JPS5848854A - Analysis for rhodium phase of planted film of rhodium- ruthenium alloy - Google Patents
Analysis for rhodium phase of planted film of rhodium- ruthenium alloyInfo
- Publication number
- JPS5848854A JPS5848854A JP56147260A JP14726081A JPS5848854A JP S5848854 A JPS5848854 A JP S5848854A JP 56147260 A JP56147260 A JP 56147260A JP 14726081 A JP14726081 A JP 14726081A JP S5848854 A JPS5848854 A JP S5848854A
- Authority
- JP
- Japan
- Prior art keywords
- rhodium
- ruthenium alloy
- phase
- alloy plating
- plated film
- 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
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/20—Metals
- G01N33/205—Metals in liquid state, e.g. molten metals
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/20—Metals
- G01N33/202—Constituents thereof
- G01N33/2028—Metallic constituents
Abstract
Description
【発明の詳細な説明】
この発明は、ロジウム−ルテニウム合金めっき皮膜のロ
ジウム相分析方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for analyzing the rhodium phase of a rhodium-ruthenium alloy plating film.
ロジウム−ルテニウム合金めっき皮膜は、光沢のある白
色の優雅な色調と汚ｎにくい表面が得らするため、工業
用にも装飾用にも用いら牡ているが、王水にはもちろん
、逆圧水にも溶解しにくいため、従来、ロジウム相の分
析は困難であシ、わずかに、硫酸水素カリウム“または
、硫酸水素ナトリウムとともに、約７００℃で加熱溶融
後、水溶液として、原子吸光分析法によシ、ロジウム濃
度を求める方法が知らｔていた。Rhodium-ruthenium alloy plating has an elegant glossy white color and a stain-resistant surface, so it is used for both industrial and decorative purposes. Conventionally, it has been difficult to analyze the rhodium phase because it is difficult to dissolve in water, and after heating and melting it at about 700°C with potassium hydrogen sulfate or sodium hydrogen sulfate, it is analyzed as an aqueous solution by atomic absorption spectrometry. Yes, I knew how to determine the rhodium concentration.
しかしながら、この方法は、ロジウム−ルテニウム合金
めっき皮膜を細粉状にしなけｎばならず、また、細粉状
にしても、完全にカロ熱溶融することは難かしく、加え
て、加熱溶融後の水溶液に多量の硫酸イオンが存在する
ため、原子吸光分析時の干渉が大きくなり、正確なロジ
ウム相の分析ができにくいという欠点を有していた。However, in this method, the rhodium-ruthenium alloy plating film must be made into a fine powder, and even if it is made into a fine powder, it is difficult to completely melt the rhodium-ruthenium alloy plating film. The presence of a large amount of sulfate ions in the aqueous solution increases interference during atomic absorption spectrometry, making it difficult to accurately analyze the rhodium phase.
この発明は、上記の欠点を改良するためになされたもの
であシ、ロジウム−ルテニウム合金メっき皮膜の正確な
ロジウム相分析方法の提供を目的としｔものである。This invention was made to improve the above-mentioned drawbacks, and its purpose is to provide an accurate method for analyzing the rhodium phase of a rhodium-ruthenium alloy plating film.
この発明の特徴は、ロジウム−ルテニウム合金めっき皮
膜を、ニッケルるつぼ中で過酸化ナトリウムまたは、過
酸化カリウムとともに、加熱溶融することにある。この
方法を用いると、ロジウム−ルテニウム合金めっき皮膜
を、細粉状にすることなく完全に加熱溶融することがで
き、しかも、原子吸光分析時の干渉となるナトリウム、
カリウ ムの影響は、同時バックグラウンド補正をする
ことにより増り除かれるため正確なロジウム濃度の測定
が可能である。The feature of this invention is that a rhodium-ruthenium alloy plating film is heated and melted together with sodium peroxide or potassium peroxide in a nickel crucible. Using this method, it is possible to completely heat and melt the rhodium-ruthenium alloy plating film without turning it into fine powder, and it is possible to completely heat and melt the rhodium-ruthenium alloy plating film without turning it into fine powder.
Accurate rhodium concentration measurements are possible because the effect of potassium is increased or eliminated by simultaneous background correction.
以下、この発明の実施例について述べる。Examples of the present invention will be described below.
実施例１
０ジウム（硫酸ロジウムとして）５ｙ／ｌ、、スルファ
ミンＨ２０ｙ ／ ｔ ％ ＩＡ ｅマグネシウム２０
．９ ／′ｔ１ルテニウム〔塩化ルテニウムとして〕０
゜５１１／ｌのロジウム−ルテニウム合金めっき液を建
浴した後、浴温ｆ、５０℃とし、電流密度１゜３Ａ／
ｔｌｍ” テ９０ 分間、ステンレス板（５０ｍｍ Ｘ
２５濶１日）にめっきを施した。このロジウム−ルテ
ニウム合金めっき皮膜を剥離し、その０゜２１１程度を
天秤で正確にはかり取り、ニッケルるつほに入ｎ１過酸
化ナトリウム３ｇとともに、約８００℃で加分間、加熱
溶融した。室温まで冷却後、溶融物ｋ ２００ ｍＡの
メスフラスコに移し変え、さらに）ニッケルるつは中の
残留物ヲ、１０％の塩酸で洗浄ｇ、２００ ｍｌのメス
フラスコにカｌえ、１０％ノ塩酸でメスフラスコを定容
とした。この水溶液中のロジウム症度ｆ ３４３ ｎ
ｒｎの波長で、同時バックグラウンド補正を行いながら
、標章添加法を用いた原子吸光法で測定し、測定結果を
得た。この測定結果と、最初にはかシ取つ；′？：、ロ
ジウムールテニウム合金めっき皮膜の重量からロジウム
相は、５９．２％と算出さ詐た。一方、めっき浴中のロ
ジウム濃度の減少量を、同様に原子吸光法で測定したと
ころ、ロジウムの減少量と、上記析出量は、一致した。Example 1 0dium (as rhodium sulfate) 5y/l, Sulfamine H20y/t% IA e Magnesium 20
．． 9 /'t1 Ruthenium [as Ruthenium chloride] 0
After preparing a rhodium-ruthenium alloy plating solution of ゜511/l, the bath temperature was set to f and 50°C, and the current density was set to 1゜3A/l.
tlm" for 90 minutes on a stainless steel plate (50mm
Plating was applied after 25 hours and 1 day). This rhodium-ruthenium alloy plating film was peeled off, and approximately 0°211 of it was accurately weighed with a balance, and heated and melted at about 800° C. with 3 g of n1 sodium peroxide in a nickel melting box. After cooling to room temperature, the melt was transferred to a 200 mA volumetric flask, and the residue inside the nickel melt was washed with 10% hydrochloric acid. The volumetric flask was brought to volume with hydrochloric acid. Rhodium disease degree f 343 n in this aqueous solution
The measurement results were obtained by measuring by atomic absorption spectrometry using the mark addition method at a wavelength of rn while performing simultaneous background correction. With this measurement result, first take a candle ;'? : The rhodium phase was calculated to be 59.2% from the weight of the rhodium ruthenium alloy plating film. On the other hand, when the amount of decrease in rhodium concentration in the plating bath was similarly measured by atomic absorption spectrometry, the amount of decrease in rhodium and the amount of precipitation coincided with each other.
実施例２
０ジウム（硫酸ロジウムとして）５１１／ｌ、ス／Ｉ／
７ アミンｆｔ ２０１ ／ １％ （ｉｉｔｔ酸マ
グネシウム２０１／／１１ルテニウム（塩化ルテニウム
として）２ｙ／ｌのロジウム−ルテニウム合金めっき液
を建浴した後、浴温を５０℃とし、電流密度１．３Ａ／
ｄｍ”で１２０分間、ステンレス板（５０ｍ Ｘ ２５
ｍＸ１ｍｍ）にめっきを施した。このロジウム−ルテ
ニウム合金めつき皮膜を剥離し、その０．２＃程度を天
秤で正確にはかり取シ、ニッケルるつぼに入れ、過酸化
ナトリウム３１１とともに、約８００℃で（資）分間、
加熱溶融した。室温まで冷却後、溶融物を２００ ｍｌ
のメスフラスコに移し変え、さらに、ニッケルるつぼ中
の残留物’ｔ、ｉｏ％の塩酸で洗浄後、２００ｔｎＬの
メスフラスコに力１え、１０％の塩酸でメスフラスコ會
定容とした。この水溶液中のロジウム濃度’１３４３ｚ
ｔｒＬの波長で、同時バックグラウンド補正を行いなが
ら、標準添加法を用いた原子吸光法で測定し、測定結果
を得た。この測定結果と、最初にはかシ取ったロジウム
−ルテニウム合金めっき皮膜の重量からロジウム相は、
４９゜０％と算出され友。一方、めっき浴中のロジウム
濃度の減少量を、同様に原子吸光法で測定したところ、
ロジウムの減少量と、上記析出量は、一致した。Example 2 0dium (as rhodium sulfate) 511/l, Su/I/
After preparing a rhodium-ruthenium alloy plating solution containing 7 amine ft 201/1% (magnesium iitt acid 201//11 ruthenium (as ruthenium chloride) 2y/l, the bath temperature was set to 50°C, and the current density was set to 1.3 A/l.
dm" for 120 minutes on a stainless steel plate (50m x 25
m x 1 mm) was plated. This rhodium-ruthenium alloy plating film was peeled off, about 0.2# of it was accurately weighed out using a balance, placed in a nickel crucible, and heated at about 800°C for minutes with 311 sodium peroxide.
Melted by heating. After cooling to room temperature, 200 ml of the melt
The residue in the nickel crucible was then washed with io% hydrochloric acid, and then poured into a 200 tnL volumetric flask, and the volume of the volumetric flask was brought to a constant volume with 10% hydrochloric acid. Rhodium concentration in this aqueous solution '1343z
The measurement results were obtained by measuring at the wavelength of trL by atomic absorption spectrometry using the standard addition method while simultaneously performing background correction. From this measurement result and the weight of the rhodium-ruthenium alloy plating film that was initially scraped off, the rhodium phase was determined to be
It was calculated to be 49.0%. On the other hand, when the decrease in the rhodium concentration in the plating bath was similarly measured using atomic absorption spectrometry, it was found that
The amount of rhodium decreased and the amount of precipitation were consistent.
以上述べたように、この発明によ牡は、従来の方法ト異
なり、ロジウム−ルテニウム合金めっき皮膜を、過酸化
ナトリウムま几は、過酸化カリウ５−
ムとともに加熱溶融するという簡単な操作で、完全に加
熱溶融することができ、しかも、原子吸光分析時の干渉
が小さいため、ロジウム−ルテニウム合金めっき皮膜の
ロジウム相を簡潔に精度よく分析できるという効果を有
する。As described above, the present invention differs from the conventional method in that a rhodium-ruthenium alloy plating film can be melted by heating with sodium peroxide or potassium peroxide. Since it can be completely heated and melted and has little interference during atomic absorption analysis, it has the effect of allowing the rhodium phase of a rhodium-ruthenium alloy plating film to be analyzed simply and accurately.
以上 出願人 株式会社第二精工舎 ６−that's all Applicant: Daini Seikosha Co., Ltd. 6-
Claims (1)
皮膜を過酸化ナトリウムまたは、過酸化カリウムととも
に加熱溶融し、溶融後のロジウム−ルテニウム合金めっ
き皮膜中のロジウム量を、原子吸光分析法により求める
ことを特徴とするロジウム−ルテニウム合金めっき皮膜
のロジウム相分析方法。A rhodium-ruthenium alloy plating film is heated and melted together with sodium peroxide or potassium peroxide in a nickel crucible, and the amount of rhodium in the rhodium-ruthenium alloy plating film after melting is determined by atomic absorption spectrometry. A method for analyzing the rhodium phase of a rhodium-ruthenium alloy plating film.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP56147260A JPS5848854A (en) | 1981-09-18 | 1981-09-18 | Analysis for rhodium phase of planted film of rhodium- ruthenium alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP56147260A JPS5848854A (en) | 1981-09-18 | 1981-09-18 | Analysis for rhodium phase of planted film of rhodium- ruthenium alloy |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS5848854A true JPS5848854A (en) | 1983-03-22 |
Family
ID=15426203
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP56147260A Pending JPS5848854A (en) | 1981-09-18 | 1981-09-18 | Analysis for rhodium phase of planted film of rhodium- ruthenium alloy |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5848854A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007138768A1 (en) | 2006-05-26 | 2007-12-06 | Nippon Mining & Metals Co., Ltd. | Zirconium crucible for analytical sample melting, method of preparing analytical sample and method of analysis |
| JP2009041947A (en) * | 2007-08-06 | 2009-02-26 | Nikko Kinzoku Kk | Nickel crucible |
| WO2010110064A1 (en) | 2009-03-23 | 2010-09-30 | 日鉱金属株式会社 | Zirconium crucible |
-
1981
- 1981-09-18 JP JP56147260A patent/JPS5848854A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007138768A1 (en) | 2006-05-26 | 2007-12-06 | Nippon Mining & Metals Co., Ltd. | Zirconium crucible for analytical sample melting, method of preparing analytical sample and method of analysis |
| JP2009041947A (en) * | 2007-08-06 | 2009-02-26 | Nikko Kinzoku Kk | Nickel crucible |
| WO2010110064A1 (en) | 2009-03-23 | 2010-09-30 | 日鉱金属株式会社 | Zirconium crucible |
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