for storing the fluctuation range of the liquid level, and the sample liquid level in the fractionation container at the start and end of distillation when the distillation point is actually measured. Are detected by the liquid level detection mechanism, respectively. The liquid level fluctuation range between is stored by the storage means,
A boiling point meter characterized in that the distillation point is measured with the liquid level fluctuation range between these two liquid levels as zero-span.
（請求項３） 試料が導入される容器と、この容器内の試料を加熱する
加熱装置と、容器内に生じた試料の蒸気が導入されると
共に、この蒸気を冷却して液化する冷却管と、前記冷却
管で液化した試料が滴下される分留容器と、前記容器内
に生じた試料蒸気の温度を検出する温度検出器とを有
し、前記分留容器内に滴下された試料の液面を検出する
ことにより求めた試料の留出量と温度検出器で検出した
容器内の試料温度とから試料の蒸留点を測定する沸点計
において、所定量の試料を計量し、この試料を前記容器
に導入する計量装置と、この計量装置と前記分留容器と
を連通する切換可能に設けられたバイパス管と、分留容
器内の試料の液面変動を検出する液面検出機構と、この
液面の変動幅を記憶する記憶手段とを具備してなり、前
記分留容器から試料を排出したとき及び前記計量装置か
らバイパス管を通して分留容器に所定量の試料を導入し
たときにおける分留容器内の試料液面をそれぞれ前記液
面検出機構によって検出すると共に、これら両液面間の
液面変動幅を前記記憶手段によって記憶し、これら両液
面間の液面変動幅をゼロ−スパンとして蒸留点を測定す
るようにしたことを特徴とする沸点計。(Claim 3) A container in which the sample is introduced, a heating device for heating the sample in the container, and a cooling pipe for introducing the sample vapor generated in the container and cooling the vapor to liquefy it. , A fractionation container in which the sample liquefied in the cooling pipe is dropped, and a temperature detector for detecting the temperature of the sample vapor generated in the container, and the liquid of the sample dropped in the fractionation container In the boiling point meter which measures the distillation point of the sample from the distillation amount of the sample obtained by detecting the surface and the sample temperature in the container detected by the temperature detector, a predetermined amount of sample is weighed, and this sample is A metering device to be introduced into the container, a switchable bypass pipe communicating the metering device with the fractionation container, a liquid level detection mechanism for detecting the liquid level fluctuation of the sample in the fractionation container, and A storage means for storing the fluctuation range of the liquid level, The sample liquid level in the fractionating container when the sample is discharged from the container and when a predetermined amount of the sample is introduced from the measuring device to the fractionating container through the bypass pipe is detected by the liquid level detection mechanism, and both of these are detected. A boiling point meter characterized in that the liquid level fluctuation range between the liquid levels is stored by the storage means, and the distillation point is measured with the liquid level fluctuation range between the two liquid levels as zero-span.
この場合、請求項１〜３の沸点計における液面変動を検
出する液面検出機構としては、イメージセンサや液面上
昇と共に上昇するタイプのレベルセンサなどを用いるこ
とができる。また、請求項２及び３の沸点計における液
面の変動幅を記憶する記憶手段は、液面検出機構と接続
した制御部に液面変動幅の記憶回路を設けることなどに
より構成することができる。In this case, an image sensor or a level sensor of a type that rises as the liquid level rises can be used as the liquid level detection mechanism for detecting the liquid level fluctuation in the boiling point meter according to the first to third aspects. Further, the storage means for storing the fluctuation range of the liquid level in the boiling point meter according to claims 2 and 3 can be configured by providing a storage circuit for the fluctuation level of the liquid level in the control unit connected to the liquid level detection mechanism. .
［作用］ 請求項１の沸点計においては、分留容器内の試料液面の
変動を検出すると共に、温度検出器で検出した容器内の
試料温度が所定の値になったときに液面検出機構で分留
容器内の試料液面を検出するようにしたため、どのよう
な留出温度であってもその温度に対応する留出量を測定
することができる。[Operation] In the boiling point meter according to claim 1, the fluctuation of the sample liquid level in the fractionation container is detected, and the liquid level is detected when the sample temperature in the container detected by the temperature detector reaches a predetermined value. Since the mechanism detects the sample liquid level in the fractionation container, the amount of distillate corresponding to the temperature can be measured at any distillate temperature.
請求項２の沸点計においては、実際の測定を行い、この
ときの全留出量を対応した液面変動幅を記憶手段で記憶
しておき、この変動幅（ゼロ−スパン）を基準として測
定を行うことにより、補正を行うことなくJISに定めら
れた減失分加算留出点に近似したJISの許容範囲内の留
出点を直接求めることができる。すなわち、実際の測定
により求めた全留出量に対応する液面変動幅をゼロ−ス
パンとして測定を行った場合、減失分が差し引かれた留
出量を基準とすることができるため、測定後に減失分に
応じた補正を行うことなく減失分加算留出点に近似した
値を直読できるものである。In the boiling point meter according to claim 2, actual measurement is performed, and the liquid level fluctuation width corresponding to the total amount of distillate at this time is stored in the storage means, and the fluctuation width (zero-span) is used as a reference for measurement. By performing the above, it is possible to directly obtain the distillation point within the allowable range of JIS that is close to the addition point for loss reduction specified in JIS without correction. That is, when the liquid level fluctuation width corresponding to the total distillate amount obtained by actual measurement is measured as zero-span, the distillate amount from which the loss is subtracted can be used as the reference, It is possible to directly read the value approximated to the diminished amount addition distillation point without performing the correction according to the lost amount later.
請求項３の沸点計においては、計量装置からバイパス管
を通して分留容器内に試料を導入してゼロ−スパンの設
定を行うようにしたので、計量装置によるゼロ−スパン
の精密な設定を容易に行うことができる。また、上記計
量装置によるゼロ−スパンを記憶手段で記憶すると共
に、実際の測定を行ってそのときの全留出量に対応した
液面変動幅（ゼロ−スパン）を記憶手段で記憶し、前者
の計量装置によるゼロ−スパンの値から後者の実際の測
定により求めたゼロ−スパンの値を引くことにより、減
失分を簡単に算出することができる。従って、この減失
分の値を用いてJISに定められた補正計算を行うことに
より、減失分加算留出点を得ることができ、この場合は
もちろんJISの規定と完全に合致した値を得ることがで
きる。In the boiling point meter according to claim 3, since the sample is introduced from the measuring device through the bypass pipe into the fractionating container to set the zero-span, the precise setting of the zero-span by the measuring device is facilitated. It can be carried out. In addition, the zero-span by the above-mentioned measuring device is stored in the storage means, the actual measurement is performed, and the liquid level fluctuation width (zero-span) corresponding to the total amount of distillate at that time is stored in the storage means. The loss amount can be easily calculated by subtracting the zero-span value obtained by the latter actual measurement from the zero-span value measured by the measuring device of FIG. Therefore, by performing the correction calculation specified in JIS using the value of this loss, it is possible to obtain the loss addition distillation point, and in this case, of course, the value that completely conforms to the JIS Obtainable.
次に実施例を示し、本発明を具体的に説明するが、本発
明は下記実施例に限定されるものではない。EXAMPLES Next, the present invention will be specifically described with reference to examples, but the present invention is not limited to the following examples.
〔実施例〕 第１図は本発明沸点計の一実施例を示す。なお、第１図
において第３図の沸点計と同一構成の部分には同一参照
符号を付してその説明を省略する。Example FIG. 1 shows an example of the boiling point meter of the present invention. In FIG. 1, the same components as those of the boiling point meter of FIG. 3 are designated by the same reference numerals and the description thereof will be omitted.
本実施例においては、液面検出管14にイメージセンサ19
が配設され、このイメージセンサ19によって検出管14内
の液面が連続的に検出されるようになっている。このイ
メージセンサ19は制御部18と連絡していると共に、この
制御部18はイメージセンサ19が検出した液面の変動幅を
記憶できるように構成されている。また、試料導入管３
には第１電磁バルブ６の下流側に存して三方電磁バルブ
20が介装され、このバルブ20の通路口にバイパス管21の
一端が連結されていると共に、バイパス管21の他端は試
料留出管12に連結されている。更に、試料排出管16の上
端は第２図に示すように分留容器13内部にまで延出され
ている。In this embodiment, the image sensor 19 is attached to the liquid level detection tube 14.
The image sensor 19 continuously detects the liquid level in the detection tube 14. The image sensor 19 is in communication with the control unit 18, and the control unit 18 is configured to be able to store the fluctuation range of the liquid level detected by the image sensor 19. In addition, the sample introduction tube 3
Is located on the downstream side of the first solenoid valve 6 and is a three-way solenoid valve.
20 is interposed, one end of a bypass pipe 21 is connected to the passage opening of the valve 20, and the other end of the bypass pipe 21 is connected to the sample distillation pipe 12. Furthermore, the upper end of the sample discharge pipe 16 extends to the inside of the fractionation container 13 as shown in FIG.
ここで、上記イメージセンサ19は第２図に示す構成を有
する。即ち、発行ダイオード等の発光素子19aが縦方向
に沿って連続的に多数配設された発光体19bと、ホトダ
イオード等の受光素子19cが縦方向に沿って連続的に多
数配設された受光体19dとが互に対向配置されてなるも
ので、発光素子19aから発光され、検出管14を透過した
光を受光素子19cで検知することにより検出管14内の液
面変動を連続的に検出するものである。Here, the image sensor 19 has the structure shown in FIG. That is, a light emitting body 19b in which a large number of light emitting elements 19a such as issuing diodes are continuously arranged along the vertical direction, and a light receiving body in which a large number of light receiving elements 19c such as photodiodes are continuously arranged along the vertical direction. 19d are arranged to face each other, and the light emitted from the light emitting element 19a and transmitted through the detection tube 14 is detected by the light receiving element 19c to continuously detect the liquid level fluctuation in the detection tube 14. It is a thing.
本実施例の沸点計によって蒸留点の測定を行なう場合、
まずゼロ−スパン（留出量０〜100％の液面変動幅）の
調整を行なう。即ち、第１電磁バルブ６を閉じ、第２電
磁バルブ８を開けて計量カップ４に所定量の試料を溜め
た後、第２電磁バルブ８を閉じ、試料の流通を止めた状
態で第１電磁バルブ６を開けると共に、三方電磁バルブ
20を作動させて計量カップ４内の試料をバイパス管21に
導き、この試料全てを分留容器13内に入れた後、第３電
磁バルブ17を開いて分留容器13内の試料を排出する。す
ると、分留容器13内の試料液面は試料排出管16の上端面
と同じ位置（第２図中Ａ）になるので、このときのイメ
ージセンサ19の出力を制御部18で読み取り、再度行い、
計量カップで定まる量の100％留出点とする。これによ
りゼロ−スパンが制御部18で記憶され、このゼロ−スパ
ンによって留出量を管理することができる。なお、この
ゼロ−スパン調整は、定期的に行なうことにより測定値
の信頼性が向上すると共に、ゼロ−スパンの値の変動か
ら計量ミス等の装置不良の診断にも役立つ。When measuring the distillation point by the boiling point meter of the present embodiment,
First, adjust the zero-span (fluid level fluctuation range of distillate amount 0 to 100%). That is, the first electromagnetic valve 6 is closed, the second electromagnetic valve 8 is opened to store a predetermined amount of sample in the measuring cup 4, and then the second electromagnetic valve 8 is closed to stop the flow of the sample to the first electromagnetic valve. 3-way solenoid valve with valve 6 open
20 is operated to guide the sample in the measuring cup 4 to the bypass pipe 21, all the sample is put in the fractionation container 13, and then the third electromagnetic valve 17 is opened to discharge the sample in the fractionation container 13. . Then, the sample liquid level in the fractionation container 13 will be at the same position as the upper end face of the sample discharge pipe 16 (A in FIG. 2), and the output of the image sensor 19 at this time is read by the control unit 18 and the process is performed again. ,
The distillation point is 100% of the amount determined by the measuring cup. As a result, the zero-span is stored in the controller 18, and the amount of distillate can be controlled by this zero-span. Note that this zero-span adjustment improves the reliability of the measured value by performing the adjustment periodically, and is useful for diagnosing a device failure such as a measurement error due to the fluctuation of the zero-span value.
上記ゼロ−スパンの調整後、このゼロ−スパンを基準と
して試料の蒸留点を測定するものであるが、このときの
測定動作は第３図の沸点計と同じであるからその説明を
省略する。After adjusting the zero-span, the distillation point of the sample is measured with the zero-span as a reference. The measuring operation at this time is the same as that of the boiling point meter in FIG. 3, and the description thereof is omitted.
この場合、複数回のバッチ測定を連続して行うときに
は、最初に設定したゼロ−スパンを基準として全ての測
定を行うことができ、その測定時に減失する減失分も管
理することができる。即ち、最初に設定したゼロ−スパ
ン（計量装置によるゼロ−スパン）と、実際の測定によ
って得られたゼロ−スパンとを制御部18で記憶してお
き、前者の値から後者の値を引くことにより、減失分を
算出することができ、この減失分の値を用いてJISに定
められた補正計算を行うことにより、JISの規定に完全
に合致した減失分加算留出点を得ることができる。In this case, when a plurality of batch measurements are continuously performed, all the measurements can be performed with the initially set zero-span as a reference, and the loss amount lost at the time of the measurement can be managed. That is, the zero-span initially set (zero-span by the measuring device) and the zero-span obtained by actual measurement are stored in the control unit 18, and the latter value is subtracted from the former value. The loss amount can be calculated by using the value of this loss amount, and the correction calculation stipulated in JIS is used to obtain the loss-addition distillate point that completely conforms to JIS regulations. be able to.
また、実際の測定時に得られたゼロ−スパンを制御部18
で記憶しておき、このゼロ−スパンを基準として測定を
行うこともできる。即ち、実際の測定により求めたゼロ
−スパンを基準として測定を行った場合、減失分を差し
引かれた留出量を基準とすることができるため、減失分
に応じた補正を行うことなくJISに定められた減失分加
算留出点に近似した留出点を直接求めることができる。In addition, the zero-span obtained during actual measurement is used as the control unit 18
It is also possible to store the value in step S3 and store it in the memory, and perform the measurement based on this zero-span. That is, when the measurement is performed with the zero-span obtained from the actual measurement as the reference, the distillate amount after subtracting the loss can be used as the reference, so that correction is not performed according to the loss. It is possible to directly obtain a distillation point that is similar to the JIS point for diminishing loss addition.
本実施例の沸点計は、液面の検出に液面変動を連続的に
検出し得るイメージセンサ19を用いたことにより、いわ
ば液面の検出幅に無数のレベルセンサが設置されたのと
同じこととなり、液面の高さを正確に測定することがで
きると共に、検出ポイントの変更は制御部18に対する指
示を変えるだけで行なうことができ、従って装置に手を
加えることなく簡単に検出ポイントを変更することがで
きる。The boiling point meter of the present embodiment, by using the image sensor 19 capable of continuously detecting the liquid level fluctuation in the detection of the liquid level, so to speak, the same as innumerable level sensors are installed in the detection width of the liquid level. Therefore, the height of the liquid surface can be accurately measured, and the detection point can be changed only by changing the instruction to the control unit 18, and therefore the detection point can be easily changed without changing the device. Can be changed.
また、本沸点計においては液面を連続的に検出できるた
め、所望の留出量における試料留出温度を測定すること
ができるのみならず、所望の留出温度における留出量を
も測定することができ、しかも留出量とこれに対応する
留出温度を連続的に制御部18で保持することにより、こ
の値に基づいて蒸留曲線を表示させることも可能であ
る。Further, since the liquid level can be continuously detected in this boiling point meter, not only the sample distilling temperature at the desired distilling amount can be measured but also the distilling amount at the desired distilling temperature can be measured. Further, the distillation curve can be displayed based on this value by continuously holding the distillation amount and the distillation temperature corresponding thereto by the control unit 18.
更に、上述したように、バイパス管21を用いることによ
り測定開始前にゼロ−スパンを容易に設定できるのみな
らず、連続的にバッチ測定を行なうときに一回の測定に
おけるゼロ−スパンを記憶すると共に、このゼロ−スパ
ンを基準として測定を行なうことにより、実際の測定に
よって求めたゼロ−スパンを基準として蒸留点の測定を
行なうことができるため、蒸留時に減失分があってもこ
の減失分が差し引かれた全留出量を100％としてゼロ−
スパンを設定することができ、従って減失分を測定した
り減失分に応じた補正を行なうことなくJISに対応するJ
ISの許容範囲内の測定値を直接得ることができるもので
ある。Further, as described above, by using the bypass pipe 21, not only the zero-span can be easily set before the measurement is started, but also the zero-span in one measurement is stored when continuously performing batch measurement. At the same time, by performing measurement with this zero-span as a reference, the distillation point can be measured with reference to the zero-span obtained by actual measurement. Zero with 100% as the total amount of distillate minus
The span can be set, so the JIS corresponding to JIS can be used without measuring the loss or correction according to the loss.
It is possible to directly obtain the measured value within the allowable range of IS.
なお、上記実施例においては液面変動を連続的に検出す
る液面検出機構としてイメージセンサを用いたが、液面
上昇と共に上昇するタイプのレベルセンサを用いてもよ
い。また、その他の構成についても本発明の要旨を逸脱
しない範囲で種々変更して差し支えない。Although the image sensor is used as the liquid level detecting mechanism for continuously detecting the liquid level fluctuation in the above embodiment, a level sensor of a type that rises as the liquid level rises may be used. Further, other configurations may be variously modified without departing from the scope of the present invention.
以上説明したように、請求項１の沸点計は、分留容器内
の液面変動を検出すると共に、試料温度が所定の値にな
ったときに分留容器内の液面を検出するように構成した
ので、所望の留出温度における留出量を測定することが
できる。As described above, the boiling point meter according to claim 1 detects the liquid level fluctuation in the fractionation container and also detects the liquid level in the fractionation container when the sample temperature reaches a predetermined value. Since it is configured, the amount of distillate at a desired distilling temperature can be measured.
請求項２の沸点計は、分留容器内の液面変動を検出する
と共に、この液面変動を記憶するように構成したので、
実際の測定によって得られたゼロ−スパンを記憶し、こ
れを基準として測定を行うことにより、減失分や補正計
算を行うことなく減失分加算留出点に近似した留出点を
容易に求めることができる。Since the boiling point meter according to claim 2 is configured to detect the liquid level fluctuation in the fractionating container and store the liquid level fluctuation,
By storing the zero-span obtained by actual measurement and performing measurement with this as a reference, it is possible to easily obtain a distilling point that is close to the diminishing component addition distilling point without performing loss calculation and correction calculation. You can ask.
請求項３の沸点計は、バイパス管を用いることにより、
測定開始前にゼロ−スパンを簡単かつ精密に設定でき
る。また、測定開始前のゼロ−スパンと実際の測定によ
り求めたゼロ−スパンとから算出した減失分の値を用い
て補正計算を行うことにより、減失分加算留出点を簡単
に得ることができる。The boiling point meter according to claim 3 uses a bypass pipe,
Zero-span can be set easily and precisely before starting measurement. In addition, it is possible to easily obtain the loss-added distillation point by performing a correction calculation using the value of the loss component calculated from the zero-span before the start of measurement and the zero-span obtained from the actual measurement. You can
第１図は本発明の一実施例に係る沸点計を示す概略図、
第２図は同沸点計の分留容器、液面検出管部分を示す一
部省略拡大断面図、第３図は従来の沸点計の一例を示す
概略図である。 １…容器、２…ヒータ（加熱装置） ４…計量装置、９…試料冷却管 11…温度検出器、13…分留容器 18…制御部、19…イメージセンサ 21…バイパス管FIG. 1 is a schematic view showing a boiling point meter according to an embodiment of the present invention,
FIG. 2 is a partially omitted enlarged cross-sectional view showing a fractional distillation container and a liquid level detecting tube portion of the same boiling point meter, and FIG. 3 is a schematic view showing an example of a conventional boiling point meter. DESCRIPTION OF SYMBOLS 1 ... Container, 2 ... Heater (heating device) 4 ... Metering device, 9 ... Sample cooling pipe 11 ... Temperature detector, 13 ... Fractionation container 18 ... Control part, 19 ... Image sensor 21 ... Bypass pipe
───────────────────────────────────────────────────── フロントページの続き (72)発明者 那須 英輔 東京都武蔵野市吉祥寺北町４丁目13番14号 電気化学計器株式会社内 (56)参考文献 特開 昭49−31397（ＪＰ，Ａ) ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Eisuke Nasu 4-13-14 Kitacho, Kichijoji, Musashino City, Tokyo Electrochemical Instruments Co., Ltd. (56) Reference JP-A-49-31397 (JP, A)
Claims (3)
料を加熱する加熱装置と、容器内に生じた試料の蒸気が
導入されると共に、この蒸気を冷却して液化する冷却管
と、前記冷却管で液化した試料が滴下される分留容器
と、前記容器内に生じた試料蒸気の温度を検出する温度
検出器とを有し、前記分留容器内に滴下された試料の液
面を検出することにより求めた試料の留出量と温度検出
器で検出した容器内の試料温度とから試料の蒸留点を測
定する沸点計において、分留容器内の試料の液面変動を
検出する液面検出機構を具備してなり、温度検出器で検
出した容器内の試料温度が所定の値になったときに前記
液面検出機構で分留容器内の試料液面を検出するように
したことを特徴とする沸点計。1. A container for introducing a sample, a heating device for heating the sample in the container, and a cooling pipe for introducing the sample vapor generated in the container and cooling the vapor to liquefy it. , A fractionation container in which the sample liquefied in the cooling pipe is dropped, and a temperature detector for detecting the temperature of the sample vapor generated in the container, and the liquid of the sample dropped in the fractionation container In the boiling point meter, which measures the distillation point of the sample from the amount of sample distilled out by detecting the surface and the sample temperature in the container detected by the temperature detector, the change in the liquid level of the sample in the fractionation container is detected. A liquid level detection mechanism is provided, and when the sample temperature in the container detected by the temperature detector reaches a predetermined value, the liquid level detection mechanism detects the sample liquid level in the fractionation container. A boiling point meter characterized in that
料を加熱する加熱装置と、容器内に生じた試料の蒸気が
導入されると共に、この蒸気を冷却して液化する冷却管
と、前記冷却管で液化した試料が滴下される分留容器
と、前記容器内に生じた試料蒸気の温度を検出する温度
検出器とを有し、前記分留容器内に滴下された試料の液
面を検出することにより求めた試料の留出量と温度検出
器で検出した容器内の試料温度とから試料の蒸留点を測
定する沸点計において、分留容器内の試料の液面変動を
検出する液面検出機構と、この液面の変動幅を記憶する
記憶手段とを具備してなり、実際に蒸留点を測定したと
きの蒸留開始時及び蒸留終了時における分留容器内の試
料液面をそれぞれ前記液面検出機構によって検出すると
共に、これら両液面間の液面変動幅を前記記憶手段によ
って記憶し、これら両液面間の液面変動幅をゼロ−スパ
ンとして蒸留点を測定するようにしたことを特徴とする
沸点計。2. A container into which a sample is introduced, a heating device for heating the sample in the container, and a cooling pipe for introducing the sample vapor generated in the container and cooling the vapor to liquefy it. , A fractionation container in which the sample liquefied in the cooling pipe is dropped, and a temperature detector for detecting the temperature of the sample vapor generated in the container, and the liquid of the sample dropped in the fractionation container In the boiling point meter, which measures the distillation point of the sample from the amount of sample distilled out by detecting the surface and the sample temperature in the container detected by the temperature detector, the change in the liquid level of the sample in the fractionation container is detected. Liquid level detection mechanism and a storage means for storing the fluctuation range of the liquid level, and the sample liquid level in the fractionation container at the start and end of distillation when the distillation point is actually measured. Are detected by the liquid level detection mechanism, respectively. Of the liquid level fluctuation width stored by said storing means, the liquid level fluctuation width between the both liquid level zero - boiling meter is characterized in that so as to measure the distillation points as span.
料を加熱する加熱装置と、容器内に生じた試料の蒸気が
導入されると共に、この蒸気を冷却して液化する冷却管
と、前記冷却管で液化した試料が滴下される分留容器
と、前記容器内に生じた試料蒸気の温度を検出する温度
検出器とを有し、前記分留容器内に滴下された試料の液
面を検出することにより求めた試料の留出量と温度検出
器で検出した容器内の試料温度とから試料の蒸留点を測
定する沸点計において、所定量の試料を計量し、この試
料を前記容器に導入する計量装置と、この計量装置と前
記分留容器とを連通する切換可能に設けられたバイパス
管と、分留容器内の試料の液面変動を検出する液面検出
機構と、この液面の変動幅を記憶する記憶手段とを具備
してなり、前記分留容器から試料を排出したとき及び前
記計量装置からバイパス管を通して分留容器に所定量の
試料を導入したときにおける分留容器内の試料液面をそ
れぞれ前記液面検出機構によって検出すると共に、これ
ら両液面間の液面変動幅を前記記憶手段によって記憶
し、これら両液面間の液面変動幅をゼロ−スパンとして
蒸留点を測定するようにしたことを特徴とする沸点計。3. A container for introducing a sample, a heating device for heating the sample in the container, and a cooling pipe for introducing the vapor of the sample generated in the container and cooling the vapor to liquefy it. , A fractionation container in which the sample liquefied in the cooling pipe is dropped, and a temperature detector for detecting the temperature of the sample vapor generated in the container, and the liquid of the sample dropped in the fractionation container In the boiling point meter which measures the distillation point of the sample from the distillation amount of the sample obtained by detecting the surface and the sample temperature in the container detected by the temperature detector, a predetermined amount of sample is weighed, and this sample is A metering device to be introduced into the container, a switchable bypass pipe communicating the metering device with the fractionation container, a liquid level detection mechanism for detecting the liquid level fluctuation of the sample in the fractionation container, and A storage means for storing the fluctuation range of the liquid level, The sample liquid level in the fractionating container when the sample is discharged from the container and when a predetermined amount of the sample is introduced from the measuring device into the fractionating container through the bypass pipe is detected by the liquid level detection mechanism. A boiling point meter characterized in that the liquid level fluctuation range between the liquid levels is stored by the storage means, and the distillation point is measured with the liquid level fluctuation range between the two liquid levels as zero-span.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1142587A JPH06100557B2 (en) | 1989-06-05 | 1989-06-05 | Boiling point |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1142587A JPH06100557B2 (en) | 1989-06-05 | 1989-06-05 | Boiling point |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH039253A JPH039253A (en) | 1991-01-17 |
| JPH06100557B2 true JPH06100557B2 (en) | 1994-12-12 |
Family
ID=15318778
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1142587A Expired - Lifetime JPH06100557B2 (en) | 1989-06-05 | 1989-06-05 | Boiling point |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH06100557B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012181134A (en) * | 2011-03-02 | 2012-09-20 | Dkk Toa Corp | Boiling-point meter |
| CN104597072A (en) * | 2015-01-20 | 2015-05-06 | 兰州大学 | Boiling point testing instrument |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5225116B2 (en) * | 1972-07-13 | 1977-07-05 |
-
1989
- 1989-06-05 JP JP1142587A patent/JPH06100557B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH039253A (en) | 1991-01-17 |
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