JP2009079902A - Quantitative analysis method of nickel or nickel alloy plating layer - Google Patents
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本発明は、銅または黄銅からなる基材に、ニッケルまたはニッケル合金からなるめっき層（以下、「ニッケルめっき層」ともいう）を形成してなる試料における前記めっき層を定量分析する方法に関する。 The present invention relates to a method for quantitatively analyzing the plating layer in a sample formed by forming a plating layer made of nickel or a nickel alloy (hereinafter also referred to as “nickel plating layer”) on a base material made of copper or brass.
電気機器や電子機器の電極や端子として銅や黄銅が広く使用されており、耐食性の向上や、接触抵抗の低減、挿入力の低減等の目的でニッケルめっき層で被覆されることが多い。しかし、ニッケルめっき層には、鉛やカドミウム、水銀、クロム等の環境負荷物質が混入していることがあり、それらの含有量を定量する必要がある。 Copper and brass are widely used as electrodes and terminals of electrical and electronic devices, and are often coated with a nickel plating layer for the purpose of improving corrosion resistance, reducing contact resistance, and reducing insertion force. However, environmental impact substances such as lead, cadmium, mercury, and chromium may be mixed in the nickel plating layer, and it is necessary to quantify their contents.
ニッケルめっき層の定量分析方法としては、簡便であることから、試料をめっき剥離液に浸漬してニッケルめっき層を溶解し、溶解分を含有するめっき剥離液について定量することが主流になっている（例えば、非特許文献１及び非特許文献２参照）。 As a quantitative analysis method for the nickel plating layer, since it is simple, the sample is immersed in the plating stripper to dissolve the nickel plating layer, and the plating stripper containing the dissolved component is quantified. (For example, refer nonpatent literature 1 and nonpatent literature 2).
めっき剥離液は、めっき層だけを選択的に溶解する必要がある。しかし、非特許文献１及び非特許文献２に記載の定量方法では、めっき剥離液に硝酸や塩酸等の酸や混酸を用いるため、基材が銅や黄銅、鉄系材料である場合、これらを溶解する。従って、基材側にも測定対象の金属成分が含まれていると、その分を定量値から差し引く必要があるが、測定精度を高めるためにめっき層の溶解量を多くしようとすると、基材の溶解量も多くなるため、測定対象の金属成分が基材側に多く含まれていると、めっき層における測定対象の金属成分の定量値がマイナスになることがあり、定量できない。 The plating stripping solution needs to selectively dissolve only the plating layer. However, in the quantitative methods described in Non-Patent Document 1 and Non-Patent Document 2, since an acid or mixed acid such as nitric acid or hydrochloric acid is used for the plating stripper, when the base material is copper, brass, or an iron-based material, these are used. Dissolve. Therefore, if the metal component to be measured is also included on the substrate side, it is necessary to subtract that amount from the quantitative value. However, if the dissolution amount of the plating layer is increased in order to increase the measurement accuracy, the substrate Therefore, if a large amount of the metal component to be measured is contained on the substrate side, the quantitative value of the metal component to be measured in the plating layer may be negative and cannot be quantified.
このような不具合を防ぐために、金属イオンを含有するめっき剥離液も知られている。例えば、鉄イオンを含有するめっき剥離液が知られているが、定量下限値が高く、分析結果を示すスペクトルが良好ではない。また、クロムイオンを含有するめっき剥離液も知られているが、クロムの定量はできず、またＰｂ：２２０．３５３ｎｍに干渉があるため鉛の測定にも不適である。 In order to prevent such problems, plating stripping solutions containing metal ions are also known. For example, although a plating stripper containing iron ions is known, the lower limit of quantification is high, and the spectrum indicating the analysis result is not good. Also, a plating stripping solution containing chromium ions is known, but chromium cannot be quantified, and Pb: 220.353 nm interferes with it, which is not suitable for lead measurement.
このように、従来のめっき剥離液は銅系材料を溶解しやすく、銅や黄銅を基材とするニッケルめっき層には不適である。 Thus, the conventional plating stripper easily dissolves the copper-based material and is not suitable for a nickel plating layer based on copper or brass.
また、非特許文献１に記載の定量方法では、規格化半定量値を得ているため、データの精度は湿式分解によるＩＣＰ−ＡＥＳ法及びＩＣＰ−ＭＳ法との比較が必要であり、操作が複雑になる。 Further, in the quantification method described in Non-Patent Document 1, since a normalized semi-quantitative value is obtained, the accuracy of the data needs to be compared with the ICP-AES method and ICP-MS method by wet decomposition, and the operation is It becomes complicated.
そこで本発明は、銅や黄銅からなる基材にニッケルめっき層を形成した試料について、ニッケルめっき層をより正確に定量する方法を提供することを目的とする。 Then, this invention aims at providing the method of quantifying a nickel plating layer more correctly about the sample which formed the nickel plating layer in the base material which consists of copper or brass.
上記課題を解決するために、本発明は下記に示す定量分析方法を提供する。
（１） 銅または黄銅からなる基材に、ニッケルまたはニッケル合金からなるめっき層を形成してなる試料、もしくは金属製の基材に、銅または黄銅からなる下地層を介して、ニッケルまたはニッケル合金からなるめっき層を形成してなる試料における前記めっき層の定量分析方法であって、
硫酸を１３〜１４質量％、硝酸を９〜１０質量％、リン酸を０．５〜９質量％及び酢酸を５〜７質量％の割合で含む水溶液からなるめっき剥離液を前記試料に接触させて前記めっき層を溶解し、溶解分を含有する前記めっき剥離液について定量することを特徴とするニッケルまたはニッケル合金めっき層の定量分析方法。
（２）前記試料が電極または端子であることを特徴とする上記（１）記載のニッケルまたはニッケル合金めっき層の定量分析方法。
In order to solve the above problems, the present invention provides the following quantitative analysis method.
(1) A sample formed by forming a plating layer made of nickel or nickel alloy on a base material made of copper or brass, or nickel or nickel alloy on a metal base material through an underlayer made of copper or brass A method for quantitative analysis of the plating layer in a sample formed by forming a plating layer comprising:
A plating stripping solution comprising an aqueous solution containing 13 to 14% by mass of sulfuric acid, 9 to 10% by mass of nitric acid, 0.5 to 9% by mass of phosphoric acid and 5 to 7% by mass of acetic acid is brought into contact with the sample. A method for quantitative analysis of a nickel or nickel alloy plating layer, wherein the plating layer is dissolved, and the plating stripping solution containing the dissolved content is quantified.
(2) The method for quantitative analysis of a nickel or nickel alloy plating layer according to (1), wherein the sample is an electrode or a terminal.
本発明で用いる特定組成のめっき剥離剤は、実質的にニッケルめっき層のみを選択的に溶解することができるため、該めっき層の定量を正確に行なうことができる。 Since the plating stripper having a specific composition used in the present invention can substantially selectively dissolve only the nickel plating layer, the plating layer can be accurately quantified.
以下、本発明に関して詳細に説明する、 Hereinafter, the present invention will be described in detail.
本発明の定量方法は、基本的には従来と同様に、ニッケルめっき層が形成された試料をめっき剥離液に浸漬してニッケルめっき層を溶解し、溶解分を含有するめっき剥離液を定量するが、その際、下記に示す特定組成のめっき剥離液を用いる。 The quantification method of the present invention basically immerses a sample with a nickel plating layer in a plating stripper to dissolve the nickel plating layer and quantifies the plating stripper containing the dissolved component, as in the conventional method. However, at that time, a plating stripping solution having a specific composition shown below is used.
めっき剥離液は、 硫酸を１３〜１４質量％、硝酸を９〜１０質量％、リン酸を０．５〜９質量％及び酢酸を５〜７質量％の割合で含む水溶液からなる。また、必要に応じて、分散剤を０．１〜２質量％配合してもよい。 The plating stripper comprises an aqueous solution containing 13 to 14% by mass of sulfuric acid, 9 to 10% by mass of nitric acid, 0.5 to 9% by mass of phosphoric acid, and 5 to 7% by mass of acetic acid. Moreover, you may mix | blend a 0.1-2 mass% dispersing agent as needed.
測定精度を高めるためにはニッケルめっき層の溶出量が多いほど好ましいため、めっき剥離液との接触は、基材が露出するまで行なう。液温は３５〜４５℃が好ましい。尚、基材の露出は、目視により十分可能である。 In order to increase the measurement accuracy, the larger the amount of elution of the nickel plating layer, the better. Therefore, contact with the plating stripper is performed until the substrate is exposed. The liquid temperature is preferably 35 to 45 ° C. It should be noted that the substrate can be sufficiently exposed by visual observation.
そして、ニッケルめっき層の溶解分を含有するめっき剥離液について、定量分析を行なう。定量分析は、簡便で、高精度の定量ができる等の理由から、ＩＣＰ−ＡＥＳ（誘導結合プラズマ発光分光分析法）を行なうことが好ましい。本発明では、特にニッケルめっき層中の環境負荷物質である鉛、カドミウム、クロムの定量を目的とするが、ＩＣＰ−ＡＥＳによりこれらを高精度で測定することができる。 And the quantitative analysis is performed about the plating stripper containing the melt | dissolution content of a nickel plating layer. Quantitative analysis is preferably performed by ICP-AES (inductively coupled plasma emission spectroscopy) for reasons such as simple and highly accurate quantification. The purpose of the present invention is to determine lead, cadmium, and chromium, which are environmentally hazardous substances, in the nickel plating layer, and these can be measured with high accuracy by ICP-AES.
本発明で用いる上記のめっき剥離液は、銅、並びに黄銅成分である亜鉛を、測定に影響を与えるレベルまで溶解せず、実質的にニッケルめっき層のみを溶解する。従って、測定値をそのままニッケルめっき層における含有量と見做して問題ない。しかし、後述する実施例１のように、銅や亜鉛の測定値を試料量から差し引いて新たな試料量とし、鉛やカドミウム、クロム等の各成分の含有量を補正することでより、高精度の定量ができる。 The plating stripping solution used in the present invention does not dissolve copper and zinc, which is a brass component, to a level that affects measurement, but substantially dissolves only the nickel plating layer. Therefore, there is no problem when the measured value is regarded as the content in the nickel plating layer as it is. However, as in Example 1 to be described later, the measured value of copper or zinc is subtracted from the sample amount to obtain a new sample amount, and by correcting the content of each component such as lead, cadmium, chromium, etc., high accuracy Can be quantified.
また、同じく環境負荷物質である水銀を定量する場合には、ＣＶ−ＡＡＳ（冷蒸気還元気化原子吸光法）を行なうことが好ましい。 Similarly, when quantifying mercury, which is an environmentally hazardous substance, it is preferable to perform CV-AAS (cold vapor reduction vaporization atomic absorption spectrometry).
尚、本発明で用いるめっき剥離液は銅及び黄銅を溶解しないため、試料は、銅や黄銅からなる基材にニッケルめっき層が形成されたものの他に、銅や黄銅以外の金属製基材で、銅や黄銅を下地層としてその上にニッケルめっき層を形成したものであってもよい。このような試料として、電極や端子類が挙げられる。 In addition, since the plating stripper used in the present invention does not dissolve copper and brass, the sample is made of a metal substrate other than copper or brass, in addition to a substrate made of copper or brass with a nickel plating layer formed. Alternatively, a nickel plating layer may be formed thereon using copper or brass as a base layer. Examples of such a sample include electrodes and terminals.
（実施例１〜２）
メルテックス株式会社製めっき剥離液「メルストリップＮ−９５０Ａ」（硫酸１６質量％、硝酸１１質量％、リン酸１〜１０質量％、残部水）５００ｍＬ、メルテックス株式会社製めっき剥離液「メルストリップＮ−９５０Ｂ」（酢酸３０〜４０質量％、分散剤１〜１０質量％、残部水）１００ｍＬ、３５％過酸化水素水１００ｍＬ及び超純水３００ｍＬを混合してめっき剥離液を調製した。
(Examples 1-2)
Plating stripper "Melstrip N-950A" manufactured by Meltex Co., Ltd. (500% sulfuric acid, 11% by weight nitric acid, 1-10% by weight phosphoric acid, remaining water) 500 mL, Plating stripper manufactured by Meltex Co., Ltd. N-950B "(acetic acid 30 to 40% by mass, dispersant 1 to 10% by mass, remaining water) 100 mL, 35% hydrogen peroxide solution 100 mL and ultrapure water 300 mL were mixed to prepare a plating stripping solution.
また、高純度ニッケルに、鉛３０ｐｐｍ、カドミウム５ｐｐｍ、クロム５ｐｐｍ、水銀１ｐｐｍとなるように添加してめっき液を調製し、黄銅製基材に銅下地めっきを施した後、無電解めっき法によりニッケルめっき層を形成して試験片とした。 In addition, a plating solution is prepared by adding high purity nickel to 30 ppm lead, 5 ppm cadmium, 5 ppm chromium, and 1 ppm mercury. A plating layer was formed to obtain a test piece.
そして、試験片を、４０℃に維持した上記のめっき剥離液に浸漬し、黄銅製基材が露出した時点で試験片を取り出し、浸漬前との重量差からニッケルめっき層の溶解量を求めた。次いで、めっき剥離液におけるニッケルめっき層の溶解量が０．１ｇ／２５ｍＬ（実施例１）または０．０５ｇ／２５ｍＬ（実施例２）となるように水で調整し、試料とした。 And the test piece was immersed in said plating peeling liquid maintained at 40 degreeC, the test piece was taken out when the base material made from brass was exposed, and the dissolution amount of the nickel plating layer was calculated | required from the weight difference with before immersion. . Next, the sample was adjusted with water so that the dissolution amount of the nickel plating layer in the plating stripper was 0.1 g / 25 mL (Example 1) or 0.05 g / 25 mL (Example 2).
次いで、各試料について、ＩＣＰ−ＡＥＳにより鉛、カドミウム及びクロムの含有量を、またＣＶ−ＡＡＳにより水銀の含有量をそれぞれ定量した。結果を表１に示す。 Subsequently, about each sample, content of lead, cadmium, and chromium was quantified by ICP-AES, and mercury content was quantified by CV-AAS, respectively. The results are shown in Table 1.
（比較例１）
硝酸と塩酸との混合液に実施例と同一の試験片を浸漬してニッケルめっき層を溶解し、ニッケルめっき層の溶解量が０．０５ｇ／２５ｍＬとなるように水で調整して試料を得た。そして、試料について、ＩＣＰ−ＡＥＳにより鉛、カドミウム及びクロムの含有量を、またＣＶ−ＡＡＳにより水銀の含有量をそれぞれ定量した。結果を表１に示す。
(Comparative Example 1)
The same test piece as in the example is immersed in a mixed solution of nitric acid and hydrochloric acid to dissolve the nickel plating layer, and the sample is obtained by adjusting with water so that the dissolution amount of the nickel plating layer is 0.05 g / 25 mL. It was. And about the sample, content of lead, cadmium, and chromium was quantified by ICP-AES, and content of mercury was quantified by CV-AAS, respectively. The results are shown in Table 1.
表１に示すように、本発明に従うめっき剥離液を用いた実施例１及び実施例２の測定結果は、硫酸と硝酸との混合液を用いた比較例１に比べて、試験片のニッケルめっき層の組成との相関が高くなっている。このことから、本発明によれば、黄銅製基材にニッケルめっき層を形成した試験片に対し、基材の溶解を抑え、ニッケルめっき層を高精度で定量できることがわかる。 As shown in Table 1, the measurement results of Example 1 and Example 2 using the plating stripper according to the present invention were compared to Comparative Example 1 using a mixed solution of sulfuric acid and nitric acid, and the nickel plating of the test piece The correlation with the composition of the layer is high. From this, it can be seen that according to the present invention, the dissolution of the base material can be suppressed and the nickel plating layer can be quantified with high accuracy with respect to the test piece in which the nickel plating layer is formed on the brass base material.
Claims (2)
硫酸を１３〜１４質量％、硝酸を９〜１０質量％、リン酸を０．５〜９質量％及び酢酸を５〜７質量％の割合で含む水溶液からなるめっき剥離液を前記試料に接触させて前記めっき層を溶解し、溶解分を含有する前記めっき剥離液について定量することを特徴とするニッケルまたはニッケル合金めっき層の定量分析方法。 Sample made by forming a plating layer made of nickel or nickel alloy on a base material made of copper or brass, or plating made of nickel or nickel alloy on a metal base material through an underlayer made of copper or brass A method for quantitative analysis of the plating layer in a sample formed by forming a layer,
A plating stripping solution comprising an aqueous solution containing 13 to 14% by mass of sulfuric acid, 9 to 10% by mass of nitric acid, 0.5 to 9% by mass of phosphoric acid and 5 to 7% by mass of acetic acid is brought into contact with the sample. A method for quantitative analysis of a nickel or nickel alloy plating layer, wherein the plating layer is dissolved, and the plating stripping solution containing the dissolved content is quantified.
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| JP2009162727A (en) * | 2008-01-10 | 2009-07-23 | Yazaki Corp | Method for analyzing poisonous metal in silver-plated layer |
| JP2010256214A (en) * | 2009-04-27 | 2010-11-11 | Yazaki Corp | Recovery method and analysis method of gold-containing plating layer |
| KR101873242B1 (en) * | 2016-10-17 | 2018-07-04 | 주식회사 필머티리얼즈 | METHOD FOR ANALYZING COMPONENT RATIO OF ELECTROFORMED Fe-Ni ALLOY FILM |
| KR20200054550A (en) * | 2018-11-12 | 2020-05-20 | 주식회사 포스코 | Liquefaction reagent composition for plating layer of nickel plated steel sheet, and analyzing method of plating layer of nickel plated steel sheet using thereof |
| CN112323107A (en) * | 2020-09-16 | 2021-02-05 | 歌尔科技有限公司 | Brass material with nano rare earth nickel coating and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009162727A (en) * | 2008-01-10 | 2009-07-23 | Yazaki Corp | Method for analyzing poisonous metal in silver-plated layer |
| JP2010256214A (en) * | 2009-04-27 | 2010-11-11 | Yazaki Corp | Recovery method and analysis method of gold-containing plating layer |
| KR101873242B1 (en) * | 2016-10-17 | 2018-07-04 | 주식회사 필머티리얼즈 | METHOD FOR ANALYZING COMPONENT RATIO OF ELECTROFORMED Fe-Ni ALLOY FILM |
| KR20200054550A (en) * | 2018-11-12 | 2020-05-20 | 주식회사 포스코 | Liquefaction reagent composition for plating layer of nickel plated steel sheet, and analyzing method of plating layer of nickel plated steel sheet using thereof |
| KR102218457B1 (en) | 2018-11-12 | 2021-02-19 | 주식회사 포스코 | Liquefaction reagent composition for plating layer of nickel plated steel sheet, and analyzing method of plating layer of nickel plated steel sheet using thereof |
| CN112323107A (en) * | 2020-09-16 | 2021-02-05 | 歌尔科技有限公司 | Brass material with nano rare earth nickel coating and preparation method thereof |
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