CN105784919A - Method for eliminating bismuth interference in determination of lead content of mineral by EDTA (ethylenediaminetetraacetic acid) volumetric method - Google Patents
Method for eliminating bismuth interference in determination of lead content of mineral by EDTA (ethylenediaminetetraacetic acid) volumetric method Download PDFInfo
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Abstract
The invention discloses a method for eliminating bismuth interference in the determination of lead content of a mineral by EDTA (ethylenediaminetetraacetic acid) volumetric method. The method using the mineral as a specimen includes the steps of specimen digesting, acid driving, lead sulfate precipitate forming, lead sulfate precipitate dissolving, and titrating. The method is differed from the prior art in that before titrating lead acetate solution obtained in the step of lead sulfate precipitate dissolving, 2,3-dimercaprol is added; the 2,3-dimercaprol is used to react with bismuth to generate a substance with a stability constant higher than that of Bi-EDTA, the interference due to the presence of bismuth in the determination of lead content of the mineral by EDTA volumetric method is effectively eliminated accordingly, and the method is simple and quick, has reliable results and can meet the production analytical requirement.
Description
Technical field
The present invention relates to non-ferrous metal analysis and testing technology, be specifically related to use EDTA volumetric determination ore deposit
The method eliminating bismuth interference in thing during lead content.
Background technology
Leaded polymetallic ore and alloy are that lead is smelted and highly important raw material in processing industry.Right
For instructing mine development and Mineral Processing Enterprises processing, in Accurate Determining polymetallic ore and alloy
Lead (Pb) content is particularly important.A lot, for lead ore (lead content >=5%) for measuring the method for lead
Speech, Analysis on amount of lead assay method generally selects EDTA volumetric method.But, using showing of lead concentrate
When having national standard to analyze the lead content that method measures the lead ore of bismuth-containing and alloy, the existence meeting of a large amount of bismuths
Produce larger interference, applicant it is thought that because bismuth partial hydrolysis formed alkali formula bismuth sulfate and lead sulfate
It is co-precipitated so that while EDTA complexometry lead, bismuth also consumes EDTA, so that point
Analysis result is higher.Prior art is not yet found to have and eliminates bismuth by addition 2,3-dimercaprol dimercaptopropanol (BAL)
The relevant report of interference.
Summary of the invention
The technical problem to be solved in the present invention is to provide lead in a kind of use EDTA volumetric determination mineral and contains
The method eliminating bismuth interference during amount.The method can effectively eliminate the bismuth impact on Determination of Pb in mineral,
And the degree of accuracy is high, accuracy is good.
For solve above-mentioned technical problem, the present invention by the following technical solutions:
The method eliminating bismuth interference when using lead content in EDTA volumetric determination mineral, the method is with ore deposit
Thing is sample, including sample digestion step, catches up with acid step, formation lead sulfate settling step, lead sulfate to sink
Shallow lake dissolving step and titration step, unlike the prior art: dissolving step to through lead sulfate precipitation
Before the lead acetate solution of rapid gained titrates, adding 2,3-dimercaprol dimercaptopropanol (is called for short BAL).
In technique scheme, the addition volume (V of described 2,3-dimercaprol dimercaptopropanolBAL) molten with lead acetate
Bismuth ion content (M in liquidBi) ratio be: 0.125~0.3ml:1mg, more preferably 0.2~0.3ml:
1mg。
The method of the invention is applicable to detect the content of lead in sample, and contains bismuth in sample simultaneously
Situation, be preferably applied to lead content >=1% and the mineral of bi content >=0.1% or alloy, be particularly suited for
Lead content >=5% and the mineral of bi content >=0.5% or alloy.
In the method for the invention, described mineral can be selected from lead content >=1% and bi content >=0.1%
Polymetallic ore, lead concentrate and metal in one or more combination.
In order to make 2,3-dimercaprol dimercaptopropanol being scattered in lead acetate solution evenly, reduce further bismuth from
Lead detection is disturbed thus is improved accuracy and the accuracy of lead content detection further by son, preferably will
2,3-dimercaprol dimercaptopropanol joins in lead acetate solution with the form of the 2,3-dimercaprol dimercaptopropanol aqueous solution.Applicant
Thinking on the basis of test, by 2,3-dimercaprol dimercaptopropanol water is configured to 2,3-that concentration is 1~40v/v%
Dimercaprol dimercaptopropanol solution is then added in lead acetate solution to obtain preferable effect;And by 2,3-bis-mercapto
Base propyl alcohol is configured to the 2,3-dimercaprol dimercaptopropanol aqueous solution that concentration is 5~15v/v%, and to be then added to lead acetate molten
Liquid can obtain more preferably effect.
When in lead acetate solution containing iron ion, in order to avoid iron ion produces dry when lead content detects
Disturbing, preferably adding 2, adding ascorbic acid while 3-dimercaprol dimercaptopropanol (can be with solid or the aqueous solution
Form adds).Applicant thinks on the basis of test, and the addition of ascorbic acid is in lead acetate solution
In more than 1 times of iron ion mole, preferably lead acetate solution 1.5 times of iron ion mole.
In the method for the invention, except adding 2, outside 3-dimercaprol dimercaptopropanol before titration step, its
What it was described clears up step, catches up with acid step, formation lead sulfate settling step, lead sulfate precipitation dissolving step
And the concrete operations of titration step are the most same as the prior art.
Specifically, method of the present invention specifically includes following steps:
1) sample digestion: with mineral as sample, is cleared up sample by existing conventional method;
2) acid is caught up with: remove for clearing up the acid used by sample as existing conventional method;
3) formed lead sulfate precipitation: to through above-mentioned steps 2) process gained material in add water, boil after the coldest
But, add proper amount of methanol or ethanol, stand until lead sulfate precipitation is complete;
4) lead sulfate precipitation is dissolved: above-mentioned steps 3) gained reactant Filter paper filtering at a slow speed, by filter paper and
Precipitation on filter paper is placed in container, adds acetic acid-sodium acetate buffer solution and xylenol orange indicator, boils
Boiling, cooling, obtain lead acetate solution;
5) titration: to step 4) the lead acetate solution of gained adds 2,3-dimercaprol dimercaptopropanol, dilute with water
After, become glassy yellow, the EDTA standard that record consumes with EDTA standard liquid volumetric soiutions from redness
The volume of solution, and it is calculated as follows the content of lead in sample:
ω/10-2=VS×fT/mS/10
Wherein: fT=mB/VB
ω is the content of lead, %, V in sampleB、VSIt is respectively metallic lead and sample consumption EDTA standard is molten
The volume of liquid, mL;fTFor the EDTA standard liquid titer to lead, mg/mL;mB、mSIt is respectively
Alleged metallic lead and the quality of sample, g.
More specifically, the method for the invention comprises the following steps:
1) sample digestion: with mineral as sample, the sample weighing constant weight (such as 0.1~0.3g, is accurate to
0.0001g) in container (such as beaker), use a small amount of water-wet, add by the solid-to-liquid ratio of 1g:50~100mL
Concentrated hydrochloric acid, close the lid (such as surface plate), after 120~150 DEG C of heating for dissolving 3~5min, then presses 1g:
The solid-to-liquid ratio of 15~30mL adds red fuming nitric acid (RFNA), continues to be heated to sample and decomposes completely, obtains test portion;
2) acid is caught up with: add by the sulfuric acid solution of 50% in test portion by the solid-to-liquid ratio of 1g:150~200mL,
It is heated to emitting the white cigarette of dense sulfur trioxide, cooling, continues after rinsing lid and chamber wall with a small amount of water afterwards
It is heated to emitting the white cigarette of sulfur trioxide, makes the hydrochloric acid of excess and nitric acid catch up with to the greatest extent, take off cooling;
3) lead sulfate precipitation is formed: to step 2) material of gained is pressed the solid-liquid of 1g:500~800mL
Ratio adds water, and heating is boiled and made soluble-salt dissolve, and the solid-to-liquid ratio pressing 1g:50~80mL after cooling adds
Ethanol or methyl alcohol, shake up, and stands until lead sulfate precipitation completely (time of standing generally >=2h);
4) lead sulfate precipitation is dissolved: above-mentioned steps 3) gained reactant Filter paper filtering at a slow speed is (dense with dilute sulfuric acid
Degree is 3~the sulfuric acid scrubbing of 8% (volumetric concentration), afterwards together with filter paper, lead sulfate precipitation is put back to former container
In, dropping xylenol orange indicator (concentration of xylenol orange indicator can determine as required, usually 1~
5g/L), with ammoniacal liquor, solution is adjusted to aubergine, by 1g (referring to the amount that lead sulfate precipitates): 200~250mL
Solid-to-liquid ratio add acetic acid-sodium acetate buffer solution (pH ≈ 5.8), boil 5~10min, cooling, obtain second
Lead plumbate solution;
5) titration: to step 4) the lead acetate solution of gained adds 2,3-dimercaprol dimercaptopropanol, dilute with water
(it is typically diluted to 100~120mL) afterwards, is become bright orange with EDTA standard liquid volumetric soiutions from redness
Look, the volume of the EDTA standard liquid that record consumes, and it is calculated as follows the content of lead in sample:
ω/10-2=VS×fT/mS/10
Wherein: fT=mB/VB
ω is the content of lead, %, V in sampleB、VSIt is respectively metallic lead and sample consumption EDTA standard is molten
The volume of liquid, mL;fTFor the EDTA standard liquid titer to lead, mg/mL;mB、mSIt is respectively
Alleged metallic lead and the quality of sample, g.
Compared with prior art, the present invention utilizes 2, and 3-dimercaprol dimercaptopropanol and bismuth react and can generate stability constant
Higher than the material of Bi-EDTA, thus when effectively eliminating lead content in use EDTA volumetric determination mineral
The interference produced because of the existence of bismuth, the method for the invention is easy, quick, and reliable results can meet
Producing to analyze needs.
The following is applicant and the method for the invention is included preparation and demarcation, experimental technique, the lead ore of reagent
In stone and alloy, bismuth enters that lead sulfate Precipitation, BAL shelter the principle of bismuth and blank assay, BAL adds
The angle of incidence and addition choice experiment:
1, the preparation of reagent and demarcation
Metallic lead, bismuth (99.99%), ascorbic acid, hydrochloric acid, nitric acid, sulfuric acid, ammoniacal liquor, ethanol, ice
Acetic acid, sodium acetate trihydrate, disodium ethylene diamine tetraacetate (Na2EDTA), xylenol orange, 2,3-dimercapto
Propyl alcohol (BAL) etc., the not marked AR that is, test water is first water.
Xylenol orange indicator: 5g/L.
Acetic acid-sodium acetate buffer solution (pH ≈ 5.8): weigh 500g sodium acetate trihydrate soluble in water, add
Enter about 50mL glacial acetic acid, be diluted with water to 2500mL, mixing.
Bismuth standard liquid: weigh 0.1000g bismuth metal in 100mL beaker, with 10mL nitric acid (1+1)
After low-temperature decomposition, move in 100mL volumetric flask, be diluted with water to scale, mixing.This solution contains 1mg/mL
Bismuth.
EDTA standard liquid c (EDTA) ≈ 0.01mol/L: weigh 3.72g Na2EDTA is dissolved in 1000mL
In water, mixing.
Demarcate: weigh three parts of 0.1000g metallic leads and be respectively placed in 250mL beaker, add 10mL (1+1)
Nitric acid, low-temperature heat, to being completely dissolved, is taken off the coldest, adds 20mL (1+1) sulfuric acid and continues to be heated to emitting
Cigarette, takes off cooling, carries out by sample analysis step below.Take the mean value of 3 parts of calibration results, three parts
The extreme difference of calibration result should be not more than 0.0010mg/mL.
2, experimental technique
Weigh 0.1~0.3g (being accurate to 0.0001g) sample and, in 250mL beaker, use a small amount of water-wet,
Add 15mL hydrochloric acid, cap upper surface ware, after 120~150 DEG C of heating for dissolving 5min, add 5mL nitre
Acid, continues to be heated to sample and decomposes completely, adds 20mL (1+1) sulfuric acid afterwards, is heated to emitting dense by three
The white cigarette of sulfur oxide, takes off cooling, continues to be heated to smoldering, take after rinsing surface plate and wall of cup with a small amount of water
Lower cooling.Being added thereto to 50mL water again, heating is boiled and is made soluble-salt dissolve, and adds 10 after cooling
ML absolute ethyl alcohol, places 2h, afterwards with Filter paper filtering the most at a slow speed, with 5% sulfuric acid solution washing
Precipitation.Precipitation is put back in former beaker together with filter paper, adds 2 xylenol orange indicator, with ammoniacal liquor by molten
Liquid is adjusted to aubergine, adds 40mL acetic acid-sodium acetate buffer solution (pH ≈ 5.8), boils 10min, cold
But, after, adding 10mL concentration is the 10v/v%BAL aqueous solution and 0.1g ascorbic acid, dilute with water
To 100mL, making the color of solution be become glassy yellow from redness with the titration of EDTA standard liquid is terminal.
3, in lead ore, bismuth enters the orthogonal experiment of lead sulfate Precipitation
Investigate bismuth and enter lead sulfate Precipitation situation, after different lead standards add bismuth standard, record lead amount
The results are shown in Table 1.
The impact on lead test result of table 1 bismuth element
From table 1, when content one timing of lead in sample, enter the bismuth amount of lead sulfate precipitation with bismuth
Content increases and increases;Content one timing of bismuth, the bismuth amount entering lead sulfate precipitation increases with the content of lead
And increase.
4, the experiment with BAL as screening agent
(1) BAL shelters principle and the blank assay of bismuth
Applicant thinks that bismuth is owing to bismuth can be complexed with EDTA to the mensuration interference of lead content in lead ore,
Bi-EDTA complex compound quite stable, its constant is k=27.94, although bismuth and the stability constant of BAL
Unclear, but BAL can discharge the EDTA in Bi-EDTA complex compound, illustrates that its stability constant is certain
Stability constant higher than Bi-EDTA.
40mL acetic acid-sodium acetate caching solution is joined in the 10mL 10v/v%BAL aqueous solution
In (pH ≈ 5.8), adding 2 xylenol orange indicator, solution immediately becomes yellow, i.e. BAL does not disappears
Consumption EDTA standard liquid.
(2) selection of joining day
The interference of result is got off by bismuth mainly due to being mixed in coprecipitation in lead sulfate precipitation, and BAL
Meeting high temperature easily to decompose and make solution blackening, have influence on the color judgement dripping timed end, therefore we select
Select and add before titration.
(3) addition experiment
40mL acetic acid-sodium acetate caching solution is added in the bismuth standard liquid of one group of different content
(pH ≈ 5.8), adds 2 xylenol orange solution, is titrated to claret with 10v/v%BAL solution and becomes bright
Yellow is terminal.The results are shown in Table 2.
The selection consumption of table 2BAL screening agent
MBi/mg | 2 | 4 | 6 | 8 | 10 |
VBAL/mL | 2.5 | 5.0 | 7.5 | 10 | 12.5 |
Table 2 result shows, VBAL/MBi≈ 1.25mL:1mg, in order to make the interference of bismuth in sample to fill
Divide and eliminate, and the addition of BAL the most additionally consumes EDTA, preferably presses VBAL/MBiThe amount of ≈ mL:1mg
Add 10v/v%BAL solution.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail, to be more fully understood that the present invention's
Content, but the present invention is not limited to following example.
Embodiment 1: standard sample analysis
Select national standard sample GBW07172, be separately added in every part of sample before precipitation lead
6mg bismuth standard, is respectively adopted the method for the invention (specific as follows) and by GB/T 8152.1-2006
Described methods analyst sample:
The method of the invention: weigh 0.20g (being accurate to 0.0001g) sample, 0.006g bismuth standard in 250
In mL beaker, using a small amount of water-wet, add 15mL hydrochloric acid, cap upper surface ware, 120~150 DEG C add
After heat of solution 5min, add 5mL nitric acid, continue to be heated to sample and decompose completely, be subsequently adding 6mL
Bismuth standard liquid, adds 20mL (1+1) sulfuric acid afterwards, is heated to emitting the white cigarette of dense sulfur trioxide, takes off
Cooling, continues to be heated to smoldering after rinsing surface plate and wall of cup with a small amount of water, takes off cooling.The most wherein
Adding 50mL water, heating is boiled and is made soluble-salt dissolve, and adds 10mL absolute ethyl alcohol, put after cooling
Put 2h, afterwards with Filter paper filtering the most at a slow speed, with 5% sulfuric acid solution washing precipitation.To precipitate together with filter
Paper is put back in former beaker, adds 2 xylenol orange indicator, with ammoniacal liquor, solution is adjusted to aubergine, adds
40mL acetic acid-sodium acetate buffer solution (pH ≈ 5.8), boils 10min, cooling, obtains lead acetate solution,
Being added thereto to 12mL concentration is 10v/v%BAL solution and 0.1g ascorbic acid, is diluted with water to
100mL, makes the color of solution be become bright orange from redness with EDTA standard liquid (about 0.01mol/L) titration
Look is terminal, the EDTA standard liquid volume that record consumes, lead content according to the following formula, result
As described in Table 3:
ω/10-2=VS×fT/mS/10
Wherein: fT=mB/VB
ω is the content of lead, %, V in sampleB、VSIt is respectively metallic lead and sample consumption EDTA standard is molten
The volume of liquid, mL;fTFor the EDTA standard liquid titer to lead, mg/mL;mB、mSIt is respectively
Alleged metallic lead and the quality of sample, g.
The analysis result contrast of lead in table 3 standard sample
Embodiment 2: standard sample analysis
Select national standard sample GBW07167, be separately added in every part of sample before precipitation lead
10mg bismuth standard, is respectively adopted the method for the invention (specific as follows) and by GB/T 8152.1-2006
Described methods analyst sample:
The method of the invention: weigh 0.10g (being accurate to 0.0001g) sample, 0.010g bismuth standard in 250
In mL beaker, using a small amount of water-wet, add 15mL hydrochloric acid, cap upper surface ware, 120~150 DEG C add
After heat of solution 5min, add 5mL nitric acid, continue to be heated to sample and decompose completely, add 20 afterwards
ML (1+1) sulfuric acid, is heated to emitting the white cigarette of dense sulfur trioxide, takes off cooling, rinses surface plate with a small amount of water
And continue after wall of cup to be heated to smoldering, take off cooling.Being added thereto to 50mL water again, heating is boiled and is made
Soluble-salt dissolves, and adds 10mL absolute ethyl alcohol after cooling, places 2h, afterwards with filter paper the most at a slow speed
Filter, with 5% sulfuric acid solution washing precipitation.Precipitation is put back in former beaker together with filter paper, adds 2 two
Cresols orange indicator, is adjusted to aubergine with ammoniacal liquor by solution, adds 40mL acetic acid-sodium acetate buffer solution
(pH ≈ 5.8), boils 10min, cooling, obtains lead acetate solution, and being added thereto to 5mL concentration is 40
The v/v%BAL aqueous solution and 0.1g ascorbic acid, be diluted with water to 100mL, molten by EDTA standard
It is terminal that liquid (about 0.01mol/L) titration makes the color of solution be become glassy yellow from redness, and record consumes
EDTA standard liquid volume, as described in embodiment 1, formula calculates lead content.
Measurement result is shown in Table 4.
The analysis result contrast of lead in table 4 standard sample
Embodiment 3:
Select institute of Guilin City Jin Zeli mining industry Co., Ltd feeding sample A, analyze method through national standard
It is 4.68% that GB/T15926-2010 measures the content of bismuth in this sample, is respectively adopted the method for the invention
The content of lead in (specific as follows) and methods analyst sample as described in GB/T 8152.1-2006:
The method of the invention: weigh 0.10g (being accurate to 0.0001g) sample, 0.010g bismuth standard in 250
In mL beaker, using a small amount of water-wet, add 15mL hydrochloric acid, cap upper surface ware, 120~150 DEG C add
After heat of solution 5min, add 5mL nitric acid, continue to be heated to sample and decompose completely, add 20 afterwards
ML (1+1) sulfuric acid, is heated to emitting the white cigarette of dense sulfur trioxide, takes off cooling, rinses surface plate with a small amount of water
And continue after wall of cup to be heated to smoldering, take off cooling.Being added thereto to 50mL water again, heating is boiled and is made
Soluble-salt dissolves, and adds 10mL absolute ethyl alcohol after cooling, places 2h, afterwards with filter paper the most at a slow speed
Filter, with 5% sulfuric acid solution washing precipitation.Precipitation is put back in former beaker together with filter paper, adds 2 two
Cresols orange indicator, is adjusted to aubergine with ammoniacal liquor by solution, adds 40mL acetic acid-sodium acetate buffer solution
(pH ≈ 5.8), boils 10min, cooling, obtains lead acetate solution, and being added thereto to 12mL concentration is
The 10v/v%BAL aqueous solution and 0.1g ascorbic acid, be diluted with water to 100mL, uses EDTA standard
It is terminal that solution (about 0.01mol/L) titration makes the color of solution be become glassy yellow from redness, and record consumes
EDTA standard liquid volume, as described in embodiment 1, formula calculates lead content.
Measurement result is shown in Table 5.
Table 5 unit selects and recommends the analysis result contrast of lead in sample
By above 3 examples it can be seen that the method for the invention can effectively eliminate bismuth by adding BAL
EDTA measures interference during lead, and method is easy, quick, reliable results, can meet production and analyze need
Want.
Claims (10)
1. the method eliminating bismuth interference when using lead content in EDTA volumetric determination mineral, the party
Method with mineral as sample, including sample digestion step, catch up with acid step, formed lead sulfate settling step,
Lead sulfate precipitation dissolving step and titration step, it is characterised in that: dissolving through lead sulfate precipitation
Before the lead acetate solution of step gained titrates, add 2,3-dimercaprol dimercaptopropanol.
Method the most according to claim 1, it is characterised in that: described 2,3-dimercaprol dimercaptopropanol
Addition volume VBALWith bismuth ion content M in lead acetate solutionBiRatio be: VBAL: MBi=
0.125~0.3mL:1mg.
Method the most according to claim 1, it is characterised in that: described 2,3-dimercaprol dimercaptopropanol
Addition volume VBALWith bismuth ion content M in lead acetate solutionBiRatio be: VBAL: MBi=
0.2~0.3mL:1mg.
Method the most according to claim 1, it is characterised in that: described mineral are lead content
>=1% and the ore of bi content >=0.1% or alloy.
Method the most according to claim 1, it is characterised in that: described mineral are lead content
>=5% and the ore of bi content >=0.1% or alloy.
6. according to the method according to any one of Claims 1 to 5, it is characterised in that: described
2,3-dimercaprol dimercaptopropanol joins in lead acetate solution with the form of the 2,3-dimercaprol dimercaptopropanol aqueous solution.
Method the most according to claim 6, it is characterised in that: by 2,3-dimercaprol dimercaptopropanol is joined
Make the 2,3-dimercaprol dimercaptopropanol aqueous solution that concentration is 1~40v/v% to be then added in lead acetate solution.
8. according to the method according to any one of Claims 1 to 5, it is characterised in that: adding
Ascorbic acid is added while 2,3-dimercaprol dimercaptopropanol.
Method the most according to claim 8, it is characterised in that: the addition of described ascorbic acid
Amount is in lead acetate solution more than 1 times of iron ion mole.
Method the most according to claim 9, it is characterised in that: the addition of described ascorbic acid
Amount is in lead acetate solution 1.5 times of iron ion mole.
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CN106940357A (en) * | 2017-04-14 | 2017-07-11 | 广东省矿产应用研究所 | Method for detecting bismuth in bismuth slag containing high selenium and tellurium |
CN108593839A (en) * | 2018-04-24 | 2018-09-28 | 长春黄金研究院有限公司 | A kind of method of lead amount in measurement silver alloy |
CN112378899A (en) * | 2020-10-27 | 2021-02-19 | 西北矿冶研究院 | Method for determining gold in crude lead sample by low-temperature separation ICP-AES (inductively coupled plasma-atomic emission Spectrometry) method |
CN113607880A (en) * | 2021-09-15 | 2021-11-05 | 中冶北方(大连)工程技术有限公司 | Method for determining lead content in lead ore by EDTA volumetric method |
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