CN103308646A - Method for measuring zinc and cadmium in copper slag and copper-cadmium slag by using EDTA (Ethylene Diamine Tetraacetic Acid) volumetric method - Google Patents
Method for measuring zinc and cadmium in copper slag and copper-cadmium slag by using EDTA (Ethylene Diamine Tetraacetic Acid) volumetric method Download PDFInfo
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Abstract
The invention provides a method for measuring zinc and cadmium in copper slag and copper-cadmium slag by using an EDTA (Ethylene Diamine Tetraacetic Acid) volumetric method. In the presence of interference elements of a great amount of copper ions, iron, aluminum and the like, hydrogen peroxide is taken as the oxidizing agent and potassium fluoride as the masking agent, the pH value is controlled to be 6-6.2 by using a hexamethylenetetramine buffer solution, and the influence of the interference elements to a final point is eliminated; and the zinc-cadmium content is measured by using an EDTA complexometric titration method, and the zinc content is obtained by subtracting the cadmium content which is measured through atom absorption. The method is simple and rapid to operate; an analysis method is good in accuracy and precision and is applicable to analysis on zinc content and cadmium content in copper slag, copper-cadmium slag and sponge cadmium in a zinc hydrometallurgy system; the method plays an important role in accurate and reliable production conduction; a factory does not need to invest a great deal of extra equipment purchase expense, and the zinc content and the cadmium content in the copper slag, the copper-cadmium slag and the sponge cadmium can be rapidly and accurately measured through slight improvement on medicines.
Description
Technical field
The invention belongs to technical field of wet metallurgy, particularly the analytical approach of zinc, cadmium resultant in the samples such as copper ashes, copper-cadmium slag in a kind of wet zinc-making system.
Background technology
The copper ashes produced in hydrometallurgy process, copper-cadmium slag generally will carry out recycling, this just requires to determine quickly and accurately the content of topmost zinc impurities and cadmium in copper ashes, copper-cadmium slag, just can have accurately and instruct follow-up production after measuring this parameter, otherwise can cause a large amount of medicaments and energy dissipation.But the copper content in copper ashes and copper-cadmium slag is generally up to 20%～60%, when using classical EDTA compleximetry, the copper of high-load can have a strong impact on measurement result, in production scale, than hour this result impact, not to give prominence to especially, along with production-scale continuous expansion and vigorously advocate rule out raw material and energy dissipation instantly, this classical titrimetry be take acetic acid-sodium acetate and is controlled the appearance that pH value cadmium when 5.5～6.0 can cause titration affects terminal as buffer solution, cause titration end-point not sharp, make to analyze data unstable, can not effectively instruct production.
" Hunan non-ferrous metal " the 6th interim Wang Yong green grass or young crops in 2010 has proposed a kind of method of utilizing copper, cadmium, lead, zinc in the Rapid Determination copper-cadmium slag.The method precision is very high, but equipment investment is huge, and the test sample process is loaded down with trivial details, requires the mensuration of laboratory efficient quick in the time of can not well being applicable to factory's large-scale production.
After this in 208～209 pages of " Yunnan geology " the 30th the 2nd phases of volume in 2011, Yang Yi and Huang Xiaolin have also pointed out a large amount of drawbacks of conventional method, proposed the secondary separation method can be in laboratory the content of Accurate Determining zinc, but there is larger error at copper content in this kind of method in up to 20%～60% Specimen Determination, do not reach the purpose that actual guidance is produced, therefore be badly in need of finding a kind of energy fast, the method for zinc, cadmium in Accurate Determining copper ashes, copper-cadmium slag, and do not need extra equipment investment.
Summary of the invention
The objective of the invention is deficiency and the present situation that is not suitable with industrialization production for prior art, proposed zinc, cadmium method in a kind of EDTA volumetric determination copper ashes, copper-cadmium slag.
For reaching above-mentioned technique effect, the present invention adopts following technical scheme, and in a kind of EDTA volumetric determination copper ashes, copper-cadmium slag, zinc, cadmium method, comprise the steps:
(1) sample and sal prunella nitration mixture are added in heating container, be heated with stirring to without obvious moisture;
(2) wash chamber wall with clear water, add hydrogen peroxide to be no more than 5 minutes lower than 100 ℃ of micro-heating;
(3) add while hot the potassium fluoride saturated solution after taking off heating container, shake up and rinse the heating container wall with clear water, drip xylenol orange indicator, ascorbic acid and thiocarbamide saturated solution and shake up;
(4) add hexamethylenetetramine buffer solution in heating container, control the interior pH of heating container between 6.0～6.2, with the EDTA standard solution titration of 0.08 moL/L, it is terminal that the interior solution of heating container becomes glassy yellow by aubergine;
(5) calculate with EDTA complexometric titration zinc cadmium resultant, deduct the cadmium amount recorded by Atomic absorption, be the zinc amount.
Preferably, described sal prunella nitration mixture is used the nitric acid of ρ=1.37g/mL and the hydrochloric acid of ρ=1.19g/mL, and the mass percent of hydrogen peroxide is 30%, and xylenol orange density is 0.5g/L, the pH=5.8 of hexamethylenetetramine buffer solution～6.2, potassium fluoride, ascorbic acid and thiocarbamide are all used analysis pure.
Preferably, when the tested sample unit mass is 0.20g, the using dosage of other medicaments is hydrochloric acid 8～15mL, nitric acid 2～5mL, hydrogen peroxide is less than 1 mL, potassium fluoride saturated solution 3～10mL, 1～2 of xylenol orange indicator, ascorbic acid 0.1g, thiocarbamide saturated solution 10～25mL.
Preferably, when the tested sample unit mass is 0.20g, the using dosage of other medicaments is hydrochloric acid 10mL, nitric acid 3mL, 5 of hydrogen peroxide, potassium fluoride saturated solution 5mL, 1～2 of xylenol orange indicator, ascorbic acid 0.1g, thiocarbamide saturated solution 20mL.
Beneficial effect of the present invention:
The invention provides zinc, cadmium method in a kind of EDTA volumetric determination copper ashes, copper-cadmium slag, under the existence of the interference elements such as a large amount of copper ions and iron, aluminium, take hydrogen peroxide as oxygenant, take potassium fluoride as screening agent, control the pH value 6～6.2 with hexamethylenetetramine buffer solution, eliminate the impact of interference element on terminal, with EDTA complexometric titration zinc cadmium resultant, deduct the cadmium amount recorded by Atomic absorption, be the zinc amount.
This method is simple to operate fast, and the accuracy of analytical approach, precision are good, be applicable to very much the analysis of zinc, cadmium content in copper ashes in wet zinc-making system, copper-cadmium slag, Spongy Cadmium, for instructing accurately and reliably to produce, important effect is arranged, factory need not additionally drop into a large amount of equipment purchasing expenses, and only aspect medicament, a small amount of improvement can be measured again zinc, cadmium content in copper ashes, copper-cadmium slag, Spongy Cadmium fast accurately.
Embodiment
Following example can further illustrate the present invention, the reagent that uses:
Potassium fluoride (analyzing pure);
Ascorbic acid (analyzing pure);
Nitric acid (ρ=1.37g/mL);
Hydrochloric acid (ρ=1.19g/mL);
Hydrogen peroxide (30%);
Xylenol orange (0.5g/L);
Hexamethylenetetramine buffer solution (PH=5.8～6.2);
Thiocarbamide (analyzing pure);
EDTA standard titration solution (0.08mol/L): prepare according to a conventional method, demarcate.
Embodiment 1-5
Accurately take sample 0.2000g in 500mL circular cone beaker, add respectively hydrochloric acid 5mL, 8mL, 10mL, 15mL, 20mL
,nitric acid 3mL heats near dry on electric hot plate, takes off to wash wall of cup, adds 5 hydrogen peroxide low-grade fever numbers minute, takes off and adds while hot 5mL potassium fluoride saturated solution, shakes up, with the washing wall of cup.Add water to after cooling the about 80mL of volume left and right, add 1～2 xylenol orange indicator, 0.1g ascorbic acid, 20mL thiocarbamide saturated solution, shake up, add 20mL hexamethylenetetramine buffer solution, controlling pH value is between 6～6.2, and being titrated to solution with the EDTA standard solution of 0.08 mol/L, to become glassy yellow by aubergine be terminal.The results are shown in Table 1.
Result shows, the hydrochloric acid consumption at 5～20mL on measurement result without obvious impact, hydrochloric acid consumption 10mL when this determination experiment is chosen in sample and is 0.2g.
Embodiment 6～10
Accurately take sample 0.2000g in 500mL circular cone beaker, add hydrochloric acid 10mL, add respectively nitric acid 2mL, 3mL, 5mL, 10mL, 15mL to heat on electric hot plate near dry, take off to wash wall of cup, add 5 hydrogen peroxide low-grade fever numbers minute, take off and add while hot 5mL potassium fluoride saturated solution, shake up, with the washing wall of cup.Add water to after cooling the about 80mL of volume left and right, add 1～2 xylenol orange indicator, 0.1g ascorbic acid, 20mL thiocarbamide saturated solution, shake up, add 20mL hexamethylenetetramine buffer solution, controlling pH value is between 6～6.2, and being titrated to solution with the EDTA standard solution of 0.08 mol/L, to become glassy yellow by aubergine be terminal.The results are shown in Table 2.
Experimental data shows, when sample is 0.2g, nitric acid dosage is influential to measuring too greatly, should strictly control nitric acid dosage between 2～5mL, and it is 3mL that this determination experiment is selected nitric acid dosage.
embodiment 11-14
Accurately take sample 0.2000g in 500mL circular cone beaker, add hydrochloric acid 10mL, nitric acid 3mL heats near dry on electric hot plate, take off to wash wall of cup, add respectively 2～3,0.5mL, 1mL, 2mL hydrogen peroxide low-grade fever number minute, take off and add while hot 5mL potassium fluoride saturated solution, shake up, with the washing wall of cup.Add water to after cooling the about 80mL of volume left and right, add 1～2 xylenol orange indicator, 0.1g ascorbic acid, 20mL thiocarbamide saturated solution, shake up, add 20mL hexamethylenetetramine buffer solution, controlling pH value is between 6～6.2, and being titrated to solution with the EDTA standard solution of 0.08 mol/L, to become glassy yellow by aubergine be terminal.The results are shown in Table 3.
Result shows, when sample is 0.2g, the consumption of hydrogen peroxide 1mL with interior on measurement result without obvious impact, should strictly control the consumption of hydrogen peroxide, it is 0.5mL that this determination experiment is selected the consumption of hydrogen peroxide.
Result shows, when sample is 0.2g, the consumption of hydrogen peroxide 1mL with interior on measurement result without obvious impact, should strictly control the consumption of hydrogen peroxide, it is 0.5mL that this determination experiment is selected the consumption of hydrogen peroxide.
embodiment 15-19
Accurately take sample 0.2000g in 500mL circular cone beaker, add hydrochloric acid 10mL, nitric acid 3mL heats near dry on electric hot plate, take off to wash wall of cup, add 5 hydrogen peroxide low-grade fever numbers minute, take off and add respectively while hot 3mL, 5mL, 10mL, 15mL, 20mL potassium fluoride saturated solution, shake up, with the washing wall of cup.Add water to after cooling the about 80mL of volume left and right, add 1～2 xylenol orange indicator, 0.1g ascorbic acid, 20mL thiocarbamide saturated solution, shake up, add 20mL hexamethylenetetramine buffer solution, controlling pH value is between 6～6.2, and being titrated to solution with the EDTA standard solution of 0.08 mol/L, to become glassy yellow by aubergine be terminal.The results are shown in Table 4.
Result shows, when sample is 0.2g, the potassium fluoride consumption should strictly be controlled the consumption of potassium fluoride with interior to measuring without significantly impact at 10mL, and it is 5mL that this determination experiment is selected potassium fluoride consumption
.
embodiment 20-24
Accurately take sample 0.2000g in 500mL circular cone beaker, add hydrochloric acid 10mL, nitric acid 3mL heats near dry on electric hot plate, take off to wash wall of cup, add 5 hydrogen peroxide low-grade fever numbers minute, take off and add while hot 5mL potassium fluoride saturated solution, shake up, with the washing wall of cup.Add water to after cooling the about 80mL of volume left and right, add 1～2 xylenol orange indicator, 0.1g ascorbic acid, add respectively 5mL, 10mL, 15mL, 20mL, 25mL thiocarbamide saturated solution, shake up, add 20mL hexamethylenetetramine buffer solution, controlling the pH value is between 6～6.2, and being titrated to solution with the EDTA standard solution of 0.08 mol/L, to become glassy yellow by aubergine be terminal.The results are shown in Table 5.
Result shows, thiocarbamide can't be eliminated the interference of copper during by quantity not sufficient, affects measurement result, and it is 20mL that this determination experiment is selected thiocarbamide consumption.
embodiment 25
Take tri-parts of parallel samples of 0.2000g, add respectively zinc standard 20mg, 30mg, 100mg, add hydrochloric acid 10mL, nitric acid 3mL heats near dry on electric hot plate, take off to wash wall of cup, add 5 hydrogen peroxide low-grade fever numbers minute, take off and add while hot 5mL potassium fluoride saturated solution, shake up, with the washing wall of cup.Add water to after cooling the about 80mL of volume left and right, add 1～2 xylenol orange indicator, 0.1g ascorbic acid, add 20mL thiocarbamide saturated solution, shake up, add hexamethylenetetramine buffer solution, controlling pH value is between 6～6.2, and being titrated to solution with the EDTA standard solution of 0.08 mol/L, to become glassy yellow by aubergine be terminal.The results are shown in Table 6.
From the table, in laboratory the accuracy of this method higher, can meet the analysis of zinc, cadmium resultant in the sample such as copper ashes, copper-cadmium slag in Zinc hydrometallurgy process fully.
embodiment 26
In actual production, take sample 0.2000g in 500mL circular cone beaker, add 10mL hydrochloric acid, 3mL nitric acid, on electric hot plate, heating is near does, and takes off to wash wall of cup, adds 5 hydrogen peroxide low-grade fever numbers minute, take off and add while hot 5mL potassium fluoride saturated solution, shake up, with the washing wall of cup.Add water to after cooling the about 80mL of volume left and right, add 1～2 xylenol orange indicator, 0.1g ascorbic acid, 20mL thiocarbamide saturated solution, shake up, add 20mL hexamethylenetetramine buffer solution, controlling pH value is between 6～6.2, and being titrated to solution with the EDTA standard solution of 0.08 mol/L, to become glassy yellow by aubergine be terminal.The results are shown in Table 7.
The invention provides zinc, cadmium method in a kind of EDTA volumetric determination copper ashes, copper-cadmium slag, under the existence of the interference elements such as a large amount of copper ions and iron, aluminium, take hydrogen peroxide as oxygenant, take potassium fluoride as screening agent, control the pH value 6～6.2 with hexamethylenetetramine buffer solution, eliminate the impact of interference element on terminal, with EDTA complexometric titration zinc cadmium resultant, deduct the cadmium amount recorded by Atomic absorption, be the zinc amount.
This method is simple to operate fast, and the accuracy of analytical approach, precision are good, be applicable to very much the analysis of zinc, cadmium content in copper ashes in wet zinc-making system, copper-cadmium slag, Spongy Cadmium, for instructing accurately and reliably to produce, important effect is arranged, factory need not additionally drop into a large amount of equipment purchasing expenses, and only aspect medicament, a small amount of improvement can be measured again zinc, cadmium content in copper ashes, copper-cadmium slag, Spongy Cadmium fast accurately.
Above-described is only preferred embodiment of the present invention.Should be understood that for the person of ordinary skill of the art, under technology enlightenment provided by the present invention, as the common practise of this area, can also make other equivalent modifications and improvement, also should be considered as protection scope of the present invention.
Claims (4)
1. zinc, cadmium method in an EDTA volumetric determination copper ashes, copper-cadmium slag, it is characterized in that: described method comprises the steps:
(1) sample and sal prunella nitration mixture are added in heating container, be heated with stirring to without obvious moisture;
(2) wash chamber wall with clear water, add hydrogen peroxide to be no more than 5 minutes lower than 100 ℃ of micro-heating;
(3) add while hot the potassium fluoride saturated solution after taking off heating container, shake up and rinse the heating container wall with clear water, drip xylenol orange indicator, ascorbic acid and thiocarbamide saturated solution and shake up;
(4) add hexamethylenetetramine buffer solution in heating container, control the interior pH of heating container between 6.0～6.2, with the EDTA standard solution titration of 0.08 moL/L, it is terminal that the interior solution of heating container becomes glassy yellow by aubergine;
(5) calculate with EDTA complexometric titration zinc cadmium resultant, deduct the cadmium amount recorded by Atomic absorption, be the zinc amount.
2. zinc, cadmium method in a kind of EDTA volumetric determination copper ashes, copper-cadmium slag according to claim 1, it is characterized in that: described sal prunella nitration mixture is used the nitric acid of ρ=1.37g/mL and the hydrochloric acid of ρ=1.19g/mL, the mass percent of hydrogen peroxide is 30%, xylenol orange density is 0.5g/L, the pH=5.8 of hexamethylenetetramine buffer solution～6.2, potassium fluoride, ascorbic acid and thiocarbamide are all used analysis pure.
3. zinc, cadmium method in a kind of EDTA volumetric determination copper ashes, copper-cadmium slag according to claim 1, it is characterized in that: when the tested sample unit mass is 0.20g, the using dosage of other medicaments is hydrochloric acid 8～15mL, nitric acid 2～5mL, hydrogen peroxide is less than 1 mL, potassium fluoride saturated solution 3～10mL, 1～2 of xylenol orange indicator, ascorbic acid 0.1g, thiocarbamide saturated solution 10～25mL.
4. zinc, cadmium method in a kind of EDTA volumetric determination copper ashes, copper-cadmium slag according to claim 1, it is characterized in that: when the tested sample unit mass is 0.20g, the using dosage of other medicaments is hydrochloric acid 10mL, nitric acid 3mL, 5 of hydrogen peroxide, potassium fluoride saturated solution 5mL, xylenol orange indicator 1-2 drips, ascorbic acid 0.1g, thiocarbamide saturated solution 20mL.
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| CN102590122A (en) * | 2012-01-17 | 2012-07-18 | 佛山市邦普循环科技有限公司 | Method for measuring cadmium content in waste nickel-cadmium battery |
| CN103512881A (en) * | 2013-09-22 | 2014-01-15 | 南通新邦化工科技有限公司 | Method for detecting metal ion contents in zinc stearate and calcium stearate composite salt |
| CN104749318A (en) * | 2013-12-30 | 2015-07-01 | 北京有色金属与稀土应用研究所 | Method for volumetric method determination of zinc content in silver copper zinc cadmium nickel solder |
| CN105181691A (en) * | 2015-09-29 | 2015-12-23 | 聊城市鲁西化工工程设计有限责任公司 | Detection method for content of zinc in benzene hydrogenation catalyst |
| CN105445414A (en) * | 2015-12-17 | 2016-03-30 | 天津神能科技有限公司 | Chemical analysis determination method of zinc content of molecular sieve |
| CN107132219A (en) * | 2017-05-15 | 2017-09-05 | 长春黄金研究院 | A kind of method for continuously measuring of Zinc in Zinc Concentrates and iron content |
| CN110132956A (en) * | 2019-06-14 | 2019-08-16 | 云南三环中化化肥有限公司 | The rapid assay methods of Zn content in a kind of fertilizer |
| CN110596032A (en) * | 2019-10-25 | 2019-12-20 | 贺州学院 | Method for detecting zinc content in tea |
| CN110907594A (en) * | 2019-11-22 | 2020-03-24 | 西北矿冶研究院 | Chemical analysis method for measuring cadmium in crude cadmium based on increased complexing stability constant |
| CN111458332A (en) * | 2020-05-11 | 2020-07-28 | 西安西北有色地质研究院有限公司 | Method for measuring lead, zinc and cadmium from mixed lead-zinc-cadmium concentrate |
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| CN102590122A (en) * | 2012-01-17 | 2012-07-18 | 佛山市邦普循环科技有限公司 | Method for measuring cadmium content in waste nickel-cadmium battery |
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| CN103512881A (en) * | 2013-09-22 | 2014-01-15 | 南通新邦化工科技有限公司 | Method for detecting metal ion contents in zinc stearate and calcium stearate composite salt |
| CN104749318A (en) * | 2013-12-30 | 2015-07-01 | 北京有色金属与稀土应用研究所 | Method for volumetric method determination of zinc content in silver copper zinc cadmium nickel solder |
| CN105181691A (en) * | 2015-09-29 | 2015-12-23 | 聊城市鲁西化工工程设计有限责任公司 | Detection method for content of zinc in benzene hydrogenation catalyst |
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| CN107132219A (en) * | 2017-05-15 | 2017-09-05 | 长春黄金研究院 | A kind of method for continuously measuring of Zinc in Zinc Concentrates and iron content |
| CN110132956A (en) * | 2019-06-14 | 2019-08-16 | 云南三环中化化肥有限公司 | The rapid assay methods of Zn content in a kind of fertilizer |
| CN110596032A (en) * | 2019-10-25 | 2019-12-20 | 贺州学院 | Method for detecting zinc content in tea |
| CN110907594A (en) * | 2019-11-22 | 2020-03-24 | 西北矿冶研究院 | Chemical analysis method for measuring cadmium in crude cadmium based on increased complexing stability constant |
| CN111458332A (en) * | 2020-05-11 | 2020-07-28 | 西安西北有色地质研究院有限公司 | Method for measuring lead, zinc and cadmium from mixed lead-zinc-cadmium concentrate |
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Application publication date: 20130918 |