JPS63163154A - Analysis of metal ion type - Google Patents
Analysis of metal ion typeInfo
- Publication number
- JPS63163154A JPS63163154A JP31494486A JP31494486A JPS63163154A JP S63163154 A JPS63163154 A JP S63163154A JP 31494486 A JP31494486 A JP 31494486A JP 31494486 A JP31494486 A JP 31494486A JP S63163154 A JPS63163154 A JP S63163154A
- Authority
- JP
- Japan
- Prior art keywords
- concentration
- metal ion
- analysis
- density
- ions
- 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.)
- Pending
Links
- 229910021645 metal ion Inorganic materials 0.000 title claims abstract description 39
- 238000004458 analytical method Methods 0.000 title claims abstract description 32
- 150000002500 ions Chemical class 0.000 claims abstract description 24
- 238000007747 plating Methods 0.000 claims abstract description 15
- 239000011651 chromium Substances 0.000 claims abstract description 12
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 claims abstract description 11
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 6
- 230000002596 correlated effect Effects 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 abstract description 12
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 230000002226 simultaneous effect Effects 0.000 abstract 1
- 238000000034 method Methods 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004993 emission spectroscopy Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000007705 chemical test Methods 0.000 description 1
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 1
- 230000000875 corresponding effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
Landscapes
- Analysing Materials By The Use Of Radiation (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
Description
【発明の詳細な説明】
〈産業［二の利用分野〉
本発明は、クロムめっきまたはクロメート処理を行うに
際してのそわらの処理液中の金属イオン形態を分析する
方法に関する。DETAILED DESCRIPTION OF THE INVENTION <Industry [Second Field of Application] The present invention relates to a method for analyzing the form of metal ions in a treatment solution for chromium plating or chromate treatment.
〈先行核ｊ４ｔとその問題点〉
クロムめっきまたはクロメート処理を行うに際しては、
その処理液中の各構成金属イオンの濃度バランスか特に
重要視されていることから、処理液組成を直接測定して
、その測定値に基づいて、消費された金属イオンの星を
算出し、その補充を行なうことが・般に行われている。<Advanced nucleus j4t and its problems> When performing chromium plating or chromate treatment,
Since the concentration balance of each component metal ion in the processing solution is particularly important, the composition of the processing solution is directly measured, and based on the measured value, the star of consumed metal ions is calculated. Replenishment is a common practice.
近年、製品の高級化（合金化、多層化）に伴ない、例え
ばクロムめっきにおけるめっき液中の全成分を迅速に測
定する心霊性が高まり、多元素同時分析法である蛍光Ｘ
線分析法、または発光分光分析法を用いた分析装置が導
入され始めている。これらの多元素同時分析法は、瞬時
にしてめっき液中の全成分の濃度を測定できるという利
点があるが、その反面、［：、３４、Ｃｒ６＋などの金
属イオン形態の別が分析できず、Ｃ「の総量しか測定す
ることができないため、結局、トータル元素量管理しか
できないという欠点がある。In recent years, as products have become more sophisticated (alloyed, multi-layered), the spirituality of rapidly measuring all components in a plating solution in chrome plating, for example, has increased, and fluorescence
Analyzers using line analysis or emission spectrometry are beginning to be introduced. These multi-element simultaneous analysis methods have the advantage of being able to instantly measure the concentration of all components in the plating solution, but on the other hand, they cannot analyze the different forms of metal ions such as [:, 34, Cr6+, etc.]. Since only the total amount of C can be measured, there is a drawback that only the total amount of elements can be managed.
このような金属イオンの形態分析を行なうことはめっき
付着効率、めっき液の劣化判断等の管理面で１ｎ要であ
り、従来は吸光光度計、中和滴定などによって測定して
いた。しかし、これらの方法では、めっき液中の各金属
成分毎に分析するため同時分析を行うためには複数の装
置か必要であり、また測定に要する時間も測定成分の種
類に比例して長くなるいう欠点がある。Such morphological analysis of metal ions is necessary in terms of management such as plating adhesion efficiency and deterioration judgment of plating solution, and conventionally, measurements have been carried out using an absorptiometer, neutralization titration, or the like. However, these methods require multiple devices to perform simultaneous analysis because each metal component in the plating solution is analyzed, and the time required for measurement increases in proportion to the type of component to be measured. There is a drawback.
〈発明の目的〉
本発明の目的は、卜述した従来技術の欠点を解消し、多
元素同時分析法により処理液中の必要な各元素の濃度を
測定するとともに、金属イオン形態の分析をも可能とす
る金属イオン形態の分析法を提供することにある。<Objective of the Invention> The object of the present invention is to solve the above-mentioned drawbacks of the prior art, to measure the concentration of each necessary element in a processing liquid by a multi-element simultaneous analysis method, and to also analyze the form of metal ions. The purpose of this invention is to provide a method for analyzing metal ion forms that makes it possible.
〈発明の構成〉 このような目的は以下の本発明によって達成される。<Structure of the invention> These objects are achieved by the following invention.
即ち１本発明は、クロムめっきまたはクロメート処理時
に金属イオンの形態を分析するに際し、多元素同時分析
法により処理液中の必要な各元素濃度を測定するととも
に、
測定ずへき金属イオン形態と、この金属イオン形態と相
関のある元素の濃度との関係から求められる相関式をｒ
め計算機に入力し、
＋ｉｉｆ記元素の濃度の測定値を前記相関式に代入する
ことにより、前記金属イオン形態を演算して求めること
を特徴とする金属イオン形態の分析法を提供するもので
ある。That is, 1. When analyzing the form of metal ions during chromium plating or chromate treatment, the required concentration of each element in the treatment solution is measured by a simultaneous multi-element analysis method, and the form of the metal ions to be measured and this The correlation equation obtained from the relationship between the metal ion form and the concentration of the correlated element is expressed as r
The present invention provides an analysis method for a metal ion form, characterized in that the metal ion form is calculated and determined by inputting it into a calculator and substituting the measured value of the concentration of the +iif element into the correlation equation. .
以ド、本発明の金属イオン形態の分析法について詳細に
説明する。Hereinafter, the method for analyzing the metal ion form of the present invention will be explained in detail.
本発明は、次のような原理に基づくものである。The present invention is based on the following principle.
Ｊ、１本的には、クロムめっきにおけるめっき液または
クロメート処理液（以下これらを総称して「処理液」と
いう）を仕立てた時は、その処理液中のイオン形態は、
１種の状態、即ちＣｒ６＋の形で存在すると考えられる
。J. Basically, when a plating solution or chromate treatment solution (hereinafter collectively referred to as "treatment solution") for chrome plating is prepared, the ion form in the treatment solution is
It is believed to exist in one state, namely the form of Cr6+.
しかし、処理液が使用されるに従い、酸化逼元反応など
の品種反応が進み、その結果、イオンの形態が変化する
。ここで、電子という１つのｍに注１−１すれば、処理
液中の電子の総ｈ１には変化はなく、異種元素間開［で
電子のやりとりがあるだけである（他の元素の状態を変
えている）。そこで、本発明者らは、管理（測定）した
い金属イオンに対し、その形態を変化させる要因となっ
ている元素を見つけ、この元素の濃度を測定することに
より、前記管理したい金属イオンの濃度を間接的に知る
ことが可能であると考えられた。However, as the treatment liquid is used, various reactions such as oxidation and hydrogenation reactions progress, resulting in changes in the form of the ions. Here, if we note 1-1 to one m called electron, there is no change in the total h1 of electrons in the processing solution, there is only an exchange of electrons between different elements (states of other elements ). Therefore, the present inventors discovered the element that causes the shape of the metal ion to be controlled (measured), and by measuring the concentration of this element, the concentration of the metal ion to be controlled can be determined. It was thought that it was possible to know indirectly.
本発明は、クロムめっきまたはクロメート処理を行うに
際し、
１） 多元素同時分析法により処理液中の必要な各元素
濃度を測定しつつ、
２） 測定すべき金属イオン形態と、この金属イオン形
態と相関のある元素の濃度との関係をｒめ求め、
３） この関係を数式化して計算機に入力しておき、
４） この数式に、前記多元素同時分析法により測定し
た航記金属イオン形態と相関のある元素の濃度の測定値
を代入し、演算して、
５）測定すべき金属イオン形態を間接的に求めるｂので
ある。The present invention, when performing chromium plating or chromate treatment, 1) measures the necessary concentration of each element in the treatment solution using a multi-element simultaneous analysis method, and 2) determines the metal ion form to be measured and this metal ion form. 3) Convert this relationship into a mathematical formula and input it into a computer. 4) Incorporate the metal ion morphology measured by the multi-element simultaneous analysis method into this formula. By substituting the measured values of the concentrations of correlated elements and performing calculations, 5) indirectly determine the metal ion form to be measured.
多元素同時分析法には蛍光Ｘ線分析法、発光分光分析法
等がありこれらを実施する多元素同時分析装置には蛍光
Ｘ線分析装置、ＩＣＰ発光分光分析装置等がある。 本
発明の金属イオンの分析法を実施するための装置の好適
例を第１図に示す。Multi-element simultaneous analysis methods include fluorescent X-ray analysis, emission spectrometry, etc., and multi-element simultaneous analysis devices that carry out these methods include fluorescent X-ray analyzers, ICP emission spectrometers, and the like. A preferred example of an apparatus for carrying out the metal ion analysis method of the present invention is shown in FIG.
同図に示すように、処理槽ｌ内の処理液２をサンプリン
グして多元素同時分析装置３にて必要な各元素濃度を分
析する。これらの分析値は、データ処理が可能な計算機
４に随時入力される。As shown in the figure, the processing liquid 2 in the processing tank 1 is sampled and the necessary concentration of each element is analyzed by the multi-element simultaneous analysis device 3. These analytical values are inputted into the computer 4 capable of data processing at any time.
一方、計算機４には、測定しようとする金属イオン形態
（例えば（：ｒ３”）の濃度と、これと相関のある元素
Ｘ（例えばＦｅ）の濃度との相関式がｒめ入力されてい
る。On the other hand, a correlation equation between the concentration of a metal ion form to be measured (for example (:r3'')) and the concentration of an element X (for example Fe) having a correlation therewith is input into the computer 4.
１】１算機４内では、前記多元素同時分析装置３により
分析された各元素の濃度のうち元素Ｘの濃度に関するデ
ータを相関式に代入し、演算して、測定しようとする１
？η記金属イオン形態の濃度を求める。1) In the calculator 4, data regarding the concentration of element
? Determine the concentration of the metal ion form η.
処理液２の管理として、求めた金属イオン形態の濃度と
、その適正濃度とを比較し、その差を求め、これに相当
する量を処理槽ｌ内へ補充するという作業をリアルタイ
ムに行うことも可能である。To manage the processing solution 2, it is possible to compare the obtained concentration of the metal ion form with its appropriate concentration, find the difference, and replenish the corresponding amount into the processing tank 1 in real time. It is possible.
なお、本発明法においては、不溶性陽極、可溶性陽極の
いずれを用いてもよいが、不溶性陽極を用いて処理する
のが好ましい。In the method of the present invention, either an insoluble anode or a soluble anode may be used, but it is preferable to use an insoluble anode.
以下、金属イオン形態の求め方について、クロメート処
理液中のＣｒ３＋とＣｒ叶の金属イオン形態分析を行う
場合を例にとって説明する。Hereinafter, how to obtain the metal ion form will be explained by taking as an example a case where metal ion form analysis of Cr3+ and Cr leaf in the chromate treatment solution is performed.
Ｃｒ３＋は、Ｆ記式（１）に示す還元反応によって生成
すると考えられる。Cr3+ is considered to be generated by the reduction reaction shown in F-formula (1).
Ｃｒ’ｉ” ＋ ３ａ−−＋ Ｃｒ” ・
・・−（１）また、処理液中ではト記反応に対して他の
元素の酸化反応が行なわれていると考えられる。そこで
、クロム酸３０ｇ／Ｉｔ、硫酸０．：ｌ ｇｉｎなる組
成の処理液について調査した結果、下記式（２）に示す
鉄の酸化反応がＬ記りロムの還元反応に対応しているこ
とが判明した。即ち、処理液中のＦｅ３＋濃度と（、ｒ
”十濃度との間には、第２図のグラフに示す関係がある
。Cr'i" + 3a--+ Cr"・
...-(1) Furthermore, in addition to the above reaction, it is thought that oxidation reactions of other elements are taking place in the treatment liquid. Therefore, chromic acid 30g/It, sulfuric acid 0. As a result of investigating a treatment liquid having a composition of :l gin, it was found that the oxidation reaction of iron shown in the following formula (2) corresponds to the reduction reaction of ROM (L). That is, the Fe3+ concentration in the treatment solution and (, r
``There is a relationship between the concentration and the concentration shown in the graph in Figure 2.
ＦＱ → １・ｅ３” ＋ ３ｃｍ
−・・・ （２）なお、多
元素同時分析法では、トータル元素量（Ｔ・Ｆｃｆｉ度
）しか測定することができないので。FQ → 1・e3” + 3cm
-... (2) Note that in the multi-element simultaneous analysis method, only the total element content (T/Fcfi degree) can be measured.
処理液中におけるＦｅ３＋濃度とＴ−Ｆｅ濃度の関係を
調べた。The relationship between Fe3+ concentration and T-Fe concentration in the treatment solution was investigated.
その結果を第３図のグラフに示す。同図に示すようにＦ
ｅ３＋濃度とＴ−Ｆｅ１度とは直線的な関係を示してお
り、このＴ−Ｆｅｆｉ度を知ることによってｐｃ３＋４
度を知り、このＦｅ３＋濃度から第２図に示す関係にＪ
、（づいてＧｃ３＋濃度を推定することができる。The results are shown in the graph of FIG. As shown in the figure, F
There is a linear relationship between e3+ concentration and T-Fe1 degree, and by knowing this T-Fefi degree, pc3+4
From this Fe3+ concentration, the relationship shown in Figure 2 can be drawn from J
, (The Gc3+ concentration can then be estimated.
第２図および第３図の関係からＣｒ３＋の濃度ｙは下記
式（３）によって！ｊえられる。From the relationship shown in Figures 2 and 3, the concentration y of Cr3+ is determined by the following formula (3)! I can get it.
ｙ ＝ −７，８９ｘ２ ＋ ４．９３ｘ ＋
０．１６ ・・・・軸 （３）ｙ：Ｃｒ３
＋の濃度（ｇ／ＩＬ）
ｘ： Ｔ−ＦＣの濃度 （ｇ／Ｊり
このようにしてＣｒ３＋の濃度が求まれば、下記式（４
）より（Ｈｒ（ｉ＋の濃度も求まる。y = -7,89x2 + 4.93x +
0.16 ...Axis (3) y: Cr3
+ concentration (g/IL) x: T-FC concentration (g/J) If the concentration of Cr3+ is found in this way, the following formula
), the concentration of (Hr(i+) can also be found.
Ｏｒ’十濃度＝’ｒ−Ｃｒ濃度−ｃｒ３＋ｎ度 ・−
・−（４）なお、 Ｔ−Ｃｒ濃度は、多元素同時分析法
によりＴ−Ｆｅｆｉ度と同時に求めることができる。Or'10 concentration='r-Cr concentration-cr3+n degrees ・-
-(4) Note that the T-Cr concentration can be determined simultaneously with the T-Fefi degree by a multi-element simultaneous analysis method.
ト述したようにしてクロメート処理液中のＣ「３＋濃度
および（：ｒ６＋濃度を分析することができる。The C'3+ concentration and (:r6+ concentration) in the chromate treatment solution can be analyzed as described above.
また、ト述した本発明法による金属イオン形態（Ｃｒ３
＋とに、Ｉｉ＋）の分析結果の正確さを確めるために、
同 クロメート処理液について化学試験分析を行い、そ
の分析値と本発明法による分析イハの比較を行った。そ
の結果を下記表１に示す。In addition, the metal ion form (Cr3
In order to confirm the accuracy of the analysis results of Ii+),
A chemical test analysis was conducted on the same chromate treatment solution, and the analytical values were compared with the analysis results obtained by the method of the present invention. The results are shown in Table 1 below.
表 １
Ｌ記表１に示すように、本発明法による分析値は、その
積度が極めて高いことがわかる。Table 1 L As shown in Table 1, it can be seen that the analysis values obtained by the method of the present invention have an extremely high degree of integration.
〈発明の効果〉
本発明の金属イオンＪｆ３ ！！３の分析法によれば、
多元素同時分析法により処理液中の必要な谷元素濃度を
分析するとともに、従来の多元素同時分析法では不可能
であった金属イオン形態の分析をも可能とし、これによ
り弔−の分析装置にて金属イオン形態をも含めた処理液
中の全成分（または必要な全成分）を瞬時にして分析す
ることができるようになった。<Effect of the invention> Metal ion Jf3 of the present invention! ! According to the analysis method of 3.
The multi-element simultaneous analysis method not only analyzes the necessary concentration of elements in the processing liquid, but also enables the analysis of metal ion forms, which was impossible with the conventional multi-element simultaneous analysis method. It has become possible to instantly analyze all components (or all necessary components) in the processing solution, including metal ion forms.
その結果、処理液劣化の判断が容易に可能となり、また
処理液が適正濃度から外れた場合の補充すべき金属イオ
ン形態の川を正確かつ即時に求め、これを補充して、均
一なりロムめっきまたクロメート処理（付着けの安定性
等）を図ることができる等、処理液の管理を高精度で行
うことができる。As a result, it becomes possible to easily judge whether the processing solution has deteriorated, and when the processing solution deviates from the appropriate concentration, it is possible to accurately and immediately determine the river of metal ion forms that should be replenished, and to replenish it to achieve uniform ROM plating. In addition, it is possible to perform chromate treatment (stability of adhesion, etc.), and to manage the treatment liquid with high precision.
第１図は、本発明の金属イオンの分析法を実施するため
の装置の好適例を示す説明図である。
第２図は、処理液中のＦｃ３＋濃度とＣｒｓ＋の関係を
示すグラフである。
第３図は、処理液中のＦｅ３＋濃度とＴ・Ｐｃの濃度の
関係を示すグラフである。
符号の説明
！・・・処理槽、２・・・処理液、
３・・・多元素同時分析装置、４・・・計算機ＦＩＧ、
３
Ｔ−Ｆｅ濠窪（９／ｌ）FIG. 1 is an explanatory diagram showing a preferred example of an apparatus for carrying out the metal ion analysis method of the present invention. FIG. 2 is a graph showing the relationship between the Fc3+ concentration in the treatment liquid and Crs+. FIG. 3 is a graph showing the relationship between the Fe3+ concentration and the T.Pc concentration in the treatment liquid. Explanation of symbols! ... Processing tank, 2... Processing liquid, 3... Multi-element simultaneous analysis device, 4... Computer FIG,
3 T-Fe Horikubo (9/l)
Claims (1)
ンの形態を分析するに際し、 多元素同時分析法により処理液中の必要な各元素濃度を
測定するとともに、 測定すべき金属イオン形態と、この金属イオン形態と相
関のある元素の濃度との関係から求められる相関式を予
め計算機に入力し、 前記元素の濃度の測定値を前記相関式に代入することに
より、前記金属イオン形態を演算して求めることを特徴
とする金属イオン形態の分析法。(1) When analyzing the form of metal ions during chromium plating or chromate treatment, the required concentration of each element in the treatment solution is measured using a multi-element simultaneous analysis method, and the form of the metal ion to be measured and the form of this metal ion are determined. The metal ion form can be calculated by inputting in advance into a computer a correlation equation obtained from the relationship between the concentration of the element and the concentration of the element that is correlated with Analysis method for characteristic metal ion forms.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP31494486A JPS63163154A (en) | 1986-12-25 | 1986-12-25 | Analysis of metal ion type |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP31494486A JPS63163154A (en) | 1986-12-25 | 1986-12-25 | Analysis of metal ion type |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63163154A true JPS63163154A (en) | 1988-07-06 |
Family
ID=18059531
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP31494486A Pending JPS63163154A (en) | 1986-12-25 | 1986-12-25 | Analysis of metal ion type |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63163154A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003057184A (en) * | 2001-08-10 | 2003-02-26 | Toyota Motor Corp | Method for quantitative determining of hexavalent chromium |
| JP2007139754A (en) * | 2005-10-19 | 2007-06-07 | Rigaku Industrial Co | Fluorescence x-ray spectrometer, and program used therefor |
-
1986
- 1986-12-25 JP JP31494486A patent/JPS63163154A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003057184A (en) * | 2001-08-10 | 2003-02-26 | Toyota Motor Corp | Method for quantitative determining of hexavalent chromium |
| JP2007139754A (en) * | 2005-10-19 | 2007-06-07 | Rigaku Industrial Co | Fluorescence x-ray spectrometer, and program used therefor |
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