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JPH07109397B2 - Method for measuring iron content in soluble oil - Google Patents
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JPH07109397B2 - Method for measuring iron content in soluble oil - Google Patents

Method for measuring iron content in soluble oil

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Publication number
JPH07109397B2
JPH07109397B2 JP1278536A JP27853689A JPH07109397B2 JP H07109397 B2 JPH07109397 B2 JP H07109397B2 JP 1278536 A JP1278536 A JP 1278536A JP 27853689 A JP27853689 A JP 27853689A JP H07109397 B2 JPH07109397 B2 JP H07109397B2
Authority
JP
Japan
Prior art keywords
oil
iron
container
iron content
rolling
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
Application number
JP1278536A
Other languages
Japanese (ja)
Other versions
JPH03140837A (en
Inventor
健吾 妹尾
稔 川原田
勝二 面高
春男 小金森
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.)
Nippon Steel Corp
Original Assignee
Nippon Steel Corp
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 Nippon Steel Corp filed Critical Nippon Steel Corp
Priority to JP1278536A priority Critical patent/JPH07109397B2/en
Publication of JPH03140837A publication Critical patent/JPH03140837A/en
Publication of JPH07109397B2 publication Critical patent/JPH07109397B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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  • Metal Rolling (AREA)
  • Investigating Or Analyzing Materials By The Use Of Magnetic Means (AREA)

Description

【発明の詳細な説明】 産業上の利用分野 本発明は、ソルブン油中の鉄分測定方法に関するもので
ある。
Description: TECHNICAL FIELD The present invention relates to a method for measuring iron content in a solvent oil.

従来の技術 ソルブン油として例えば、鋼帯などの冷間圧延油は、圧
延機の圧延性を良好にするとともに、工程間における簡
易防錆機能を付与するものであり、圧延油中の鉄分含有
量の測定は、鋼帯等の清浄性及び疵防止の観点から、品
質保持に必須の管理項目である。
As a conventional oil, for example, cold rolling oil such as steel strip improves rolling property of a rolling mill and imparts a simple rust preventive function between processes. The measurement of is an essential control item for quality maintenance from the viewpoint of cleanliness of steel strips and prevention of flaws.

従って、圧延油中の鉄分を測定することが行なわれ、例
えば特開昭49-75197号のごとく、圧延油流中にブリッジ
回路の一辺からなる静電容量測定電極を浸漬し、高周波
の搬送波を印加し、圧延油中の金属粉が混在した場合の
静電容量の変化を電気信号にして鉄分を測定する方法が
開示されている。
Therefore, the iron content in the rolling oil is measured, and for example, as in JP-A-49-75197, a capacitance measuring electrode composed of one side of a bridge circuit is immersed in a rolling oil flow, and a high frequency carrier wave is applied. A method is disclosed in which the iron content is measured by applying a change in the capacitance when the metal powder in the rolling oil is mixed and using the change as an electric signal.

しかし、このような測定方法は、油中の鉄粉の粒径分布
が不均一なため誘電率変化が鉄粉量変化に対して一様で
ないことや、静電容量測定電極への鉄の油との化合物等
油劣化物の付着による静電容量の変化により測定精度が
悪いため、現場には不向きであることから一般的には、
フラスコに圧延油の一部を取り出して加熱灰化し、塩酸
などの鉱酸にて溶解したのち、一定量に水で希釈したの
ち、例えば原紙吸光分析計にて圧延油中の鉄分を測定し
ており、所要時間は約200分を必要とする。
However, in such a measurement method, the particle size distribution of the iron powder in the oil is non-uniform, so the change in the dielectric constant is not uniform with respect to the change in the amount of iron powder, and the oil content of the iron on the capacitance measuring electrode Since the measurement accuracy is poor due to the change in capacitance due to the adhesion of oil-degraded substances such as
Take out a part of the rolling oil into a flask, heat it to ash, dissolve it with mineral acid such as hydrochloric acid, and dilute it with water to a certain amount, and then measure the iron content in the rolling oil with a base paper absorption spectrometer, for example. It takes about 200 minutes.

しかし、鋼帯の連続冷間圧延においては、40tコイルの
場合で、圧延時間は平均10分位であり、圧延油の測定中
に40tコイルで20本(800t)もの圧延がなされることに
なり、例えば、圧延油中(循環使用)の鉄分濃度が上昇
し、所定の濃度以上になっていたときは、鋼帯の汚れ、
ロールの摩耗のほかにロールに鉄分が付着し、鋼帯に疵
が転写される等の不良コイルとなる等の大きな欠陥をと
もなうものである。
However, in continuous cold rolling of steel strip, the rolling time is about 10 minutes on average in the case of 40t coil, and as many as 20 (800t) are rolled with 40t coil during measurement of rolling oil. , For example, if the iron concentration in rolling oil (recycled) has risen above a certain level, the steel strip becomes dirty,
In addition to the abrasion of the roll, iron is attached to the roll, which causes a large defect such as a defective coil in which a flaw is transferred to the steel strip.

又鋼材等の切削加工においては、切削油の1部を切りだ
し、同様に油中の鉄分を測定するため、長時間を要し、
切削具(グラインダー等)の偏摩耗などによる処理材表
面の疵発生、切削面が平滑にならない等の欠点をともな
うものである。
Also, when cutting steel, etc., it takes a long time to cut out a part of the cutting oil and similarly measure the iron content in the oil.
This is accompanied by defects such as the occurrence of flaws on the surface of the treated material due to uneven wear of the cutting tool (grinder, etc.), and the cut surface is not smooth.

発明が解決しようとする課題 本発明は、このような従来技術の欠点を確実に解決する
ためになされたものでソルブン油中の鉄分の迅速・簡易
な測定方法を提供するものである。
DISCLOSURE OF THE INVENTION Problems to be Solved by the Invention The present invention has been made in order to surely solve the above-mentioned drawbacks of the prior art, and provides a quick and simple method for measuring iron content in a solvent oil.

課題を解決するための手段 本発明の特徴とするところは、含鉄ソルブル油を容器内
に気泡を混入しないように収納して秤量し、続いて磁石
を接近させ、油中の鉄分を重力とつりあうように容器上
部に移動せしめて磁力で保持して含鉄ソルブル油中の重
量減少量を計測することを特徴とする、ソルブル油中の
鉄分測定方法に関するものである。
Means for Solving the Problems A feature of the present invention is that iron-containing solvel oil is stored and weighed so as not to mix bubbles in a container, and subsequently a magnet is brought close to balance iron in oil with gravity. As described above, the present invention relates to a method for measuring an iron content in a soluble oil, which comprises moving the container to the upper portion of the container and holding it by magnetic force to measure the weight reduction amount in the iron-containing soluble oil.

即ち、本発明においては、例えば使用中(循環使用)の
ソルブル油の一部を取り出し、これを非磁性の容器内へ
収納後、天秤等にて秤量し、一定距離に磁石を容器の上
方又は横方向から近接し鉄粉をすべて容器上方に移動し
た状態(つまり無重力状態)とし、この重量変化を測定
するものであり、天秤、磁石共に市販されているもので
十分である。
That is, in the present invention, for example, a part of the soluble oil in use (recycled use) is taken out, stored in a non-magnetic container, and then weighed by a balance or the like, and the magnet is placed at a fixed distance above the container or The weight change is measured while the iron powder is moved close to the horizontal direction and all the iron powder is moved to the upper side of the container (that is, the weightless state), and both the balance and the magnet are commercially available.

磁石の強さおよび秤量の性能としては、鉄濃度が10ppm
以上のソルブル油30ccの場合では磁力は1000ガウス以
上、秤量の最少感度は1mg以上でよく、磁石は永久磁石
の他に電磁石で、秤量も天秤の他圧力センサー等の力セ
ンサーで、代替しても同様の効果が得られる。
As for the strength of the magnet and the weighing performance, the iron concentration is 10 ppm.
In the case of the above 30 cc of soluble oil, the magnetic force may be 1000 gauss or more, the minimum sensitivity of weighing may be 1 mg or more, the magnet may be an electromagnet in addition to the permanent magnet, and the weighing may be replaced by a force sensor such as a pressure sensor other than the balance. Also has the same effect.

このようにして鉄分を測定するソルブル油としては、鋼
帯の冷間圧延油、切削加工用の切削油、プレス加工用の
プレス油、加工離型用の離型油、エンジンオイル等の潤
滑油、加工成型用の成型油等の分散油、乳化型油等があ
る。
As the soluble oil for measuring the iron content in this way, cold rolling oil for steel strip, cutting oil for cutting, press oil for press working, release oil for mold release, lubricating oil such as engine oil, etc. , Dispersed oils such as molding oils for processing and molding, and emulsified oils.

またソルブル油を収納する容器としては、磁力を通す性
質(透磁性)を有する材質であればよく、例えば、非磁
性金属・合金(Al、オーステナイト系ステンレス等)、
ガラス、セラミック、プラスチック等がある。そして、
その容器の形状は、磁力線に対して容器の上方が垂直に
交わる形状が望ましく、例えば、秤量器に設定時の安定
性および磁力をかけた時の鉄粉の浮上性の点で直方体状
(各形)が好ましいが、専用の受け台を設ければ円柱状
の容器でもかまわない。尚、容器内面の親油性が高い
(例えば、内面の凹凸が大きい等)と、鉄粉付着油が容
器内壁に付着し、浮上が困難になるので、容器内面の親
油性は低い方が好ましい。含鉄ソルブル油を充満収納す
るには、気泡が混入しない方が好ましいので、気泡の混
入状況を監視するには、少なくとも容器の上方(例えば
容器上面、容器の側面上部等)が透明または半透明の素
材であることが望ましい。
The container for storing the solvel oil may be any material that has a property of transmitting magnetic force (magnetic permeability). For example, non-magnetic metal / alloy (Al, austenitic stainless steel, etc.),
There are glass, ceramics, plastics, etc. And
The shape of the container is preferably such that the upper part of the container intersects perpendicularly to the magnetic field lines, for example, in the shape of a rectangular parallelepiped (in each case) in terms of stability when the weighing machine is set and floatability of iron powder when a magnetic force is applied. The shape is preferable, but a cylindrical container may be used if a dedicated pedestal is provided. When the lipophilicity of the inner surface of the container is high (for example, the unevenness of the inner surface is large), the iron powder-adhering oil adheres to the inner wall of the container, making it difficult to float. Therefore, the lipophilicity of the inner surface of the container is preferably low. It is preferable that air bubbles are not mixed in to store iron-containing soluble oil. Therefore, at least the upper part of the container (for example, the upper surface of the container, the upper part of the side surface of the container, etc.) should be transparent or translucent to monitor the mixed condition of the air bubbles. It is desirable to be a material.

次に本発明の一例を図面により説明する。Next, an example of the present invention will be described with reference to the drawings.

第1図において、秤量器1にガラス製等の非磁性体によ
り構成した容器2内に含鉄ソルブル油3を充満収納(気
泡を混入しないように)し、これを秤量する。次いで磁
石4を接近して含鉄ソルブン油3中の鉄粉5を容器2上
部に磁力で移動せしめて磁力で保持することにより、鉄
粉5は無重力状態になり、このときの重量を秤量する。
In FIG. 1, iron-containing solvable oil 3 is stored in a container 2 made of a non-magnetic material such as glass in a weighing device 1 (to prevent bubbles from being mixed) and weighed. Next, the iron powder 5 in the iron-containing solvent oil 3 is moved to the upper part of the container 2 by magnetic force and held by the magnetic force by approaching the magnet 4, and the iron powder 5 becomes weightless, and the weight at this time is weighed.

しかして前記のごとく、容器2内に含鉄ソルブル油3を
充満収納後の秤量値と、上記のごとく、磁石4を接近し
て、容器2内の含鉄ソルブル油3中の鉄粉5が無重力状
態のときの秤量値の差が鉄粉5量となる。
Therefore, as described above, the weighed value after the iron-containing soluble oil 3 is filled in the container 2 and the magnet 4 as described above are brought close to each other, and the iron powder 5 in the iron-containing soluble oil 3 in the container 2 is in a weightless state. The difference between the weighed values at this time is the amount of iron powder 5.

実施例 次に本発明の実施例を比較例とともに挙げる。Examples Next, examples of the present invention will be given together with comparative examples.

実施例1 鋼帯の連続冷間圧延機で鋼帯圧延中の圧延油(循環使用
中の圧延油)を、容積100ml(外寸100×52×20mm)のキ
ャップ付きのガラス製容器に気泡を巻き込まないように
収納し、天秤で重量を測定し、次いで磁力1000ガウスの
板状永久磁石(100×100×30mm)を、上方20mmの距離に
固定したときの重量減から、鉄分濃度30ppmと測定し
た。所定時間は、圧延油収納、天秤へのセット等を加味
して15分であった。
Example 1 Using a continuous cold rolling mill for steel strips, rolling oil during rolling of steel strips (rolling oil in circulation use) was bubbled into a glass container with a cap having a volume of 100 ml (outer dimensions 100 × 52 × 20 mm). It was stored so that it would not get caught, the weight was measured with a balance, and then the iron concentration was measured as 30 ppm from the weight loss when a plate-shaped permanent magnet (100 x 100 x 30 mm) with a magnetic force of 1000 Gauss was fixed at a distance of 20 mm above. did. The predetermined time was 15 minutes in consideration of rolling oil storage, setting on a balance, and the like.

このときの圧延油を分析したところ鉱物油50%、合成エ
ステルと油脂40%、脂肪酸3%、乳化剤4%、酸化防止
剤1%、極圧剤2%であった。
When the rolling oil at this time was analyzed, it was found to be mineral oil 50%, synthetic ester and fat 40%, fatty acid 3%, emulsifier 4%, antioxidant 1%, extreme pressure agent 2%.

比較例1 実施例1と同条件の圧延油中の圧延油を100ml取り出し
(実施例1の分と併せ200ml抽出)容器に収納し、120℃
熱板上にて90分加熱し、水分を除去したのち、800℃電
気炉内にて30分加熱灰化し、30分室温にて冷却後、18%
HClを30ml添加し、20分間熱板上で加温溶解したのち冷
却し、100mlメスフラスコにメスアップし、原子吸光分
析法にて鉄分濃度30ppmと測定した。所要時間は圧延油
収納、加熱灰化、酸添加加温溶解、メスアップ、原子吸
光測定等を含め、214分と長時間を要した。
Comparative Example 1 100 ml of the rolling oil in the rolling oil under the same conditions as in Example 1 was taken out (combined with Example 1 and 200 ml was extracted) and stored in a container at 120 ° C.
After heating on a hot plate for 90 minutes to remove water, heat ash in an electric furnace at 800 ° C for 30 minutes, cool at room temperature for 30 minutes, and then cool to 18%.
After adding 30 ml of HCl, heating and dissolving on a hot plate for 20 minutes, the mixture was cooled, the volume was increased to a 100 ml measuring flask, and the concentration of iron was determined to be 30 ppm by atomic absorption spectrometry. The time required was 214 minutes, including rolling oil storage, heating ashing, acid addition heating dissolution, measuring up, and atomic absorption measurement.

このときの圧延油を分析したところ鉱物油50%、合成エ
ステルと油脂40%、脂肪酸3%、乳化剤4%、酸化防止
剤1%、極圧剤2%であった。
When the rolling oil at this time was analyzed, it was found to be mineral oil 50%, synthetic ester and fat 40%, fatty acid 3%, emulsifier 4%, antioxidant 1%, extreme pressure agent 2%.

実施例2 鋼材表面をグラインダーにて切削油を供給しつつ切削中
の切削油を、容積100ml(外寸100×52×20mm)のキャッ
プ付きのガラス製容器に気泡を巻き込まないように収納
し、非磁性体(ポリプロピレン製100×100×200mm)の
角柱を介して圧力センサーと連結された磁力2000ガウス
の磁石(100×100×50mm)の上方20mmの位置に固定した
ときの磁石に働く力の変化を圧力センサーにて計測し、
鉄分濃度50ppmと測定した。所要時間は、切削油収納、
測定位置へのセット等を加味し、14分であった。このと
きの切削油を分析したところ鉱物油80%、界面活性剤9
%、脂肪酸5%、アミン類4%、防菌防ばい剤2%であ
った。
Example 2 While supplying cutting oil to the surface of a steel material with a grinder, the cutting oil is stored in a glass container with a cap having a volume of 100 ml (outer dimension 100 × 52 × 20 mm) so as not to entrap air bubbles, The force that acts on the magnet when fixed at a position 20 mm above the magnet (100 × 100 × 50 mm) with a magnetic force of 2000 Gauss connected to the pressure sensor through the prism of a non-magnetic material (100 × 100 × 200 mm made of polypropylene). Measure the change with a pressure sensor,
The iron concentration was measured as 50 ppm. The time required is cutting oil storage,
It took 14 minutes, including the setting to the measurement position. When the cutting oil at this time was analyzed, mineral oil 80%, surfactant 9
%, Fatty acids 5%, amines 4%, antibacterial and antifungal agents 2%.

比較例2 実施例2と同条件で切削中の切削油を100ml取り出し
(実施例2の分と合わせ200ml抽出)容器へ収納し、120
℃熱板上にて90分加熱し、水分を除去したのち、800℃
電気炉内にて30分加熱灰化し、30分室温にて冷却後、20
%HClを30ml添加し、20分間熱板上で加温溶解したのち
冷却し、100mlメスフラスコにメスアップし、原子吸光
分析法にて鉄分濃度50ppmと測定し、所要時間は圧延油
収納、加熱灰化、酸添加加温溶解、メスアップ、原子吸
光測定等を含め、210分と長時間を要した。
Comparative Example 2 Under the same conditions as in Example 2, 100 ml of cutting oil during cutting was taken out (combined with the amount of Example 2 and extracted in 200 ml) and stored in a container, and
After heating on a hot plate for 90 minutes to remove water, 800 ℃
Heat ash in an electric furnace for 30 minutes, cool at room temperature for 30 minutes, then
Add 30 ml of% HCl, heat and dissolve on a hot plate for 20 minutes, cool, and make up to a 100 ml volumetric flask. Measure the iron concentration to be 50 ppm by atomic absorption spectrometry. It took a long time of 210 minutes, including ashing, acid addition heating dissolution, measuring up, and atomic absorption measurement.

このときの切削油を分析したところ鉱物油80%、界面活
性剤9%、脂肪酸5%、アミン類4%、防菌防ばい剤2
%であった。
Analyzing the cutting oil at this time, mineral oil 80%, surfactant 9%, fatty acid 5%, amines 4%, antibacterial and antibacterial agent 2
%Met.

発明の効果 本発明により、ソルブル油中の鉄分の測定が著しく短縮
でき、油中鉄分濃度増による処理材の品質の低下を防止
することができる。
EFFECTS OF THE INVENTION According to the present invention, the measurement of the iron content in the soluble oil can be significantly shortened, and the deterioration of the quality of the treated material due to the increase of the iron content in the oil can be prevented.

又、処理材の歩留を向上することができる。In addition, the yield of treated material can be improved.

更に圧延ロールの疵発生および摩耗によるロール組替を
延長でき、ロール原単位を向上することができる。
Further, roll reshuffling due to flaw generation and wear of the rolling roll can be extended, and the roll unit can be improved.

更にまたグラインダー等の切削機具の損耗を軽減し、コ
ストを低下するとともに、処理材の疵発生も低下させ品
質を向上させることができる等の効果が得られる。
Furthermore, it is possible to reduce wear of a cutting machine tool such as a grinder, reduce costs, and reduce defects in the treated material to improve quality.

【図面の簡単な説明】[Brief description of drawings]

第1図は、本発明の一例を示す説明図である。 1……秤量器、2……容器、3……ソルブル油、4……
磁石、5……鉄粉。
FIG. 1 is an explanatory diagram showing an example of the present invention. 1 ... Weighing machine, 2 ... Container, 3 ... Soluble oil, 4 ...
Magnet, 5 ... iron powder.

───────────────────────────────────────────────────── フロントページの続き (72)発明者 小金森 春男 愛知県東海市東海町5―3 新日本製鐵株 式會社名古屋製鐵所内 (56)参考文献 特開 昭49−50995(JP,A) ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Haruo Koganemori 5-3 Tokai-cho, Tokai City, Aichi Pref. Nippon Steel Co., Ltd. Inside the Nagoya Works (56) References JP-A-49-50995 (JP, A) )

Claims (1)

【特許請求の範囲】[Claims] 【請求項1】含鉄ソルブル油を容器内に気泡を混入しな
いように収納して秤量し、続いて磁石を接近させ、油中
の鉄分を重力とつりあうように容器上部に移動せしめて
磁力で保持して含鉄ソルブル油中の重量減少量を計測す
ることを特徴とする、ソルブル油中の鉄分測定方法。
1. An iron-containing solvel oil is stored and weighed in a container so as not to mix air bubbles, and then a magnet is brought close to the iron, and iron in the oil is moved to the upper part of the container so as to balance with gravity and retained by magnetic force. A method for measuring iron content in a soluble oil, comprising measuring the amount of weight loss in the iron-containing soluble oil.
JP1278536A 1989-10-27 1989-10-27 Method for measuring iron content in soluble oil Expired - Lifetime JPH07109397B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP1278536A JPH07109397B2 (en) 1989-10-27 1989-10-27 Method for measuring iron content in soluble oil

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP1278536A JPH07109397B2 (en) 1989-10-27 1989-10-27 Method for measuring iron content in soluble oil

Publications (2)

Publication Number Publication Date
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CN102305749A (en) * 2011-05-25 2012-01-04 山东大学 A Method for Rapid Determination of Fe3O4 Content in Minerals
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US3787761A (en) * 1972-05-15 1974-01-22 Gen Electric Method of detecting magnetic additives in nuclear fuel material by noting change in weight of material when weighed in a magnetic field

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