JPS58205840A - Assay of copper in copper-stainless steel-bismuth alloy - Google Patents

Assay of copper in copper-stainless steel-bismuth alloy

Info

Publication number
JPS58205840A
JPS58205840A JP8801382A JP8801382A JPS58205840A JP S58205840 A JPS58205840 A JP S58205840A JP 8801382 A JP8801382 A JP 8801382A JP 8801382 A JP8801382 A JP 8801382A JP S58205840 A JPS58205840 A JP S58205840A
Authority
JP
Japan
Prior art keywords
copper
sample
assay
calibration curve
alloy
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
Application number
JP8801382A
Other languages
Japanese (ja)
Inventor
Hideo Hara
原　秀夫
Kumiko Ito
久美子 伊藤
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.)
Meidensha Corp
Meidensha Electric Manufacturing Co Ltd
Original Assignee
Meidensha Corp
Meidensha Electric Manufacturing Co Ltd
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 Meidensha Corp, Meidensha Electric Manufacturing Co Ltd filed Critical Meidensha Corp
Priority to JP8801382A priority Critical patent/JPS58205840A/en
Publication of JPS58205840A publication Critical patent/JPS58205840A/en
Pending legal-status Critical Current

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/3103—Atomic absorption analysis

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

PURPOSE:To achieve a quick assay of copper in an alloy with a relatively high content of copper by a method wherein after dissolved in aqua regia, the sample is heated with addition of Hcl and partially taken to assay copper therein by calibration curve employing an atomic absorption spectrophotometer. CONSTITUTION:0.2g of a copper alloy is sampled and dissolved in 20ml of aqua regia. Immediately before the hardened dry in evaporation, it is heated with addition of HCl 10ml and H2O 20ml. After the dissolution of the sample, the solution is rendered 100ml constant and partially taken by 10ml. Then it is rendered 100ml constant again and then partially taken by 10ml. After addition of HCl 20ml, it is rendered 100ml constant. Then, the solution is measured in 327.4nm with an atomic absorption spectrophotometer and copper in the sample is assayed by the calibration curve. The analysis in such a manner enables a quick assay of copper in an alloy with such relatively high content of copper as about 50%.

Description

【発明の詳細な説明】 本発明は、銅−ステンレス−ビスマス合金中の銅の分析
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 copper in a copper-stainless steel-bismuth alloy.

従来、銅合金中の銅の分析方法として、電解型がある。Conventionally, there is an electrolytic method for analyzing copper in copper alloys.

例えば、Ｃｕが０．０１％以上０．５チ未満といった微
量の銅を含む合金の場合、鉄を添加する方法がＪＩＳ　
　Ｇ　１２５７　　（鉄及び鋼の原子吸光分析方法）に
規定されている。For example, in the case of an alloy containing a trace amount of copper, such as 0.01% or more and less than 0.5% Cu, the method of adding iron is JIS
Specified in G 1257 (Atomic absorption spectrometry method for iron and steel).

本発明は、銅の含有量が例えば５０チといった比較的高
い合金中の銅の分析を迅速に行うことのできる分析方法
を提供しようとするものである。The present invention aims to provide an analysis method that can rapidly analyze copper in an alloy having a relatively high copper content, such as 50 tchi.

本発明に係る分析方法は、試料の溶解に王水を用いると
ともに、これにＨＣｌを加えて加熱し、分取後、原子吸
光光度計を用いて、検量線法によシ試料中の銅の分析を
行なうことを特徴とするものである。The analysis method according to the present invention uses aqua regia to dissolve the sample, adds HCl to it and heats it, and after fractionation, uses an atomic absorption spectrophotometer to analyze copper in the sample using the calibration curve method. It is characterized by conducting analysis.

第１図は、本発明に係る分析方法の一例を示すフローシ
ートである。まず、試料たる銅合金を、０．２ｇ採取し
、王水２０−を用いて溶解する。なお、試料の溶解に、
塩酸、硝酸、塩酸−加圧ルツボ、塩酸−フツ化水素−加
圧ルツボ等を試みた力瓢試料の溶解はできず、また、王
水、塩酸−過酸化水素では、王水による場合が最も良好
であった。FIG. 1 is a flow sheet showing an example of the analysis method according to the present invention. First, 0.2 g of a copper alloy as a sample is taken and dissolved using 20% of aqua regia. In addition, for dissolving the sample,
Hydrochloric acid, nitric acid, hydrochloric acid-pressure crucible, hydrochloric acid-hydrogen fluoride-pressure crucible, etc., were used to dissolve the sample. It was good.

ここで蒸発乾固寸前にＨＣＬ　１０　ｍ／、Ｈ，０２０
ｍを加えて加熱する。試料溶解後、１００ｔｎｔ一定と
し、１〇−分増、再び１００−一定とし、１〇−分取、
ＨＣＬ２．Ｏ−添加し、１００−一定とし、これを原子
吸光光度計を用いて、３２７．４％ｍで測定し、検量線
法によって、試料中の銅の分析を行なう。Here, just before evaporation to dryness, add HCL 10 m/, H,020
Add m and heat. After dissolving the sample, keep it constant at 100 tnt, increase by 10 minutes, keep it constant at 100 again, take 10 minutes,
HCL2. Add O to make the sample constant at 100, measure it at 327.4% m using an atomic absorption spectrophotometer, and analyze copper in the sample using the calibration curve method.

第２図は銅の検量線である。この検量線は、Ｃｕ（０，
５，０，８，１，０，１，５ｑ）ＫＨｃｔ２−を加え、
水で１００−一定にしたものを用いて作製したもので、
Ｉ＝１１．８Ｃ＋０．１３で表わされる。なお相関係数
ｒ＝ｏ、９９９７、濃度換算の標準偏差Ｓｃ−〇、１０
　ｐｐｍである。この検量線は、２〜１５　ｐｐｍ間で
直線を示し、＃１ソ原点を通り、非常に精度が良いこと
が認められる。原子吸光光度計で分析を行うに際し、分
析線を、２〜１５　ｐｐｍ間において、２２２．５７％
ｍ、２４９．２２％ｍ、２４４．１６％ｍと種々変えた
ところ、これらの場合はいずれも感度不足であった。、
また、３２４．７４％ｍ　ではスケールオーバし、３２
７．４％ｍの分析線を用いるのが最も良好であつた。Figure 2 is a copper calibration curve. This calibration curve is Cu(0,
5,0,8,1,0,1,5q) Add KHct2-,
It was made using water adjusted to a constant value of 100.
It is expressed as I=11.8C+0.13. Note that correlation coefficient r=o, 9997, standard deviation of concentration conversion Sc-〇, 10
It is ppm. This calibration curve shows a straight line between 2 and 15 ppm, passes through the #1 origin, and is recognized to have very high accuracy. When performing analysis with an atomic absorption spectrophotometer, the analytical line is 222.57% between 2 and 15 ppm.
When various changes were made to m, 249.22%m, and 244.16%m, the sensitivity was insufficient in all of these cases. ,
Also, at 324.74%m, there is overscale and 324.74%m.
It was best to use the 7.4% m analysis line.

第６図は分解試薬の影響を調べた線図である、試料を王
水で溶解し１００分の１に希釈すると、酸濃度が低下し
て、ビスマスなどが析出し測定の妨げとなる。一方酸濃
度が低ければ低いはど酸自身の影響は少くなる。塩酸０
．２４〜０．３６　Ｎにした時の銅への影響は、第６図
に示すように約５チ程度の回収率の低下をみた。しかし
添加量による有意差は認められない。従って、検量線に
塩酸を添加して、試料の酸濃度と合せることとした。FIG. 6 is a diagram examining the influence of decomposition reagents. When a sample is dissolved in aqua regia and diluted to 1/100, the acid concentration decreases and bismuth etc. precipitate, interfering with measurements. On the other hand, the lower the acid concentration, the less the influence of the acid itself. Hydrochloric acid 0
．． When the pressure was set to 24 to 0.36 N, the effect on copper was that the recovery rate decreased by about 5 cm, as shown in Figure 6. However, no significant difference was observed depending on the amount added. Therefore, it was decided to add hydrochloric acid to the calibration curve to match the acid concentration of the sample.

第４図〜第８図は試料に共存する元素の影響を調べた線
図で、第４図は鉄、第５図はニッケル、第６図はクロム
、第７図はモリブデン、第８図はビスマスのそれぞれの
銅の回収率を示している。Figures 4 to 8 are diagrams examining the influence of elements coexisting in the sample. Figure 4 is iron, Figure 5 is nickel, Figure 6 is chromium, Figure 7 is molybdenum, and Figure 8 is The recovery rate of copper for each bismuth is shown.

これらの結果から明らかなように１回収率はいずれも許
容範囲内であり、銅への影響はないことがわかった、次
に組成が、（Ｃｕ　：　０．９６７ｗｇ、　Ｆｅ：　　
ｏ、ａＩｌｖ、　Ｎｉ　：　０．０８Ｗ、　Ｃｒ　：　
０．２”％’、　Ｍｏ　：０．０２■、　Ｂｔ　：　０
．１ｖ、　Ｈｃｔ　２ｍｇ）／１００ｍｇの疑似試料を
１０個作製し、Ｃｕの回収率を調べた結果、Ｃｕの回収
率は平均で１００．８％、変動係数０、４５　％で、・
十分満足できる結果が得られた。As is clear from these results, the 1 recovery rate was all within the allowable range, and it was found that there was no effect on copper.Next, the composition was (Cu: 0.967 wg, Fe:
o, aIlv, Ni: 0.08W, Cr:
0.2"%', Mo: 0.02■, Bt: 0
．． 1v, Hct 2mg)/100mg were prepared, and the recovery rate of Cu was investigated. As a result, the recovery rate of Cu was 100.8% on average, and the coefficient of variation was 0.45%.
A fully satisfactory result was obtained.

また、金属標準銅と８ｕ８３０４　を約１：１に混ぜ本
発明に係る方法によ９５回の測定を行なった結果では、
銅の回収率９９．２　％　、変動係数１．３チとな妙、
実用上満足できることが確認された。また、実試料６個
について分析した結果では、平均値４６．８　％　、変
動係数０．９４　％であった。In addition, the results of 95 measurements conducted using the method of the present invention by mixing metal standard copper and 8u8304 at a ratio of approximately 1:1 show that
Copper recovery rate is 99.2%, coefficient of variation is 1.3ch,
It was confirmed that it is practically satisfactory. Furthermore, the results of analysis of six actual samples showed an average value of 46.8% and a coefficient of variation of 0.94%.

以上説明した。ように、本発明に係る分析方法によれば
、銅の含有率が５〇チ前後といった比較的高い合金中の
銅の分析を迅速に行うことができる。This has been explained above. As described above, according to the analysis method according to the present invention, it is possible to rapidly analyze copper in an alloy having a relatively high copper content of around 50%.

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

第１図は本発明に係る分析方法の一例を示すフローシー
ト図、第２図はＣｕの検量線図、第３図は分解試薬の影
響を調べた線図、第４図〜第８図は共存元素の影響につ
いて調べた線図である。 代理人　弁理士　　木　村　三　朗 第１図 試料Figure 1 is a flow sheet diagram showing an example of the analysis method according to the present invention, Figure 2 is a calibration curve diagram for Cu, Figure 3 is a diagram examining the influence of decomposition reagents, and Figures 4 to 8 are It is a diagram in which the influence of coexisting elements was investigated. Agent Patent Attorney Sanro Kimura Sample Figure 1

Claims (2)

【特許請求の範囲】[Claims] （１）試料の溶解に王水を用いるとともにこれにＨＣｌ
を加えて加熱し、分取後原子吸光光度針を用いて、検量
線法により前記試料中の銅の分析を行なうことを特徴と
する銅−ステンレス−ビスマス合金中の銅の分析方法。(1) Use aqua regia to dissolve the sample and add HCl to it.
1. A method for analyzing copper in a copper-stainless steel-bismuth alloy, which comprises adding and heating the sample, and after fractionation, using an atomic absorption spectrometer needle, the copper in the sample is analyzed by a calibration curve method. （２）検量線に塩酸を添加し、試料の酸濃度と合せるよ
うにした特許請求の範囲第１項記載の銅−ステンレス−
ビスマス合金中の銅の分析方法。(2) Copper stainless steel according to claim 1, in which hydrochloric acid is added to the calibration curve to match the acid concentration of the sample.
Method for analyzing copper in bismuth alloys.
JP8801382A 1982-05-26 1982-05-26 Assay of copper in copper-stainless steel-bismuth alloy Pending JPS58205840A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP8801382A JPS58205840A (en) 1982-05-26 1982-05-26 Assay of copper in copper-stainless steel-bismuth alloy

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP8801382A JPS58205840A (en) 1982-05-26 1982-05-26 Assay of copper in copper-stainless steel-bismuth alloy

Publications (1)

Publication Number Publication Date
JPS58205840A true JPS58205840A (en) 1983-11-30

Family

ID=13930956

Family Applications (1)

Application Number Title Priority Date Filing Date
JP8801382A Pending JPS58205840A (en) 1982-05-26 1982-05-26 Assay of copper in copper-stainless steel-bismuth alloy

Country Status (1)

Country Link
JP (1) JPS58205840A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104764704A (en) * 2015-04-22 2015-07-08 阳谷祥光铜业有限公司 Method for determining copper phase in flash converting furnace slag

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104764704A (en) * 2015-04-22 2015-07-08 阳谷祥光铜业有限公司 Method for determining copper phase in flash converting furnace slag
CN104764704B (en) * 2015-04-22 2017-10-24 阳谷祥光铜业有限公司 Copper thing molybdenum determination method in flash blowing clinker

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