CN108872469A - A kind of method of lead bronze METHOD FOR CONTINUOUS DETERMINATION in efficient ore - Google Patents
A kind of method of lead bronze METHOD FOR CONTINUOUS DETERMINATION in efficient ore Download PDFInfo
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Abstract
The present invention relates to a kind of methods of lead bronze METHOD FOR CONTINUOUS DETERMINATION in efficient ore, belong to the method for lead bronze METHOD FOR CONTINUOUS DETERMINATION in ore.Use nitric acid-potassium chlorate saturated solution sample dissolution, the lead in solution is set to form lead sulfate precipitation using the concentrated sulfuric acid, lead is isolated after filtering, after separating obtained lead sulfate is using ammonium acetate dissolution, using xylenol orange as indicator, lead content can be obtained using the titration of EDTA standard solution, filtrate recycling, after simple process, using starch as indicator, titrated using sodium thiosulfate standard solution for measuring copper content.The invention has the advantages that only needing primary molten sample, it can simultaneously obtain lead content and copper content, experimental procedure is simplified to the full extent, workload needed for reducing test, reduce amount of reagent, quickly can measure sample in batches, reduce chemical examination cost, working efficiency is effectively increased, it is as a result reliable and stable.
Description
Technical field
The present invention relates to a kind of methods of lead bronze METHOD FOR CONTINUOUS DETERMINATION in ore, in particular to lead content is 5-40%, copper content
For the measuring method of the ore of 2-50%.
Background technique
Much it is related to the measuring method of copper content in the measurement of lead content and ore in ore in existing national standard method.But nothing
One exception, needs respectively using different molten sample prescription case independent analysis lead content and copper content, and individual analytical procedure is all longer,
And two kinds of elements cannot be analyzed simultaneously, chemical examination is time-consuming also longer.
Summary of the invention
The present invention provides a kind of method of lead bronze METHOD FOR CONTINUOUS DETERMINATION in efficient ore, with solve presently, there are individually point
It is all longer to analyse step, and two kinds of elements cannot be analyzed simultaneously, the time-consuming also longer problem of chemical examination.
Step of the invention is as follows：
(1) 0.28-0.30g sample m is accurately weighed, is placed in 400mL beaker, nitric acid-chloric acid of 20-25mL saturation is added
It is complete to be heated to Specimen eliminating on electric furnace for potassium solution, cap upper surface ware；
(2) it is cooling to remove beaker, the 8-10mL concentrated sulfuric acid is added into beaker, continuation is heated to emitting dense white cigarette 2- on electric furnace
3 minutes, beaker cooling is removed, slow water supplement to 80-90mL heats slightly boiled 8-10min on electric furnace；
(3) beaker is removed, it is 10-20 minutes cooling, 5-6mL dehydrated alcohol is added, shakes up, stands 1-1.5 hours；
(4) using double-layer filter paper filtering precipitating, filtrate is accepted with clean beaker, is washed after transfer completely with sulfuric acid lotion
For several times, filtrate, which retains, surveys copper for beaker and precipitating；
(5) filter paper in funnel is transferred in former beaker together with precipitating, 100mL acetic acid-is added into former beaker
Sodium acetate buffer solution, low-grade fever are boiled the solution containing filter paper 8-10 minutes, dissolution lead precipitating, be then washed with a small amount watch glass and
Wall of cup, it is 20-30 minutes cooling after 80-100mL water is added into former beaker, it is titrated using EDTA, according to titration volumes V and sky
White titration volumes V0Calculate lead content w1；
(6) after 5mL concentrated nitric acid being added in the filtrate retained into step (4), in steaming on electric furnace pan to volume residue 1-
2mL removes cooling, purges watch glass and wall of cup respectively three times with water 10-15mL, places back in heating on electric furnace pan and boils sample 1-2
Minute, remove cooling；
(7) acetic acid-ammonium acetate solution solution is added dropwise to red no longer intensification and excessive 3-4mL, 3-4mL fluorination is then added
Hydrogen ammonium saturated solution mixes, and 2-3g potassium iodide solid is added and shakes dissolution, is titrated immediately with sodium thiosulfate standard titration solution
To light yellow, addition 2-3mL starch solution, continue to drop to light blue, addition 4-5mL potassium thiocyanate solution, fierce shake to indigo plant
Color is deepened, then being titrated to blue and just disappearing is terminal, the volume V of record consumption sodium thiosulfate standard titration solution3And it is empty
White titration volumes V2Calculate copper content w2；
(8) blank assay is done in company with sample.
In step (1) of the present invention, when sample has the insoluble matter of black, 0.5-0.8g potassium chlorate solid can be added,
It is added and boils again, if there is insoluble matter, continuously add 0.5-0.8g potassium chlorate solid and 3-5mL nitric acid, until insoluble matter is complete
Portion's dissolution.
In step (2) of the present invention, need to after solution is completely cooled down to room temperature slow water supplement again.
In step (3) of the present invention, dehydrated alcohol is added for reducing the solubility of lead sulfate.
In step (4) of the present invention, the filter paper used is quantitative filter paper at a slow speed, the preparation side of used sulfuric acid lotion
Method is：The 50mL concentrated sulfuric acid is slowly added in water, after be settled to 2500mL.
In step (5) of the present invention, before being titrated using EDTA, 0.5-0.8g ascorbic acid is added and shelters iron, 2-3 is added
The xylenol orange of 1g/L is dripped as indicator；
The preparation method of the acetic acid-sodium acetate solution is：1500g sodium acetate is dissolved in water, and 200mL acetic acid is added,
It is diluted to 10000mL；
The preparation method of EDTA titrating solution is：68-70g disodium ethylene diamine tetraacetate is dissolved in 10L tubualted bottle, it is dilute with water
It releases to scale, shakes up, placement is demarcated two days later；
The scaling method of EDTA titrating solution is：4 parts of 20mL lead standard solution 0.004g/mL are drawn in parallel to close up in 400mL
In beaker, 28-30mL ammonium acetate solution is added, adds 80-100ml water, then plus 2-3 drop xylenol orange indicator, titrated with EDTA
Liquid, which is titrated to solution, becomes glassy yellow, as terminal from red, according to titration volumes V1It is calculated by (1) formula, obtains EDTA titrating solution
Titer T1；As a result it calculates：
In formula：
ω1The mass fraction of-lead, %；
V-sample consumption titrating solution volume, unit is ml；
V0- blank consumes the volume of titrating solution, and unit is ml；
V1The volume of titrating solution is consumed when-calibration, unit is mL；
M-sample quality, unit are g；
T1The titer of-EDTA titrating solution, unit are g/mL.
In step (7) of the present invention, if sample solution does not redden when acetic acid-ammonium acetate is added dropwise, it can be mended into solution
Add 1mL liquor ferri trichloridi 100g/L；
The preparation method of the acetic acid-ammonium acetate solution is：90g acetic acid adds 100mL water, 100mL glacial acetic acid, is diluted to
300mL；
The preparation method of ammonium acid fluoride saturated solution is：Ammonium hydrogen fluoride solid is added into 300mL water, until ammonium acid fluoride
It is not redissolved, takes supernatant to use after standing；
The preparation method of potassium thiocyanate solution is：100g potassium rhodanide solid is weighed, is dissolved in 1000mL water；
The preparation method of starch solution is：0.5g starch is weighed, is dissolved in 100mL water, heating is boiled molten to starch solution
Solution uniformly, uses after cooling；
The preparation method of sodium thiosulfate titrating solution is：50g sodium thiosulfate is weighed, the distilled water for boiling and cooling down is used
It is dissolved in 10L brown tubualted bottle, 2g natrium carbonicum calcinatum is added, 10mL chloroform stands calibration and usage after two weeks；
The scaling method of sodium thiosulfate titrating solution is：In parallel draw 4 parts of 20mL copper standard solution 0.002g/mL in
In 400mL closing in beaker, copper standard solution is handled by step (6) and step (7), and molten using sodium thiosulfate titration copper standard
Liquid, according to titration volumes V4It can be calculated the titer T of sodium thiosulfate titrating solution by (3) formula2；As a result it calculates：
In formula：
T2The titer of-sodium thiosulfate titrating solution, unit are g/mL；
ω2The mass fraction of-copper, %；
V2- blank consumes the volume of titrating solution, and unit is ml；
V3- sample consumes the volume of titrating solution, and unit is ml；
V4The volume of titrating solution is consumed when-calibration, unit is mL；
M-sample quality, unit are g.
It is 5-40% the present invention is more particularly directed to lead content, copper content is the measurement of the ore of 2-50%.
The present invention uses nitric acid-potassium chlorate saturated solution sample dissolution, so that the lead in solution is formed sulfuric acid using the concentrated sulfuric acid
Lead precipitating, isolates lead after filtering.After separating obtained lead sulfate is using ammonium acetate dissolution, using xylenol orange as indicator, use
The titration of EDTA standard solution can obtain lead content, and filtrate recycling after simple process, using starch as indicator, uses thio sulphur
Sour sodium standard solution titration is for measuring copper content.
Present invention uses simple and effective molten sample loading modes, while carrying out lead content and copper content to gained ore solution
Measurement, it is creative to separate lead from ore solution, individually measure, the solution after separating lead is used to measure copper content,
Primary molten sample METHOD FOR CONTINUOUS DETERMINATION lead bronze is achieved the effect that.
Beneficial effects of the present invention：It establishes primary molten sample and letter is taken to the method for lead in ore and copper METHOD FOR CONTINUOUS DETERMINATION
Single effective molten sample loading mode is capable of the obtaining accurately as a result, significantly reducing production cost of efficient stable.
The present invention is compared with current method, it is only necessary to which primary molten sample can simultaneously obtain lead content and copper content, utmostly
On simplify experimental procedure, reduce test needed for workload, reduce amount of reagent, can batch quickly measure sample, drop
Low chemical examination cost, effectively increases working efficiency, as a result reliable and stable.
Specific embodiment
Embodiment 1
(1) 0.28g sample m is accurately weighed, is placed in 400mL beaker, nitric acid-potassium chlorate solution of 20mL saturation is added,
It is complete to be heated to Specimen eliminating on electric furnace for cap upper surface ware；
(2) it is cooling to remove beaker, is added the 8mL concentrated sulfuric acid into beaker, continuation, which is heated to emitting dense white cigarette 2 on electric furnace, to divide
Clock, removes beaker cooling, and slow water supplement to 80mL heats slightly boiled 8min on electric furnace；
(3) beaker is removed, it is 10 minutes cooling, 5mL dehydrated alcohol is added, shakes up, stands 1 hour；
(4) using double-layer filter paper filtering precipitating, filtrate is accepted with clean beaker, is washed after transfer completely with sulfuric acid lotion
For several times, filtrate, which retains, surveys copper for beaker and precipitating；
(5) filter paper in funnel is transferred in former beaker together with precipitating, 100mL acetic acid-is added into former beaker
Sodium acetate buffer solution, low-grade fever are boiled the solution containing filter paper 8 minutes, then watch glass and cup is washed with a small amount in dissolution lead precipitating
Wall, it is 20 minutes cooling after 80mL water is added into former beaker, it is titrated using EDTA, according to titration volumes V and blank titration volume
V0Calculate lead content ω1；
(6) after 5mL concentrated nitric acid being added into the filtrate retained in step (4), in being steamed on electric furnace pan to volume residue 1mL,
Cooling is removed, purges watch glass and wall of cup respectively three times with water 10mL, heating on electric furnace pan is placed back in and boils sample 1 minute, remove
It is cooling；
(7) acetic acid-ammonium acetate solution solution is added dropwise to red no longer intensification and excessive 3mL, 3mL ammonium acid fluoride is then added
Saturated solution mixes, and 2g potassium iodide solid is added and shakes dissolution, is titrated to immediately with sodium thiosulfate standard titration solution pale yellow
2mL starch solution is added in color, continues to drop to light blue, addition 4mL potassium thiocyanate solution, fierce shake to blue intensification, then drip
Fixed just disappear to blue is terminal, the volume V of record consumption sodium thiosulfate standard titration solution3And blank titration volume V2
Calculate copper content ω2；
(8) blank assay is done in company with sample.
Calculate to obtain lead content and copper content.
Embodiment 2
(1) 0.30g sample m is accurately weighed, is placed in 400mL beaker, nitric acid-potassium chlorate solution of 25mL saturation is added,
It is complete to be heated to Specimen eliminating on electric furnace for cap upper surface ware；
(2) it is cooling to remove beaker, is added the 10mL concentrated sulfuric acid into beaker, continuation, which is heated to emitting dense white cigarette 3 on electric furnace, to divide
Clock, removes beaker cooling, and slow water supplement to 90mL heats slightly boiled 10min on electric furnace；
(3) beaker is removed, it is 20 minutes cooling, 6mL dehydrated alcohol is added, shakes up, stands 1.5 hours；
(4) using double-layer filter paper filtering precipitating, filtrate is accepted with clean beaker, is washed after transfer completely with sulfuric acid lotion
For several times, filtrate, which retains, surveys copper for beaker and precipitating；
(5) filter paper in funnel is transferred in former beaker together with precipitating, 100mL acetic acid-is added into former beaker
Sodium acetate buffer solution, low-grade fever are boiled the solution containing filter paper 10 minutes, then watch glass and cup is washed with a small amount in dissolution lead precipitating
Wall, it is 30 minutes cooling after 100mL water is added into former beaker, it is titrated using EDTA, according to titration volumes V and blank titration body
Product V0Calculate lead content ω1；
(6) after 5mL concentrated nitric acid being added into the filtrate retained in step (4), in being steamed on electric furnace pan to volume residue 2mL,
Cooling is removed, purges watch glass and wall of cup respectively three times with water 15mL, heating on electric furnace pan is placed back in and boils sample 2 minutes, remove
It is cooling；
(7) acetic acid-ammonium acetate solution solution is added dropwise to red no longer intensification and excessive 4mL, 4mL ammonium acid fluoride is then added
Saturated solution mixes；3g potassium iodide solid is added and shakes dissolution, is titrated to immediately with sodium thiosulfate standard titration solution pale yellow
3mL starch solution is added in color, continues to drop to light blue, addition 5mL potassium thiocyanate solution, fierce shake to blue intensification, then drip
Fixed just disappear to blue is terminal, the volume V of record consumption sodium thiosulfate standard titration solution3And blank titration volume V2
Calculate copper content ω2；
(8) blank assay is done in company with sample.
Calculate to obtain lead content and copper content.
Embodiment 3
(1) 0.29g sample m is accurately weighed, is placed in 400mL beaker, nitric acid-potassium chlorate that 22.5mL saturation is added is molten
It is complete to be heated to Specimen eliminating on electric furnace for liquid, cap upper surface ware；
(2) it is cooling to remove beaker, is added the 9mL concentrated sulfuric acid into beaker, continuation, which is heated to emitting dense white cigarette 2.5 on electric furnace, to divide
Clock, removes beaker cooling, and slow water supplement to 85mL heats slightly boiled 9min on electric furnace；
(3) beaker is removed, it is 15 minutes cooling, 5.5mL dehydrated alcohol is added, shakes up, stands 1.25 hours；
(4) using double-layer filter paper filtering precipitating, filtrate is accepted with clean beaker, is washed after transfer completely with sulfuric acid lotion
For several times, filtrate, which retains, surveys copper for beaker and precipitating；
(5) filter paper in funnel is transferred in former beaker together with precipitating, 100mL acetic acid-is added into former beaker
Sodium acetate buffer solution, low-grade fever are boiled the solution containing filter paper 9 minutes, then watch glass and cup is washed with a small amount in dissolution lead precipitating
Wall, it is 25 minutes cooling after 90mL water is added into former beaker, it is titrated using EDTA, according to titration volumes V and blank titration volume
V0Calculate lead content ω1；
(6) remaining to volume in being steamed on electric furnace pan after 5mL concentrated nitric acid being added in the filtrate retained into step (4)
1.5mL removes cooling, purges watch glass and wall of cup respectively three times with water 12.5mL, places back in heating on electric furnace pan and boils sample 1.5
Minute, remove cooling；
(7) acetic acid-ammonium acetate solution solution is added dropwise to red no longer intensification and excessive 3.5mL, 3.5mL fluorination is then added
Hydrogen ammonium saturated solution mixes；2.5g potassium iodide solid is added and shakes dissolution, is titrated immediately with sodium thiosulfate standard titration solution
To light yellow, addition 2.5mL starch solution, continue to drop to light blue, addition 4.5mL potassium thiocyanate solution, fierce shake to indigo plant
Color is deepened, then being titrated to blue and just disappearing is terminal, the volume V of record consumption sodium thiosulfate standard titration solution3And it is empty
White titration volumes V2Calculate copper content ω2；
(8) blank assay is done in company with sample.
In the various embodiments described above：
In the step (1), when sample has the insoluble matter of black, 0.5-0.8g potassium chlorate solid can be added, again plus
Enter to boil, if there is insoluble matter, continuously add 0.5-0.8g potassium chlorate solid and 3-5mL nitric acid, until insoluble matter all dissolves；
In the step (2), need to after solution is completely cooled down to room temperature slow water supplement again；
In the step (3), dehydrated alcohol is added for reducing the solubility of lead sulfate；
In the step (4), the filter paper used is that quantitative filter paper, the preparation method of used sulfuric acid lotion are at a slow speed：
The 50mL concentrated sulfuric acid is slowly added in water, after be settled to 2500mL；
In the step (5), before being titrated using EDTA, 0.5-0.8g ascorbic acid is added and shelters iron, 2-3 drop 1g/L is added
Xylenol orange as indicator；
The preparation method of the acetic acid-sodium acetate solution is：1500g sodium acetate is dissolved in water, and 200mL acetic acid is added,
It is diluted to 10000mL；
The preparation method of EDTA titrating solution is：68-70g disodium ethylene diamine tetraacetate is dissolved in 10L tubualted bottle, it is dilute with water
It releases to scale, shakes up, placement is demarcated two days later；
The scaling method of EDTA titrating solution is：4 parts of 20mL lead standard solution 0.004g/mL are drawn in parallel to close up in 400mL
In beaker, 28-30mL ammonium acetate solution is added, adds 80-100ml water, then plus 2-3 drop xylenol orange indicator, titrated with EDTA
Liquid, which is titrated to solution, becomes glassy yellow, as terminal from red, according to titration volumes V1It is calculated by (1) formula, obtains EDTA titrating solution
Titer T1；As a result it calculates：
In formula：
ω1The mass fraction of-lead, %；
V-sample consumption titrating solution volume, unit is ml；
V0- blank consumes the volume of titrating solution, and unit is ml；
V1The volume of titrating solution is consumed when-calibration, unit is mL；
M-sample quality, unit are g；
T1The titer of-EDTA titrating solution, unit are g/mL.
In the step (7), if sample solution does not redden when acetic acid-ammonium acetate is added dropwise, 1mL tri- can be added into solution
Ferric chloride solution 100g/L；
The preparation method of the acetic acid-ammonium acetate solution is：90g acetic acid adds 100mL water, 100mL glacial acetic acid, is diluted to
300mL；
The preparation method of ammonium acid fluoride saturated solution is：Ammonium hydrogen fluoride solid is added into 300mL water, until ammonium acid fluoride
It is not redissolved, takes supernatant to use after standing；
The preparation method of potassium thiocyanate solution is：100g potassium rhodanide solid is weighed, is dissolved in 1000mL water；
The preparation method of starch solution is：0.5g starch is weighed, is dissolved in 100mL water, heating is boiled molten to starch solution
Solution uniformly, uses after cooling；
The preparation method of sodium thiosulfate titrating solution is：50g sodium thiosulfate is weighed, the distilled water for boiling and cooling down is used
It is dissolved in 10L brown tubualted bottle, 2g natrium carbonicum calcinatum is added, 10mL chloroform stands calibration and usage after two weeks；
The scaling method of sodium thiosulfate titrating solution is：In parallel draw 4 parts of 20mL copper standard solution 0.002g/mL in
In 400mL closing in beaker, copper standard solution is handled by step (6) and step (7), and molten using sodium thiosulfate titration copper standard
Liquid, according to titration volumes V4It can be calculated the titer T of sodium thiosulfate titrating solution by (3) formula2；As a result it calculates：
In formula：
T2The titer of-sodium thiosulfate titrating solution, unit are g/mL；
ω2The mass fraction of-copper, %；
V2- blank consumes the volume of titrating solution, and unit is ml；
V3- sample consumes the volume of titrating solution, and unit is ml；
V4The volume of titrating solution is consumed when-calibration, unit is mL；
M-sample quality, unit are g.
Effect of the invention is further illustrated in conjunction with specific experiment example below.
Experimental example 1：Mark-on reclaims measurement is carried out to sample 1 (lead content 10.18%, copper content 17.26%)
(1) 0.28g sample m is accurately weighed, is placed in 400mL beaker, nitric acid-potassium chlorate solution of 20mL saturation is added,
It is complete to be heated to Specimen eliminating on electric furnace for cap upper surface ware；
(2) it is cooling to remove beaker, is added the 8mL concentrated sulfuric acid into beaker, continuation, which is heated to emitting dense white cigarette 2 on electric furnace, to divide
Clock, removes beaker cooling, and slow water supplement to 80mL heats slightly boiled 8min on electric furnace；
(3) beaker is removed, it is 10 minutes cooling, 5mL dehydrated alcohol is added, shakes up, stands 1 hour；
(4) using double-layer filter paper filtering precipitating, filtrate is accepted with clean beaker, is washed after transfer completely with sulfuric acid lotion
For several times, filtrate, which retains, surveys copper for beaker and precipitating；
(5) filter paper in funnel is transferred in former beaker together with precipitating, 100mL acetic acid-is added into former beaker
Sodium acetate buffer solution, low-grade fever are boiled the solution containing filter paper 8 minutes, then watch glass and cup is washed with a small amount in dissolution lead precipitating
Wall, it is 20 minutes cooling after 80mL water is added into former beaker, it is titrated using EDTA, according to titration volumes V and blank titration volume
V0Calculate lead content ω1；
(6) after 5mL concentrated nitric acid being added into the filtrate retained in step (4), in being steamed on electric furnace pan to volume residue 1mL,
Cooling is removed, purges watch glass and wall of cup respectively three times with water 10mL, heating on electric furnace pan is placed back in and boils sample 1 minute, remove
It is cooling；
(7) acetic acid-ammonium acetate solution solution is added dropwise to red no longer intensification and excessive 3mL, 3mL ammonium acid fluoride is then added
Saturated solution mixes, and 2g potassium iodide solid is added and shakes dissolution, is titrated to immediately with sodium thiosulfate standard titration solution pale yellow
2mL starch solution is added in color, continues to drop to light blue, addition 4mL potassium thiocyanate solution, fierce shake to blue intensification, then drip
Fixed just disappear to blue is terminal, the volume V of record consumption sodium thiosulfate standard titration solution3And blank titration volume V2
Calculate copper content ω2。
(8) blank assay is done in company with sample；
Calculate the rate of recovery of lead is 99.82%, the rate of recovery of copper is 99.76%.
Experimental example 2：Mark-on reclaims measurement is carried out to sample 2 (lead content 6.39%, copper content 10.22%)
(1) 0.30g sample m is accurately weighed, is placed in 400mL beaker, nitric acid-potassium chlorate solution of 25mL saturation is added,
It is complete to be heated to Specimen eliminating on electric furnace for cap upper surface ware；
(2) it is cooling to remove beaker, is added the 10mL concentrated sulfuric acid into beaker, continuation, which is heated to emitting dense white cigarette 3 on electric furnace, to divide
Clock, removes beaker cooling, and slow water supplement to 90mL heats slightly boiled 10min on electric furnace；
(3) beaker is removed, it is 20 minutes cooling, 6mL dehydrated alcohol is added, shakes up, stands 1.5 hours；
(4) using double-layer filter paper filtering precipitating, filtrate is accepted with clean beaker, is washed after transfer completely with sulfuric acid lotion
For several times, filtrate, which retains, surveys copper for beaker and precipitating；
(5) filter paper in funnel is transferred in former beaker together with precipitating, 100mL acetic acid-is added into former beaker
Sodium acetate buffer solution, low-grade fever are boiled the solution containing filter paper 10 minutes, then watch glass and cup is washed with a small amount in dissolution lead precipitating
Wall, it is 30 minutes cooling after 100mL water is added into former beaker, it is titrated using EDTA, according to titration volumes V and blank titration body
Product V0Calculate lead content ω1；
(6) after 5mL concentrated nitric acid being added into the filtrate retained in step (4), in being steamed on electric furnace pan to volume residue 2mL,
Cooling is removed, purges watch glass and wall of cup respectively three times with water 15mL, heating on electric furnace pan is placed back in and boils sample 2 minutes, remove
It is cooling；
(7) acetic acid-ammonium acetate solution solution is added dropwise to red no longer intensification and excessive 4mL, 4mL ammonium acid fluoride is then added
Saturated solution mixes, and 3g potassium iodide solid is added and shakes dissolution, is titrated to immediately with sodium thiosulfate standard titration solution pale yellow
3mL starch solution is added in color, continues to drop to light blue, addition 5mL potassium thiocyanate solution, fierce shake to blue intensification, then drip
Fixed just disappear to blue is terminal, the volume V of record consumption sodium thiosulfate standard titration solution3And blank titration volume V2
Calculate copper content ω2；
(8) blank assay is done in company with sample；
Calculate the rate of recovery of lead is 100.18%, the rate of recovery of copper is 99.66%.
This method is verified using verifyings means such as mark-on reclaims by experimental example, from the results of view, this method
It is reliable and stable.
Claims (7)
1. a kind of method of lead bronze METHOD FOR CONTINUOUS DETERMINATION in efficient ore, which is characterized in that include the following steps：
(1) 0.28-0.30g sample m is accurately weighed, is placed in 400mL beaker, nitric acid-potassium chlorate that 20-25mL saturation is added is molten
It is complete to be heated to Specimen eliminating on electric furnace for liquid, cap upper surface ware；
(2) it is cooling to remove beaker, the 8-10mL concentrated sulfuric acid is added into beaker, continuation is heated to emitting dense white cigarette 2-3 points on electric furnace
Clock, removes beaker cooling, and slow water supplement to 80-90mL heats slightly boiled 8-10min on electric furnace；
(3) beaker is removed, it is 10-20 minutes cooling, 5-6mL dehydrated alcohol is added, shakes up, stands 1-1.5 hours；
(4) using double-layer filter paper filtering precipitating, filtrate is accepted with clean beaker, washs beaker with sulfuric acid lotion after transfer completely
For several times with precipitating, filtrate, which retains, surveys copper；
(5) filter paper in funnel is transferred in former beaker together with precipitating, 100mL acetic acid-acetic acid is added into former beaker
Sodium buffer solution, low-grade fever are boiled the solution containing filter paper 8-10 minutes, then watch glass and cup is washed with a small amount in dissolution lead precipitating
Wall, it is 20-30 minutes cooling after 80-100mL water is added into former beaker, it is titrated using EDTA, according to titration volumes V and blank
Titration volumes V0Calculate lead content ω1；
(6) it after 5mL concentrated nitric acid being added in the filtrate retained into step (4), in steaming on electric furnace pan to volume residue 1-2mL, takes
Lower cooling purges watch glass and wall of cup respectively three times with water 10-15mL, places back in heating on electric furnace pan and boils sample 1-2 minutes, takes
Lower cooling；
(7) acetic acid-ammonium acetate solution solution is added dropwise to red no longer intensification and excessive 3-4mL, 3-4mL ammonium acid fluoride is then added
Saturated solution mixes, and 2-3g potassium iodide solid is added and shakes dissolution, is titrated to shallowly with sodium thiosulfate standard titration solution immediately
Yellow, be added 2-3mL starch solution, continue to drop to it is light blue, be added 4-5mL potassium thiocyanate solution, fierce shake to blue plus
It is deep, then being titrated to blue and just disappearing is terminal, the volume V of record consumption sodium thiosulfate standard titration solution3And blank drop
Determine volume V2Calculate copper content ω2；
(8) blank assay is done in company with sample.
2. the method for lead bronze METHOD FOR CONTINUOUS DETERMINATION in a kind of efficient ore according to claim 1, it is characterised in that：The step
Suddenly in (1), when sample has the insoluble matter of black, 0.5-0.8g potassium chlorate solid can be added, be added boil again, if there is not
Molten object continuously adds 0.5-0.8g potassium chlorate solid and 3-5mL nitric acid, until insoluble matter all dissolves.
3. the method for lead bronze METHOD FOR CONTINUOUS DETERMINATION in a kind of efficient ore according to claim 1, it is characterised in that：The step
Suddenly in (2), need to after solution is completely cooled down to room temperature slow water supplement again.
4. the method for lead bronze METHOD FOR CONTINUOUS DETERMINATION in a kind of efficient ore according to claim 1, it is characterised in that：The step
Suddenly in (3), dehydrated alcohol is added for reducing the solubility of lead sulfate.
5. the method for lead bronze METHOD FOR CONTINUOUS DETERMINATION in a kind of efficient ore according to claim 1, it is characterised in that：The step
Suddenly in (4), the filter paper used is that quantitative filter paper, the preparation method of used sulfuric acid lotion are at a slow speed：The 50mL concentrated sulfuric acid is delayed
Slowly be added to the water, after be settled to 2500mL.
6. the method for lead bronze METHOD FOR CONTINUOUS DETERMINATION in a kind of efficient ore according to claim 1, it is characterised in that：The step
Suddenly in (5), before being titrated using EDTA, 0.5-0.8g ascorbic acid is added and shelters iron, the xylenol orange conduct of 2-3 drop 1g/L is added
Indicator；
The preparation method of the acetic acid-sodium acetate solution is：1500g sodium acetate is dissolved in water, and 200mL acetic acid, dilution is added
To 10000mL；
The preparation method of EDTA titrating solution is：68-70g disodium ethylene diamine tetraacetate is dissolved in 10L tubualted bottle, is diluted with water to
Scale shakes up, and placement is demarcated two days later；
The scaling method of EDTA titrating solution is：4 parts of 20mL lead standard solution 0.004g/mL are drawn in parallel in 400mL closing in beaker
In, 28-30mL ammonium acetate solution is added, adds 80-100ml water, then plus 2-3 drop xylenol orange indicator, with EDTA titration drop
It is fixed to become glassy yellow, as terminal to solution from red, according to titration volumes V1It is calculated by (1) formula, obtains the drop of EDTA titrating solution
Surely T is spent1；As a result it calculates：
In formula：
ω1The mass fraction of-lead, %；
V-sample consumption titrating solution volume, unit is ml；
V0- blank consumes the volume of titrating solution, and unit is ml；
V1The volume of titrating solution is consumed when-calibration, unit is mL；
M-sample quality, unit are g；
T1The titer of-EDTA titrating solution, unit are g/mL.
7. the method for lead bronze METHOD FOR CONTINUOUS DETERMINATION in a kind of efficient ore according to claim 1, it is characterised in that：The step
Suddenly in (7), if sample solution does not redden when acetic acid-ammonium acetate is added dropwise, 1mL liquor ferri trichloridi can be added into solution
100g/L；
The preparation method of the acetic acid-ammonium acetate solution is：90g acetic acid adds 100mL water, 100mL glacial acetic acid, is diluted to 300mL；
The preparation method of ammonium acid fluoride saturated solution is：Ammonium hydrogen fluoride solid is added into 300mL water, until ammonium acid fluoride is no longer
It dissolves, takes supernatant to use after standing；
The preparation method of potassium thiocyanate solution is：100g potassium rhodanide solid is weighed, is dissolved in 1000mL water；
The preparation method of starch solution is：0.5g starch is weighed, is dissolved in 100mL water, heating is boiled equal to starch solution dissolution
It is even, it is used after cooling；
The preparation method of sodium thiosulfate titrating solution is：50g sodium thiosulfate is weighed, is dissolved using the distilled water for boiling and cooling down
In 10L brown tubualted bottle, 2g natrium carbonicum calcinatum is added, 10mL chloroform stands calibration and usage after two weeks；
The scaling method of sodium thiosulfate titrating solution is：4 parts of 20mL copper standard solution 0.002g/mL are drawn in parallel to receive in 400mL
In mouth beaker, copper standard solution is handled by step (6) and step (7), and titrate copper standard solution using sodium thiosulfate, according to
Titration volumes V4It can be calculated the titer T of sodium thiosulfate titrating solution by (3) formula2；As a result it calculates：
In formula：
T2The titer of-sodium thiosulfate titrating solution, unit are g/mL；
ω2The mass fraction of-copper, %；
V2- blank consumes the volume of titrating solution, and unit is ml；
V3- sample consumes the volume of titrating solution, and unit is ml；
V4The volume of titrating solution is consumed when-calibration, unit is mL；
M-sample quality, unit are g.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111693643A (en) * | 2020-06-17 | 2020-09-22 | 浙江天能电池(江苏)有限公司 | Free lead testing method for green plate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102226800A (en) * | 2011-06-14 | 2011-10-26 | 白银有色集团股份有限公司 | Chemical analysis method of complex crude copper sample |
| CN104792931A (en) * | 2015-05-05 | 2015-07-22 | 梧州市产品质量检验所 | Method of detecting copper content in metallic ores |
| CN105467068A (en) * | 2015-12-24 | 2016-04-06 | 阳谷祥光铜业有限公司 | Method for detecting copper, iron and calcium in flash converting furnace slag |
| CN106053366A (en) * | 2016-06-17 | 2016-10-26 | 长春黄金研究院 | Efficient accurate continuous measurement method for lead and zinc in lead concentrate and gold concentrate |
| CN107515273A (en) * | 2017-09-05 | 2017-12-26 | 长春黄金研究院 | A kind of method of lead content in simple, efficient measure Gold Concentrate under Normal Pressure |
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2018
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102226800A (en) * | 2011-06-14 | 2011-10-26 | 白银有色集团股份有限公司 | Chemical analysis method of complex crude copper sample |
| CN104792931A (en) * | 2015-05-05 | 2015-07-22 | 梧州市产品质量检验所 | Method of detecting copper content in metallic ores |
| CN105467068A (en) * | 2015-12-24 | 2016-04-06 | 阳谷祥光铜业有限公司 | Method for detecting copper, iron and calcium in flash converting furnace slag |
| CN106053366A (en) * | 2016-06-17 | 2016-10-26 | 长春黄金研究院 | Efficient accurate continuous measurement method for lead and zinc in lead concentrate and gold concentrate |
| CN107515273A (en) * | 2017-09-05 | 2017-12-26 | 长春黄金研究院 | A kind of method of lead content in simple, efficient measure Gold Concentrate under Normal Pressure |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111693643A (en) * | 2020-06-17 | 2020-09-22 | 浙江天能电池(江苏)有限公司 | Free lead testing method for green plate |
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