JPS592343B2 - Method for measuring the amount of metallic Al in a composite plated coating layer - Google Patents

Method for measuring the amount of metallic Al in a composite plated coating layer

Info

Publication number
JPS592343B2
JPS592343B2 JP53087049A JP8704978A JPS592343B2 JP S592343 B2 JPS592343 B2 JP S592343B2 JP 53087049 A JP53087049 A JP 53087049A JP 8704978 A JP8704978 A JP 8704978A JP S592343 B2 JPS592343 B2 JP S592343B2
Authority
JP
Japan
Prior art keywords
amount
coating layer
measuring
metallic
plated coating
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
Application number
JP53087049A
Other languages
Japanese (ja)
Other versions
JPS5515005A (en
Inventor
敬久 吉原
俊一 原田
肇 木村
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.)
JFE Steel Corp
Original Assignee
Kawasaki 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 Kawasaki Steel Corp filed Critical Kawasaki Steel Corp
Priority to JP53087049A priority Critical patent/JPS592343B2/en
Publication of JPS5515005A publication Critical patent/JPS5515005A/en
Publication of JPS592343B2 publication Critical patent/JPS592343B2/en
Expired legal-status Critical Current

Links

Landscapes

  • Investigating And Analyzing Materials By Characteristic Methods (AREA)

Description

【発明の詳細な説明】 この発明は複合めつき法により複合めつき被覆層中に共
析含有した金属Al(以下Alと略す)量を簡単な装置
で迅速に測定する方法に関するものである。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for quickly measuring the amount of metal Al (hereinafter abbreviated as Al) eutectoidally contained in a composite plating coating layer using a composite plating method using a simple device.

複合めつき被覆層中にAlが共析含有(以下共析と略す
)すると、その共析量に応じて、耐食性あるいは耐酸化
性などの表面特性が顕著に改善されることについては、
すでに特開昭51一143534号あるいは特開昭53
−18435号各公報で開示した。
Regarding the fact that when Al is eutectoid contained in the composite plated coating layer (hereinafter abbreviated as eutectoid), surface properties such as corrosion resistance and oxidation resistance are significantly improved depending on the amount of eutectoid.
JP-A-51-143534 or JP-A-53
-18435 disclosed in each publication.

このような複合めつき被覆層中のAl量を測定する方法
として、従来から容量法、重量法による化学分析あるい
は螢光X線法、原子吸光法、比色法による機器分析など
が用いられているが、それぞれ次のような不利がある。
すなわち、容量法、重量法、原子吸光法、比色法などに
おいては、複合めつき被覆層を酸などで溶解し、溶液状
態としたのち、分析操作を行なわねばならず、さらにA
i分析を行なう上で、妨害となる元素、化合物を分離し
、あるいはマスキングするなどの複雑な操作が必要であ
わ、迅速にAll共析量を測定することは困難である。
一方、螢光X線法では、Ai共析量を迅速に測定するこ
とはできるが、装置が高価であり、保守、点検などの調
整を必要とし、据付場所(環境、スペースなど)にも押
動をうける。複合めつき被覆層を形成するマトリックス
としては、Zn、Sn、Pb、Cd、Cr、Mn、Ni
、Co、Cu、Fe、Ag、Auなどの金属がある。
Conventionally, methods for measuring the amount of Al in such a composite plated coating layer include chemical analysis using a volumetric method or gravimetric method, or instrumental analysis using a fluorescent X-ray method, atomic absorption method, or colorimetric method. However, each has the following disadvantages:
That is, in the volumetric method, gravimetric method, atomic absorption method, colorimetric method, etc., it is necessary to dissolve the composite plated coating layer with acid etc. to make it into a solution state, and then perform the analytical operation.
In performing i-analysis, complicated operations such as separating or masking interfering elements and compounds are required, and it is difficult to quickly measure the amount of All eutectoid.
On the other hand, with the fluorescent X-ray method, although it is possible to quickly measure the amount of Ai eutectoid, the equipment is expensive, requires adjustments such as maintenance and inspection, and is also difficult to install (environment, space, etc.). be moved. The matrix forming the composite plating layer includes Zn, Sn, Pb, Cd, Cr, Mn, and Ni.
, Co, Cu, Fe, Ag, and Au.

これらの金属のなかで、Zn、Sn、Pb、CdぱPH
12以上の強アルカリ溶液中で徐々に溶解するが、他の
金属はほとんど溶解しない゜一方、金属Alはアルカリ
溶液つまわ水酸化ナトリウム又ぱ水酸化カリウムの1N
〜10N濃度の水溶液に極めて活性で、水素ガスを発生
しながら激しく溶解する。したがつて、上記のマトリッ
クス中にAlが共析した複合めつき被覆層を上記の強ア
ルカリ溶液中に浸漬した場合、1〜5分以内の短時間に
発生するガス量はほとんどA11の溶解によるものであ
わ、一方、マトリックスの溶解によるガス発生量は無視
できることを知見した。
Among these metals, Zn, Sn, Pb, Cd, PH
It gradually dissolves in a strong alkaline solution of 12 or higher, but other metals hardly dissolve.On the other hand, metal Al is dissolved in an alkaline solution of 1N sodium hydroxide or potassium hydroxide.
It is extremely active in aqueous solutions with a concentration of ~10N, and dissolves violently while generating hydrogen gas. Therefore, when the composite plated coating layer in which Al is eutectoided in the above matrix is immersed in the above strong alkaline solution, the amount of gas generated within a short period of 1 to 5 minutes is mostly due to the dissolution of A11. On the other hand, we found that the amount of gas generated due to matrix dissolution can be ignored.

この発明は上記の知見をもとに、前述のように不利、欠
点を解決することを目的とするもので、複合めつき被覆
層中のAl共析量を測定する方法において、該複合めつ
き被覆材をアルカリ溶液に浸漬し、上記の時間内に発生
するガス量を測定することを特徴とするものである。
This invention is based on the above knowledge, and aims to solve the disadvantages and drawbacks as mentioned above. The method is characterized in that the coating material is immersed in an alkaline solution and the amount of gas generated within the above-mentioned period of time is measured.

ここで、アルカリ溶液はすでに触れた水酸化ナトリウム
、水酸化カリウムなどの強アルカリ性水溶液がよく、そ
の濃度は1N〜10Nの範囲が必要である。
Here, the alkaline solution is preferably a strong alkaline aqueous solution such as sodium hydroxide or potassium hydroxide mentioned above, and its concentration needs to be in the range of 1N to 10N.

これよりもアルカリ濃度が低b場合、Al溶解速度が遅
くなり、複合めつき被覆層中のAl共析量を測定するの
に長時間を必要とする。一方、濃共が高くなわすぎると
、Al溶解速度は速くなるが、液調整に多量のアルカリ
が必要であるとともに、調整時の発熱が激しくなるなど
の不利がある。ガス発生量の測定時間は1〜5分が必要
であり、これよりも測定時間が短い場合、Al共析量の
測定誤差が大きく、一方、測定時間が長くなvすぎると
、能率の低下が顕著になる。ガス発生量の測定装置は発
生したガスを捕集し、その量(体積または圧力)を測定
できるものであれば、とくに測定方法に限定されない。
たとえば、強アルカリ溶液を入れた容器と水を満たした
ビユーレツトを三方コツクで接続した装置、あるいはビ
ユーレツトのかわりにガス圧変換器とレコーダーを取シ
付けた装置などでもよい。このような、ガス発生量の測
定装置は簡単に組立てることができ、保守、点検などの
調整をほとんど必要とせず、据付場所の制約をうけるこ
とはほとんどない。
When the alkali concentration is lower than this, the Al dissolution rate becomes slow and it takes a long time to measure the amount of Al eutectoid in the composite plated coating layer. On the other hand, if the concentration is too high, the Al dissolution rate will increase, but there will be disadvantages such as a large amount of alkali being required for liquid preparation and increased heat generation during preparation. The measurement time for the amount of gas generated is 1 to 5 minutes; if the measurement time is shorter than this, the measurement error in the amount of Al eutectoid will be large; on the other hand, if the measurement time is too long, the efficiency will decrease. become noticeable. The measuring device for measuring the amount of gas generated is not particularly limited to a measuring method as long as it can collect the gas generated and measure its amount (volume or pressure).
For example, a device in which a container containing a strong alkaline solution and a burette filled with water are connected via a three-way connection, or a device in which a gas pressure transducer and a recorder are attached instead of the burette may be used. Such a gas generation amount measuring device can be easily assembled, requires almost no maintenance, inspection, or other adjustments, and is hardly subject to any restrictions on installation location.

次にこの発明を実施例について、さらに詳細に説明する
Next, the present invention will be described in more detail with reference to examples.

実施例 電気Znめつき液にAノ粉末を添加して調製した複合め
つき液を電解浴として、鋼板の片面にZn−Al複合め
つき被覆を施した三種の試験材を作製した。
Example Three types of test materials were prepared by applying a Zn--Al composite plating coating to one side of a steel plate using a composite plating solution prepared by adding A powder to an electric Zn plating solution as an electrolytic bath.

複合めつき被覆層の成分は原子吸光法による分析の結果
、Zn付着量15,30,52f1/01′、Al共析
量0.9〜6.89/m″であつた。試験材から10c
Ti1(25X40m1)の試験片を採取し、25゜±
1℃の5NNに肘溶液中で、3分間のガス発生量を測定
した。結果を第1図に示す。第1図から明らかなように
、原子吸光法により分析したAl分析量とガス発生量と
は極めてよい一致を示すことがわかつた。さらに、ガス
発生量はZn付着量(マトリツクス)の影響をほとんど
うけないことがわかつた。なお、同一の材料を螢光X線
で分析したところ、Zn付着量によつてAlのカウント
数力吠きく変化し、マトリツクスの影響を無視できない
ことがわかつた。
As a result of analysis by atomic absorption spectrometry, the components of the composite plated coating layer were found to have a Zn adhesion amount of 15, 30, 52 f1/01' and an Al eutectoid amount of 0.9 to 6.89/m''.
A test piece of Ti1 (25 x 40 m1) was taken, and the angle of 25°±
The amount of gas generated during 3 minutes was measured in 5NN solution at 1°C. The results are shown in Figure 1. As is clear from FIG. 1, it was found that the amount of Al analyzed by atomic absorption spectrometry and the amount of gas generated were in very good agreement. Furthermore, it was found that the amount of gas generated was hardly affected by the amount of Zn deposited (matrix). Incidentally, when the same material was analyzed by fluorescent X-rays, it was found that the Al count value changed dramatically depending on the amount of Zn deposited, and it was found that the influence of the matrix could not be ignored.

かくしてこの発明によれば、複合めつき被覆層中の金属
Al量を高い精度で簡便に測定することができる。
Thus, according to the present invention, the amount of metallic Al in the composite plated coating layer can be easily measured with high accuracy.

【図面の簡単な説明】[Brief explanation of the drawing]

第1図は複合めつき被覆層中のAI!共析量と5NNa
0H浸漬3分後のガス発生量の関係を示すグラフである
Figure 1 shows AI in the composite plating layer! Eutectoid amount and 5NNa
It is a graph showing the relationship between the amount of gas generated after 3 minutes of 0H immersion.

Claims (1)

【特許請求の範囲】[Claims] 1 複合めつき被覆層中に含有する金属Al量を測定す
る方法において、該複合めつき被覆材を水酸化ナトリウ
ム又は水酸化カリウムの1N〜10N濃度の水溶液中に
浸漬し、1〜5分以内に発生するガス量と含有Al量と
の相関によつて定量することを特徴とする複合めつき被
覆層中の金属Al量測定方法。
1. In the method of measuring the amount of metallic Al contained in a composite plating coating layer, the composite plating coating material is immersed in an aqueous solution of sodium hydroxide or potassium hydroxide with a concentration of 1N to 10N, and the method is performed within 1 to 5 minutes. A method for measuring the amount of metallic Al in a composite plated coating layer, characterized in that the amount of metallic Al in a composite plated coating layer is determined by the correlation between the amount of gas generated and the amount of Al contained.
JP53087049A 1978-07-19 1978-07-19 Method for measuring the amount of metallic Al in a composite plated coating layer Expired JPS592343B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP53087049A JPS592343B2 (en) 1978-07-19 1978-07-19 Method for measuring the amount of metallic Al in a composite plated coating layer

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP53087049A JPS592343B2 (en) 1978-07-19 1978-07-19 Method for measuring the amount of metallic Al in a composite plated coating layer

Publications (2)

Publication Number Publication Date
JPS5515005A JPS5515005A (en) 1980-02-01
JPS592343B2 true JPS592343B2 (en) 1984-01-18

Family

ID=13904076

Family Applications (1)

Application Number Title Priority Date Filing Date
JP53087049A Expired JPS592343B2 (en) 1978-07-19 1978-07-19 Method for measuring the amount of metallic Al in a composite plated coating layer

Country Status (1)

Country Link
JP (1) JPS592343B2 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0253749U (en) * 1988-10-07 1990-04-18
JPH02116457U (en) * 1989-03-02 1990-09-18

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS57191998A (en) * 1981-05-22 1982-11-25 Japan Atomic Energy Res Inst Controller for neutral particle incident unit
JP4769045B2 (en) * 2005-08-10 2011-09-07 積水化学工業株式会社 Vacuum injection molding method for fiber reinforced resin molded products
CN102460266B (en) 2009-04-16 2014-10-15 奥林巴斯医疗株式会社 objective optical system
WO2011070930A1 (en) 2009-12-11 2011-06-16 オリンパスメディカルシステムズ株式会社 Objective optical system
CN104198329B (en) * 2014-09-05 2016-07-06 天津立中合金集团有限公司 A kind of method quick and precisely detecting metal aluminum content in aluminum ash and device

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0253749U (en) * 1988-10-07 1990-04-18
JPH02116457U (en) * 1989-03-02 1990-09-18

Also Published As

Publication number Publication date
JPS5515005A (en) 1980-02-01

Similar Documents

Publication Publication Date Title
Radu et al. Guidelines for improving the lower detection limit of ion‐selective electrodes: a systematic approach
Foley Localized corrosion of aluminum alloys—a review
TWI226439B (en) Plating bath analysis
Materlik et al. X-ray standing-wave fluorescence analysis of electrodeposited Tl on clean and oxygen-reconstructed Cu (111)
Hei et al. Sensing atmospheric corrosion of carbon steel and low-alloy steel using the electrochemical noise technique: effects of weather conditions
ATE414901T1 (en) MEASURING THE COMPLEX FORMING CONCENTRATION IN A POWERLESS GALVANIZING BATH
JPS592343B2 (en) Method for measuring the amount of metallic Al in a composite plated coating layer
KR101511408B1 (en) Method for control of stabilizer additives in electroless metal and metal alloy plating electroylytes
US5262022A (en) Method of assessing solderability
Sung et al. Adsorption characteristics by a radiochemical method on smooth electrode surfaces
Chen et al. Stripping Voltammetry of Pb (II), Cu (II), and Hg (II) at a Nafion‐Coated Glassy Carbon Electrode Modified by Neutral Ionophores
Sargent et al. Probing the mechanism of electroless gold plating using an electrochemical quartz crystal microbalance I. Elucidating the nature of reactive intermediates in dimethylamine borane
O'Sullivan et al. Characterization of PdSn catalysts for electroless metal deposition
EP1471347A1 (en) Method of determining organic additives in an electroplating bath
Korolczuk et al. Determination of thallium in a flow system by anodic stripping voltammetry at a bismuth film electrode
Su et al. Cathodic reduction of copper oxides
JP3824011B2 (en) Determination method of alloy phase in plating layer
JP3184375B2 (en) Method for evaluating and restoring solderability of electronic components
Carra et al. A" Hybrid" Mercury Film Electrode for the Voltammetric Analysis of Copper and Lead in Acidified Seawater and Other Media
Sheremet et al. Standardless electrochemical method for mercury, cadmium, lead and copper determination in aqueous solution
JP3778037B2 (en) Determination method of alloy phase in plating layer
Yen et al. Electrochemical characterization of gold-nanostructured platinum substrates and application to determination of Hg (II) at trace levels
Du et al. Underpotential deposition study and determination of bismuth on gold electrode by using voltammetry
Montañés et al. Evolution with exposure time of copper corrosion in a concentrated lithium bromide solution. Characterization of corrosion products by energy-dispersive X-ray analysis and X-ray diffraction
JP2616320B2 (en) Analysis method of metal ion concentration in plating bath