CN104049028A - Determination method for cadmium amount in copper slag - Google Patents
Determination method for cadmium amount in copper slag Download PDFInfo
- Publication number
- CN104049028A CN104049028A CN201410260300.3A CN201410260300A CN104049028A CN 104049028 A CN104049028 A CN 104049028A CN 201410260300 A CN201410260300 A CN 201410260300A CN 104049028 A CN104049028 A CN 104049028A
- Authority
- CN
- China
- Prior art keywords
- hydrochloric acid
- ammonium acetate
- cadmium
- sample
- solution
- 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.)
- Granted
Links
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Electrolytic Production Of Metals (AREA)
Abstract
The invention discloses a determination method for cadmium amount in copper slag. The determination method disclosed by the invention adopts an oscillographic polarography which comprises the following steps: taking hydrochloric acid-ammonium acetate as a base solution, pouring a prepared sample solution into an electrolysis cup for oscillographic polarograph photoplotting, and anodizing dipolar derivative waves, starting scanning when an origin potential is -224 mV, and measuring an output peak value; transferring and taking a pure cadmium standard solution along with a sample to obtain the output peak value of the pure cadmium standard solution; calculating the cadmium content in the copper slag sample by using a standard contrast method according to the concentration and the output peak value of the standard solution. Compared with a classic hydrochloric acid base solution method and an ammoniacal base solution method, the analysis method for determining the cadmium amount in copper slag by using the oscillographic polarography disclosed by the invention is stable in waveform and quite high in accuracy; the method is easy and fast, and also eliminates the influence of ammonia gas on a human body; moreover, the determination method is good in precision and high in analysis speed, can meet the requirement for rapid analysis in production, meanwhile provides accurate and reliable data, so as to play a good role in guiding production.
Description
Technical field
The present invention relates to a kind of detection method, relate to specifically the method for cadmium content in the copper ashes of the clean liquid of a kind of rapid and accurate determination workshop.
Background technology
In Zinc Hydrometallurgy Process, output copper-cadmium slag during Purification of zinc sulfate solution, mainly contains the valuable metal elements such as copper, cadmium, zinc in copper-cadmium slag.Comprehensive these valuable metal elements that reclaim, not only can fully utilize raw material, protection of the environment, and can improve metal recovery rate, reduce production costs.The product reclaiming from copper-cadmium slag after valuable metal zinc, cadmium is copper ashes, for cadmium quantitative determination in copper ashes, adopts atom absorption spectrophotometry method to measure cadmium amount always, and the method analytical error is large, and interference element is many; ICP-AES method measurement result is relatively stable reliable, but analysis cost is large, should not apply.
Summary of the invention
Object of the present invention is exactly in order to overcome atom absorption spectrophotometry method, to measure deficiency and the shortcoming of cadmium metering method, and cadmium quantitative analysis method in the mensuration copper ashes that a kind of accuracy is high, precision good, analysis speed is fast is provided.
In order to address the above problem, the present invention adopts following technical scheme:
A method of measuring cadmium amount in copper ashes, specifically comprises the following steps:
A) configuration of liquid at the bottom of polarogram: liquid at the bottom of configuration hydrochloric acid-ammonium acetate polarogram;
B) the cadmium standard solution that configuration concentration is 1mg/mL: take cadmium metal (99.999%) 1.0000g in 300mL beaker, add 20mL nitric acid (1+1) heating for dissolving near dry, add 10mL hydrochloric acid (1+1), in cooling rear immigration 1000mL volumetric flask, constant volume, shakes up, standby;
C) measure the cadmium amount in copper ashes: the copper ashes that takes 0.1000g is that sample is put into container, add 5 ~ 15mL hydrochloric acid heating, then add 1 ~ 5mL nitric acid sample is decomposed completely, steam to small size, add 3 ~ 5mL hydrochloric acid again and steam near dry, micro-boiling dissolved the soluble salt in sample completely; Take off, add ascorbic acid ferric yellow in solution is disappeared and excessive about 0.1g completely; Solution is moved in the 50 mL volumetric flasks fill liquid at the bottom of 15 ~ 35mL hydrochloric acid-ammonium acetate, clean beaker, constant volume, shakes up, standby.The sample solution configuring is poured in electrolysis cup, carried out oscillographic polarograph, and take the photograph figure, anodization, two utmost point derivative ripples, initial point current potential starts scanning for-224mV, surveys it and goes out peak-to-peak value; In company with sample, to pipette 1 ~ 10mL concentration be the pure cadmium standard solution of 1mg/mL to filling in 50 mL volumetric flasks of liquid at the bottom of 15 ~ 35mL hydrochloric acid-ammonium acetate, and constant volume, shakes up, and below by the analytical procedure of said sample solution, operates, and obtains it and go out peak-to-peak value; With criterion keying method, according to the concentration of cadmium standard solution and go out the cadmium content that peak-to-peak value calculates sample solution, further draw the cadmium content of copper ashes sample.
?in described step a or c, at the bottom of hydrochloric acid-ammonium acetate polarogram, liquid is any one in liquid at the bottom of mass percent concentration 10% ammonium acetate-5% hydrochloric acid, 10% ammonium acetate-9% hydrochloric acid, 10% ammonium acetate-10% hydrochloric acid, 10% ammonium acetate-12% hydrochloric acid, 10% ammonium acetate-15% hydrochloric acid, 10% hydrochloric acid-5% ammonium acetate, 10% hydrochloric acid-9% ammonium acetate, 10% hydrochloric acid-10% ammonium acetate, 10% hydrochloric acid-15% ammonium acetate, 10% hydrochloric acid-20% ammonium acetate.
Preferably, in described step a or c, at the bottom of hydrochloric acid-ammonium acetate polarogram, liquid is that mass percent concentration is 10% hydrochloric acid-10% ammonium acetate.
?preferred best testing scheme is: the copper ashes that takes 0.1000g is that sample is put into container, add 10mL hydrochloric acid heating, then add 3mL nitric acid copper ashes sample is decomposed completely, steam to small size, add 3-5mL hydrochloric acid again and steam near dry, micro-boiling dissolved the soluble salt in copper ashes sample completely; Take off, add ascorbic acid ferric yellow in solution is disappeared and excessive about 0.1g completely; Solution is moved into and to be filled in the 50 mL volumetric flasks that 25 mL mass percent concentrations are liquid at the bottom of 10% hydrochloric acid-10% ammonium acetate, clean beaker, constant volume, shakes up, standby.The sample solution configuring is poured in electrolysis cup, carried out oscillographic polarograph, and take the photograph figure, anodization, two utmost point derivative ripples, initial point current potential starts scanning for-224mV, surveys it and goes out peak-to-peak value; In company with sample, to pipette 5mL concentration be the pure cadmium standard solution of 1mg/mL to filling in the 50 mL volumetric flasks that 25 mL mass percent concentrations are liquid at the bottom of 10% hydrochloric acid-10% ammonium acetate, constant volume, shake up, below by the analytical procedure of said sample solution, operate, obtain it and go out peak-to-peak value; With criterion keying method, according to the concentration of standard solution and go out the cadmium content that peak-to-peak value calculates sample solution, further draw the cadmium content of copper ashes sample.
The invention has the beneficial effects as follows: the present invention adopts oscilloscopic polarography, utilize resolution characteristic and the anti-features such as interference of first reducing ion that oscillographic polarograph, is higher to measure the cadmium amount in copper ashes, while solving existing aas determination cadmium metering method, interference element is many, analysis speed is slow, the shortcoming that data are inaccurate and cost is large; The present invention proposes with hydrochloric acid-ammonium acetate is that end liquid is measured cadmium quantitative analysis method in copper ashes, and this method is compared with liquid method, ammoniac base solution method at the bottom of general hydrochloric acid, waveform stabilization, and accuracy is suitable; And the method is simple and quick, avoid the impact of ammonia on human body; And precision is good, analysis speed is fast, can meet the express-analysis in production, and data are accurately and reliably provided simultaneously, has played directive function well for producing.
The result of comparing with ICP-AES measurement result is as shown in table 6,
This oscillopolarographic detection of table 6. result and the comparison of ICP-AES measurement result
Table 6 result shows: adopt the method and measurement result is reliable and stable but ICP-AES method measurement result that analysis cost is large is close.
Take two parts of the copper ashes of 0.1000g, handle well in 50 milliliters of volumetric flasks that move into respectively liquid at the bottom of 10% hydrochloric acid-10% ammonium acetate that fills in advance 25 milliliters after sample, in a volumetric flask, add wherein cadmium standard solution (1m ɡ ∕ mL) 2.00mL, in company with sample, do pure code test, below by sample analysis step, operate.Its experiment the results are shown in Table 7.
The test of table 7. recovery
Table 7 shows that the recovery is 99.30%, meets analysis requirement.
Same sample is done to 11 experiments by the determination step of embodiment is parallel.Experimental result is in Table 8.
The test of table 8. precision
Table 8 result shows that precision is 0.43%, shows that precision is good.
By can show above that the method accuracy higher data is reliable, precision is good, the recovery is high meets analysis requirement, is used for measuring the cadmium amount in copper ashes, has certain practical value.
Accompanying drawing explanation
Fig. 1. be the polarogram crest figure of the pure cadmium of the present invention;
Fig. 2. be the polarogram crest figure of copper ashes sample of the present invention.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described:
Instrument: JP-2c type oscillographic polarograph.
Reagent and compound method are as follows:
Hydrochloric acid: ρ 1.19g/mL;
Nitric acid: ρ 1.42g/mL;
The configuration of liquid at the bottom of polarogram: take a certain amount of ammonium acetate distilled water heating for dissolving, slightly cold, add (ρ 1.19g/mL) hydrochloric acid, after solution is cooling, be diluted with water to scale, constant volume, shake up, configuration quality percent concentration is 10% ammonium acetate-5% hydrochloric acid respectively, 10% ammonium acetate-9% hydrochloric acid, 10% ammonium acetate-10% hydrochloric acid, 10% ammonium acetate-12% hydrochloric acid, 10% ammonium acetate-15% hydrochloric acid, 10% hydrochloric acid-5% ammonium acetate, 10% hydrochloric acid-9% ammonium acetate, 10% hydrochloric acid-10% ammonium acetate, 10% hydrochloric acid-15% ammonium acetate, the end liquid of 10% hydrochloric acid-20% ammonium acetate, standby,
Hydrochloric acid (1+1);
Nitric acid (1+1);
The configuration of cadmium standard solution: the cadmium standard solution that configuration concentration is 1mg/mL, take cadmium metal (99.999%) 1.0000g in 300mL beaker, add 20mL nitric acid (1+1) heating for dissolving near dry, add 10mL hydrochloric acid (1+1), in cooling rear immigration 1000mL volumetric flask, constant volume, shakes up, standby.
Measure the cadmium amount in copper ashes: take 0.1000g copper ashes in 100mL beaker, add 10mL hydrochloric acid (ρ 1.19g/mL) to heat after several minutes, adding 3mL nitric acid (ρ 1.42g/mL) decomposes sample completely again, steam to small size, then add 3-5mL hydrochloric acid (ρ 1.19g/mL) steaming near dry.Water purge table ware and wall of cup, micro-boiling dissolved soluble salt completely.Take off, add ascorbic acid ferric yellow in solution is disappeared and excessive about 0.1g completely.Solution is moved in the 50mL volumetric flask of liquid at the bottom of 10% hydrochloric acid-10% ammonium acetate fill 25mL, clean beaker, and be diluted to scale, shake up, standby.The above-mentioned sample solution configuring is poured in electrolysis cup, carry out oscillographic polarograph, and take the photograph figure, anodization, two utmost point derivative ripples, initial point current potential-224mV, goes out spike potential for-600mv left and right, survey it and go out peak-to-peak value, in company with sample, pipette in the 50mL volumetric flask of 1mg ∕ mL cadmium standard solution liquid at the bottom of the mass concentration that fills 25mL is 10% hydrochloric acid-10% ammonium acetate of 5.00mL, below by the analytical procedure of copper ashes sample, operate, obtain it and go out peak-to-peak value; The polarogram crest figure of pure cadmium, as shown in Figure 1; The polarogram crest figure of copper ashes sample, as shown in Figure 2; In figure, horizontal ordinate is all for going out spike potential (mv), and ordinate is for going out peak-to-peak value (uA), with criterion keying method result of calculation.By criterion keying method, learn cadmium concentration in sample solution, further draw cadmium content in copper ashes.
embodiment 1
Take 5 parts of 0.1000g copper ashes in 100mL beaker, add respectively 5,8,10,12,15mL hydrochloric acid (ρ 1.19g/mL) heats after several minutes, then add 3mL nitric acid (ρ 1.42g/mL) sample is decomposed completely.Steam to small size, add 3-5mL hydrochloric acid (ρ 1.19g/mL) and steam near dry.Water purge table ware and wall of cup, micro-boiling dissolved soluble salt.Take off, add ascorbic acid ferric yellow in solution is disappeared and excessive about 0.1g completely.Solution is moved in the 50mL volumetric flask of liquid at the bottom of 10% hydrochloric acid-10% ammonium acetate fill 25mL, clean beaker, and be diluted to scale, shake up, standby.The above-mentioned sample solution configuring is poured in electrolysis cup, carried out oscillographic polarograph, and take the photograph figure.Anodization, two utmost point derivative ripples, initial point current potential-224mV, go out spike potential-600mV left and right, survey it and go out peak-to-peak value, in company with sample, pipette 5.00mL cadmium standard solution (1mg ∕ mL) in 50mL volumetric flask, by sample analysis step, operate below, with criterion keying method result of calculation.Its experiment the results are shown in Table 1.
?table 1. hydrochloric acid consumption on polarogram go out peak-to-peak value impact
Hydrochloric acid addition can obtain maximum, the most stable polarogram crest when 8 ~ 12mL as can be seen from Table 1, and on measurement result, without obvious impact, and waveform is good herein, so the present invention selects and adds 10mL hydrochloric acid to measure as optimum value.
embodiment 2
Take 5 parts of 0.1000g copper ashes in 100mL beaker, add 10mL hydrochloric acid (ρ 1.19g/mL) to heat after several minutes, add respectively again 1,2,3,4,5mL nitric acid (ρ 1.42g/mL) decomposes sample completely, steam to small size, add 3-5mL hydrochloric acid (ρ 1.19g/mL) and steam near dry.Water purge table ware and wall of cup, micro-boiling dissolved soluble salt.Take off, add ascorbic acid ferric yellow in solution is disappeared and excessive about 0.1g completely.Solution is moved in the 50mL volumetric flask of liquid at the bottom of 10% hydrochloric acid-10% ammonium acetate fill in advance 25mL, clean beaker, and be diluted to scale, shake up, standby.The above-mentioned sample solution configuring is poured in electrolysis cup, carried out oscillographic polarograph, and take the photograph figure.Anodization, two utmost point derivative ripples, initial point current potential-224mV, goes out spike potential-600mV left and right, surveys it and goes out peak-to-peak value.In company with sample, pipette 5.00mL cadmium standard solution (1mg ∕ mL) in the 50mL volumetric flask of liquid at the bottom of 10% hydrochloric acid-10% ammonium acetate that fills 25mL, below by sample analysis step, operate, with criterion keying method result of calculation.Its experiment the results are shown in Table 2.
Table 2. nitric acid dosage goes out the impact of peak-to-peak value on polarogram
Nitric acid addition can obtain maximum, the most stable polarogram crest when 3mL as can be seen from Table 2, and waveform is good herein, so the present invention adopts, and while adding nitric acid 3mL, to measure effect best.
embodiment 3
Take 10 parts of 0.1000g copper ashes in 100mL beaker, add 10mL hydrochloric acid (ρ 1.19g/mL) to heat after several minutes, add respectively again 3mL nitric acid (ρ 1.42g/mL) sample is decomposed completely, steam to small size, add 3-5mL hydrochloric acid (ρ 1.19g/mL) and steam near dry.Water purge table ware and wall of cup, micro-boiling dissolved soluble salt.Take off, add ascorbic acid ferric yellow in solution is disappeared and excessive about 0.1g completely.Solution is moved into respectively and filled in advance in the 50mL volumetric flask that 25mL concentration is respectively liquid at the bottom of 10% ammonium acetate-5% hydrochloric acid, 10% ammonium acetate-9% hydrochloric acid, 10% ammonium acetate-10% hydrochloric acid, 10% ammonium acetate-12% hydrochloric acid, 10% ammonium acetate-15% hydrochloric acid, 10% hydrochloric acid-5% ammonium acetate, 10% hydrochloric acid-9% ammonium acetate, 10% hydrochloric acid-10% ammonium acetate, 10% hydrochloric acid-15% ammonium acetate, 10% hydrochloric acid-20% ammonium acetate, clean beaker, and be diluted to scale, shake up, standby.The above-mentioned sample solution configuring is poured in electrolysis cup, carried out oscillographic polarograph, and take the photograph figure.Anodization, two utmost point derivative ripples, initial point current potential-224mV, goes out spike potential-600mV left and right, surveys it and goes out peak-to-peak value.In company with sample, pipette 5.00mL cadmium standard solution (1mg ∕ mL) in 50mL volumetric flask, below by sample analysis step, operate, with criterion keying method result of calculation.Its experiment the results are shown in Table 3.
The impact of the selection of table 3. bottom liquid concentration on peak value
While showing that from table 3 fixedly the concentration of ammonium acetate is 10%, only change hydrochloric acid consumption from 5%～15%, other operates by operation steps, and from experimental result, hydrochloric acid consumption is 9%～12% time, and polarogram peak is more stable.This law adopts 10% hydrochloric acid consumption.When fixedly the consumption of hydrochloric acid is 10%, change accordingly the concentration of ammonium acetate from 5%～20%, experimental result shows, the concentration of ammonium acetate is little to the determination influences of copper ashes, because solution viscosity increases, crest current value is slightly shown in reduction, therefore adopt the concentration of 10% ammonium acetate proper.
embodiment 4
Take 5 parts, 0.1000g sample in 100mL beaker, add 10 mL hydrochloric acid (ρ 1.19g/mL) to heat after several minutes, add again 3mL nitric acid (ρ 1.42g/mL) sample is decomposed completely, steam at least volume, add 3-5mL hydrochloric acid (ρ 1.19g/mL) and steam near dry.Water purge table ware and wall of cup, micro-boiling dissolved soluble salt.Take off, add ascorbic acid ferric yellow in solution is disappeared and excessive about 0.1g completely.Solution is moved into respectively in the 50mL volumetric flask of liquid at the bottom of 10% hydrochloric acid-10% ammonium acetate that fills in advance 15mL, 20 mL, 25mL, 30 mL, 35 mL, clean beaker, and be diluted to scale, shake up, standby.The above-mentioned sample solution configuring is poured in electrolysis cup, carried out oscillographic polarograph, and take the photograph figure.Anodization, two utmost point derivative ripples, initial point current potential-224mV, goes out spike potential-600mV left and right, surveys it and goes out peak-to-peak value., in 50mL volumetric flask, its experiment the results are shown in Table 4 in company with sample, to pipette 5.00mL cadmium standard solution (1mg ∕ mL).
At the bottom of table 4. 10% hydrochloric acid-10% ammonium acetate liquid consumption on go out peak-to-peak value impact
Table 4 shows, during the change of end liquid consumption, peak height is had to impact in various degree, and when 25 mL, crest is stable, therefore liquid at the bottom of employing 25 mL.
embodiment 5
Take 0.1000g copper ashes in 100mL beaker, add 10mL hydrochloric acid (ρ 1.19g/mL) to heat after several minutes, add again 3mL nitric acid (ρ 1.42g/mL) sample is decomposed completely, steam to small size, add 3-5mL hydrochloric acid (ρ 1.19g/mL) and steam near dry.Water purge table ware and wall of cup, micro-boiling dissolved soluble salt.Take off, add ascorbic acid ferric yellow in solution is disappeared and excessive about 0.1g completely.Solution is moved in the 50mL volumetric flask of liquid at the bottom of 10% hydrochloric acid-10% ammonium acetate fill in advance 25mL, clean beaker, and be diluted to scale, shake up, standby.In company with sample, do pure cadmium standard test, pipetting respectively concentration is cadmium standard solution 1mL, 2mL, the 3mL of 1mg/mL, 5 mL, 10 mL are to filling in advance in 5 volumetric flasks of 50 mL of liquid at the bottom of 10% hydrochloric acid-10% ammonium acetate of 25mL, by sample analysis step, undertaken below, solution is poured in electrolysis cup, carried out oscillographic polarograph, and take the photograph figure.Anodization, two utmost point derivative ripples, initial point current potential-224mV, goes out spike potential-600mV left and right, surveys its content.Analysis result is pressed criterion keying method and is calculated in Table 5.
The impact of table 5. cadmium standard solution addition on test result
Add the accurate solution of cadmium (1mg/mL), 1 mL is more stable to 10mL, the range while adding the accurate solution 5mL of cadmium to measure in this method with go out peak-to-peak value and sample is more approaching, can effectively reduce error at measurment, therefore select the cadmium standard solution that adds 5mL.
Claims (4)
1. a method of measuring cadmium amount in copper ashes, is characterized in that: specifically comprise the following steps:
A) configuration of liquid at the bottom of polarogram: liquid at the bottom of configuration hydrochloric acid-ammonium acetate polarogram;
B) the cadmium standard solution that configuration concentration is 1mg/mL: take cadmium metal (99.999%) 1.0000g in beaker, add 20mL nitric acid (1+1) heating for dissolving near dry, add 10mL hydrochloric acid (1+1), in cooling rear immigration 1000mL volumetric flask, constant volume, shakes up, standby;
C) measure the cadmium amount in copper ashes: taking 0.1000g copper ashes is that sample is put into beaker, add 5 ~ 15mL hydrochloric acid heating, then add 1 ~ 5mL nitric acid sample is decomposed completely, steam to small size, add 3 ~ 5mL hydrochloric acid again and steam near dry, micro-boiling dissolved the soluble salt in sample completely; Take off, add ascorbic acid ferric yellow in solution is disappeared and excessive about 0.1g completely; Solution is moved in the 50 mL volumetric flasks fill liquid at the bottom of 15 ~ 35mL hydrochloric acid-ammonium acetate, clean beaker, constant volume, shakes up, standby; The said sample solution configuring is poured in electrolysis cup, carried out oscillographic polarograph, and take the photograph figure, anodization, two utmost point derivative ripples, initial point current potential starts scanning for-224mV, surveys it and goes out peak-to-peak value; In company with sample, to pipette 1 ~ 10mL concentration be the pure cadmium standard solution of 1mg/mL to filling in 50 mL volumetric flasks of liquid at the bottom of hydrochloric acid-ammonium acetate of 15 ~ 35mL, constant volume, shake up, below operation is undertaken by the analytical procedure of said sample solution, records the peak-to-peak value that of cadmium standard solution; With criterion keying method, according to the concentration of cadmium standard solution with go out peak-to-peak value and calculate the cadmium concentration in sample solution, further draw the cadmium content of copper ashes sample.
2. a kind of method of measuring cadmium amount in copper ashes according to claim 1, is characterized in that: in described step a or c, at the bottom of hydrochloric acid-ammonium acetate, the mass percent concentration of liquid is any one in 10% ammonium acetate-5% hydrochloric acid, 10% ammonium acetate-9% hydrochloric acid, 10% ammonium acetate-10% hydrochloric acid, 10% ammonium acetate-12% hydrochloric acid, 10% ammonium acetate-15% hydrochloric acid, 10% hydrochloric acid-5% ammonium acetate, 10% hydrochloric acid-9% ammonium acetate, 10% hydrochloric acid-10% ammonium acetate, 10% hydrochloric acid-15% ammonium acetate, 10% hydrochloric acid-20% ammonium acetate.
3. a kind of method of measuring cadmium amount in copper ashes according to claim 1, is characterized in that: in described step a or c, preferred mass percent concentration is liquid at the bottom of 10% hydrochloric acid-10% ammonium acetate.
4. a kind of method of measuring cadmium amount in copper ashes according to claim 1, it is characterized in that: described step c is that the copper ashes that takes 0.1000g is that sample is put into container, add the heating of 10mL hydrochloric acid, adding 3mL nitric acid decomposes sample completely again, steam to small size, add 3-5mL hydrochloric acid again and steam near dry, micro-boiling dissolved the soluble salt in sample completely; Take off, add ascorbic acid ferric yellow in solution is disappeared and excessive about 0.1g completely; Solution is moved into and to be filled in the 50 mL volumetric flasks that 25 mL mass percent concentrations are liquid at the bottom of 10% hydrochloric acid-10% ammonium acetate, clean beaker, constant volume, shakes up, standby.The sample solution configuring is poured in electrolysis cup, carried out oscillographic polarograph, and take the photograph figure, anodization, two utmost point derivative ripples, initial point current potential starts scanning for-224mV, surveys it and goes out peak-to-peak value; In company with sample, to pipette 5mL concentration be the pure cadmium standard solution of 1mg/mL to filling in the 50 mL volumetric flasks that 25 mL mass percent concentrations are liquid at the bottom of 10% hydrochloric acid-10% ammonium acetate, constant volume, shake up, below operation is undertaken by the analytical procedure of said sample solution, obtains it and goes out peak-to-peak value; With criterion keying method, according to the concentration of cadmium standard solution with go out peak-to-peak value and calculate the cadmium concentration in sample solution, further draw the cadmium content of copper ashes sample.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410260300.3A CN104049028B (en) | 2014-06-12 | 2014-06-12 | Determination method for cadmium amount in copper slag |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410260300.3A CN104049028B (en) | 2014-06-12 | 2014-06-12 | Determination method for cadmium amount in copper slag |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104049028A true CN104049028A (en) | 2014-09-17 |
| CN104049028B CN104049028B (en) | 2017-02-15 |
Family
ID=51502135
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410260300.3A Active CN104049028B (en) | 2014-06-12 | 2014-06-12 | Determination method for cadmium amount in copper slag |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104049028B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105203616A (en) * | 2015-09-08 | 2015-12-30 | 江苏绿扬电子仪器集团有限公司 | Oscillographic polarograph |
| CN109738381A (en) * | 2018-08-01 | 2019-05-10 | 刘茂诚 | Minimal feeding device and its detection method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1687753A (en) * | 2005-04-29 | 2005-10-26 | 农业部环境保护科研监测所 | Test paper for detecting heavy metal cadmium rapidly, preparation method and application |
| CN103675074A (en) * | 2013-11-01 | 2014-03-26 | 白银有色集团股份有限公司 | Method for continuously determining content of zinc and cadmium in zinc sulfate procedure |
-
2014
- 2014-06-12 CN CN201410260300.3A patent/CN104049028B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1687753A (en) * | 2005-04-29 | 2005-10-26 | 农业部环境保护科研监测所 | Test paper for detecting heavy metal cadmium rapidly, preparation method and application |
| CN103675074A (en) * | 2013-11-01 | 2014-03-26 | 白银有色集团股份有限公司 | Method for continuously determining content of zinc and cadmium in zinc sulfate procedure |
Non-Patent Citations (3)
| Title |
|---|
| 桂义军: "示波极谱法同时测定铅精矿中的铜镉锌", 《山东化工》 * |
| 桃林铅锌矿质检科化验室: "锌精矿中铜、铅、锡的连续测定（盐酸-乙酸铵底液示波极谱法）", 《湖南冶金》 * |
| 陈梅安等: "单扫描示波极谱法直接测定废水、矿渣、矿石中的铀及其机理的初步探讨", 《铀矿冶》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105203616A (en) * | 2015-09-08 | 2015-12-30 | 江苏绿扬电子仪器集团有限公司 | Oscillographic polarograph |
| CN109738381A (en) * | 2018-08-01 | 2019-05-10 | 刘茂诚 | Minimal feeding device and its detection method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104049028B (en) | 2017-02-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103196880B (en) | Method for determining content of arsenic in iron ore by using hydride generation-atomic fluorescence spectroscopy | |
| CN101566611B (en) | Method for quickly measuring acid value of lubricating oil by thermometric titration | |
| CN103913506A (en) | Method for simultaneous measurement of 17 trace elements in reconstituted tobacco by using inductively coupled plasma mass spectrometry | |
| CN101344489A (en) | Method for measuring calcium constituent in silicon aluminum calcium barium alloy | |
| CN101609049A (en) | The method of nickel and cobalt content in a kind of titrimetry test nickel compound | |
| CN103134849A (en) | Quick method for simultaneously measuring potassium content and sodium content and calcium content and magnesium content in cigarette paper | |
| CN104215738B (en) | A kind of method of Zr, Cu, Ni content in simultaneous determination Zr-Cu-Ni-Al non-crystaline amorphous metal | |
| CN105021545A (en) | Method for measuring contents of bismuth and lead ions in tin lead bismuth alloy electroplating solution | |
| CN104297226A (en) | Method for detecting content of aluminum and calcium in nodulizing agent by ICP-AES process | |
| CN104049028A (en) | Determination method for cadmium amount in copper slag | |
| CN105548115B (en) | The assay method of Mercury In Soil | |
| CN103543134B (en) | The method of lead content in Hg-afs Determination iron ore | |
| CN106290705A (en) | Utilize the method for manganese amount in volumetric determination ferrous ammonium sulfate carbon manganese ball | |
| CN104764793A (en) | Method of measuring arsenic and lead in steelmaking blast furnace slag | |
| CN104792853A (en) | Method for determining acid value in lubricating oil | |
| CN103344628B (en) | The ICP-AES of Determination of Arsenic In Iron And Steel measures | |
| CN107894414B (en) | Method for determining release amount of heavy metal elements in buccal cigarette | |
| CN112881587A (en) | Method and device for jointly measuring concentrations of free acid and divalent tin in electrotinning solution | |
| CN104819982A (en) | Determination method for content of calcium in calcium-containing silicon-aluminum alloy | |
| CN101576529A (en) | Determination of sliver using precision electric potential titration | |
| CN104316499A (en) | A method of indirectly measuring gold in seawater by adoption of an atomic fluorescence spectrophotometer | |
| CN103675074A (en) | Method for continuously determining content of zinc and cadmium in zinc sulfate procedure | |
| CN104237216A (en) | Method for detecting phosphorus content in metallurgy raw materials | |
| CN104280368A (en) | Method for efficiently and accurately detecting main content of industrial magnesium oxide | |
| CN102507487B (en) | Method for analyzing and measuring silver content in chromium bronze alloy |
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 |