CN101995381A - Method for measuring cobalt in cobalt-containing material by using 5-Cl-PADAB photometry - Google Patents
Method for measuring cobalt in cobalt-containing material by using 5-Cl-PADAB photometry Download PDFInfo
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- CN101995381A CN101995381A CN 201010538494 CN201010538494A CN101995381A CN 101995381 A CN101995381 A CN 101995381A CN 201010538494 CN201010538494 CN 201010538494 CN 201010538494 A CN201010538494 A CN 201010538494A CN 101995381 A CN101995381 A CN 101995381A
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Abstract
The invention discloses a method for measuring cobalt in a cobalt-containing material by using 5-Cl-PADAB photometry and a testing agent preparation method thereof. The cobalt is complexed with a color developer testing agent under the pH of 5.5 to 6.0, and the cobalt is developed obviously and stably under the action of sulfur-phosphorus mixed acid so as to perform colorimetric determination. Over high cobalt content of purified liquid and electrolyzed new liquid affects the next process; in particular in the purification process of the cobalt, the cobalt content in the flow needs well control; and the method for measuring the cobalt by the testing agent spectrophotometry has the advantages of high accuracy, good precision and high analysis speed, can meet quick analysis in the production, and provides accurate and reliable data for well guiding the production.
Description
Technical field
The invention belongs to the analytical approach of cobalt element in a kind of zinc lixiviating solution, scavenging solution, the new liquid of electrolysis, particularly a kind of 5-Cl-PADAB spectrphotometric method for measuring contains the method and the test agent preparation method thereof of cobalt in the cobalt material.
Background technology
Prior art is measured zinc all the time and is smelted atomic absorption spectrography (AAS) commonly used of the cobalt in the various liquid and nitroso-R salt photometry in the wet method system, but because the interference of zinc-base body makes that the result of cobalt is higher, had a strong impact on the accuracy that cobalt is analyzed during the cobalt in the above material of aas determination.And the nitroso-R salt photometry is because the interference of zinc-base body makes the analysis poor stability of cobalt, the accuracy of cobalt analysis can not be satisfied with precision produce the analysis requirement.
Summary of the invention
The object of the present invention is to provide a kind of spectrphotometric method for measuring of test agent accurately and reliably to contain the method for cobalt in the cobalt material, solved the inaccurate reliable problem of use atomic absorption spectrography (AAS) and nitroso-R salt spectrphotometric method for measuring result.
The method step that 5-Cl-PADAB spectrphotometric method for measuring of the present invention contains cobalt in the cobalt material is as follows:
Accurately pipette 2.00ml and contain the cobalt test solution in the 100ml beaker, add 2.0-10.0ml acetate-sodium acetate buffer then, mixing accurately moves into 1.00-4.00ml test agent ethanol liquid, mixing again, with water purge walls of beaker, cover the table ware, be heated to boiling again, and keep taking off behind the 1-6min, add 2.0-15.0ml sulphur-phosphorus nitration mixture immediately, mixing is cooled to room temperature, moves in the 50ml color comparison tube, be diluted with water to scale 50ml, mixing is measured on spectrophotometer behind the placement 5-120 min, is reference with the reagent blank, use the 2cm cuvette, carry out absorbance measurement at the 560-580nm place.
The preferred 5.0ml of the consumption of acetate-sodium acetate buffer, preferred 2.00 ml of the consumption of test agent, preferred 3 min of boiling time, preferred 10.0 ml of the consumption of sulphur-phosphorus nitration mixture, preferred 5 min of developing time, wavelength is selected 570nm.
This method is achieved in that cobalt and the complexing of developer test agent under the condition of PH5.5-6.0, and colour developing is obvious and stable under the effect of mixture of sulfuric phosphoric acid, carries out colorimetric estimation.
The too high levels of cobalt can influence next process in the new liquid of scavenging solution and electrolysis, especially in the purification process of cobalt, the content that needs cobalt in the control flow well, test agent spectrophotometry cobalt, the method has the accuracy height, and precision is good, the advantage that analysis speed is fast, can satisfy the express-analysis in the production, data accurately and reliably are provided simultaneously, instruct production well.
Embodiment
The following examples can further specify the present invention, but do not limit the present invention in any way.
The collocation method of reagent is as follows:
Acetate-sodium acetate buffer (PH=5.5 ~ 6.0): the 150g anhydrous sodium acetate is dissolved in the suitable quantity of water, adds the 20ml glacial acetic acid, is diluted to 1000ml with water, mixing;
New cobalt reagent ethanolic solution (0.0016mol/l): accurately take by weighing the new cobalt reagent of 0.2000 g, put into 500 ml volumetric flasks, behind an amount of anhydrous alcohol solution, use the absolute ethyl alcohol constant volume, shake up;
Sulphur-phosphorus nitration mixture (14.4mol/L ~ 2.92mol/L): accurately measure 1000 ml water in 2000 ml beakers, measure the 800 ml concentrated sulphuric acids, slowly pour in the beaker that 1000 ml are housed, constantly stir, add 200 ml phosphoric acid again, stir, cooling with glass bar;
Accurately pipette 2.00ml and contain the cobalt test solution in the 100ml beaker, add 5.0ml acetate-sodium acetate buffer, mixing accurately moves into the new cobalt reagent ethanol of 2.00ml liquid, mixing, with water purge walls of beaker, lid table ware, heated and boiled 3min takes off, add 10.0ml sulphur ~ phosphorus nitration mixture immediately, mixing is cooled to room temperature, moves in the 50ml color comparison tube, be diluted with water to scale, mixing is placed and is measured on spectrophotometer after 5 minutes, is reference with the reagent blank, use the 2cm cuvette, carry out absorbance measurement at the 570nm place.
Embodiment 1
Get the scavenging solution sample, accurately pipette 2.00ml in the 100ml beaker, add 5.0ml acetate-sodium acetate buffer, mixing, accurately move into 2.00ml test agent ethanol liquid, mixing, with water purge walls of beaker, lid table ware, be heated to and boil and keep 3min, take off, add 10.0ml sulphur-phosphorus nitration mixture immediately, mixing, be cooled to room temperature, move in the 50ml color comparison tube, be diluted with water to scale, mixing, place and on spectrophotometer, measure after 5 minutes, with the reagent blank is reference, uses the 2cm cuvette, carries out absorbance measurement at the 570nm place.
The mean value of cobalt content is 0.32mg/l in 10 working samples, standard deviation 0.02, relative standard deviation 0.062%.
Embodiment 2-6
Accurately pipette 2.00ml scavenging solution 1 and place the 100ml beaker with scavenging solution 2, add 5.0ml acetate-sodium acetate buffer, mixing accurately moves into 2.00ml test agent ethanol liquid, mixing, with water purge walls of beaker, lid table ware is heated to and boils and keep 3min, takes off, add 10.0ml sulphur-phosphorus nitration mixture immediately, mixing is cooled to room temperature, moves in the 50ml color comparison tube, be diluted with water to scale, mixing is placed and is measured on spectrophotometer after 5 minutes, is reference with the reagent blank, use the 2cm cuvette, respectively at spectrophotometer 560nm, 565 nm, 570 nm, 575 nm, 580 nm places carry out absorbance measurement.Its experiment the results are shown in Table 1.
Table 1 wavelength is to the influence of absorbance
| ? | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| Wavelength (nm) | 560 | 565 | 570 | 575 | 580 |
| Scavenging solution 1 absorbance | 0.111 | 0.122 | 0.144 | 0.112 | 0.092 |
| Scavenging solution 2 absorbances | 0.211 | 0.219 | 0.236 | 0.214 | 0.191 |
The absorbance maximum that records at 570 nm places of wavelength as can be seen from Table 1, and analyze linear well herein, so the present invention adopts 570 nm place measurement effects best.
Embodiment 7-12
Accurately pipetting 2.00ml contains the cobalt test solution and places the 100ml beaker, add 5.0ml acetate-sodium acetate buffer, mixing accurately moves into 2.00ml test agent ethanol liquid, mixing, with water purge walls of beaker, lid table ware is heated to and boils and keep 3min, takes off, add 10.0ml sulphur-phosphorus nitration mixture immediately, mixing is cooled to room temperature, moves in the 50ml color comparison tube, be diluted with water to scale, mixing places 5,15,30,60,90, respectively at measuring on the spectrophotometer, be reference after 120 minutes with the reagent blank, use the 2cm cuvette, 570 nm places carry out absorbance measurement in spectrophotometer.Its experiment the results are shown in Table 2
Table 2 chromophoric solution stability
| ? | Embodiment 7 | Embodiment 8 | Embodiment 9 | Embodiment 10 | Embodiment 11 | Embodiment 12 |
| Time (branch) | 5 | 15 | 30 | 60 | 90 | 120 |
| Light absorption value | 0.142 | 0.144 | 0.143 | 0.143 | 0.142 | 0.142 |
As seen after placing 5 minutes colour developing fully, and one hour internal absorbance do not have significant change, places and measures after 5 minutes in order to adapt to this test and Selection of express-analysis.
Implement 13-16
Accurately pipetting 2.00ml respectively contains the cobalt test solution and places the 100ml beaker respectively for 4 parts, add 5.0ml acetate-sodium acetate buffer, mixing accurately moves into 1.00 respectively, 2.00,3.00,4.00ml test agent ethanol liquid, mixing, with water purge walls of beaker, lid table ware is heated to and boils and keep 3min, takes off, add 10.0ml sulphur-phosphorus nitration mixture immediately, mixing is cooled to room temperature, moves in the 50ml color comparison tube, be diluted with water to scale, mixing is placed after 5 minutes respectively at measuring on the spectrophotometer, is reference with the reagent blank, use the 2cm cuvette, 570 nm places carry out absorbance measurement in spectrophotometer.Its experiment the results are shown in Table 3
Table 3 test agent consumption is to the influence of absorbance
| ? | Embodiment 13 | Embodiment 14 | Embodiment 15 | Embodiment 16 |
| Developer (ml) | 1.00 | 2.00 | 3.00 | 4.00 |
| Light absorption value | 0.137 | 0.143 | 0.144 | 0151 |
As seen add the 2.00-3.00ml test agent, light absorption value is constant substantially, and 2.00ml is selected in test determination.
Embodiment 17-22
Accurately pipetting 2.00ml respectively contains the cobalt test solution and places the 100ml beaker respectively for 6 parts, add 2.0 respectively, 4.0,5.0,6.0,8.0,10.0ml acetate-sodium acetate buffer, mixing accurately moves into 2.00ml test agent ethanol liquid, mixing, with water purge walls of beaker, lid table ware is heated to and boils and keep 3min, takes off, add 10.0ml sulphur-phosphorus nitration mixture immediately, mixing is cooled to room temperature, moves in the 50ml color comparison tube, be diluted with water to scale, mixing is placed after 5 minutes respectively at measuring on the spectrophotometer, is reference with the reagent blank, use the 2cm cuvette, 570 nm places carry out absorbance measurement in spectrophotometer.Its experiment the results are shown in Table 4
Table 4 acetate-sodium acetate buffer solution consumption is to the influence of absorbance
| ? | Embodiment 17 | Embodiment 18 | Embodiment 19 | Embodiment 20 | Embodiment 21 | Embodiment 22 |
| Damping fluid (ml) | 2.0 | 4.0 | 5.0 | 6.0 | 8.0 | 10.0 |
| Light absorption value | 0.131 | 0.140 | 0.143 | 0.144 | 0.151 | 0.155 |
As seen acetate-sodium acetate buffer addition during at 5.0-6.0ml absorbance constant substantially, select 5.0ml during mensuration.
Embodiment 23-27
Accurately pipetting 2.00ml respectively contains the cobalt test solution and places the 100ml beaker respectively for 4 parts, add 5.0ml acetate-sodium acetate buffer respectively, mixing accurately moves into 2.00ml test agent ethanol liquid, mixing, with water purge walls of beaker, lid table ware, being heated to boils keeps 3min, takes off, add 2.0 respectively immediately, 5.0,10.0,15.0ml sulphur-phosphorus nitration mixture, mixing is cooled to room temperature, moves in the 50ml color comparison tube, be diluted with water to scale, mixing is placed after 5 minutes respectively at measuring on the spectrophotometer, is reference with the reagent blank, use the 2cm cuvette, 570 nm places carry out absorbance measurement in spectrophotometer.Its experiment the results are shown in Table 5.
Table 5 sulphur-phosphorus nitration mixture consumption is to the influence of absorbance
| ? | Embodiment 24 | Embodiment 25 | Embodiment 26 | Embodiment 27 |
| Sulphur-phosphorus nitration mixture (ml) | 2.0 | 5.0 | 10.0 | 15.0 |
| Light absorption value | 0.130 | 0.143 | 0.144 | 0.156 |
As seen sulphur-phosphorus nitration mixture addition absorbance when 5.0-10.0ml is constant substantially, selects 10.0ml during mensuration.
Embodiment 28-27
Accurately pipetting 2.00ml respectively contains the cobalt test solution and places the 100ml beaker respectively for 6 parts, add 5.0ml acetate-sodium acetate buffer respectively, mixing accurately moves into 2.00ml test agent ethanol liquid, mixing, with water purge walls of beaker, lid table ware is heated to respectively and boils and keep 1,2,3,4,5,6min takes off, add 10.0ml sulphur-phosphorus nitration mixture immediately respectively, mixing is cooled to room temperature, moves in the 50ml color comparison tube, be diluted with water to scale, mixing is placed after 5 minutes respectively at measuring on the spectrophotometer, is reference with the reagent blank, use the 2cm cuvette, 570 nm places carry out absorbance measurement in spectrophotometer.Its experiment the results are shown in Table 6.
The influence of table 6 boiling time absorbance
| ? | Embodiment 28 | Embodiment 29 | Embodiment 30 | Embodiment 31 | Embodiment 32 | Embodiment 33 |
| Boiling time (branch) | 1 | 2 | 3 | 4 | 5 | 6 |
| Light absorption value | 0.136 | 0.143 | 0.143 | 0.143 | 0.144 | 0.143 |
As seen boiling time light absorption value after 2 minutes is stable.It is 3 minutes that this method is selected boiling time.
Embodiment 34-39
ZnSO in zinc lixiviating solution, scavenging solution, the new liquid of electrolysis
4Content draws 1 respectively now at 140-170g/l
#Sample 2.00,3.00,4.00,5.00,6.00,7.00ml two groups in the 100ml beaker, wherein one group accurately adds 2.00ug cobalt standard respectively, every group of sample adds 5.0ml acetate-sodium acetate buffer respectively then, mixing, accurately move into 2.00ml test agent ethanol liquid, mixing, with water purge walls of beaker, lid table ware, be heated to respectively and boil and keep 3min, take off, add 10.0ml sulphur-phosphorus nitration mixture immediately respectively, mixing, be cooled to room temperature, move in the 50ml color comparison tube, be diluted with water to scale, mixing, place after 5 minutes respectively at measuring on the spectrophotometer, with the reagent blank is reference, uses the 2cm cuvette, and 570 nm places carry out absorbance measurement in spectrophotometer.Its experiment the results are shown in Table 7.
Table 7 zinc-base body is to the influence of absorbance
| ? | Embodiment 34 | Embodiment 35 | Embodiment 36 | Embodiment 37 | Embodiment 38 | Embodiment 39 |
| Sample (ml) | 2.00 | 3.00 | 4.00 | 5.00 | 6.00 | 7.00 |
| Absorbance (sample adds standard) | 0.193 | 0.213 | 0.238 | 0.263 | 0.286 | 0.309 |
| Absorbance (sample) | 0.049 | 0.071 | 0.096 | 0.119 | 0.142 | 0.164 |
| Absorbance (standard) | 0.144 | 0.142 | 0.142 | 0.144 | 0.144 | 0.145 |
As seen the zinc sulfate matrix does not obviously disturb the method.
Embodiment 40
Draw 1 respectively now
#4 parts of sample 2.00ml are in the 100ml beaker, accurately add certain cobalt standard solutions in three parts of difference wherein, add 5.0ml acetate-sodium acetate buffer, mixing then respectively, accurately move into 2.00ml test agent ethanol liquid, mixing, with water purge walls of beaker, lid table ware, be heated to respectively and boil and keep 3min, take off, add 10.0ml sulphur-phosphorus nitration mixture immediately respectively, mixing, be cooled to room temperature, move in the 50ml color comparison tube, be diluted with water to scale, mixing, place after 5 minutes respectively at measuring on the spectrophotometer, with the reagent blank is reference, uses the 2cm cuvette, and 570 nm places carry out absorbance measurement in spectrophotometer.Its experiment the results are shown in Table 7
Table 7 mark-on reclaims experiment
Test as can be seen by recovery of standard addition that this method has high accuracy, can satisfy the express-analysis of cobalt fully, can be used for checking the cobalt in zinc lixiviating solution, the new liquid of electrolysis, certain practical value is arranged.
Claims (6)
1. a 5-Cl-PADAB spectrphotometric method for measuring contains the method for cobalt in the cobalt material, and it is characterized in that: the step of described this method is as follows,
Accurately pipette 2.00ml and contain the cobalt test solution in the 100ml beaker, add 2.0-10.0ml acetate-sodium acetate buffer then, mixing accurately moves into 1.00-4.00ml test agent ethanol liquid, mixing again, with water purge walls of beaker, cover the table ware, be heated to boiling again, and keep taking off behind the 1-6min, add 2.0-15.0ml sulphur-phosphorus nitration mixture immediately, mixing is cooled to room temperature, moves in the 50ml color comparison tube, be diluted with water to scale 50ml, mixing is measured on spectrophotometer behind the placement 5-120 min, is reference with the reagent blank, use the 2cm cuvette, carry out absorbance measurement at the 560-580nm place.
2. a kind of 5-Cl-PADAB spectrphotometric method for measuring according to claim 1 contains the method for cobalt in the cobalt material, it is characterized in that: the preferable amount of acetate-sodium acetate buffer is 5.0ml.
3. a kind of 5-Cl-PADAB spectrphotometric method for measuring according to claim 1 contains the method for cobalt in the cobalt material, it is characterized in that: the preferable amount of test agent is 2.00 ml.
4. a kind of 5-Cl-PADAB spectrphotometric method for measuring according to claim 1 contains the method for cobalt in the cobalt material, it is characterized in that: boiling the preferred time is 3 min.
5. a kind of 5-Cl-PADAB spectrphotometric method for measuring according to claim 1 contains the method for cobalt in the cobalt material, it is characterized in that: the preferable amount of sulphur-phosphorus nitration mixture is 10.0 ml.
6. a kind of 5-Cl-PADAB spectrphotometric method for measuring according to claim 1 contains the method for cobalt in the cobalt material, it is characterized in that: developing time is preferably 5 min, and wavelength is chosen as 570nm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103063590A (en) * | 2012-12-25 | 2013-04-24 | 攀钢集团江油长城特殊钢有限公司 | Spectrophotometry for cobalt content in steel |
| CN103267761A (en) * | 2013-05-31 | 2013-08-28 | 攀钢集团江油长城特殊钢有限公司 | Method for measuring cobalt content in steel |
| CN103308646A (en) * | 2013-06-30 | 2013-09-18 | 白银有色集团股份有限公司 | Method for measuring zinc and cadmium in copper slag and copper-cadmium slag by using EDTA (Ethylene Diamine Tetraacetic Acid) volumetric method |
| CN106841180A (en) * | 2015-12-03 | 2017-06-13 | 北京有色金属研究总院 | A kind of method for continuously measuring of Platinum in Ore, palladium |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103063590A (en) * | 2012-12-25 | 2013-04-24 | 攀钢集团江油长城特殊钢有限公司 | Spectrophotometry for cobalt content in steel |
| CN103063590B (en) * | 2012-12-25 | 2015-12-23 | 攀钢集团江油长城特殊钢有限公司 | Spectrophotometry for cobalt content in steel |
| CN103267761A (en) * | 2013-05-31 | 2013-08-28 | 攀钢集团江油长城特殊钢有限公司 | Method for measuring cobalt content in steel |
| CN103308646A (en) * | 2013-06-30 | 2013-09-18 | 白银有色集团股份有限公司 | Method for measuring zinc and cadmium in copper slag and copper-cadmium slag by using EDTA (Ethylene Diamine Tetraacetic Acid) volumetric method |
| CN106841180A (en) * | 2015-12-03 | 2017-06-13 | 北京有色金属研究总院 | A kind of method for continuously measuring of Platinum in Ore, palladium |
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Application publication date: 20110330 |