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JPS6035024B2 - How to measure aniline point - Google Patents
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JPS6035024B2 - How to measure aniline point - Google Patents

How to measure aniline point

Info

Publication number
JPS6035024B2
JPS6035024B2 JP9741078A JP9741078A JPS6035024B2 JP S6035024 B2 JPS6035024 B2 JP S6035024B2 JP 9741078 A JP9741078 A JP 9741078A JP 9741078 A JP9741078 A JP 9741078A JP S6035024 B2 JPS6035024 B2 JP S6035024B2
Authority
JP
Japan
Prior art keywords
temperature
mixed liquid
heating
aniline
circuit
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
Application number
JP9741078A
Other languages
Japanese (ja)
Other versions
JPS5524631A (en
Inventor
貞夫 森田
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Idemitsu Kosan Co Ltd
Original Assignee
Idemitsu Kosan Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Idemitsu Kosan Co Ltd filed Critical Idemitsu Kosan Co Ltd
Priority to JP9741078A priority Critical patent/JPS6035024B2/en
Publication of JPS5524631A publication Critical patent/JPS5524631A/en
Publication of JPS6035024B2 publication Critical patent/JPS6035024B2/en
Expired legal-status Critical Current

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  • Investigating Or Analyzing Materials Using Thermal Means (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Description

【発明の詳細な説明】 本発明はァニリン点の測定方法に関し、詳しくは温度制
御回、微分回路および演算回路等を併用することによっ
て精度の高いアニリン点の測定方法に関する。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for measuring an aniline point, and more particularly to a method for measuring an aniline point with high accuracy by using a temperature control circuit, a differentiation circuit, an arithmetic circuit, etc. in combination.

一般に石油製品の組成を調べるためにアニリン点の測定
が広く行なわれており、アニリン点試験方法としてはJ
ISK2256が確立されている。
The aniline point is generally measured to determine the composition of petroleum products, and the aniline point test method is J.
ISK2256 is established.

従釆からこのJISの方法に準拠して様々なアニリン点
試験器あるいは方法が開発されている。しかし従釆の試
験器あるいは方法では、測定値の誤差(たとえば66.
900の場合は測定値が66.5〜67.5oo)が大
きく、また晴色油等の試料油に適用できないなどの欠点
があった。
Various aniline point testers and methods have been developed based on this JIS method. However, depending on the test device or method, the error in the measurement value (for example, 66.
In the case of 900, the measured value was large (66.5 to 67.5 oo), and there were drawbacks such as inability to apply to sample oils such as fair-colored oil.

本発明者は上記従釆技術の欠点を克服して、測定の精度
が高くしかも広範囲の石油類に適用しうる方法を関発す
べ〈鋭意研究を重ねた。
The present inventor has conducted extensive research to overcome the drawbacks of the conventional techniques described above and develop a method that has high measurement accuracy and can be applied to a wide range of petroleum products.

その結果、試料油とアニリンの混合液の白濁度を透過光
量により検知してアニリン点を測定するに際して、温度
制御回路、微分回路および演算回路等を併用することに
より目的を達成しうろことを見出し、本発明を完成する
に至った。すなわち本発明は、試料油とアニリンとの混
合液の白濁度の温度変化を透過光量の変化により検知し
てアニリン点を測定する方法において、{ィ} 該混合
液を昇温用温度制御回路を介して加熱昇温せしめ、{〇
ー 該混合液の昇温速度が一定範囲に達したときに微分
回路を作動せしめてdl/dT(ここで1は透過光量に
対応する出力を示し、Tは混合液の温度あるいは時間の
出力を示す。
As a result, it was discovered that when measuring the aniline point by detecting the white turbidity of a mixed solution of sample oil and aniline by the amount of transmitted light, the purpose could be achieved by using a temperature control circuit, a differentiation circuit, an arithmetic circuit, etc. , we have completed the present invention. That is, the present invention provides a method for measuring the aniline point by detecting a temperature change in the white turbidity of a mixed liquid of a sample oil and aniline by a change in the amount of transmitted light. When the heating rate of the mixed liquid reaches a certain range, the differential circuit is activated to calculate dl/dT (where 1 indicates the output corresponding to the amount of transmitted light, and T is Indicates the temperature or time output of the mixed liquid.

)を測定し、し一 前記dl/dTの値が零になったと
きに昇溢用温度制御回路による混合液の加熱を停止ある
いは低下させると共に、微分回路を停止しかつその際の
1をlsとして演算回路に記憶せしめ、0 次いで前記
混合液を昇温用温度制御回路を介して冷却すると共に前
記演算回路を作動せしめて△1=ls−1を計算し、【
ホー △1が所定値に達したときにその際の混合液の温
度を記録することを特徴とするアニリン点の測定方法を
提供するものである。
), and when the value of dl/dT becomes zero, stop or reduce the heating of the mixed liquid by the overflow temperature control circuit, stop the differential circuit, and set 1 at that time to ls. Then, the mixed liquid is cooled through the temperature control circuit for heating up, and the arithmetic circuit is operated to calculate Δ1=ls-1, and
The present invention provides a method for measuring an aniline point, which is characterized by recording the temperature of a liquid mixture when Δ1 reaches a predetermined value.

本発明の方法を図面に基づいてさらに詳しく説明すれば
次の如くである。
The method of the present invention will be explained in more detail based on the drawings as follows.

第1図において、槽1内に試料セル2が入れてあり、こ
のセル2の両側に光源3および受光器4が備えられてい
る。
In FIG. 1, a sample cell 2 is placed in a tank 1, and a light source 3 and a light receiver 4 are provided on both sides of the cell 2.

この試料セル2に測定すべき試料油とアニリンを等量(
通常は10の【ずつ)注ぎ入れ、櫨梓棒5で充分に鷹杵
混合しながら、昇温用温度制御回路6を介して加熱器7
により糟1を加熱して、試料油とアニリンの混合液を加
熱昇温する。昇温速度が一定範囲、通常は1〜200の
昇温速度に達したときに、前記混合液の温度計8ならび
に受光器4に接続してある微分回路9を作動せしめる。
この微分回路9においては温度計8、受光器4からの情
報に従ってdl/dTが測定され、このdl/dTの値
が零になったとき、すなわち透明点に達したときに、微
分回路9を停止する。またこれと同時に昇温用温度制御
回路6による試料混合液の加熱を停止するかあるいは弱
くして昇温をストップされる。さらにこの透明点におけ
る透過光量に対応する出力1をlsとして演算回路1川
こ記憶させておく。この演算回路10は受光器4と接続
してあり、微分回路9の停止と同時に作動しはじめ△1
=ls−1(あるいは△1=logls−logl)を
計算する。一方、試料混合液は、降温用温度制御回路1
1を介して冷却される。降温速度は特に制限はないが、
通常は毎分0.5〜1℃程度となるように制御すべきで
ある。冷却は一般に加熱器7のスイッチを切ったり、強
さを弱めたりすることによって行ない得るが、所定の降
温速度が得られない場合は、電磁弁12等を通して槽1
内に冷却用空気を吹き込めばよい。試料混合液の冷却を
行ないながら演算回路10による△1=ls−1の計算
を続け、△1の値が予め設定した値になったときに、そ
の際の混合液の温度をアニリン点としてプリンターある
いはディジタル表示器13に記録する。なお本発明の方
法に用いる微分回路、演算回路、温度制御回路等はすべ
て総合制御回路14によって総括的にコントロールすべ
きである。
Equal amounts of the sample oil and aniline to be measured (
Usually, 10 [at a time] is poured into the heater 7 through the temperature control circuit 6 for heating while thoroughly mixing with a hawk rod 5.
The mixture of sample oil and aniline is heated to raise its temperature by heating the cassette 1. When the temperature increase rate reaches a certain range, usually 1 to 200, the differential circuit 9 connected to the mixed liquid thermometer 8 and the light receiver 4 is activated.
In this differentiating circuit 9, dl/dT is measured according to the information from the thermometer 8 and the light receiver 4, and when the value of this dl/dT becomes zero, that is, when the clear point is reached, the differentiating circuit 9 is Stop. At the same time, the heating of the sample mixture by the heating temperature control circuit 6 is stopped or weakened to stop the heating. Furthermore, the output 1 corresponding to the amount of transmitted light at this transparent point is stored as ls in one calculation circuit. This arithmetic circuit 10 is connected to the light receiver 4 and starts operating at the same time as the differentiation circuit 9 stops △1
=ls-1 (or Δ1=logls-logl). On the other hand, the sample mixture liquid is
1. There is no particular limit to the cooling rate, but
Normally, the temperature should be controlled to be about 0.5 to 1°C per minute. Cooling can generally be achieved by turning off the heater 7 or weakening its strength, but if a predetermined temperature reduction rate cannot be obtained, the tank 1 can be cooled down through the solenoid valve 12 or the like.
Just blow cooling air inside. The arithmetic circuit 10 continues to calculate △1=ls-1 while cooling the sample liquid mixture, and when the value of △1 reaches a preset value, the temperature of the liquid mixture at that time is set as the aniline point and is printed on the printer. Alternatively, it is recorded on the digital display 13. It should be noted that all the differentiating circuits, arithmetic circuits, temperature control circuits, etc. used in the method of the present invention should be totally controlled by the general control circuit 14.

また本発明の方法は、前述した如き操作手順にてアニリ
ン点を測定するものであるが、さらにその精度を高めた
い場合には、記録したアニリン点が所定の誤差範囲内で
一致するまでイ〜木までの操作を繰り返せばよい。この
場合、一般には記録したアニリン点が3回連続0.ro
あるいは0.ぞ0℃の範囲内で一致したときに真のアニ
リン点として記録する。叙上の如く、本発明の方法によ
れば、極めて高い精度でアニリン点を測定することがで
き、またA重油等の燃料油、ブライトストック、シリン
ダー油等の重質潤滑油、エキストラクト蟹分等の広範囲
の石油についてのアニリン点測定が可能である。
Furthermore, in the method of the present invention, the aniline point is measured using the operating procedure as described above, but if you want to further improve the accuracy, repeat the steps from step to step until the recorded aniline points match within a predetermined error range. Just repeat the operation up to the tree. In this case, generally the recorded aniline point is 0.3 times in a row. ro
Or 0. When they agree within a range of 0°C, it is recorded as a true aniline point. As described above, according to the method of the present invention, it is possible to measure the aniline point with extremely high accuracy, and it is also possible to measure the aniline point with extremely high accuracy, and it is also possible to measure the aniline point with extremely high accuracy, and it is also possible to measure the aniline point with extremely high accuracy. It is possible to measure the aniline point of a wide range of petroleum products, such as:

【図面の簡単な説明】[Brief explanation of the drawing]

第1図は本発明の方法に使用する制御機構の一例を示す
概略図である。 図中1は糟、2は試料セル、3は光源、4は受光器、5
は縄洋棒、6は昇温用温度制御回路、7は加熱器、8は
温度計、9は微分回路、1川ま演算回路、11は降温用
温度制御回路、12は電磁弁、13はプリンターあるい
はディジタル表示器、14は総合制御回路を示す。 第1図
FIG. 1 is a schematic diagram showing an example of a control mechanism used in the method of the present invention. In the figure, 1 is a cell, 2 is a sample cell, 3 is a light source, 4 is a light receiver, and 5
6 is a temperature control circuit for increasing temperature, 7 is a heater, 8 is a thermometer, 9 is a differential circuit, 1 is a calculation circuit, 11 is a temperature control circuit for decreasing temperature, 12 is a solenoid valve, 13 is a A printer or digital display, 14 indicates a general control circuit. Figure 1

Claims (1)

【特許請求の範囲】 1 試料油とアニリンとの混合液の白濁度の温度変化を
透過光量の変化により検知してアニリン点を測定する方
法において、(イ)該混合液を昇温用温度制御回路を介
して加熱昇温せしめ、(ロ)該混合液の昇温速度が一定
範囲に達したときに微分回路を作動せしめてdI/dT
(ここでIは透過光量に対応する出力を示し、Tは混合
液の温度あるいは時間の出力を示す。 )を測定し、(ハ)前記dI/dTの値が零になつたと
きに昇温用温度制御回路による混合液の加熱を停止ある
いは低下させると共に、微分回路を停止しかつその際の
IをI_sとして演算回路に記憶せしめ、(ニ)次いで
前記混合液を昇温用温度制御回路を介して冷却すると共
に前記演算回路を作動せしめてΔI=I_s−Iを計算
し、(ホ)ΔIが所定値に達したときにその際の混合液
の温度を記録する。 ことを特徴とするアニリン点の測定方法。 2 測定したアニリン点が所定の誤差範囲内で一致する
まで(イ)〜(ホ)の操作を繰り返すことを特徴とする
特許請求の範囲第1項記載の方法。 3 混合液の昇温速度を毎分1〜2℃に調節する特許請
求の範囲第1項記載の方法。
[Scope of Claims] 1. A method for measuring the aniline point by detecting a temperature change in the white turbidity of a mixed liquid of a sample oil and aniline by a change in the amount of transmitted light, comprising: (a) temperature control for heating the mixed liquid; (b) When the temperature increase rate of the mixed liquid reaches a certain range, a differential circuit is activated to calculate dI/dT.
(Here, I indicates the output corresponding to the amount of transmitted light, and T indicates the temperature or time output of the mixed liquid.), and (c) the temperature is increased when the value of dI/dT becomes zero. At the same time as stopping or reducing the heating of the mixed liquid by the temperature control circuit for heating, the differential circuit is stopped and the I at that time is stored as I_s in the arithmetic circuit, and (d) the mixed liquid is then heated by the temperature control circuit for heating. and (e) when ΔI reaches a predetermined value, the temperature of the mixed liquid at that time is recorded. A method for measuring aniline points characterized by the following. 2. The method according to claim 1, characterized in that operations (a) to (e) are repeated until the measured aniline points match within a predetermined error range. 3. The method according to claim 1, wherein the rate of temperature increase of the liquid mixture is adjusted to 1 to 2°C per minute.
JP9741078A 1978-08-11 1978-08-11 How to measure aniline point Expired JPS6035024B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP9741078A JPS6035024B2 (en) 1978-08-11 1978-08-11 How to measure aniline point

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP9741078A JPS6035024B2 (en) 1978-08-11 1978-08-11 How to measure aniline point

Publications (2)

Publication Number Publication Date
JPS5524631A JPS5524631A (en) 1980-02-21
JPS6035024B2 true JPS6035024B2 (en) 1985-08-12

Family

ID=14191713

Family Applications (1)

Application Number Title Priority Date Filing Date
JP9741078A Expired JPS6035024B2 (en) 1978-08-11 1978-08-11 How to measure aniline point

Country Status (1)

Country Link
JP (1) JPS6035024B2 (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0614017B2 (en) * 1985-12-27 1994-02-23 大阪瓦斯株式会社 Method and apparatus for measuring softening point distribution of thermosoftening substance
US4804274A (en) * 1986-12-30 1989-02-14 Mobil Oil Corporation Method and apparatus for determining phase transition temperature using laser attenuation

Also Published As

Publication number Publication date
JPS5524631A (en) 1980-02-21

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