JP3482760B2 - How to measure plating weight - Google Patents
How to measure plating weightInfo
- Publication number
- JP3482760B2 JP3482760B2 JP07773596A JP7773596A JP3482760B2 JP 3482760 B2 JP3482760 B2 JP 3482760B2 JP 07773596 A JP07773596 A JP 07773596A JP 7773596 A JP7773596 A JP 7773596A JP 3482760 B2 JP3482760 B2 JP 3482760B2
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- Prior art keywords
- time
- potential
- amount
- curve
- plating
- Prior art date
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- Investigating And Analyzing Materials By Characteristic Methods (AREA)
- Electroplating Methods And Accessories (AREA)
Description
【発明の詳細な説明】
【０００１】
【発明の属する技術分野】本発明は、めっき付着量の測
定方法に関し、詳しくは電解剥離法によってぶりき板等
のめっき付着量を求める際に測定した電位−時間曲線の
変曲点位置を従来法より正確に判定する技術に係わる。
【０００２】
【従来の技術】高品質のめっき鋼板を製造するには、そ
のめっき付着量を正確に測定してめっき条件を調整し、
常に適正なめっき厚みになるよう管理する必要がある。
そのためには、めっき付着量を迅速、且つ正確に測定す
ることが必要で、従来より種々のめっき付着量測定方法
が知られている。例えば、ぶりき板の錫付着量やティン
フリー鋼板の金属クロム付着量に対しては、ＪＩＳ−Ｇ
−３３０３（付属書１）及びＪＩＳ−Ｇ−３３１５（付
属書１）で規定されている所謂電解剥離法、蛍光Ｘ線法
と称する試験方法がよく利用される。
【０００３】このうち、電解剥離法は、電解槽中に炭素
棒電極（陰極）、試験片保持器及び銀製の照合電極を取
付け、該試験片を陽極として所定の電解液中で定電流電
解を行うものである。そして、電解中に試験片の電位を
電位差計で連続的に記録紙に描いて電位−時間曲線（ｖ
−ｔ曲線）を求め、その曲線からある特定電位値までに
流れた電気量が算出され、ファラデーの法則によって付
着量に換算される。
【０００４】ところで、上記電解剥離法で、電位−時間
曲線より具体的にめっき付着量を求めるに際しては、電
解が進行し試料の溶解が錫層（クロム層）等のめっき層
から地鉄に移る時に該電位−時間曲線１に図４に示すよ
うな変曲点Ａが出現するので、その変曲点Ａを利用す
る。つまり、該変曲点Ａを上記の「ある特定電位」と
し、電解開始からその点までの間に通じた電流量を用い
て付着量を算出するのが一般的である（通称、変曲点法
という）。しかし、試料がぶりき板の場合には、この変
曲点Ａが明確に現れないことが多いので、該変曲点Ａを
人が判断するには問題があった。そこで、図４に示すよ
うに、電位−時間曲線１の変曲点Ａと思われる位置に仮
に接線ｄ1 を引き、また該曲線１の電位が一定になった
部分に水平線ｄ2 を引き、該接線ｄ1 と水平線ｄ2 との
交点Ｂまでの時間ｔ1 内に流した電流量に基づき付着量
を求める方法が提案され、多用されるようになった（以
後’接線法’と呼ぶ）。
【０００５】
【発明が解決しようとする課題】しかしながら、この接
線法を用いても、電位−時間曲線を描いた記録紙から手
作業で上記接線ｄ1 を引く場合、作業者によって接線ｄ
1 が異なり、測定データの信頼性に欠けるという問題が
あった。さらに、この接線法を人手によらず機器で自動
的に行う方法もあり、その方法で接線ｄ1 及び水平線ｄ
2 を引くと、地鉄側の水平線ｄ2 が無数に現れ、特定困
難となる別の問題がある。これは、一定電位の部分は各
瞬間での傾きの変化が小さいので、どこで一定になった
か機器で明確に判断できないからである。これを精度よ
く行なうとすると、電圧の極微小な変化をキャッチする
必要があり、現状の機器ではほとんど実行不可能であ
る。
【０００６】そこで、本発明は、かかる事情を鑑み、電
解剥離法のうち所謂「接線法」でめっき付着量を求める
に際し、電位−時間曲線１上に引いた接線ｄ1 と該曲線
の一定電位部分に引いた水平線ｄ2 と交点Ｂの位置を人
手を介さずに容易、かつ迅速に定めるようにしためっき
付着量の測定方法を提供することを目的としている。
【０００７】
【課題を解決するための手段】本発明者は、上記目的を
達成するために、電位−時間曲線を時間で２回微分した
電位変化速度の加速度が極小値を有することに着眼し、
それを利用すれば一義的に上記交点が定まると考え、本
発明を創案した。すなわち、本発明は、めっき板から採
取した試験片を電解液中で定電流電解して電位の経時変
化を測定し、ある特定電位に対応する時間を電解開始か
ら試験片付着物の剥離に要した時間と定め、その時間に
至るまでに流れた電流値にファラデーの法則を適用して
該試験片のめっき付着量を算出する方法において、上記
測定した電位値を時間に関し２回微分し、その微分値
（Ｅ”）が極小となる時間の前後のＥ”＝０となる２点
の中点を上記のある特定電位に対応する時間とすること
を特徴とするめっき付着量の測定方法である。
【０００８】
【発明の実施の形態】本発明では、めっき板から採取し
た試験片を陽極として電解液中で定電流電解して電位の
経時変化を測定し、ある特定電位に対応する時間を電解
開始から試験片付着物の剥離に要した時間と定め、その
時間に至るまでに流れた電流値にファラデーの法則を適
用して該試験片のめっき付着量を算出する方法におい
て、上記測定した電位値を時間に関し２回微分し、その
微分値が極小となる時間の前後のＥ”＝０となる２点の
中点を上記のある特定電位に対応する時間とするように
したので、それは、電位変化の加速度が極小になる時間
となる。つまり、前記電位−時間曲線上に引いた接線と
一定電位の部分に引いた水平線の交点Ｂの位置に相当
し、該位置が容易に、しかも正確且つ一義的に求められ
るようになる。また、電位−時間曲線を記録しなくて
も、測定した電位値と時間とをコンピュータの自動ロジ
ックに組み込めば、従来の接線法と同等の値が迅速かつ
容易に得られるようになる。
【０００９】なお、具体的な微分値は、電位−時間曲線
上において、微小時間（秒）を仮定し、その時間内で変
化する電位値の差をその時間で除して１回目の値とし、
２回目の微分値は、上記で得た電位変化速度−時間曲線
において同様の演算を行なうことによって求められる。
以下、実施例において、図１〜３に基づき本発明の内容
を説明する。
【００１０】
【実施例】図３は、Ｆｅ素地上に目標量２．８０ｇ／ｍ
2 としてＳｎめっきを施したぶりき板で得た電位−時間
曲線を示している。該曲線を得るに際しては、まず、上
記ぶりき板から大きさ９０ｍｍφの試験片を採取して陽
極とした。そして、電解液に１規定塩酸水溶液を、陰極
に炭素棒を用いて、電圧５ｍＶ、電流２５０ｍＡの定電
流電解を行った。その結果が、上記図３の電位−時間曲
線１である。
【００１１】次に、この電位−時間曲線を用いて、前記
（１）変曲点法（変極点はａ）、（２）接線法（交点は
ｂ）及び（３）本発明に係る２回微分法（中点ｃ）によ
り、それぞれの場合に対応するめっき付着量を求めた。
その際、各ケースについての電解時間と電流値とから、
前記ＪＩＳ規定に記載された下記式で付着量を換算し
た。
すずめっき量、ｇ／ｍ2 ＝０．６１５５７×（１／Ｓ）×Ｆ×Ｄ ・・・（Ａ）
ここで、Ｓは試験片の面積（ｍｍ2 ）、Ｄは電解開始か
ら各交点（ａ，ｂ）や上記中点（ｃ）までの時間（ｓｅ
ｃ）、Ｆはその間の電流値（ｍＡ）である。
【００１２】従って、変曲点法によるめっき付着量は、
図３のａまでの時間ｔa を上記（Ａ）式に代入、接線法
による値は、同じく図３のｂまでの時間ｔb を代入する
ことで得られる。一方、本発明に係る２回微分法での値
は、以下のようにして求める。まず、図３の電位−時間
曲線１を時間で１回微分した電位変化速度−時間曲線２
を得る。その結果を図２に示す。引続いて、この図２の
電位変化速度をさらに時間で微分し、電位変化加速度
（Ｅ”）−時間曲線３を得る。その結果を図１に示す。
【００１３】図１は、Ｅ”が極小値を示す点（ｂ）の前
後において、Ｅ”＝０に対応する点は、ａとｄである。
従って、本発明では、このａとｄの中点ｃを前記「ある
特定電位に対応する時間ｔc とし、めっき付着量はこの
ｔc を前記（Ａ）式に代入することで求める。ところ
で、図１〜図３より、ａ点とｂ点は明らかに異なる時間
であるが、ｂ点とｃ点間にはほとんど時間の違いが見ら
れないことがわかる。そこで、本発明法で求めた付着量
が妥当なものであるかどうかを判断するため、試験片数
ｎ＝１０で電解試験を行い、上記３つの方法についての
有意差検定を行った。
【００１４】その結果は、表１及び表２に一括して示す
が、（１）の変曲点法と（２）の接線法との間では、ｔ
0 ＝−２．４２７７（≧ｔ0 （９，００５）＝２．２
６）となり、両者間に有意差が認められた。つまり、両
者で異なった付着量が得られた。
【００１５】
【表１】
【００１６】
【表２】
【００１７】一方、本発明に係る（３）の２回微分法で
は、上記（２）の接線法と比較してｔ0 ＝０．３０７８
（≦ｔ0 （９．００５）＝２．２６）と有意差は認めら
れなかった（危険率５％）。つまり、本発明に係る２回
微分法で求めためっき付着量は、（２）の接線法で求め
たものと差がないことが確認できた。（２）の接線法に
は、接線が作業者や自動機械によって一致しないという
欠点があるが、本発明に係る２回微分法には、ある特定
電位に対応する時間が一義的に定まり、コンピュータを
利用すれば、簡単で、しかも迅速にめっき付着量が測定
できるという利点がある。従って、従来の接線法を利用
するよりも、本発明に係る２回微分法が優れていること
が明らかである。
【００１８】
【発明の効果】以上述べたように、本発明では電解剥離
法において電位−時間曲線を時間で２回微分し、その極
小値前後のＥ”＝０の２点の交点までの時間で付着量を
算出するようにしたので、接線法と等価な付着量が迅速
に得られるようになった。また、人手を介さない自動測
定時でも測定点が明確となり、容易にめっき付着量が求
められるようになった。Description: BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for measuring the amount of plating applied, and more particularly, to a potential measured when the amount of plating applied to a tinplate or the like is determined by an electrolytic peeling method. The present invention relates to a technique for determining the inflection point position of the time curve more accurately than the conventional method. 2. Description of the Related Art In order to manufacture a high-quality plated steel sheet, the plating amount is accurately measured and the plating conditions are adjusted.
It is necessary to control the plating thickness to be always appropriate.
For this purpose, it is necessary to measure the coating weight quickly and accurately, and various methods for measuring the coating weight are conventionally known. For example, for the tin adhesion amount of tinplate and the metal chromium adhesion amount of tin-free steel plate, JIS-G
A so-called electrolytic stripping method and a test method called a fluorescent X-ray method defined in -3303 (Appendix 1) and JIS-G-3315 (Appendix 1) are often used. In the electrolytic stripping method, a carbon rod electrode (cathode), a test piece holder and a silver reference electrode are mounted in an electrolytic cell, and a constant current electrolysis is performed in a predetermined electrolytic solution using the test piece as an anode. Is what you do. During the electrolysis, the potential of the test piece was continuously drawn on a recording paper with a potentiometer, and a potential-time curve (v
−t curve), the amount of electricity flowing from the curve to a specific potential value is calculated, and is converted into the amount of adhesion according to Faraday's law. When the amount of plating is specifically determined from the potential-time curve by the electrolytic stripping method, the electrolysis proceeds and the dissolution of the sample shifts from a plating layer such as a tin layer (chromium layer) to ground iron. Since the inflection point A as shown in FIG. 4 sometimes appears in the potential-time curve 1, the inflection point A is used. That is, it is general that the inflection point A is set to the “certain specific potential” described above, and the amount of adhesion is calculated using the amount of current passed from the start of electrolysis to that point (commonly called the inflection point). Law). However, when the sample is a tinplate, the inflection point A often does not clearly appear, so that there is a problem in that the inflection point A is judged by a person. Therefore, as shown in FIG. 4, the potential - if a tangent is drawn to d 1 to the position that seems an inflection point A time curve 1, also draw a horizontal line d 2 in the portion where the potential of the curve 1 becomes constant, method for determining the adhesion amount based on the amount of current supplied to the time t 1 to an intersection B between該接line d 1 and the horizontal line d 2 have been proposed and come to be frequently used (hereinafter referred to as 'tangent method') . However, even if this tangent method is used, when the tangent d 1 is manually drawn from the recording paper on which the potential-time curve is drawn, the tangent d 1
1 was different, and there was a problem that the reliability of the measurement data was lacking. Furthermore, there is also a method of automatically performing by the device regardless of the tangent method to manually tangential d 1 and the horizontal line d in that way
Subtracting 2, countless appear horizon d 2 of the base steel side, there is another problem that a specific difficult. This is because the constant potential portion has a small change in the slope at each moment, so that it is not possible for the device to clearly determine where the potential has become constant. If this is performed with high accuracy, it is necessary to catch a minute change in the voltage, which is almost impossible with current equipment. In view of the above circumstances, the present invention considers the tangent d 1 drawn on the potential-time curve 1 and the constant potential of the curve when determining the amount of plating by the so-called “tangential method” of the electrolytic stripping method. and its object is to provide a coating weight measurement method to facilitate the position of the horizon d 2 and the intersection B drawn in the portion without human intervention, and quickly determined. In order to achieve the above object, the present inventors have focused on the fact that the acceleration of the potential change rate obtained by differentiating the potential-time curve twice with respect to time has a minimum value. ,
The inventor of the present invention devised that the intersection would be uniquely determined by using this. That is, according to the present invention, a test piece collected from a plating plate is subjected to constant current electrolysis in an electrolytic solution to measure a change with time in potential, and a time corresponding to a specific potential is required for peeling off a test substance deposit from the start of electrolysis. In the method of calculating the coating weight of the test piece by applying Faraday's law to the current value flowing up to that time, the measured potential value is differentiated twice with respect to time. A method for measuring a plating adhesion amount, wherein a middle point between two points where E "= 0 before and after a time when a differential value (E") becomes a minimum is a time corresponding to the above-mentioned specific potential. . DETAILED DESCRIPTION OF THE INVENTION In the present invention, a test piece taken from a plating plate is used as an anode to conduct a constant current electrolysis in an electrolytic solution to measure a change with time of the potential, and a time corresponding to a certain specific potential is measured. In the method of calculating the amount of plating applied to the test piece by applying the Faraday's law to the value of the current flowing up to that time and determining the time required for peeling off the attached matter from the start, The value is differentiated twice with respect to time, and the midpoint between the two points where E ″ = 0 before and after the time when the differential value is minimized is set as the time corresponding to the above specific potential. This is the time when the acceleration of the potential change becomes minimal, that is, it corresponds to the position of the intersection B of the tangent drawn on the potential-time curve and the horizontal line drawn at the constant potential, and the position is easily and accurately determined. And to be uniquely requested Further, even if the potential-time curve is not recorded, if the measured potential value and time are incorporated into an automatic logic of a computer, a value equivalent to the conventional tangent method can be obtained quickly and easily. As a specific differential value, a minute time (second) is assumed on a potential-time curve, and a difference between potential values changing within that time is divided by the time to obtain a first value. ,
The second differential value is obtained by performing the same calculation on the potential change speed-time curve obtained above.
Hereinafter, the contents of the present invention will be described with reference to FIGS. FIG. 3 shows a target amount of 2.80 g / m2 on an Fe substrate.
2 shows a potential-time curve obtained with a tinplate subjected to Sn plating. In obtaining the curve, first, a test piece having a size of 90 mmφ was sampled from the tinplate and used as an anode. Then, using a 1N aqueous hydrochloric acid solution as an electrolytic solution and a carbon rod as a cathode, constant current electrolysis was performed at a voltage of 5 mV and a current of 250 mA. The result is the potential-time curve 1 in FIG. Next, using this potential-time curve, the above-mentioned (1) inflection point method (inflection point is a), (2) tangent method (intersection point is b), and The plating amount corresponding to each case was determined by the differential method (middle point c).
At that time, from the electrolysis time and current value for each case,
The adhesion amount was calculated by the following equation described in the JIS regulations. Tin plating amount, g / m 2 = 0.61557 × (1 / S) × F × D (A) where S is the area (mm 2 ) of the test piece, and D is each intersection point from the start of electrolysis. a, b) and the time (se
c) and F are current values (mA) between them. Therefore, the coating weight by the inflection point method is
Substituting time t a to a of FIG. 3 in the above formula (A), the value by the tangent method can be obtained by similarly substituting the time t b until b in FIG. On the other hand, the value obtained by the second differentiation method according to the present invention is obtained as follows. First, the potential change time-time curve 2 obtained by differentiating the potential-time curve 1 of FIG.
Get. The result is shown in FIG. Subsequently, the potential change speed in FIG. 2 is further differentiated with respect to time to obtain a potential change acceleration (E ″)-time curve 3. The result is shown in FIG. Before and after the point (b) indicating the minimum value, points corresponding to E ″ = 0 are a and d.
Accordingly, in the present invention, the said middle point c of a and d and time t c corresponding to "a particular potential, coating weight is obtained by substituting the t c in the formula (A). By the way, 1 to 3, it can be seen that point a and point b are clearly different times, but there is almost no difference in time between point b and point c. In order to judge whether the amount is appropriate or not, an electrolysis test was performed with the number of test pieces n = 10, and a significance test was performed for the above three methods. 2, the difference between the inflection point method of (1) and the tangent method of (2) is t
0 = −2.4277 (≧ t 0 (9,005) = 2.2
6), and a significant difference was observed between the two. That is, different adhesion amounts were obtained in both cases. [Table 1] [Table 2] On the other hand, in the second differentiation method of (3) according to the present invention, t 0 = 0.3078 compared with the tangent method of (2).
(≦ t 0 (9.005) = 2.26) and no significant difference was found (risk rate 5%). That is, it was confirmed that the plating adhesion amount obtained by the second differentiation method according to the present invention did not differ from that obtained by the tangent method of (2). The tangent method of (2) has a drawback that the tangents do not coincide with each other by an operator or an automatic machine. However, in the twice differentiation method according to the present invention, the time corresponding to a specific potential is uniquely determined, and The advantage of using is that the amount of plating can be measured simply and quickly. Therefore, it is clear that the twice differentiation method according to the present invention is superior to using the conventional tangent method. As described above, in the present invention, the potential-time curve is differentiated twice with respect to time in the electrolytic stripping method, and the time until the intersection of two points of E ″ = 0 before and after the minimum value is obtained. Calculates the amount of coating by using the method described above, so that the amount of coating equivalent to the tangential method can be obtained quickly. It has become required.
【図面の簡単な説明】
【図１】図２の曲線をさらに時間で微分して得られた電
位変化の加速度に関する曲線を示す図である。
【図２】図３の曲線を時間で微分して得られた電位変化
速度の曲線を示す図である。
【図３】ぶりき板試料で実測した電位−時間曲線であ
る。
【図４】ＪＩＳに従った変曲点法、接線法による電位−
時間曲線の測定結果を示す図である。
【符号の説明】
１ 電位−時間曲線
２ 電位変化速度−時間曲線
３ 電位変化加速度−時間曲線BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a diagram showing a curve relating to acceleration of a potential change obtained by further differentiating the curve of FIG. 2 with time. FIG. 2 is a diagram showing a curve of a potential change speed obtained by differentiating the curve of FIG. 3 with time. FIG. 3 is a potential-time curve measured on a tinplate sample. FIG. 4 shows potentials obtained by the inflection point method and the tangent method according to JIS.
It is a figure showing the measurement result of a time curve. [Description of Signs] 1 potential-time curve 2 potential change speed-time curve 3 potential change acceleration-time curve
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 平５−332991（ＪＰ，Ａ) 特開 昭51−6614（ＪＰ，Ａ) 特開 昭49−46791（ＪＰ，Ａ) 特開 平８−94553（ＪＰ，Ａ) 特公 昭50−21148（ＪＰ，Ｂ１) (58)調査した分野(Int.Cl.7，ＤＢ名) G01N 27/42 C23C 2/00 - 2/40 ──────────────────────────────────────────────────続 き Continuation of the front page (56) References JP-A-5-332991 (JP, A) JP-A-51-6614 (JP, A) JP-A-49-46791 (JP, A) JP-A 8- 94553 (JP, A) JP 50-21148 (JP, B1) (58) Fields investigated (Int. Cl. 7 , DB name) G01N 27/42 C23C 2/00-2/40
Claims (1)
で定電流電解して、電位の経時変化を測定し、ある特定
電位に対応する時間を電解開始から試験片付着物の剥離
に要した時間とし、その当該時間までに流れた電流値に
ファラデーの法則を適用して該試験片のめっき付着量を
算出する方法において、 上記測定した電位値（Ｅ）を時間（ｔ）に関し２回微分
し、その微分値（Ｅ”）が極小となる時間の前後のＥ”
＝０となる２点の中点を上記のある特定電位に対応する
時間とすることを特徴とするめっき付着量の測定方法。(57) [Claims] [Claim 1] A test piece collected from a plating plate is subjected to constant current electrolysis in an electrolytic solution, a change with time of the potential is measured, and electrolysis is started for a time corresponding to a specific potential. A time required for the specimen to adhere to the test piece, and applying the Faraday's law to the current flowing up to that time to calculate the amount of plating applied to the test piece. ) Is differentiated twice with respect to time (t), and E ″ before and after the time when the differential value (E ″) is minimal.
A method for measuring the amount of plating applied, wherein a midpoint between two points where = 0 is a time corresponding to the above-mentioned specific potential.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP07773596A JP3482760B2 (en) | 1996-03-29 | 1996-03-29 | How to measure plating weight |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP07773596A JP3482760B2 (en) | 1996-03-29 | 1996-03-29 | How to measure plating weight |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH09264875A JPH09264875A (en) | 1997-10-07 |
| JP3482760B2 true JP3482760B2 (en) | 2004-01-06 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP07773596A Expired - Fee Related JP3482760B2 (en) | 1996-03-29 | 1996-03-29 | How to measure plating weight |
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| Country | Link |
|---|---|
| JP (1) | JP3482760B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1271406C (en) * | 2001-11-20 | 2006-08-23 | 爱科来株式会社 | Fail judging method in analysis and treatment and analyzer |
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1996
- 1996-03-29 JP JP07773596A patent/JP3482760B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH09264875A (en) | 1997-10-07 |
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