CN109030391A - The measuring method of dissoluble lead, soluble Zn in Lead and Zinc bulk concentrates - Google Patents
The measuring method of dissoluble lead, soluble Zn in Lead and Zinc bulk concentrates Download PDFInfo
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- CN109030391A CN109030391A CN201810900277.8A CN201810900277A CN109030391A CN 109030391 A CN109030391 A CN 109030391A CN 201810900277 A CN201810900277 A CN 201810900277A CN 109030391 A CN109030391 A CN 109030391A
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Abstract
The present invention relates to the measuring methods of dissoluble lead, soluble Zn in a kind of Lead and Zinc bulk concentrates, and determination step is: step 1: Lead and Zinc bulk concentrates are placed in conical beaker, acetic acid-ammonium acetate solution are added, is diluted with water；Then ascorbic acid is added into solution again, with the dry filtering of slow filter paper, divides take filtered clear liquid as needed, add nitric acid (1+1), be settled to scale with water, mix；Step 2: being returned to zero using Air-acetylene Flame with water, the absorbance of measurement lead, zinc subtracts the absorbance of sample blank solution, dissoluble lead zinc concentration is checked in from corresponding working curve；The drafting of third step working curve, and lead zinc is drawn respectively.Suitable solvent has been selected, dissoluble lead, soluble Zn can have been leached disposably, simultaneously, will shorten to analysis time 3 hours or so, error range controls within 0.5%.
Description
Technical field
The invention belongs to metal assay method and technology field, it is related to dissoluble lead in a kind of Lead and Zinc bulk concentrates, solvable
Property Direct spectrophotometry method.
Background technique
The prior art mainly has issued professional standard " YS/T 461.1-2013 Lead and Zinc bulk concentrates chemical analysis
Method part 1: the measurement precipitation and separation Na of lead amount and zinc amount2EDTA method ", this method can only measure in Lead and Zinc bulk concentrates
Total lead, total zinc amount.This method mainly passes through three kinds of strong acid (hydrochloric acid, nitric acid, sulfuric acid) and decomposes jointly, will be in lead and zinc bulk concentrate
Total lead, total zinc all dissolution completely after, analyzed using EDTA titration.
In lead zinc pyrometallurgical smelting process, effective component is mainly vulcanized lead, zinc sulphide.The prior art cannot be by mixed lead zinc
Vulcanized lead (zinc) in concentrate individually detected.Can not by indirect method by the lead zinc in Lead and Zinc bulk concentrates other
Object phase constituent, which individually determines, to be come, and is further acquired with minusing.
Now socially some illegal suppliers, in order to pursue juice, by the waste material of some leaded zinc, such as: lead skim
(leaded 20%-30%), scrap battery (lead 10%-40%), lead mud (lead 40% or so), gas ash (zinc 30% or so), flue containing zinc
Grey (10%-40%), secondary zinc oxide (zinc 40% or so), other as cobalt smelt in soaked cobalt slag (zinc up to 30%) and some imports
Leaded Zn scrap returns ... be mixed into Lead and Zinc bulk concentrates, adulterate.Lead, zinc in these waste materials is most of with sulfuric acid
Lead (zinc) form exists, and partially with ceruse (zinc), lead oxide (zinc) exists, these leaded (zinc) waste material costs are very low, much
Lower than the price of vulcanized lead (zinc) concentrate.
Dissoluble lead in Lead and Zinc bulk concentrates, soluble Zn content be affected for the production process of lead-zinc smelting.
The temperature of agglomerate, desulfurization degree and caking capacity are directly affected, and then influences lead, zinc yield.
Summary of the invention
In order to overcome the disadvantages mentioned above of the prior art, the present invention provides a kind of dissoluble lead in Lead and Zinc bulk concentrates, can
Dissolubility Direct spectrophotometry method, has selected suitable solvent, dissoluble lead, soluble Zn can be leached disposably, simultaneously, when by analyzing
Between shorten to 3 hours or so, error range control within 0.5%.
The technical solution adopted by the present invention to solve the technical problems is: a kind of dissoluble lead in Lead and Zinc bulk concentrates,
The measuring method of soluble Zn, determination step are:
Step 1: 0.1g Lead and Zinc bulk concentrates are placed in the conical beaker of 250 mL, acetic acid-ammonium acetate solution is added, then use
Water is diluted to 100 mL；Then 0.3g~0.5g ascorbic acid is added into solution again, vibrates 30min~2h, removes, it is cooling,
Solution is transferred to the volumetric flask of 250mL, is settled to scale with water, is mixed；With the dry filtering of slow filter paper, divides took as needed
Clear liquid 5mL~the 10mL filtered adds 10mL nitric acid (1+1) in the volumetric flask of 100mL, is settled to scale with water, mixes；
Step 2: at Atomic Absorption Spectrometer wavelength 283.3nm, 213.9 nm, returned to zero using Air-acetylene Flame with water,
The absorbance for measuring lead, zinc, subtracts the absorbance of sample blank solution, dissoluble lead zinc is checked in from corresponding working curve
Concentration；
The drafting of third step working curve, and lead zinc is drawn respectively:
Lead standard liquid series: 0,2.00mL, 4.00mL, 6.00mL, 8.00mL, 10.00mL lead standard solution is pipetted respectively
(100 μ g/mL) is added 10mL nitric acid (1+1) in one group of 100mL volumetric flask, is diluted with water to scale, mixes；This solution lead
Concentration is respectively as follows: 0,2.00 μ g/mL, 4.00 μ g/mL, 6.00 μ g/mL, 8.00 μ g/mL, 10.00 μ g/mL；
Zinc standard solution series: 0,0.10mL, 0.20mL, 0.50mL, 1.00mL, 2.00mL Zinc standard solution (100 is pipetted respectively
μ g/mL) in one group of 100mL volumetric flask, it is added 10mL nitric acid (1+1), is diluted with water to scale, mix；Zinc concentration is respectively as follows:
0,0.10µg/mL,0.20µg/mL,0.50µg/mL,1.00µg/mL,2.00µg/mL；
With under measurement sample solution the same terms, the absorbance of lead zinc series standard solution is measured, series standard solution is subtracted
In " zero " strength solution absorbance, using the concentration of respective element as abscissa, absorbance is ordinate, and it is bent to draw work respectively
Line.
It needs to sort out the various object phase constituents in Lead and Zinc bulk concentrates before implementing the first step, can be divided into big for three
Class: dissoluble lead zinc, vulcanized lead zinc, slightly solubility lead zinc, or it is divided into two classes, effective component: vulcanized lead zinc, unfavorable ingredient: easily
Molten lead zinc.
Acetic acid-the ammonium acetate solution is dissolved in the ratio production that glacial acetic acid 3-5mL is added in water according to 15g ammonium acetate solid,
Need to be heated to 80 DEG C~100 DEG C before addition in advance, which can also select ammonium acetate solid 10g-
20g, glacial acetic acid 2mL-10mL are used as and prepare raw material, and need for temperature to be heated to before addition between 60 DEG C~120 DEG C.
Acetic acid-the ammonium acetate solution can be replaced by ammonium hydroxide-ammonium chloride solution.
Oscillation in the first step can be replaced using magnetic agitation.
The positive effect of the present invention is: need not all analyze every kind of object phase constituent and come, but be influenced production process
Unfavorable ingredient be uniformly classified as dissoluble lead (zinc)；It solves property phase constituent in Lead and Zinc bulk concentrates is all single respectively
The problem of solely determining the time overlength come, difficulty super large (if all individually measured, needs ten days or so time-consuming), also solves
The problem of error superposition for all individually determining property phase constituent in Lead and Zinc bulk concentrates to come of having determined becomes larger (error
Superposition is up to 3%-5%)；The application has selected suitable solvent, can leach dissoluble lead, soluble Zn disposably, simultaneously.Energy will
Analysis time shorten to 3 hours or so, and error range controls within 0.5%；The mixed lead that certain factory buys is measured using this programme
Zinc concentrate, method is practical, finds within 1 year hundreds of batches containing the Lead and Zinc bulk concentrates compared with high dissolubility lead (zinc), converts into concentrate
Tens of thousands of tons.
Specific embodiment
Below with reference to embodiment, the present invention is further described.
The measuring method of dissoluble lead, soluble Zn in a kind of Lead and Zinc bulk concentrates, determination step is:
Step 1: 0.1g Lead and Zinc bulk concentrates are placed in the conical beaker of 250 mL, acetic acid-ammonium acetate solution is added, then use
Water is diluted to 100 mL；Then 0.3g~0.5g ascorbic acid is added into solution again, vibrates 30min~2h, removes, it is cooling,
Solution is transferred to the volumetric flask of 250mL, is settled to scale with water, is mixed；With the dry filtering of slow filter paper, divides took as needed
Clear liquid 5mL~the 10mL filtered adds 10mL nitric acid (1+1) in the volumetric flask of 100mL, is settled to scale with water, mixes；
Step 2: at Atomic Absorption Spectrometer wavelength 283.3nm, 213.9 nm, returned to zero using Air-acetylene Flame with water,
The absorbance for measuring lead, zinc, subtracts the absorbance of sample blank solution, dissoluble lead zinc is checked in from corresponding working curve
Concentration；
The drafting of third step working curve, and lead zinc is drawn respectively:
Lead standard liquid series: 0,2.00mL, 4.00mL, 6.00mL, 8.00mL, 10.00mL lead standard solution is pipetted respectively
(100 μ g/mL) is added 10mL nitric acid (1+1) in one group of 100mL volumetric flask, is diluted with water to scale, mixes；This solution lead
Concentration is respectively as follows: 0,2.00 μ g/mL, 4.00 μ g/mL, 6.00 μ g/mL, 8.00 μ g/mL, 10.00 μ g/mL；
Zinc standard solution series: 0,0.10mL, 0.20mL, 0.50mL, 1.00mL, 2.00mL Zinc standard solution (100 is pipetted respectively
μ g/mL) in one group of 100mL volumetric flask, it is added 10mL nitric acid (1+1), is diluted with water to scale, mix；Zinc concentration is respectively as follows:
0,0.10µg/mL,0.20µg/mL,0.50µg/mL,1.00µg/mL,2.00µg/mL；
With under measurement sample solution the same terms, the absorbance of lead zinc series standard solution is measured, series standard solution is subtracted
In " zero " strength solution absorbance, using the concentration of respective element as abscissa, absorbance is ordinate, and it is bent to draw work respectively
Line.
It needs to sort out the various object phase constituents in Lead and Zinc bulk concentrates before implementing the first step, can be divided into big for three
Class: dissoluble lead zinc, vulcanized lead zinc, slightly solubility lead zinc, or it is divided into two classes, effective component: vulcanized lead zinc, unfavorable ingredient: easily
Molten lead zinc.
Acetic acid-the ammonium acetate solution is dissolved in the ratio production that glacial acetic acid 3-5mL is added in water according to 15g ammonium acetate solid,
Need to be heated to 80 DEG C~100 DEG C before addition in advance, which can also select ammonium acetate solid 10g-
20g, glacial acetic acid 2mL-10mL are used as and prepare raw material, and need for temperature to be heated to before addition between 60 DEG C~120 DEG C.
Acetic acid-the ammonium acetate solution can be replaced by ammonium hydroxide-ammonium chloride solution.
Oscillation in the first step can be replaced using magnetic agitation.
The present invention, which need not can analyze every kind of object phase constituent, to be come, but is influenced the unfavorable ingredient of production process
Uniformly it is classified as dissoluble lead (zinc)；It solves and all individually determines by property phase constituent in Lead and Zinc bulk concentrates
Time overlength, difficulty super large the problem of (if all individually measured, need time-consuming ten days or so), also solving will mix
(error superposition is up to the problem of whole error superpositions individually determined of property phase constituent become larger in lead and zinc concentrate
3%-5%)；The application has selected suitable solvent, can leach dissoluble lead, soluble Zn disposably, simultaneously.It can be by analysis time
It shorten to 3 hours or so, error range controls within 0.5%；The Lead and Zinc bulk concentrates that certain factory buys are measured using this programme,
Method is practical, finds within 1 year hundreds of batches containing the Lead and Zinc bulk concentrates compared with high dissolubility lead (zinc), converts into the tens of thousands of tons of concentrate.
Claims (5)
1. the measuring method of dissoluble lead, soluble Zn in a kind of Lead and Zinc bulk concentrates, it is characterised in that determination step is:
Step 1: 0.1g Lead and Zinc bulk concentrates are placed in the conical beaker of 250 mL, acetic acid-ammonium acetate solution is added, then use
Water is diluted to 100 mL；Then 0.3g~0.5g ascorbic acid is added into solution again, vibrates 30min~2h, removes, it is cooling,
Solution is transferred to the volumetric flask of 250mL, is settled to scale with water, is mixed；With the dry filtering of slow filter paper, divides took as needed
Clear liquid 5mL~the 10mL filtered adds 10mL nitric acid (1+1) in the volumetric flask of 100mL, is settled to scale with water, mixes；
Step 2: at Atomic Absorption Spectrometer wavelength 283.3nm, 213.9 nm, returned to zero using Air-acetylene Flame with water,
The absorbance for measuring lead, zinc, subtracts the absorbance of sample blank solution, dissoluble lead zinc is checked in from corresponding working curve
Concentration；
The drafting of third step working curve, and lead zinc is drawn respectively:
Lead standard liquid series: 0,2.00mL, 4.00mL, 6.00mL, 8.00mL, 10.00mL lead standard solution is pipetted respectively
(100 μ g/mL) is added 10mL nitric acid (1+1) in one group of 100mL volumetric flask, is diluted with water to scale, mixes；This solution lead
Concentration is respectively as follows: 0,2.00 μ g/mL, 4.00 μ g/mL, 6.00 μ g/mL, 8.00 μ g/mL, 10.00 μ g/mL；
Zinc standard solution series: 0,0.10mL, 0.20mL, 0.50mL, 1.00mL, 2.00mL Zinc standard solution (100 is pipetted respectively
μ g/mL) in one group of 100mL volumetric flask, it is added 10mL nitric acid (1+1), is diluted with water to scale, mix；Zinc concentration is respectively as follows:
0,0.10µg/mL,0.20µg/mL,0.50µg/mL,1.00µg/mL,2.00µg/mL；
With under measurement sample solution the same terms, the absorbance of lead zinc series standard solution is measured, series standard solution is subtracted
In " zero " strength solution absorbance, using the concentration of respective element as abscissa, absorbance is ordinate, and it is bent to draw work respectively
Line.
2. the measuring method of dissoluble lead, soluble Zn in Lead and Zinc bulk concentrates as described in claim 1, it is characterised in that:
It needs to sort out the various object phase constituents in Lead and Zinc bulk concentrates before implementing the first step, can be divided into for three categories: is soluble
Lead zinc, vulcanized lead zinc, slightly solubility lead zinc, or it is divided into two classes, effective component: vulcanized lead zinc, unfavorable ingredient: readily soluble lead zinc.
3. the measuring method of dissoluble lead, soluble Zn in Lead and Zinc bulk concentrates as described in claim 1, it is characterised in that:
Acetic acid-the ammonium acetate solution is dissolved in the ratio production that glacial acetic acid 3-5mL is added in water according to 15g ammonium acetate solid, before addition
Need to be heated to 80 DEG C~100 DEG C in advance, which can also select ammonium acetate solid 10g-20g, glacial acetic acid
2mL-10mL is used as and prepares raw material, and needs for temperature to be heated to before addition between 60 DEG C~120 DEG C.
4. the measuring method of dissoluble lead, soluble Zn in Lead and Zinc bulk concentrates as described in claim 1, it is characterised in that:
Acetic acid-the ammonium acetate solution can be replaced by ammonium hydroxide-ammonium chloride solution.
5. the measuring method of dissoluble lead, soluble Zn in Lead and Zinc bulk concentrates as described in claim 1, it is characterised in that:
Oscillation in the first step can be replaced using magnetic agitation.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110660096A (en) * | 2019-10-08 | 2020-01-07 | 珠海格力电器股份有限公司 | Curve consistency detection method and storage medium |
| CN112595684A (en) * | 2020-12-31 | 2021-04-02 | 中国华冶科工集团有限公司 | Method for determining lead content in lead-zinc ore by atomic absorption method and application |
-
2018
- 2018-08-09 CN CN201810900277.8A patent/CN109030391A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110660096A (en) * | 2019-10-08 | 2020-01-07 | 珠海格力电器股份有限公司 | Curve consistency detection method and storage medium |
| CN112595684A (en) * | 2020-12-31 | 2021-04-02 | 中国华冶科工集团有限公司 | Method for determining lead content in lead-zinc ore by atomic absorption method and application |
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Address after: Room 303C, tower 2, Shenye Jinyuan Building, No. 112, Qingshuihe 1st Road, Qingshuihe community, Luohu District, Shenzhen City, Guangdong Province Applicant after: SHENZHEN ZHONGJIN LINGNAN NONFEMET Co.,Ltd. Address before: 518042 24-26 Floor, China Nonferrous Building, 6013 Shennan Avenue, Chegongmiao, Futian District, Shenzhen City, Guangdong Province Applicant before: SHENZHEN ZHONGJIN LINGNAN NONFEMET Co.,Ltd. |
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Application publication date: 20181218 |
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