CN103063590B - Spectrophotometry for cobalt content in steel - Google Patents
Spectrophotometry for cobalt content in steel Download PDFInfo
- Publication number
- CN103063590B CN103063590B CN201210569982.7A CN201210569982A CN103063590B CN 103063590 B CN103063590 B CN 103063590B CN 201210569982 A CN201210569982 A CN 201210569982A CN 103063590 B CN103063590 B CN 103063590B
- Authority
- CN
- China
- Prior art keywords
- solution
- steel
- cobalt content
- spectrophotometry
- nitroso
- 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.)
- Active
Links
Landscapes
- Investigating Or Analysing Materials By Optical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention provides spectrophotometry for cobalt content in a kind of steel.In this steel, spectrophotometry for cobalt content comprises the following steps: a) dissolve steel curved beam to prepare sample solution with acid solution; B) in sample solution, add sodium citrate solution, and the pH of sample solution is adjusted to 5.5-7.5; C) in sample solution, add nitroso-R-salt solution and heat and boil at least 30 minutes; D) in the sample solution being cooled to room temperature, sulfuric acid solution is added, thus obtained chromophoric solution; E) after cooling to room temperature, under the existence of reference liquid, measure the absorbance of chromophoric solution with visible spectrophotometer, thus calculate cobalt content.According to spectrophotometry for cobalt content in steel of the present invention have simple to operate, sensing range is wide, testing result is accurate and the reappearance of colour developing and the advantage such as good stability.
Description
Technical field
The invention belongs to steel and ferroalloy chemical analysis technology field, relate to spectrophotometry for cobalt content in a kind of steel, specifically, relate to the nitroso-R-salt spectrophotometry of cobalt content in a kind of steel.
Background technology
Cobalt is a kind of soft magnetic metal, is alloying element important in steel.Cobalt can improve and improve the thermal conductivity of steel, thermohardening, inoxidizability and corrosion resistance etc.Therefore, cobalt is mainly used in high-speed steel, heat-resisting steel and permanent-magnet alloy.Cobalt content in high-alloy steel normally 5%-10%, up to 15%-20% in some specific alloy, high temperature alloy, the cobalt content had in permanent-magnet alloy reaches 20%-35%.
In spectrophotometry steel, the method for cobalt has that instrument is simple, highly sensitive, good selective.But in existing steel there is many deficiencies in the spectrophotometric determination method of cobalt.Such as, GB/T223.22-2008 nitroso-R-salt Spectrophotometric determination of cobalt amount and CSM07052704-2003 cobalt content mensuration nitroso-R-salt photometry complicated operation, sensitivity is low, sensing range is narrow (accurately can only detect the cobalt content of 0.10%-3.00% in steel); Develop the color in nitroso-R-salt spectrophotometric method in acetic acid-sodium acetate buffer solution, the reappearance of colour developing and poor stability.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art and provide a kind of simple to operate, sensing range is wide, testing result is accurate and colour developing reappearance and good stability steel in spectrophotometry for cobalt content.
According to an aspect of the present invention, in steel, spectrophotometry for cobalt content comprises the following steps: a) dissolve steel curved beam to prepare sample solution with acid solution; B) in sample solution, add sodium citrate solution, and the pH of sample solution is adjusted to 5.5-7.5; C) in sample solution, add nitroso-R-salt solution and heat and boil at least 30 minutes; D) in the sample solution being cooled to room temperature, sulfuric acid solution is added, thus obtained chromophoric solution; E) after cooling to room temperature, under the existence of reference liquid, measure the absorbance of chromophoric solution with visible spectrophotometer, thus calculate cobalt content.
According to exemplary embodiment of the present invention, in step a, for dissolving the mixed acid solution that the acid solution of steel curved beam can be hydrochloric acid and nitric acid.
According to exemplary embodiment of the present invention, in step a, can according to the steel curved beam of the height acid dissolve difference amount of cobalt content in steel curved beam.
According to exemplary embodiment of the present invention, the sulfuric acid solution added in steps d can be 98% concentrated sulphuric acid of 1: 1 and the sulfuric acid solution of water for volume ratio.
According to exemplary embodiment of the present invention, in step e, the absorbance of chromophoric solution can be measured at 530nm wavelength place.
According to exemplary embodiment of the present invention, the sulfuric acid in reference liquid can be identical with in the concentration preparing sulfuric acid and the nitroso-R-salt added in chromophoric solution process with the concentration of nitroso-R-salt.
Use sodium citrate as buffer solution when developing the color according to the spectrophotometry of cobalt content in steel of the present invention, shelter the interference elements such as a large amount of iron, nickel and the copper in sample solution, therefore, testing result is accurate.
Embodiment
Be take nitroso-R-salt as the spectrophotometry of developer according to spectrophotometry for cobalt content in steel of the present invention, it is buffer solution when developing the color with sodium citrate solution.Sodium citrate solution as buffer solution can be formed on the one hand and be suitable for citrate ion or the hydrogen citrate radical ion buffer solution that cobalt ions and nitroso-R-salt form complex compound; On the other hand sodium citrate solution can form complex compound with the nickel of ferric iron and divalence and copper, shelters their interference to measurement.
Specifically, in mensuration process, first dissolve steel curved beam with acid solution and prepare sample solution.According to exemplary embodiment of the present invention, steel curved beam can be dissolved at low temperatures with the mixed acid solution that hydrochloric acid and nitric acid are formed.In addition, the steel curved beam can measured according to the height acid dissolve difference of cobalt content in steel curved beam (such as, the desired extent of cobalt content in steel grade to be measured), that is, when in steel curved beam, cobalt content is higher, with the steel curved beam of acid dissolve small amount; When cobalt content is lower in steel curved beam, the steel curved beam that acid dissolve is relatively large can be used, according to exemplary embodiment of the present invention, the dissolving of sample can be carried out with reference to table 1.Compared with the method for traditional dissolved samples, the more convenient operation of this dissolved samples, simple, be easy to operation.
Next, in sample solution, add sodium citrate solution, and the pH value of sample solution is adjusted to about 5.5-7.5.As mentioned above, here add sodium citrate solution can be formed and be suitable for citrate ion or the hydrogen citrate radical ion buffer solution that cobalt ions and nitroso-R-salt form complex compound, and the sodium citrate added can form complex compound with the nickel of ferric iron and divalence and copper thus shelter them to the interference of measuring.
Next, in the sample solution adding sodium citrate solution, nitroso-R-salt solution is added and heating boils at least 30 minutes.Here, heating can make the cobalt ions in sample solution and nitroso-R-salt be fully formed trivalent cobalt nitroso-R complex compound at least 30 minutes.In addition, compared to the amount of the nitroso-R-salt reacted with cobalt ions, more nitroso-R-salt can be added here, to eliminate the interference of vanadium, and make the range of linearity of colour developing wider simultaneously.
Then, sample solution is cooled to room temperature and adds sulfuric acid solution in the sample solution being cooled to room temperature, the complex compound that the nickel of ferric iron and divalence and copper and nitroso-R-salt are formed decomposes completely, can not make again the complex decomposes of trivalent cobalt and nitroso-R-salt simultaneously.According to exemplary embodiment of the present invention, can add volume ratio is here 98% concentrated sulphuric acid (density is 1.84g/mL) of 1: 1 and the sulfuric acid solution of water.
Finally, after cooling to room temperature, under the existence of reference liquid, measure the absorbance of sample solution with visible spectrophotometer, thus calculate cobalt content.According to exemplary embodiment of the present invention, sulfuric acid in reference liquid is identical with in the concentration preparing sulfuric acid and the nitroso-R-salt added in chromophoric solution process with the concentration of nitroso-R-salt, that is, the sulfuric acid added in reference liquid is identical with in the amount preparing sulfuric acid and the nitroso-R-salt added in chromophoric solution process with the amount of nitroso-R-salt, the complex compound content making in nitrite ion the copper that formed in the content of residual copper and the complex compound that nitroso-R-salt is formed and reference liquid and nitroso-R-salt be formed is consistent, and elimination copper is to the interference of cobalt thus.But, the present invention is not limited thereto, such as, in nitrite ion not cupric or copper content extremely low, water can be used as reference liquid.In addition, according to exemplary embodiment of the present invention, the absorbance of sample solution can be measured at 530nm wavelength place.
Visible, simple to operate according to spectrophotometry for cobalt content in steel of the present invention, is that buffer solution can shield the elements such as iron, nickel, copper to the interference of measuring with sodium citrate, thus makes measurement result more accurate.
Describe in detail according to spectrophotometry for cobalt content in steel of the present invention below with reference to specific embodiment, but the present invention is not by the restriction of following specific embodiment.
In the examples below, unless otherwise indicated, otherwise the reagent used is analytical reagent, and the water of use is distilled water or deionized water.Wherein, hydrochloric acid density is 1.19g/mL, and nitric acid density is 1.42g/mL, and sulfuric acid density is 1.42g/mL, and the concentration of sodium citrate solution is 294.1g/L, and the concentration of nitroso-R-salt solution is 10g/L.
Illustrate in table 1 according to the sample of embodiment and the consumption of reagent and constant volume.
Table 1
1. dissolved samples and constant volume
Take sample by the sample size in table 1, and by the sample constant volume in table 1, sample is added in corresponding volumetric flask.Add in volumetric flask by the acid mixture that 20.0mL is formed by hydrochloric acid, nitric acid and water, low-temperature heat is dissolved completely to sample.Be cooled to room temperature, use water constant volume.If any muddiness, then can cross and filter dregs.Such as, the volume ratio of the nitric acid in dissolving acid mixture, hydrochloric acid and water can be 3: 2: 5,1: 4: 4 or 1: 12: 5, but the present invention is not limited thereto.
2. prepare measurement with sample solution (chromophoric solution)
Pipette volume according to the sample solution in table 1 sample solution after constant volume in volumetric flask is pipetted in 300 or 600mL wide mouth beaker.Add sodium citrate solution according to table 2 and mix.Add 5.0mL nitroso-R-salt solution and mix.Add 5 ~ 6 zeolites, add water to solution and be about 200mL, heating is boiled and is about 50mL to solution, is cooled to room temperature.Add sulfuric acid and the sulfuric acid solution that formed of water mixing that 20.0mL by volume ratio is 1: 1, be cooled to room temperature.Carry out constant volume according to the nitrite ion constant volume in table 2 and mix.
3. prepare reference liquid
Sulfuric acid and the sulfuric acid solution that formed of water mixing that 20mL water, 20.0mL by volume ratio are 1: 1 is added in 300 or 600mL wide mouth beaker.Add the sodium citrate solution of respective amount according to table 2 and mix.Add 5.0mL nitroso-R-salt solution and mix.Pipette according to sample solution in table 2 solution that volume pipettes respective volume, be chilled to room temperature.Accurately be settled to respective volume according to table 2 and mix.
4. on 722 type visible spectrophotometers, with the reference liquid of above-mentioned preparation for reference is in the absorbance of the nitrite ion of 530nm wavelength place measurement preparation.
5. carry out drawing standard curve according to above-mentioned steps standard cobalt liquor.
6. calculate by working curve scaling results, calculate by following formula:
In above formula, m
1for cobalt amount (g) checked in from the typical curve made.
In addition, account form is not limited to calculate cobalt content by working curve above according to an exemplary embodiment of the present invention, can also calculate cobalt content by the following method.
Take cobalt content and close two standard models (standard model 1 and standard model 2) of sample to be tested cobalt content, calculate by following formula by above analytical procedure operation:
In above formula, W (Co), W (Co)
01, W (Co)
02represent the cobalt content (weight ratio) of sample to be tested, standard model 1 and standard model 2 respectively; M, m
01, m
02represent the weight (g) of sample to be tested, standard model 1 and standard model 2 respectively; A, A
01, A
02represent the absorbance of the measurement solution that sample to be tested, standard model 1, standard model 2 are formed by above-mentioned steps respectively.
Table 2 shows the situation of the cobalt content in the various steel of cobalt content spectrophotometry in the steel according to above embodiment.
Table 2
Can be found out by the above description to exemplary embodiment of the present invention, according to spectrophotometry for cobalt content in steel of the present invention have simple to operate, sensing range is wide, testing result is accurate and the reappearance of colour developing and the advantage such as good stability.
Claims (6)
1. a spectrophotometry for cobalt content in steel, is characterized in that, in described steel, spectrophotometry for cobalt content comprises the following steps:
A) steel curved beam is dissolved to prepare sample solution with acid solution;
B) in sample solution, add sodium citrate solution, and the pH value of sample solution is adjusted to 5.5-7.5;
C) in sample solution, add nitroso-R-salt solution and heat and boil at least 30 minutes;
D) in the sample solution being cooled to room temperature, sulfuric acid solution is added, thus obtained chromophoric solution;
E) after cooling to room temperature, under the existence of reference liquid, measure the absorbance of chromophoric solution with visible spectrophotometer, thus calculate cobalt content,
Wherein, described reference liquid, by adding sodium citrate solution and nitroso-R-salt solution in sulfuric acid solution, then adds sample solution to prepare.
2. spectrophotometry for cobalt content in steel according to claim 1, is characterized in that, in step a, for dissolving the mixed acid solution that the acid solution of steel curved beam is hydrochloric acid and nitric acid.
3. spectrophotometry for cobalt content in steel according to claim 1, is characterized in that, in step a, according to the steel curved beam that the height of cobalt content in steel curved beam is measured by acid dissolve difference.
4. spectrophotometry for cobalt content in steel according to claim 1, is characterized in that, the sulfuric acid solution added in steps d is volume ratio is 98% concentrated sulphuric acid of 1:1 and the sulfuric acid solution of water.
5. spectrophotometry for cobalt content in steel according to claim 1, is characterized in that, in step e, measures the absorbance of chromophoric solution at 530nm wavelength place.
6. spectrophotometry for cobalt content in steel according to claim 1, is characterized in that, the sulfuric acid in reference liquid is identical with in the concentration preparing sulfuric acid and the nitroso-R-salt added in chromophoric solution process with the concentration of nitroso-R-salt.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210569982.7A CN103063590B (en) | 2012-12-25 | 2012-12-25 | Spectrophotometry for cobalt content in steel |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210569982.7A CN103063590B (en) | 2012-12-25 | 2012-12-25 | Spectrophotometry for cobalt content in steel |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103063590A CN103063590A (en) | 2013-04-24 |
| CN103063590B true CN103063590B (en) | 2015-12-23 |
Family
ID=48106303
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210569982.7A Active CN103063590B (en) | 2012-12-25 | 2012-12-25 | Spectrophotometry for cobalt content in steel |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103063590B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103267761B (en) * | 2013-05-31 | 2014-12-10 | 攀钢集团江油长城特殊钢有限公司 | Method for measuring cobalt content in steel |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57158556A (en) * | 1981-03-26 | 1982-09-30 | Hitachi Ltd | Cobalt analyzer |
| JPS57158555A (en) * | 1981-03-26 | 1982-09-30 | Hitachi Ltd | Method for determination of cobalt |
| JPS63124933A (en) * | 1986-11-14 | 1988-05-28 | Seiko Instr & Electronics Ltd | Composite iron-cobalt standard liquid for atomic absorption analysis |
| CN101995381A (en) * | 2010-11-10 | 2011-03-30 | 白银有色集团股份有限公司 | Method for measuring cobalt in cobalt-containing material by using 5-Cl-PADAB photometry |
| CN102353642A (en) * | 2011-07-14 | 2012-02-15 | 东北大学 | Determination method for cobalt content in high-copper high-iron cobalt ores |
-
2012
- 2012-12-25 CN CN201210569982.7A patent/CN103063590B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57158556A (en) * | 1981-03-26 | 1982-09-30 | Hitachi Ltd | Cobalt analyzer |
| JPS57158555A (en) * | 1981-03-26 | 1982-09-30 | Hitachi Ltd | Method for determination of cobalt |
| JPS63124933A (en) * | 1986-11-14 | 1988-05-28 | Seiko Instr & Electronics Ltd | Composite iron-cobalt standard liquid for atomic absorption analysis |
| CN101995381A (en) * | 2010-11-10 | 2011-03-30 | 白银有色集团股份有限公司 | Method for measuring cobalt in cobalt-containing material by using 5-Cl-PADAB photometry |
| CN102353642A (en) * | 2011-07-14 | 2012-02-15 | 东北大学 | Determination method for cobalt content in high-copper high-iron cobalt ores |
Non-Patent Citations (5)
| Title |
|---|
| 姚喆 等."亚硝基R盐分光光度法测定合金钢中钴".《中国无机分析化学》.2011,第1卷(第1期),第61-64页. * |
| 张明德."不锈钢中微量钴的测定".《特钢技术》.2005, * |
| 潘文娟."萃取分离铜、掩蔽铁、亚硝基-R盐光度法测定矿样中的钴".《中小企业管理与科技(上旬刊)》.2009, * |
| 王青 等."分光光度法测定合金中钴含量".《齐齐哈尔大学学报（自然科学版）》.2008,第24卷(第4期), * |
| 黄业初 等."亚硝基R盐快速光度法测定钴".《第三届全国高速分析学术交流会论文集》.2010,第259-262页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103063590A (en) | 2013-04-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Dickman et al. | Colorimetric determination of phosphate | |
| Walinga et al. | Spectrophotometric determination of organic carbon in soil | |
| CN103323412B (en) | Thiocyanate spectrophotometry method for detecting iron content of high-temperature alloy | |
| CN103398963B (en) | The analytical approach of phosphorus in ferrosilicon | |
| CN101424644B (en) | Vanadium content measuring method in vanadium-added or chromium-vanadium-added tungsten basal body | |
| CN102967564B (en) | Rapid determination method of molybdenum content in iron and alloys | |
| KR20120085296A (en) | Method for analyzing and detecting calcium element in ore | |
| CN101609049A (en) | The method of nickel and cobalt content in a kind of titrimetry test nickel compound | |
| CN102539426A (en) | Method for determining phosphorus in silicon-manganese alloy | |
| CN107153059A (en) | A kind of preparation method of nanogold colorimetric sensor and its application in dimercurion detection | |
| CN101660995B (en) | Method of measuring total content of rare earth in rare earth chrome-manganese-silicon inoculant | |
| CN104101576A (en) | Method for determining nickel content in steel or iron alloy | |
| CN103063590B (en) | Spectrophotometry for cobalt content in steel | |
| CN102621135A (en) | Method for detecting trace chloride ions in boiler water | |
| CN105352900A (en) | Analysis method of chromium in chromium vanadium hydrogen storage alloy | |
| CN103267761B (en) | Method for measuring cobalt content in steel | |
| CN112213279A (en) | Method for measuring iron ions in denitration absorption liquid | |
| CN103543134A (en) | Method for determining lead content in iron ore through hydride generation-atomic fluorescence spectrometry | |
| CN101995381A (en) | Method for measuring cobalt in cobalt-containing material by using 5-Cl-PADAB photometry | |
| KR101235702B1 (en) | methode for analyzing iron ion conentration in hydroponic nutrients and kits analyzing iron ion conentration in hydroponic nutrients | |
| CN112595710B (en) | Rapid detection kit and detection method for iodide ions in serum sample | |
| CN103217417B (en) | Autoanalysis method of iron content in water sample | |
| CN104089958A (en) | Determination method for content of phosphorus in niobium-containing steel | |
| CN102590115A (en) | Method for determining silica-alumina ratio in iron-containing zeolite | |
| Holak | Atomic absorption determination of boron in foods |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |