CN107179339B - Method that is a kind of while measuring copper cadmium nickel cobalt content in zinc electrolyte - Google Patents
Method that is a kind of while measuring copper cadmium nickel cobalt content in zinc electrolyte Download PDFInfo
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- CN107179339B CN107179339B CN201710517844.7A CN201710517844A CN107179339B CN 107179339 B CN107179339 B CN 107179339B CN 201710517844 A CN201710517844 A CN 201710517844A CN 107179339 B CN107179339 B CN 107179339B
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Abstract
The invention discloses a kind of methods for measuring copper cadmium nickel cobalt content in zinc electrolyte simultaneously, including zinc electrolyte to be measured is reacted with the detection architecture being made of Boratex, sodium citrate and dimethylglyoxime, the Adsorptive Wave for measuring copper, cadmium, nickel and cobalt complex calculates the content of copper, cadmium, nickel and cobalt by the second dervative peak current of acquisition.Method of the invention is detection architecture by using Boratex, sodium citrate and dimethylglyoxime, and reaches while measuring the content of copper, cadmium, nickel and cobalt ions by adjusting pH value；The detection architecture can shelter the interference of zinc ion completely, without pre-processing to tested zinc electrolyte；By standard addition method, the influence of other coexisting ions in zinc electrolyte to be measured is reduced, selectivity is high, and measurement result is accurate；Instrument is cheap, easy to operate, and agents useful for same type is few, and stability is good, cheap, and detection process is generated without precipitating, and analysis speed is fast, easily realizes automation, is suitble to use in on-line checking.
Description
Technical field
The present invention relates to analysis and testing technology fields, contain more particularly, to copper cadmium cobalt nickel in a kind of measurement zinc electrolyte
The method of amount.
Background technique
Zinc is the basic material and strategic goods and materials for supporting national economy and defence and military development, current 80% or so zinc
It is to be generated by hydrometallurgy.For the hydrometallurgy of zinc, excessive foreign ion not only influences in electrolytic process
Current efficiency, and influence surface topography and the cathodic polarization of deposition zinc.The impurity being affected during electrodepositing zinc is main
There is copper cadmium nickel cobalt, therefore need to strictly monitor the content of these types of impurity in the zinc electrolyte for flowing into electrolytic cell.
Zn in zinc electrolyte2+Content be up to 130~170g/L, the mass ratio of zinc and trace impurity ion can reach
107Times or more, thus in severe jamming zinc electrolyte foreign ion measurement.Currently, measuring copper in zinc electrolyte in laboratory
The method of cadmium nickel cobalt content mainly has spectrophotometry, atomic absorption method, atomic emission spectrometry, polarography etc..Wherein, it is divided
Photometry sensitivity is low, complicated for operation, generally requires and pre-processes to zinc electrolyte, and is difficult to realize to copper cadmium nickel cobalt
It measures simultaneously；Atomic absorption method and atomic emission spectrometry, expensive equipment, and will receive Matrix effects；In addition, utilizing existing pole
When spectrometry measures copper cadmium nickel cobalt content in zinc electrolyte, since zinc ion content is excessively high in zinc electrolyte, wave crest is easily caused to be overlapped
(especially cobalt wave), and different metal ions are different in same detection architecture medium sensitivity, difficult to realize includes that copper cadmium nickel cobalt exists
It is measured while interior various metals ion, the polarography that single ion detection is also only limitted in practical application undoubtedly improves detection
Time and workload are unfavorable for the real-time monitoring to foreign ion.
In conclusion on the basis of the existing theory of testing and research achievement, in the presence of overcoming existing detection method
Defect, researchs and develops that a kind of simple and fast to be able to achieve the method that various metals ion detects simultaneously in zinc electrolyte be to need at present
The key technical problem of solution has important theoretical and practical significance.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of sides of copper cadmium content of cobalt and nickel in measurement zinc electrolyte
Method.
The present invention adopts the following technical scheme:
Method that is a kind of while measuring copper cadmium nickel cobalt content in zinc electrolyte, including, by zinc electrolyte to be measured and detection body
System's reaction, measures the Adsorptive Wave of each complex compound of copper, cadmium, nickel and cobalt of reaction mixture, passes through the second derivative wave of acquisition
Peak current calculates the content of copper in zinc electrolyte to be measured, cadmium, nickel and cobalt；The detection architecture includes Boratex, sodium citrate
And dimethylglyoxime.
In the above-mentioned technical solutions, after zinc electrolyte to be measured being reacted with detection architecture, measurement reaction mixture copper,
Before the Adsorptive Wave of nickel and each complex compound of cobalt, adjusting pH value is 8.2~10.5, preferably 9.3；In measurement reaction mixture
Cadmium complex Adsorptive Wave before, adjust pH value be 3.5~4.8, preferably 4.0.
In the above-mentioned technical solutions, the concentration of sodium citrate is 0.3~0.7mol/L in the reaction mixture, preferably
For 0.3mol/L.
In the above-mentioned technical solutions, the concentration of Boratex is 0.01~0.1 mol/L in the reaction mixture, preferably
0.06mol/L。
In the above-mentioned technical solutions, the concentration of dimethylglyoxime is 5 × 10 in the reaction mixture-4~3 × 10-3mol/
L, preferably 1.4 × 10-3mol/L。
Preferably, in the above-mentioned technical solutions, the dimethylglyoxime is added in the form of dimethylglyoxime ethanol solution, dense
Degree is 5~12g/L, preferably 11g/L.
Specifically, in said determination zinc electrolyte copper cadmium nickel cobalt content polarography, comprising the following steps:
S1, volume is taken to be V0Zinc electrolyte to be measured reacted with the detection architecture, adjusting pH value is 8.2~10.5, fixed
Hold, measure the Adsorptive Wave of each complex compound of copper, nickel and cobalt of reaction mixture, obtains the second dervative wave crest of copper, nickel and cobalt
Electric current I1、I2、I3, then adjusting pH value is 3.5~4.8, measures the Adsorptive Wave of the cadmium complex of reaction mixture, obtains cadmium
Second dervative peak current I4；
S2, volume is taken to be V respectively0Zinc electrolyte to be measured, with the detection architecture of step S1 equivalent and volume be V1
Contain C1mol/L Cu2+、C2mol/LCd2+、C3mol/L Ni2+And C4mol/L Co2+Mixed standard solution, three is mixed
It reacts, contained Cu in the mixed standard solution of the addition2+、Cd2+、Ni2+And Co2+Mole respectively with zinc electrolyte to be measured
Middle Cu2+、Cd2+、Ni2+And Co2+Mole it is suitable, adjust the suction that copper, nickel and each complex compound of cobalt are measured in pH value and step S1
PH value before attached polarogram is identical, constant volume to identical volume in step S1, measure each network of copper, nickel and cobalt of reaction mixture
The Adsorptive Wave of object is closed, the second dervative peak current I of copper, nickel and cobalt is obtained11、I22、I33, then adjust pH value and step S1
PH value before the Adsorptive Wave of middle measurement cadmium complex is identical, measures the Adsorptive Wave of the cadmium complex of reaction mixture,
Obtain the second dervative peak current I of cadmium44；
S3, Cu in zinc electrolyte to be measured respectively is calculated as follows2+、Cd2+、Ni2+And Co2+Concentration:
Wherein, a=1~4.
In the above-mentioned technical solutions, in step S1 and S2, in the suction of the copper, nickel and each complex compound of cobalt of measurement reaction mixture
Before attached polarogram, adjusting pH value is 9.3；Before the cadmium complex Adsorptive Wave of measurement reaction mixture, adjusting pH value is
4.0。
The present invention compared with the conventional method, has the advantages that
(1) polarography provided by the present invention is detection architecture by using Boratex, sodium citrate and dimethylglyoxime, is led to
Overregulate the content that pH value reaches while measuring copper, cadmium, nickel and cobalt ions；And the detection architecture can shelter the dry of zinc ion completely
It disturbs, without being pre-processed to tested zinc electrolyte；
(2) polarography provided by the present invention is further reduced in zinc electrolyte to be measured by introducing standard addition method
The influence of other coexisting ions, selectivity is high, and measurement result is accurate and reliable；The range of linearity is wide, to make the present invention to entire work
The copper of the zinc electrolyte of skill process, cadmium, nickel and cobalt ions content can detect；It is fast to detect speed, as a result reliably；
(3) analysis instrument used in polarography provided by the present invention is cheap, easy to operate；Agents useful for same type is few,
Stability is good, cheap；Detection process is generated without precipitating, is applicable not only to conventional analysis in laboratory, is easier to realize automatic
Change, convenient for being used in on-line checking.
Detailed description of the invention
Fig. 1 is the standard curve of copper ion in the zinc electrolyte of the embodiment of the present invention 1；
Fig. 2 is the standard curve of cadmium ion in the zinc electrolyte of the embodiment of the present invention 1；
Fig. 3 is the standard curve of nickel ion in the zinc electrolyte of the embodiment of the present invention 1；
Fig. 4 is the standard curve of cobalt ions in the zinc electrolyte of the embodiment of the present invention 1；
Fig. 5 is copper ion, nickel ion and the cobalt ions in 2 step of the embodiment of the present invention (1) in the measurement new liquid of zinc electrolysis
Second dervative polarogram；
Fig. 6 is the second dervative polarogram of the cadmium ion in the embodiment of the present invention 2 in step (1) in the measurement new liquid of zinc electrolysis
Wave；
Fig. 7 is copper ion, nickel ion and the cobalt ions in 2 step of the embodiment of the present invention (2) in the measurement new liquid of zinc electrolysis
Second dervative polarogram；
Fig. 8 is the second dervative polarogram of the cadmium ion in the embodiment of the present invention 2 in step (2) in the measurement new liquid of zinc electrolysis
Wave；
Fig. 9 is copper ion, nickel ion and the cobalt ions measured in neutral supernatant in 2 step of the embodiment of the present invention (1)
Second dervative polarogram；
Figure 10 is the second dervative polarogram for measuring the cadmium ion in neutral supernatant in the embodiment of the present invention 2 in step (1)
Wave；
Figure 11 is copper ion, nickel ion and the cobalt ions measured in neutral supernatant in 2 step of the embodiment of the present invention (2)
Second dervative polarogram；
Figure 12 is the second dervative polarogram for measuring the cadmium ion in neutral supernatant in the embodiment of the present invention 2 in step (2)
Wave.
Specific embodiment
Combined with specific embodiments below, specific embodiments of the present invention will be described in further detail.Following embodiment
It is merely to illustrate the present invention, the specific protection scope being not intended to limit the invention.
Particular technique or condition person are not specified in the embodiment of the present invention, according to the literature in the art described technology or
Condition, or carried out according to product description.Agents useful for same or instrument end indicate production firm person, and being can be by regular channel
Commercially available available conventional products.
Agents useful for same of the embodiment of the present invention and specification:
The ethanol solution of dimethylglyoxime: 11g/L；Sodium citrate solution: 1mol/L；Dobell's solution: 0.15mol/L；Hydrogen
Sodium hydroxide solution: 2mol/L；Sulfuric acid (1:2): 6mol/L.
Instrument of the embodiment of the present invention and test condition:
Instrument: JP-303E type oscillographic polarograph,；Survey the sweep interval of the Adsorptive Wave of copper, nickel and each complex compound of cobalt :-
250~-1400mV surveys the sweep interval of the Adsorptive Wave of cadmium complex: -400~-800mV；Scanning speed: 500mv/s；
Drip the mercury time: 9.5s；Quiescent time: 8s.
The new liquid of sample to be tested zinc electrolyte, zinc electrolysis, neutral supernatant are by zhuzhou, hunan province smeltery in following embodiment
It provides.
Embodiment 1Cu2+、Cd2+、Ni2+And Co2+The determination of the standard curve of measurement system
(1) Cu is taken2+Standard solution is diluted to the Cu of suitable concentration with secondary distilled water2+Standard solution；Respectively measure 1 ×
10-6mol/L、2×10-6mol/L、4×10-6mol/L、6×10-6mol/L、 8×10-6mol/L、2×10-5mol/L、4×
10-5mol/L、8×10-5mol/L、1×10-4mol/L、 2×10-4mol/L、3×10-4mol/L、6×10-4mol/L、8×
10-4The Cu of mol/L2+1.0mLZn is added in the volumetric flask of 13 10mL in each 0.5mL of standard solution into volumetric flask respectively2+
Solution (2.6mol/L) and 0.15mL dimethylglyoxime ethanol solution (11g/L) shake 3min, then sequentially add 3mL citric acid
Sodium solution (1mol/L), 4mL Boratex (0.15mol/L) and 1mL sodium hydroxide solution (2mol/L), constant volume stand 5min,
Solution is poured into electrolysis cup respectively the Cu for measuring generation2+Complex compound Adsorptive Wave obtains each concentration C u2+Corresponding second order
Derivative peak current, drawing standard curve, (abscissa indicates the Cu after volumetric flask constant volume as shown in Figure 12+Molar concentration, indulge sit
Mark indicates second dervative peak current).
(2) Cd is taken2+Standard solution is diluted to the Cd of suitable concentration with secondary distilled water2+Standard solution；Respectively measure 4 ×
10-6mol/L、6×10-6mol/L、8×10-6mol/L、2×10-5mol/L、 4×10-5mol/L、6×10-5mol/L、8×
10-5mol/L、2×10-4mol/L、4×10-4mol/L、 8×10-4mol/L、1×10-3mol/L、2×10-3mol/L、4×
10-3mol/L、8×10-3The Cd of mol/L2+Each 0.5mL of standard solution is in the volumetric flask of 14 10mL, respectively into volumetric flask
1.0mLZn is added2+Solution (2.6mol/L) and 0.15mL dimethylglyoxime ethanol solution (11g/L) shake 3min, then successively add
Enter 3mL sodium citrate solution (1mol/L), 4mL Boratex (0.15mol/L) and 0.5mL sulfuric acid (6mol/L), constant volume is stood
5min pours into solution in electrolysis cup the Cd for measuring generation respectively2+Complex compound Adsorptive Wave obtains each concentration C d2+It is corresponding
Second dervative peak current, drawing standard curve, (abscissa indicates the Cd after volumetric flask constant volume as shown in Figure 22+Molar concentration,
Ordinate indicates second dervative peak current).
(3) Ni is taken2+Standard solution is diluted to the Ni of suitable concentration with secondary distilled water2+Standard solution；Respectively measure 2 ×
10-7mol/L、4×10-7mol/L、6×10-7mol/L、8×10-7mol/L、 2×10-6mol/L、3×10-6mol/L、4×
10-6mol/L、6×10-6mol/L、7×10-6mol/L、 8×10-6mol/L、1×10-5mol/L、2×10-5mol/L、4×
10-5The Ni of mol/L2+Each 0.5mL of standard solution is in the volumetric flask of 13 10mL, referring to the method for step (1), surveys respectively each
Concentration Ni2+Corresponding second dervative peak current, drafting standard curve is as shown in Figure 3 (after abscissa indicates volumetric flask constant volume
Ni2+Molar concentration, ordinate indicate second dervative peak current).
(4) Co is taken2+Standard solution is diluted to the Co of suitable concentration with secondary distilled water2+Standard solution；Respectively measure 1 ×
10-7mol/L、2×10-7mol/L、4×10-7mol/L、6×10-7mol/L、 8×10-7mol/L、2×10-6mol/L、4×
10-6mol/L、6×10-6mol/L、1.2×10-5The Co of mol/L2+Each 0.5mL of standard solution in the volumetric flask of 9 10mL,
Referring to the method for step (1), each concentration C o is surveyed respectively2+It is as shown in Figure 4 to draw standard curve for corresponding second dervative peak current
(abscissa indicates the Co after volumetric flask constant volume2+Molar concentration, ordinate indicate second dervative peak current).
Cu in the new liquid of 2 zinc electrolysis of embodiment2+、Cd2+、Ni2+And Co2+The measurement of content
(1) the new liquid of zinc electrolysis for measuring 1mL is placed in 10mL volumetric flask, and the ethanol solution 0.15mL of dimethylglyoxime is added,
3min is shaken to uniform, 3mL sodium citrate solution (1mol/L) and 4mL Boratex (0.15mol/L) is then sequentially added, passes through
It is 9.4 that 2mol/L sodium hydroxide solution, which is added dropwise, and adjusts its pH value, and constant volume stands 5min, and solution is poured into and measures production in electrolysis cup
Raw Cu2+、Ni2+、Co2+The Adsorptive Wave of complex compound, obtain its corresponding second dervative peak current be respectively 125.2nA,
667.1nA, 214.7nA, testing result is as shown in Fig. 5, and it is 4.2 that 6mol/L sulfuric acid is added dropwise on this basis to adjust its pH value,
Measure the Cd generated2+The Adsorptive Wave of complex compound, obtaining its corresponding second dervative peak current is respectively 36.2nA, inspection
Survey result (abscissa indicates that scanning voltage/mV, ordinate indicate second dervative peak current/nA) as shown in Figure 6；
(2) the new liquid of zinc electrolysis of 1mL and the mixed standard solution (Cu of 0.5mL are measured2+: 2×10-5Mol/L, Cd2+: 6 ×
10-5Mol/L, Ni2+:2×10-6Mol/L, Co2+:4×10-6Mol/L it) is placed in 10mL volumetric flask, the second of dimethylglyoxime is added
Alcoholic solution 0.15mL shakes 3min to uniform, then sequentially adds 3mL sodium citrate solution (1mol/L) and 4mL Boratex
(0.15mol/L) is 9.4 by the way that 2mol/L sodium hydroxide solution is added dropwise to adjust its pH value, and constant volume stands 5min, solution is fallen
Enter to measure the Cu of generation in electrolysis cup2+、Ni2+、Co2+The Adsorptive Wave of complex compound obtains its corresponding second dervative wave crest electricity
Stream respectively 230.6nA, 813.1nA, 414.9nA, testing result as shown in fig. 7, be simultaneously added dropwise 6mol/L sulphur on this basis
It is 4.2 that acid, which adjusts its pH value, measures the Cd of generation2+The Adsorptive Wave of complex compound obtains its corresponding second dervative wave crest electricity
Stream is respectively 65.8nA, and (abscissa indicates that scanning voltage/mV, ordinate indicate second dervative wave crest to testing result as shown in Figure 8
Electric current/nA)；
(3) it is calculated according to formula, Cu in the new liquid of zinc electrolysis2+、Cd2+、Ni2+And Co2+Content is respectively Cu2+:1.188
×10-5Mol/L, Cd2+: 3.669 × 10-5Mol/L, Ni2+:4.569×10-6Mol/L, Co2+:2.145×10-6mol/L。
Cu in the neutral supernatant of embodiment 32+、Cd2+、Ni2+And Co2+The measurement of content
(1) 1mL neutrality supernatant is measured in 100mL volumetric flask, with secondary distilled water constant volume, as solution to be measured；
(2) solution to be measured for measuring 1mL is placed in 10mL volumetric flask, and the ethanol solution 0.15mL of dimethylglyoxime is added, and is shaken
Then dynamic 3min sequentially adds 3mL sodium citrate solution (1mol/L) and 4mL Boratex (0.15mol/L), passes through drop to uniform
Adding 2mol/L sodium hydroxide solution to adjust its pH value is 9.3, and constant volume stands 5min, and solution is poured into and measures generation in electrolysis cup
Cu2+、Ni2+、Co2+The Adsorptive Wave of complex compound, obtain its corresponding second dervative peak current be respectively 22.5nA,
53nA, 233.1nA, testing result as shown in figure 9, simultaneously on this basis be added dropwise 6mol/L sulfuric acid adjust its pH value be 4.0, survey
The raw Cd of fixed output quota2+The Adsorptive Wave of complex compound, obtaining its corresponding second dervative peak current is respectively 23.7nA, detection
The results are shown in Figure 10 (abscissa indicates that scanning voltage/mV, ordinate indicate second dervative peak current/nA)；
(3) mixed standard solution (Cu of the solution and 0.5mL to be measured of 1mL is measured2+:1×10-5Mol/L, Cd2+: 6 ×
10-5Mol/L, Ni2+: 1 × 10-6Mol/L, Co2+:4×10-6Mol/L it) is placed in 10mL volumetric flask, the second of dimethylglyoxime is added
Alcoholic solution 0.15mL shakes 3min to uniform, then sequentially adds 3mL sodium citrate solution (1mol/L) and 4mL Boratex
(0.15mol/L) is 9.3 by the way that 2mol/L sodium hydroxide solution is added dropwise to adjust its pH value, and constant volume stands 5min, solution is fallen
Enter to measure the Cu of generation in electrolysis cup2+、Ni2+、Co2+The Adsorptive Wave of complex compound obtains its corresponding second dervative wave crest electricity
Stream respectively 71.25nA, 124nA, 426.8nA, testing result is as shown in figure 11, and 6mol/L sulphur is added dropwise on this basis
It is 4.0 that acid, which adjusts its pH value, measures the Cd of generation2+The Adsorptive Wave of complex compound obtains its corresponding second dervative wave crest electricity
Stream is respectively 54nA, and (abscissa indicates that scanning voltage/mV, ordinate indicate second dervative wave crest to testing result as shown in figure 12
Electric current/nA)；
(4) it is calculated according to formula, Cu in neutral supernatant2+、Cd2+、Ni2+And Co2+Content is respectively Cu2+:2.308
×10-4Mol/L, Cd2+: 2.347 × 10-3Mol/L, Ni2+:3.732×10-5Mol/L, Co2+:2.407×10-4mol/L。
The influence of 1 interfering ion of comparative example is tested
Each interfering ion is to measurement Zn2+Cu in solution2+Content influences experiment:
(1) Zn of 1mL 2.6mol/L is measured2+Standard solution and 0.1mL 5 × 10-5The Cu of mol/L2+Solution is placed in
In 10mL volumetric flask, it is added the ethanol solution 0.15mL of dimethylglyoxime, shakes 3min to uniform, then sequentially add 3mL lemon
Acid sodium solution (1mol/L), 4mL Boratex (0.15mol/L) and 1mL sodium hydroxide solution (2mol/L), constant volume are stood
5min pours into solution in electrolysis cup the Cu for measuring generation2+The Adsorptive Wave of complex compound obtains its second dervative peak current
Respectively I1；
(2) Zn of 1mL 2.6mol/L is measured2+Standard solution and 0.1mL 5 × 10-5The Cu of mol/L2+Solution is placed in
In 10mL volumetric flask, it is separately added into a certain amount of solution containing interfering ion to be studied, the ethyl alcohol that dimethylglyoxime is then added is molten
Liquid 0.15mL shakes 3min to uniform, then sequentially adds 3mL sodium citrate solution (1mol/L), 4mL Boratex
(0.15mol/L) and 1mL sodium hydroxide solution (2mol/L), constant volume stand 5min, and solution is poured into and measures production in electrolysis cup
Raw Cu2+The Adsorptive Wave of complex compound, obtaining its second dervative peak current is respectively I2, take (I2-I1)/I1It is mixed when≤5%
The interfering ion concentration in solution is closed as the maximum concentration that can be added.
Using above-mentioned identical each interfering ion of technique study to measurement Zn2+Cd in solution2+ (1×10-6mol/L)、Ni2+
(2×10-7mol/L)、Co2+(2×10-7Mol/L) the influence of content.
Each interfering ion is to measurement Zn2+Cu in solution2+、Cd2+、Ni2+、Co2+The influence of assay is as shown in table 1 below.
Each interfering ion of table 1 is to measurement Cu2+、Cd2+、Ni2+、Co2+Interfering ion concentration when the influence of content≤5% with
Ion concentration to be measured
2 two methods of comparative example measure the Cu in different zinc electrolyte samples2+、Cd2+、 Ni2+、Co2+Content
In order to verify the accuracy of measurement result of the present invention, selecting different zinc electrolyte samples is test sample, is adopted respectively
Its Cu is measured with atomic absorption spectrophotometry and method provided by the present invention2+、Cd2+、Ni2+、Co2+Content, experimental result
As shown in table 2 below.
2 two methods of table measure Cu in zinc electrolyte sample2+、Cd2+、Ni2+、Co2+The result of content compares
As can be seen from Table 2, Cu in method of the invention measurement zinc electrolyte2+、Cd2+、Ni2+、 Co2+The result of content with
The measurement result goodness of fit of atomic absorption spectrophotometry is good, and relative error is -2.7%~+3.57%, illustrates survey of the invention
Determine the accurate and reliable of method.
The experiment of 3 sample recovery of standard addition of comparative example
Sample recovery testu result is as shown in table 3 below.
3 recovery testu result of table and the rate of recovery
As can be seen from Table 3, sample recovery testu, rate of recovery 97%-104.1%, card are carried out using the present invention
Bright this method is accurate and reliable.
Finally, being not intended to limit the scope of the present invention the above is only preferred embodiment of the invention.It is all this
Within the spirit and principle of invention, any modification, equivalent replacement, improvement and so on should be included in protection model of the invention
Within enclosing.
Claims (10)
1. a kind of method for measuring copper cadmium nickel cobalt content in zinc electrolyte simultaneously, which is characterized in that
The following steps are included:
S1, volume is taken to be V0Zinc electrolyte to be measured reacted with detection architecture, adjusting pH value is 8.2~10.5, constant volume, and measurement is anti-
The Adsorptive Wave of each complex compound of copper, nickel and cobalt of mixture is answered, the second dervative peak current I of copper, nickel and cobalt is obtained1、I2、
I3, then adjusting pH value is 3.5~4.8, measures the Adsorptive Wave of the cadmium complex of reaction mixture, obtains the second dervative of cadmium
Peak current I4；
S2, volume is taken to be V respectively0Zinc electrolyte to be measured, with the detection architecture of step S1 equivalent and volume be V1Contain
C1mol/L Cu2+、C2mol/LCd2+、C3mol/L Ni2+And C4mol/L Co2+Mixed standard solution, by three's hybrid reaction,
Contained Cu in the mixed standard solution2+、Cd2+、Ni2+And Co2+Mole respectively with Cu in zinc electrolyte to be measured2+、Cd2+、
Ni2+And Co2+Mole it is suitable, before adjusting the Adsorptive Wave for measuring copper, nickel and each complex compound of cobalt in pH value and step S1
PH value is identical, constant volume to identical volume in step S1, measure the absorption pole of each complex compound of copper, nickel and cobalt of reaction mixture
Wave is composed, the second dervative peak current I of copper, nickel and cobalt is obtained11、I22、I33, then adjust measurement cadmium complexing in pH value and step S1
PH value before the Adsorptive Wave of object is identical, measures the Adsorptive Wave of the cadmium complex of reaction mixture, obtains the second order of cadmium
Derivative peak current I44；
S3, Cu in zinc electrolyte to be measured is calculated separately as follows2+、Cd2+、Ni2+And Co2+Concentration:
Wherein, a=1~4；
The detection architecture includes Boratex, sodium citrate and dimethylglyoxime.
2. the method according to claim 1, wherein the concentration of sodium citrate is 0.3 in the reaction mixture
~0.7mol/L.
3. according to the method described in claim 2, it is characterized in that, the concentration of sodium citrate is in the reaction mixture
0.3mol/L。
4. the method according to claim 1, wherein in the reaction mixture Boratex concentration be 0.01~
0.1mol/L。
5. according to the method described in claim 4, it is characterized in that, the concentration of Boratex is in the reaction mixture
0.06mol/L。
6. the method according to claim 1, wherein in the reaction mixture dimethylglyoxime concentration be 5 ×
10-4~3 × 10-3mol/L。
7. according to the method described in claim 6, it is characterized in that, the concentration of dimethylglyoxime is 1.4 in the reaction mixture
×10-3mol/L。
8. according to the method described in claim 6, it is characterized in that, the dimethylglyoxime is in the form of dimethylglyoxime ethanol solution
Addition, concentration are 5~12g/L.
9. according to the method described in claim 8, it is characterized in that, the concentration of the dimethylglyoxime ethanol solution is 11g/L.
10. the method according to claim 1, wherein in step S1 and S2, measurement reaction mixture copper,
Before the Adsorptive Wave of nickel and each complex compound of cobalt, adjusting pH value is 9.3；Polarogram is adsorbed in the cadmium complex of measurement reaction mixture
Wavefront, adjusting pH value is 4.0.
Priority Applications (1)
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| Adsorption and electrochemical reduction of Co(II)-dimethylglyoxime on mercury;Fernando Cordon et al.;《Journal of Electroanalytical Chemistry》;20021025;第534卷;131-141 * |
| The reduction of nickel dimethylglyoxime complex preadsorbed on mercury;Silvana Ramirez et al.;《Journal of Electroanalytical Chemistry》;19980407;第431卷;171-181 * |
| 同一体系中铜(Ⅱ)、铅(Ⅱ)、镉(Ⅱ)、镍(Ⅱ)和钴(Ⅱ)的络合物吸附波及其分析应用;张明浩 等;《分析化学》;20020825;第30卷(第8期);967-971 * |
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