CN102645432A - Analysis method for quickly and accurately measuring zinc in zinc electrolyte - Google Patents
Analysis method for quickly and accurately measuring zinc in zinc electrolyte Download PDFInfo
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Abstract
The invention provides an analysis method for quickly and accurately measuring zinc in zinc electrolyte. The method comprises the following steps of: weighing quantitative zinc electrolyte in a container, blowing water, then adding excessive ammonium chloride, and shaking uniformly; adding excessive ammonia water and hydrogen peroxide, and shaking uniformly; boiling until no continuous air bubbles are generated; breaking the hydrogen peroxide, and performing hot filtration with quick filter paper; washing the filtering container with ammonium chloride-ammonia water washing liquid, and precipitating; uniformly shaking the filtrate, and heating for concentration; cooling and adding ascorbic acid; shaking uniformly and adding a xylenol orange indicator; adjusting with hydrochloric acid and ammonia water until the solution is yellow; adding saturated sodium fluoride and thiourea and shaking uniformly; adding acetic acid-sodium acetate buffer solution, and shaking uniformly; and titrating with the EDTA (Ethylene Diamine Tetraacetic Acid) standard titration solution until the solution becomes bright yellow from purple red. Through the invention, the influence of manganese ion on the measurement of zinc content in zinc electrolyte can be effectively shielded, the problem that the analysis data is not accurate or reliable in the existing method is solved, and the measured result has an instruction effect on the production of zinc electrolyte.
Description
Technical field
The present invention relates to a kind of detection method, relate to the analytical approach of zinc in a kind of rapid and accurate determination zinc electrolyte specifically.
Background technology
In the zinc hydrometallurgy process; Mainly be that the waste electrolyte that produces in the process in zinc electrolyzing is made solvent; To contain the process that the valuable metal dissolving in the zinc raw material gets into solution, outside dezincifying in its raw material, generally also contain elements such as iron, copper, cadmium, cobalt, nickel, arsenic, antimony and rare metal.In leaching process, dezincify to get into outside the solution, metallic impurity also in various degree dissolving and get into solution with zinc.Zinc analysis on Content method is continued to use comparatively classical EDTA compleximetry at present always in supernatant and the electrolytic solution in this process; But the content of manganese is higher in the zinc ore of present domestic application; The content that causes manganese in the zinc electrolyte is generally up to about 6-25g/l, and with EDTA complexometric titration zinc ion concentration the time, manganese can disturb the zinc Determination on content; Manganese is not effectively separated in the present practical measurement, historical facts or anecdotes border measured value is the zinc-manganese resultant.Data are inaccurate in this case, do not have directive function for the production of zinc electrolysis.
Summary of the invention
The object of the invention is exactly deficiency and the shortcoming that will eliminate above-mentioned prior art, and the method for measuring zinc in the higher zinc electrolyte of a kind of manganese content accurately and reliably is provided, and solves in the existing method and analyzes the inaccurate reliable problem of data.
For reaching above-mentioned technique effect, the present invention adopts following technical scheme: pipette quantitative zinc electrolyte in container, blow and add the excess chlorination ammonium behind the water; Shake up, shake up behind adding excessive ammonia and the oxydol, boil to no continuous air bubbles generation; With quick filter paper heat filtering, wash the filtering container postprecipitation with ammonium chloride-ammonia scrubbing liquid behind the destruction oxydol, filtrating shakes up the back heating and concentrates; The cooling back adds ascorbic acid, shakes up the back and adds the xylenol orange indicator, uses hydrochloric acid and ammoniacal liquor to be transferred to solution just for yellow; Add saturated sodium fluoride, thiocarbamide, shake up, add acetate-sodium acetate buffer solution; Shake up, use the EDTA standard titration solution to drip to become glassy yellow by aubergine to be terminal point to solution.
Preferably, pipette zinc electrolyte 1.00mL in conical beaker, blow water 20mL, add ammonium chloride; Shake up, add ammoniacal liquor, add oxydol; Shake up, boil, destroy oxydol to no continuous air bubbles generation; Use quick filter paper while hot in conical beaker, wash beaker 2 times, deposition with the ammonium chloride-ammonia scrubbing liquid of heat.Filtrating shakes up, and heating is concentrated to about 100 mL, takes off cooling; Add the 0.1g ascorbic acid, shake up, drip xylenol orange indicator 3-4 and drip; Being transferred to solution with hydrochloric acid and ammoniacal liquor is yellow just, adds saturated sodium fluoride, each 5mL of thiocarbamide, shakes up; Add 20mL acetate-sodium acetate buffer solution, shake up, use the EDTA standard titration solution to drip to become glassy yellow by aubergine to be terminal point to solution.
Preferably, blow that to add ammonium chloride after the water step be 2.0-5.0g, ammoniacal liquor 5.0-15.0ml, oxydol 3.0-9.0ml.
Preferably, the oxydol selected for use of oxygenant is substitutable for saturated bromine water or ammonium persulfate.
Preferably, ammonium chloride-ammonia scrubbing liquid concentration is 5% ammonium chloride-5% ammoniacal liquor.
Preferably, drip the xylenol orange indicator after, be in harmonious proportion and use hydrochloric acid to be hydrochloric acid and water volume ratio mixed solution as 1:1, the ammoniacal liquor that mediation is used is the mixed solution of ammoniacal liquor and water volume ratio 1:1.
Preferably, pipette zinc electrolyte 1.00ml in the 300ml conical beaker, blow water 20ml, add 3.0g ammonium chloride; Shake up, add 10ml ammoniacal liquor, add the 5.0ml oxydol; Shake up, boil produce to no continuous air bubbles till, destroy oxydol; Use quick filter paper while hot in the 500ml conical beaker, wash beaker 2 times, precipitate 6-8 time with the 5% ammonium chloride-5% ammonia scrubbing liquid of heat.Filtrating shakes up, and heating is concentrated to about 100 ml, takes off cooling; Add the 0.1g ascorbic acid, shake up, drip xylenol orange indicator 3-4 and drip; Being transferred to solution with hydrochloric acid (1+1) and ammoniacal liquor (1+1) is yellow just, adds saturated sodium fluoride, each 5ml of thiocarbamide, shakes up; Add 20ml acetate-sodium acetate buffer solution, shake up, use the EDTA standard titration solution to drip to become glassy yellow by aubergine to be terminal point to solution.
The beneficial effect of type of the present invention:
The analytical approach of zinc can effectively shield the influence that manganese ion is measured zinc content in the zinc electrolyte in the mensuration zinc electrolyte provided by the invention; Solve in the existing method and analyze the inaccurate reliable problem of data, the result who records can play directive function to the production of zinc electrolysis.
Embodiment
Following examples select for use reagent to be:
Ammonium chloride (analyzing pure);
Ammoniacal liquor (ρ=0.90g/mL);
Hydrochloric acid (ρ=1.19g/mL);
Sodium fluoride (analyzing pure), thiocarbamide (analyzing pure);
Oxydol (mass percent 30%);
Zinc (II) standard solution: 10mg/mL;
Manganese (II) standard solution: 1 mg/mL;
The zinc electrolyte that contains manganese: contain zinc (II) 100mg/mL, contain manganese (II) 10mg/mL;
Xylenol orange indicator (0.5g/L);
Hydrochloric acid (1+1): volume ratio hydrochloric acid: water=1:1
Ammoniacal liquor (1+1): volume ratio ammoniacal liquor: water=1:1
EDTA standard titration: by conventional method preparation, demarcation.
Embodiment 2-7
Pipette 6 parts of electrolytic solution that 1.00mL contains manganese in the 300mL conical beaker, blow about water 20mL, add 0.5,1.0,2.0,3.0,4.0 respectively, 5.0g ammonium chloride; Shake up, add 10mL ammoniacal liquor, add the 5.0mL oxydol; Shake up, boil produce to no continuous air bubbles till, destroy oxydol; Use quick filter paper while hot in the 500mL conical beaker, wash beaker 2 times, precipitate 6-8 time with the 5% ammonium chloride-5% ammonia scrubbing liquid of heat.Filtrating shakes up, and heating is concentrated to about 100 mL, takes off cooling; Add the 0.1g ascorbic acid, shake up, drip xylenol orange indicator 3-4 and drip; Being transferred to solution with hydrochloric acid (1+1) and ammoniacal liquor (1+1) is yellow just, adds saturated sodium fluoride, each 5mL of thiocarbamide, shakes up; Add 20mL acetate-sodium acetate buffer solution, shake up, use the EDTA standard titration solution to drip to become glassy yellow by aubergine to be terminal point to solution.The result sees the following form.
The test of table 2 ammonium chloride consumption
| ? | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 |
| Ammonium chloride consumption (g) | 0.5 | 1.0 | 2.0 | 3.0 | 4.0 | 5.0 |
| Record zinc amount (mg) | 97.51 | 98.53 | 99.54 | 99.73 | 99.38 | 99.70 |
The result shows that to measuring not obviously influence of result, selective chlorination ammonium optimum amount is 3.0g to the ammonium chloride consumption at 2.0-5.0 g.
Embodiment 8-12
Pipette 5 parts of electrolytic solution that 1.00mL contains manganese in the 300mL conical beaker, blow about water 20mL, add 3.0g ammonium chloride; Shake up, add 5.0,8.0,10.0,12.0 respectively, 15.0mL ammoniacal liquor, add the 5mL oxydol; Shake up, boil produce to no continuous air bubbles till, destroy oxydol; Use quick filter paper while hot in the 500mL conical beaker, wash beaker 2 times, precipitate 6-8 time with the 5% ammonium chloride-5% ammonia scrubbing liquid of heat.Filtrating shakes up, and heating is concentrated to about 100 mL, takes off cooling; Add the 0.1g ascorbic acid, shake up, drip xylenol orange indicator 3-4 and drip; Being transferred to solution with hydrochloric acid (1+1) and ammoniacal liquor (1+1) is yellow just, adds saturated sodium fluoride, each 5mL of thiocarbamide, shakes up; Add 20mL acetate-sodium acetate buffer solution, shake up, use the EDTA standard titration solution to drip to become glassy yellow by aubergine to be terminal point to solution.The result sees the following form.
The test of table 3 ammonia volume
| ? | Embodiment 8 | Embodiment 9 | Embodiment 10 | Embodiment 11 | Embodiment 12 |
| Ammonia volume (mL) | 5.0 | 8.0 | 10.0 | 12.0 | 15.0 |
| Record zinc amount (mg) | 99.70 | 99.82 | 99.33 | 99.45 | 99.39 |
The result shows that to measuring not obviously influence of result, selective chlorination ammonium optimum amount is 10.0mL to ammonia volume at 5.0-15.0mL.
Embodiment 13-19
Pipette 5 parts of electrolytic solution that 1.00mL contains manganese in the 300mL conical beaker, blow about water 20mL, add 3.0g ammonium chloride; Shake up, add 10mL ammoniacal liquor, add 1.0,3.0,4.0,5.0,6.0,7.0 respectively, the 9.0mL oxydol; Shake up, boil produce to no continuous air bubbles till, destroy oxydol; Use quick filter paper while hot in the 500mL conical beaker, wash beaker 2 times, precipitate 6-8 time with the 5% ammonium chloride-5% ammonia scrubbing liquid of heat.Filtrating shakes up, and heating is concentrated to about 100 mL, takes off cooling; Add the 0.1g ascorbic acid, shake up, drip xylenol orange indicator 3-4 and drip; Being transferred to solution with hydrochloric acid (1+1) and ammoniacal liquor (1+1) is yellow just, adds saturated sodium fluoride, each 5mL of thiocarbamide, shakes up; Add 20mL acetate-sodium acetate buffer solution, shake up, use the EDTA standard titration solution to drip to become glassy yellow by aubergine to be terminal point to solution.The result sees the following form.
The test of table 4 oxydol consumption
| ? | Embodiment 13 | Embodiment 14 | Embodiment 15 | Embodiment 16 | Embodiment 17 | Embodiment 18 | Embodiment 19 |
| Oxydol consumption (mL) | 1.0 | 3.0 | 4.0 | 5.0 | 6.0 | 7.0 | 9.0 |
| Record zinc amount (mg) | 105.90 | 102.07 | 99.57 | 99.50 | 99.33 | 99.35 | 99.47 |
The result shows that to measuring not obviously influence of result, select the oxydol optimum amount is 5.0mL to the oxydol consumption at 3.0-9.0mL.
Embodiment 20-25
Pipette 6 parts of electrolytic solution that 1.00mL contains manganese in the 300mL conical beaker, blow about water 20mL, add 3.0g ammonium chloride, shake up; Add 10mL ammoniacal liquor, add the 5.0mL oxydol, shake up; Preceding 5 parts were boiled respectively 0.5,1.0,2.0,3.0,4.0 minute, and last portion boils to no continuous air bubbles generation, behind the destruction oxydol; Use quick filter paper while hot in the 500mL conical beaker, wash beaker 2 times, precipitate 6-8 time with the 5% ammonium chloride-5% ammonia scrubbing liquid of heat.Filtrating shakes up, and heating is concentrated to about 100 mL, takes off cooling; Add the 0.1g ascorbic acid, shake up, drip xylenol orange indicator 3-4 and drip; Being transferred to solution with hydrochloric acid (1+1) and ammoniacal liquor (1+1) is yellow just, adds saturated sodium fluoride, each 5mL of thiocarbamide, shakes up; Add 20mL acetate-sodium acetate buffer solution, shake up, use the EDTA standard titration solution to drip to become glassy yellow by aubergine to be terminal point to solution.The result sees the following form.
The test of table 5 boiling time
The result shows, boiling time greater than 2.0min after, can record consistent results, till test and Selection is boiled and produced to no continuous air bubbles.
Embodiment 26-32
Pipette 7 parts of electrolytic solution that 1.00mL contains manganese in the 300mL conical beaker, blow about water 20mL, add 3.0g ammonium chloride, shake up, add 10mL ammoniacal liquor, wherein three parts add 3.0,5.0, the 10.0mL30% oxydol; Also has two parts of addings 5.0, the saturated bromine water of 10mL; Last two parts add 1.5, the 2.5g ammonium persulfate, shake up, boil produce to no continuous air bubbles till, destroy oxygenant, use quick filter paper while hot in the 500mL conical beaker, wash beaker 2 times with hot 5% ammonium chloride-5% ammonia scrubbing liquid, precipitate 6-8 time.Filtrating shakes up, and heating is concentrated to about 100 mL, takes off cooling; Add the 0.1g ascorbic acid, shake up, drip xylenol orange indicator 3-4 and drip; Being transferred to solution with hydrochloric acid (1+1) and ammoniacal liquor (1+1) is yellow just, adds saturated sodium fluoride, each 5mL of thiocarbamide, shakes up; Add 20mL acetate-sodium acetate buffer solution, shake up, use the EDTA standard titration solution to drip to become glassy yellow by aubergine to be terminal point to solution.The result sees the following form.
The influence test of the oxygenant of table 6 manganese
The result shows that three kinds of oxygenants all can reach oxidation effectiveness, but it is comparatively suitable to take all factors into consideration oxydol.
Embodiment 33-42
Pipette 10 parts of electrolytic solution that 1.00mL contains manganese in the 300mL conical beaker; Blow about water 20mL, add 3.0g ammonium chloride, shake up; Add 10mL ammoniacal liquor; Add the 5mL oxydol, shake up, boil till the no continuous air bubbles generation; Destroy oxydol; Use quick filter paper while hot in the 500mL conical beaker, wash beaker 2 times with 2% ammonium chloride-0.5% ammoniacal liquor, 2% ammonium chloride-2% ammoniacal liquor, 2% ammonium chloride-5% ammoniacal liquor, 2% ammonium chloride-10% ammoniacal liquor, 3% ammonium chloride-5% ammoniacal liquor, 4% ammonium chloride-5% ammoniacal liquor, 5% ammonium chloride-0.5% ammoniacal liquor, 5% ammonium chloride-2% ammoniacal liquor, 5% ammonium chloride-5% ammoniacal liquor, the 5% ammonium chloride-10% ammonia scrubbing liquid of heat respectively, precipitate 6-8 time.Filtrating shakes up, and heating is concentrated to about 100 mL, takes off cooling; Add the 0.1g ascorbic acid, shake up, drip xylenol orange indicator 3-4 and drip; Being transferred to solution with hydrochloric acid (1+1) and ammoniacal liquor (1+1) is yellow just, adds saturated sodium fluoride, each 5mL of thiocarbamide, shakes up; Add 20mL acetate-sodium acetate buffer solution, shake up, use the EDTA standard titration solution to drip to become glassy yellow by aubergine to be terminal point to solution.The result sees the following form.
The selection test of table 7 cleansing solution concentration
The result shows: wash concentration reaches 5% ammonium chloride-5% ammoniacal liquor, records the result and can satisfy the analysis requirement.
Embodiment 43-45
Pipette 3 parts of electrolytic solution that 1.00mL contains manganese in the 300mL conical beaker, blow about water 20mL, add 3.0g ammonium chloride; Shake up, add 10mL ammoniacal liquor, add the 5mL oxydol; Shake up, boil produce to no continuous air bubbles till, destroy oxydol; Use quick filter paper while hot in the 500mL conical beaker, wash beaker 2 times with the 5% ammonium chloride-5% ammonia scrubbing liquid of heat, washing precipitation is 4,6,8 times respectively.Filtrating shakes up, and heating is concentrated to about 100 mL, takes off cooling; Add the 0.1g ascorbic acid, shake up, drip xylenol orange indicator 3-4 and drip; Being transferred to solution with hydrochloric acid (1+1) and ammoniacal liquor (1+1) is yellow just, adds saturated sodium fluoride, each 5mL of thiocarbamide, shakes up; Add 20mL acetate-sodium acetate buffer solution, shake up, use the EDTA standard titration solution to drip to become glassy yellow by aubergine to be terminal point to solution.The result sees the following form.
The test of table 8 washing of precipitate number of times
Selecting washing beaker number of times according to test figure is twice, and the washing precipitation number of times is 6-8 time.
Embodiment 46-57
According to the sample of different content in producing, we mix three samples in the 300mL conical beaker with standard, wherein sample 1 (Zn
2+: 50mg, Mn
2+: 10 mg); Sample 2 (Zn
2+: 100mg, Mn
2+: 10 mg); Mix mark 1 (Cu
2+0.2mg, Ca
2+10 mg, Mg
2+5mg, Sb
3+50 μ g, Pb
2+0.5 mg, Ni
2+50 μ g, Cd
2+0.5 mg, Fe
3+5 mg, AL
3+5 mg, Co
2+50 μ g, SiO
3 2-1.0 mg).Wherein sample 1 is prepared 12 parts respectively with sample 2, and in this 12 duplicate samples, adds Ca respectively
2+10 mg, Mg
2+20 mg, Sb
3+10 μ g, Pb
2+1.0 mg, Ni
2+50 μ g, Cd
2+2.0 mg, Fe
3+3.0mg, Cu
2+0.5mg, AL
3+8.0mg, Co
2+50 μ g, NaSiO
31.0 mg, mixed mark 1.Blow respectively about water 20mL, add 3.0g ammonium chloride, shake up; Add 10mL ammoniacal liquor, add the 5mL oxydol, shake up; Boil produce to no continuous air bubbles till, destroy oxydol, use quick filter paper while hot in the 500mL conical beaker; 5% ammonium chloride-5% ammonia scrubbing liquid with heat is washed beaker 2 times, precipitates 6-8 time.Filtrating shakes up, and heating is concentrated to about 100 mL, takes off cooling; Add the 0.1g ascorbic acid, shake up, drip xylenol orange indicator 3-4 and drip; Being transferred to solution with hydrochloric acid (1+1) and ammoniacal liquor (1+1) is yellow just, adds saturated sodium fluoride, each 5mL of thiocarbamide, shakes up; Add 20mL acetate-sodium acetate buffer solution, shake up, use the EDTA standard titration solution to drip to become glassy yellow by aubergine to be terminal point to solution.The result sees the following form.
Table 9 coexisting ion interference test mg
| Add zinc, manganese amount | Zn：50、Mn：10 | Zn：150、Mn：10 | ? |
| Add the coexistence elements amount | Record the zinc amount | Record the zinc amount | Embodiment |
| Ca 2＋10 | 50.04 | 150.01 | Embodiment 46 |
| Mg 2＋20 | 50.03 | 150.01 | Embodiment 47 |
| Sb 3＋10 | 49.95 | 149.96 | Embodiment 48 |
| Pb 2＋1.0 | 49.90 | 150.10 | Embodiment 49 |
| Ni 2＋50 | 49.98 | 150.07 | Embodiment 50 |
| Cd 2＋2.0 | 50.80 | 151.00 | Embodiment 51 |
| Fe 3＋3.0 | 50.10 | 150.30 | Embodiment 52 |
| Cu 2＋0.5 | 50.05 | 150.08 | Embodiment 53 |
| AL 3＋8.0 | 49.93 | 150.10 | Embodiment 54 |
| Co 2＋50 | 49.90 | 150.10 | Embodiment 55 |
| NaSiO 31.0 | 50.08 | 150.03 | Embodiment 56 |
| Mix mark 1 | 49.97 | 150.20 | Embodiment 57 |
The result shows; No matter whether separate, cadmium all disturbs the mensuration of zinc, does not still have the method for separating preferably or sheltering at present; Therefore; In analytical approach considered in recording the result, deduct cadmium content in the sample (in the zinc electrolyte cadmium content general＜1.0mg/L, can not consider), other impurity elements of above-mentioned amount can and be sheltered elimination such as the measure of grade through precipitate and separate.
Practical operation embodiment
Pipette 7 parts of new liquid of 1.00mL electrolysis in the 300mL conical beaker, wherein 6 parts of solution that add zinc ion content 30.00 mg respectively; Pipette 7 parts of 1.00 mL electrolysis waste solutions again in the 300mL conical beaker, wherein 6 parts of solution that add zinc ion content 50.00 mg respectively.Blow respectively about water 20mL, add 3.0g ammonium chloride, shake up; Add 10mL ammoniacal liquor, add the 5mL oxydol, shake up; Boil produce to no continuous air bubbles till, destroy oxydol, use quick filter paper while hot in the 500mL conical beaker; 5% ammonium chloride-5% ammonia scrubbing liquid with heat is washed beaker 2 times, precipitates 6-8 time.Filtrating shakes up, and heating is concentrated to about 100 mL, takes off cooling; Add the 0.1g ascorbic acid, shake up, drip xylenol orange indicator 3-4 and drip; Being transferred to solution with hydrochloric acid (1+1) and ammoniacal liquor (1+1) is yellow just, adds saturated sodium fluoride, each 5mL of thiocarbamide, shakes up; Add 20mL acetate-sodium acetate buffer solution, shake up, use the EDTA standard titration solution to drip to become glassy yellow by aubergine to be terminal point to solution.The result sees the following form.
Table 10 zinc recovery test is mg as a result
Can know that from table the recovery of sample is at 99.33-99.93%, and this method has high accuracy, can satisfy the analysis of zinc element in supernatant in the wet zinc-making system, the electrolytic solution fully.
Above-described only is preferred embodiment of the present invention.Should be understood that for the person of ordinary skill of the art, under teachings provided by the present invention,, can also make other equivalent modifications and improvement, also should be regarded as protection scope of the present invention as the common practise of this area.
Claims (7)
1. the analytical approach of zinc in the rapid and accurate determination zinc electrolyte, it is characterized in that: this method may further comprise the steps: pipette quantitative zinc electrolyte in container, add the excess chlorination ammonium after blowing water; Shake up, shake up behind adding excessive ammonia and the oxydol, boil to no continuous air bubbles generation; With quick filter paper heat filtering, wash the filtering container postprecipitation with ammonium chloride-ammonia scrubbing liquid behind the destruction oxydol, filtrating shakes up the back heating and concentrates; The cooling back adds ascorbic acid, shakes up the back and adds the xylenol orange indicator, uses hydrochloric acid and ammoniacal liquor to be transferred to solution just for yellow; Add saturated sodium fluoride, thiocarbamide, shake up, add acetate-sodium acetate buffer solution; Shake up, use the EDTA standard titration solution to drip to become glassy yellow by aubergine to be terminal point to solution.
2. according to the analytical approach of zinc in the said a kind of rapid and accurate determination zinc electrolyte of claim 1, it is characterized in that: pipette zinc electrolyte 1.00mL in conical beaker, blow water 20mL, add ammonium chloride; Shake up, add ammoniacal liquor, add oxydol, shake up; Boil to no continuous air bubbles generation, destroy oxydol, use quick filter paper while hot in conical beaker, wash beaker 2 times with the ammonium chloride-ammonia scrubbing liquid of heat; Deposition filtrating shakes up, and heating is concentrated to about 100 mL, takes off cooling, adds the 0.1g ascorbic acid; Shake up, drip xylenol orange indicator 3-4 and drip, being transferred to solution with hydrochloric acid and ammoniacal liquor is yellow just, adds saturated sodium fluoride, each 5mL of thiocarbamide; Shake up, add 20mL acetate-sodium acetate buffer solution, shake up, use the EDTA standard titration solution to drip to become glassy yellow by aubergine to be terminal point to solution.
3. according to the analytical approach of zinc in the said a kind of rapid and accurate determination zinc electrolyte of claim 2, it is characterized in that: blow that to add ammonium chloride after the water step be 2.0-5.0g, ammoniacal liquor 5.0-15.0ml, oxydol 3.0-9.0ml.
4. according to the analytical approach of zinc in the said a kind of rapid and accurate determination zinc electrolyte of claim 2, it is characterized in that: the oxydol that oxygenant is selected for use is substitutable for saturated bromine water or ammonium persulfate.
5. according to the analytical approach of zinc in the said a kind of rapid and accurate determination zinc electrolyte of claim 2, it is characterized in that: ammonium chloride-ammonia scrubbing liquid concentration is 5% ammonium chloride-5% ammoniacal liquor.
6. according to the analytical approach of zinc in the said a kind of rapid and accurate determination zinc electrolyte of claim 2; It is characterized in that: after dripping the xylenol orange indicator; Be in harmonious proportion and use hydrochloric acid to be hydrochloric acid and the water volume ratio mixed solution as 1:1, the ammoniacal liquor that mediation is used is the mixed solution of ammoniacal liquor and water volume ratio 1:1.
7. according to the analytical approach of zinc in claim 1 or the 2 said a kind of rapid and accurate determination zinc electrolytes, it is characterized in that: pipette zinc electrolyte 1.00ml in the 300ml conical beaker, blow water 20ml, add 3.0g ammonium chloride; Shake up, add 10ml ammoniacal liquor, add the 5.0ml oxydol, shake up; Boil produce to no continuous air bubbles till, destroy oxydol, use quick filter paper while hot in the 500ml conical beaker, wash beaker 2 times with the 5% ammonium chloride-5% ammonia scrubbing liquid of heat; Precipitate 6-8 filtrating and shake up, heating is concentrated to about 100 ml, takes off cooling; Add the 0.1g ascorbic acid, shake up, drip xylenol orange indicator 3-4 and drip; Being transferred to solution with hydrochloric acid (1+1) and ammoniacal liquor (1+1) is yellow just, adds saturated sodium fluoride, each 5ml of thiocarbamide, shakes up; Add 20ml acetate-sodium acetate buffer solution, shake up, use the EDTA standard titration solution to drip to become glassy yellow by aubergine to be terminal point to solution.
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