CN102393394A - Method for detecting copper in stainless steel by adopting BCO - Google Patents
Method for detecting copper in stainless steel by adopting BCO Download PDFInfo
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- CN102393394A CN102393394A CN2011103371781A CN201110337178A CN102393394A CN 102393394 A CN102393394 A CN 102393394A CN 2011103371781 A CN2011103371781 A CN 2011103371781A CN 201110337178 A CN201110337178 A CN 201110337178A CN 102393394 A CN102393394 A CN 102393394A
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Abstract
A method for detecting copper in stainless steel by adopting BCO belongs to the field of chemical analysis methods. In the method, thymol blue indicator is adopted to replace neutral red for adjusting acidity (the color change is obvious), and then 1mL ammonia water with 0.9g/L concentration is accurately added into, so as to accurately adjust the acidity; and the operation of chromium volatilization when a sample is decomposed is combined, so as to realize the accurate detection to tiny copper in the stainless steel. The method is simple and accurate, has low cost, solves the problems resulted from adopting an international method that a large amount of poisonous organic reagent is used in a neocuproine-trichloromethane extraction spectrophotometric method, the operation is difficult, and the detection cost is high (since neocuproine is more expensive), thereby quickly realizing the low-pollution chemical detection to the tiny copper in stainless steel.
Description
Technical field:
The invention belongs to the chemical analysis method field, be specifically related to the detection method of copper in the own oxalyl dihydrazone of a kind of dicyclo spectrphotometric method for measuring stainless steel.
Background technology:
The method of trace copper is commonly used in the chemical gauging stainless steel has new cuprous spirit-chloroform extraction photometry and the own oxalyl dihydrazone of dicyclo photometry (abbreviation BCO photometry); The former is a national standard method; Accuracy is high, and its defective is to use the strong methenyl choloride of toxicity to extract, and is harmful; Be not easy to operation, and used new cuprous clever reagent is relatively more expensive.The latter is a former Ministry of Metallurgical Industry industry standard, and method is simple, be easy to grasp, accuracy is high, receives metallurgy industry chemical analysis worker's favor deeply, and when defective was high alloy class sample such as analysis of stainless steel, acidity adjustment was difficult to grasp, and indicator discoloration is sharp inadequately.It is pH=8.5～9.3 that this method requires color acidity; Make indicator (color change interval is 6.8～8.0) with dimethyl diaminophenazine chloride after adding the 2mL citric acid, 1+1 ammoniacal liquor is regulated acidity, and solution becomes orange colour by redness; Shown redness is very not remarkable when the orange colour of terminal point changes; Particularly for the very high sample of alloying element content, the hop that almost can't distinguish between colors makes this method be restricted in the application in stainless steel field.
Summary of the invention:
The present invention provides the detection method of copper in the own oxalyl dihydrazone of a kind of dicyclo spectrphotometric method for measuring stainless steel; Its objective is the defective of avoiding said method to exist; Improve the acuteness of acidity adjustment, realize that acidity precisely controls, reach copper in the stainless steel accurately, the purpose of fast measuring.
Technical scheme of the present invention:
It is characterized in that comprising the steps: (1) title 0.25g or 0.5g stainless steel sample in the 150mL triangular flask, in triangular flask, add the 10mL chloroazotic acid and make the stainless steel sample dissolution;
(2) in triangular flask, add 5mL hydrofluorite and perchloric acid mixed solution; Triangular flask is heated to drips twice hydrochloric acid when smoldering and wave chromium, drip 2～3mL hydrochloric acid at every turn and wave chromium;
(3) triangular flask is naturally cooled to room temperature, produce the crystalloid salt this moment, add this salt of 20mL dissolved in distilled water; Solution is changed in the 100mL volumetric flask, clean triangular flask with distilled water, washing lotion is incorporated in this volumetric flask; And be diluted to scale, shake up, as mother liquor;
(4) draw two parts of mother liquor 10mL respectively in two 50mL volumetric flasks, a copy of it is made colour developing liquid, and another part is made reference liquid;
(5) in colour developing liquid: add citric acid and 3 thymol blue ethanolic solutions that concentration is 1g/L that 2mL concentration is 500g/L; Dripping volume ratio immediately is the ammoniacal liquor adjusting acidity of 1+1; Drop to that liquid becomes yellow just by redness in the volumetric flask; After using transfer pipet accurately to add the ammoniacal liquor of 1mL density then, add the NH that 10mL acidity is pH=9.2 successively as 0.9g/L
3-NH
4Cl buffer solution, 10mL concentration are the BCO solution of 1g/L, and wherein BCO solution is the ethanolic solution preparation of 1+1 by volume ratio., to scale, shake up with distilled water diluting, place 5～10min, in the 600nm wavelength, with 1cm absorption vessel colorimetric;
(6) in reference liquid: add citric acid and 3 thymol blue ethanolic solutions that concentration is 1g/L that 2mL concentration is 500g/L; Dripping volume ratio immediately is the ammoniacal liquor adjusting acidity of 1+1; Drop to that liquid becomes yellow just by redness in the volumetric flask; After using transfer pipet accurately to add the ammoniacal liquor of 1mL density then, add the NH that 10mL acidity is pH=9.2 as 0.9g/L
3-NH
4Cl buffer solution, shakes up to scale with distilled water diluting, places 5～10min, in the 600nm wavelength, with 1cm absorption vessel colorimetric.
(7) with the reference liquid be reference, measure absorbance, on the copper solution working curve, check in the massfraction of copper according to this absorbance in the 600nm wavelength.
Said hydrofluorite and perchloric acid mixed solution are the mixed solutions of volume ratio Qing Fu Suan ︰ perchloric acid=4 ︰ 96;
Copper content took by weighing 0.5g less than 0.1% o'clock in the stainless steel sample; Copper content took by weighing 0.25g greater than 0.1% o'clock in the stainless steel sample, was accurate to 0.1mg.
Be that three samples are adopted the mensuration result that this method, ICP-OES method and new cuprous spirit-three kinds of methods of chloroform extraction photometry are measured respectively below, see table 1:
Technique effect of the present invention; Compare through the result to above-mentioned three kinds of assay methods and to show: the present invention replaces dimethyl diaminophenazine chloride with bromothymol blue (color change interval is 1.2～2.8) indicator; The liquid that develops the color when regulating acidity is become light yellow by peony, change color is very obvious, accurately adds 1mL ammoniacal liquor (density is 0.9g/L) then; And the operation of " waving chromium " when combining decomposed sample, just can reach the purpose of accurate adjusting acidity.
The present invention is simple, accurate, cost is low, has realized the accurate mensuration of trace copper in the stainless steel.Stopped the employing national standard method---new cuprous spirit-chloroform extraction Spectrophotometry for Determination is regularly a large amount of uses poisonous organic reagent, not easy to operate and detect the problem of cost high (new cuprous spirit is relatively more expensive), has realized oligosaprobic chemical detection.
Embodiment:
Embodiment of the present invention is carried out copper Determination on content step through the stainless steel sample of following three different contents, is elaborated.
Embodiment one: the operation steps of present embodiment is in regular turn:
1, accurately takes by weighing stainless steel sample 0.5g and place the 150mL triangular flask, in triangular flask, add the 10mL chloroazotic acid, the stainless steel sample dissolution;
2, the hydrofluorite and the perchloric acid mixed solution (promptly according to volume ratio Qing Fu Suan ︰ perchloric acid=4 ︰, 96 mixed solution) that in triangular flask, add 5mL;
3, triangular flask is heated to when emitting the perchloric acid cigarette, and dripping hydrochloric acid 3mL waves chromium,
4, triangular flask naturally cools to room temperature, and produce crystalloid salt in the triangular flask this moment;
5, in triangular flask, behind this salt of adding 20mL dissolved in distilled water, solution is moved in the 100mL volumetric flask, clean triangular flask with distilled water, washing lotion is incorporated in this volumetric flask, and is diluted to scale, shakes up, and is called mother liquor;
6, draw mother liquor 10mL in the 50mL volumetric flask each two parts, a copy of it is made colour developing liquid, and another part is made reference liquid,
7, in colour developing liquid: add 2mL citric acid (500g/L) and 3 thymol blue (1g/L; Ethanolic solution); Dropping ammonia (1+1) is regulated acidity immediately, drops to colour developing liquid and becomes yellow just by redness, continues accurately to add 1mL ammoniacal liquor (density is 0.9g/L) with transfer pipet; Add 10mLNH then successively
3-NH
4Cl buffer solution (pH=9.2), 10mLBCO (1g/L, 1+1 ethanolic solution) solution, shake up to scale with distilled water diluting, place 5～10min and carry out colorimetric, use the 1cm absorption vessel, are reference with the reference liquid, measure absorbance in the 600nm wavelength.Absorbance checks in the massfraction of copper on the working curve of the copper of being drawn in view of the above.
In reference liquid: different in the liquid with colour developing is in reference liquid, not add BCO solution, and all the other steps are identical with interpolation step in the liquid that develops the color.
The drafting of copper working curve: take by weighing identical with sample size, that can contain sample copper content, content and be 4～5 in series standard sample certain gradient and close with the sample steel grade in corresponding 150mL triangular flask, as follows sample operation procedure.Standard value with the series standard sample is a horizontal ordinate, and absorbance is an ordinate, draws regression curve, promptly gets the working curve of method.
Embodiment two: what present embodiment and embodiment one were different is accurately to take by weighing stainless steel sample 0.25g, and other operation steps is identical with embodiment one.
The copper working curve is the known technology of this area, omits and describes in detail.
Claims (2)
1. the detection method of copper in the own oxalyl dihydrazone of the dicyclo spectrphotometric method for measuring stainless steel is characterized in that comprising the steps: that (1) claim 0.25g or 0.5g stainless steel sample in the 150ml triangular flask, in triangular flask, adds the 10ml chloroazotic acid and makes the stainless steel sample dissolution;
(2) in triangular flask, add 5ml hydrofluorite and perchloric acid mixed solution; Triangular flask is heated to drips twice hydrochloric acid when smoldering and wave chromium, drip 2～3mL hydrochloric acid at every turn and wave chromium;
(3) triangular flask is naturally cooled to room temperature, produce the crystalloid salt this moment, add this salt of 20ml dissolved in distilled water; Solution is changed in the 100mL volumetric flask, clean triangular flask with distilled water, washing lotion is incorporated in this volumetric flask; And be diluted to scale, shake up, as mother liquor;
(4) draw two parts of mother liquor 10ml respectively in two 50ml volumetric flasks, a copy of it is made colour developing liquid, and another part is made reference liquid;
(5) in colour developing liquid: add citric acid and 3 thymol blue ethanolic solutions that concentration is 1g/L that 2ml concentration is 500g/L; Dripping volume ratio immediately is the ammoniacal liquor adjusting acidity of 1+1; Drop to that liquid becomes yellow by redness in the volumetric flask; After using transfer pipet accurately to add the ammoniacal liquor of 1mL density then, add the NH that 10ml acidity is pH=9.2 successively as 0.9g/L
3-NH
4Cl buffer solution, 10ml concentration are the BCO solution of 1g/L, and wherein BCO solution is the ethanolic solution preparation of 1+1 by volume ratio,
, to scale, shake up with distilled water diluting, place 5-10min, in the 600nm wavelength, with 1cm absorption vessel colorimetric;
(6) in reference liquid: add citric acid and 3 thymol blue ethanolic solutions that concentration is 1g/L that 2ml concentration is 500g/L; Dripping volume ratio immediately is the ammoniacal liquor adjusting acidity of 1+1; Drop to that liquid becomes yellow by redness in the volumetric flask; After using transfer pipet accurately to add the ammoniacal liquor of 1mL density then, add the NH that 10ml acidity is pH=9.2 as 0.9g/L
3-NH
4Cl buffer solution, shakes up to scale with distilled water diluting, places 5-10min, in the 600nm wavelength, with 1cm absorption vessel colorimetric;
(7) with the reference liquid be reference, measure absorbance, on the copper solution working curve, check in the massfraction of copper according to this absorbance in the 600nm wavelength.
2. the detection method of copper in the own oxalyl dihydrazone of a kind of dicyclo according to claim 1 spectrphotometric method for measuring stainless steel is characterized in that described hydrofluorite and perchloric acid mixed solution are the mixed solutions of volume ratio Qing Fu Suan ︰ perchloric acid=4 ︰ 96.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107941729A (en) * | 2018-01-22 | 2018-04-20 | 江苏佳铝实业股份有限公司 | The rapid analysis method of copper impurity in sulphuric acid anodizing tank liquor |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040043439A1 (en) * | 2002-09-03 | 2004-03-04 | Toyo B-Net Co., Ltd. | Luciferase detection reagent kits and luciferase detection method using the kit |
| CN101013087A (en) * | 2007-02-05 | 2007-08-08 | 同济大学 | Method for measuring trace copper ion by using light absorption ratio difference and continuous-flow |
| WO2008066003A1 (en) * | 2006-11-28 | 2008-06-05 | Nomura Micro Science Co., Ltd. | Method for quantitative determination of nickel and/or copper and equipment to be used in the method |
| CN101303286A (en) * | 2008-07-02 | 2008-11-12 | 新疆新鑫矿业股份有限公司 | Method for rapidly measuring copper content |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040043439A1 (en) * | 2002-09-03 | 2004-03-04 | Toyo B-Net Co., Ltd. | Luciferase detection reagent kits and luciferase detection method using the kit |
| WO2008066003A1 (en) * | 2006-11-28 | 2008-06-05 | Nomura Micro Science Co., Ltd. | Method for quantitative determination of nickel and/or copper and equipment to be used in the method |
| CN101013087A (en) * | 2007-02-05 | 2007-08-08 | 同济大学 | Method for measuring trace copper ion by using light absorption ratio difference and continuous-flow |
| CN101303286A (en) * | 2008-07-02 | 2008-11-12 | 新疆新鑫矿业股份有限公司 | Method for rapidly measuring copper content |
Non-Patent Citations (3)
| Title |
|---|
| 《连云港化工高等专科学校学报》 20000630 李艳辉等 铜_MTB_CTMAB_beta_CD显色体系的研究应用 摘要、正文第1页第6行至第18行 1-2 第13卷, 第2期 * |
| 张萍等: "BCO法快速测定钢铁及其合金中的微量铜", 《四川冶金》 * |
| 李艳辉等: "铜_MTB_CTMAB_β_CD显色体系的研究应用", 《连云港化工高等专科学校学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107941729A (en) * | 2018-01-22 | 2018-04-20 | 江苏佳铝实业股份有限公司 | The rapid analysis method of copper impurity in sulphuric acid anodizing tank liquor |
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