CN104215740A - Acidity testing method for sulfuric acid solution containing copper and iron - Google Patents
Acidity testing method for sulfuric acid solution containing copper and iron Download PDFInfo
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- CN104215740A CN104215740A CN201410494670.3A CN201410494670A CN104215740A CN 104215740 A CN104215740 A CN 104215740A CN 201410494670 A CN201410494670 A CN 201410494670A CN 104215740 A CN104215740 A CN 104215740A
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- sulfuric acid
- acidity
- iron
- sodium hydroxide
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 34
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 18
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title abstract description 7
- 229910052802 copper Inorganic materials 0.000 title abstract description 7
- 239000010949 copper Substances 0.000 title abstract description 7
- 238000012360 testing method Methods 0.000 title abstract 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 99
- 239000000243 solution Substances 0.000 claims abstract description 75
- 239000012086 standard solution Substances 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000004448 titration Methods 0.000 claims abstract description 17
- IRXRGVFLQOSHOH-UHFFFAOYSA-L dipotassium;oxalate Chemical compound [K+].[K+].[O-]C(=O)C([O-])=O IRXRGVFLQOSHOH-UHFFFAOYSA-L 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000002479 acid--base titration Methods 0.000 claims abstract description 6
- CEQFOVLGLXCDCX-WUKNDPDISA-N methyl red Chemical compound C1=CC(N(C)C)=CC=C1\N=N\C1=CC=CC=C1C(O)=O CEQFOVLGLXCDCX-WUKNDPDISA-N 0.000 claims description 25
- 238000003556 assay Methods 0.000 claims description 14
- MVZXTUSAYBWAAM-UHFFFAOYSA-N iron;sulfuric acid Chemical compound [Fe].OS(O)(=O)=O MVZXTUSAYBWAAM-UHFFFAOYSA-N 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- FRPHFZCDPYBUAU-UHFFFAOYSA-N Bromocresolgreen Chemical compound CC1=C(Br)C(O)=C(Br)C=C1C1(C=2C(=C(Br)C(O)=C(Br)C=2)C)C2=CC=CC=C2S(=O)(=O)O1 FRPHFZCDPYBUAU-UHFFFAOYSA-N 0.000 claims description 8
- PXIICSNDLZZJDL-UHFFFAOYSA-N S(O)(O)(=O)=O.[Fe].[Cu] Chemical compound S(O)(O)(=O)=O.[Fe].[Cu] PXIICSNDLZZJDL-UHFFFAOYSA-N 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- MKNQNPYGAQGARI-UHFFFAOYSA-N 4-(bromomethyl)phenol Chemical compound OC1=CC=C(CBr)C=C1 MKNQNPYGAQGARI-UHFFFAOYSA-N 0.000 abstract description 4
- 238000001556 precipitation Methods 0.000 abstract description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 10
- -1 copper iron ion Chemical class 0.000 description 8
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 5
- 229910001431 copper ion Inorganic materials 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 239000002253 acid Substances 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- IYRDVAUFQZOLSB-UHFFFAOYSA-N copper iron Chemical compound [Fe].[Cu] IYRDVAUFQZOLSB-UHFFFAOYSA-N 0.000 description 3
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910001447 ferric ion Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229910000474 mercury oxide Inorganic materials 0.000 description 1
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical class [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to an acidity testing method for a sulfuric acid solution containing copper and iron. The method includes transferring the sulfuric acid solution containing the copper and the iron into a conical bottle, adding deionzied water into the bottle, then adding appropriate potassium oxalate, shaking the bottle up to enable the potassium oxalate to be dissolved completely, dropping 6-10 drops of bromocresol green-methyl red mixed indicator into the bottle, conducting titration through a sodium hydroxide standard solution, dropping two drops of sodium hydroxide standard solution in an excessive mode to reach the terminal point when the sulfuric solution changes from dark red to dark green in the titration process and acquiring the acidity of the sulfuric acid solution containing the copper and the iron according to an acid-base titration formula. The method can well solve the problem that the terminal point is not obvious in change in the original acid-base testing method, no solution precipitation is produced in the titration process, the titration terminal point is easy to judge, and the measured acidity is accurate.
Description
Technical field
The present invention relates to a kind of acidity assaying method, particularly relate to a kind of assay method of cupric iron sulfuric acid solution acidity.
Background technology
Acidity assaying is chemical engineering experiment and conventional operation while producing, current acidity assaying is taking methyl red as indicator, adopt standard alkali solution is dropwise added in acid solution, utilize soda acid methyl red indicator to carry out titration end-point judgement, record the standard alkali solution volume of last consumption, finally calculate the potential of hydrogen of solution according to Related Formula.
For the mensuration of cupric iron sulfuric acid solution acidity, also can adopt above method.The problem existing is at present, in the time that in solution, iron copper content is less, copper is sheltered by potassium oxalate, and solution colour changes and first becomes yellow from redness, then becomes bright green, often changed during to bright green not obvious by yellow; In the time that iron content is larger, make indicator with methyl red, use standard solution of sodium hydroxide titration, terminal colour becomes yellow from redness, and produces a large amount of yellow mercury oxides, and this phenomenon affects endpoint, finally causes the acidity error of calculating according to formula larger.
Summary of the invention
The technical problem to be solved in the present invention: be difficult for judgement for solving in prior art titration end-point in acidity assaying process, measure the acidity problem existing such as inaccurate, provide a kind of titration end-point to be easy to judgement, measure the acidity assay method of cupric iron sulfuric acid solution acidity comparatively accurately.
Technical scheme of the present invention:
An assay method for cupric iron sulfuric acid solution acidity, comprises the following steps:
Pipette the sulfuric acid solution of cupric iron in conical flask, add deionized water, then add appropriate potassium oxalate, shake up potassium oxalate is fully dissolved, drip 6 ~ 10 bromcresol green-methyl red mixed indicators, carry out titration with standard solution of sodium hydroxide; In titration process, when sulfuric acid solution is when kermesinus becomes bottle green, add two standard solution of sodium hydroxide after minim and be terminal; According to acid base titration formula, obtain the acidity of this cupric iron sulfuric acid solution.
Consisting of of described bromcresol green-methyl red mixed indicator: the concentration of bromcresol green indicator is 1g/L, the concentration of methyl red indicator is 2g/L, the ethanolic solution that solvent for use is 95%, the two volume ratio is 3:1; The concentration of described standard solution of sodium hydroxide is 0.1mol/L.
Described acid base titration formula is
, in formula: W represents acidity g/L; C represents the concentration mol/L of standard solution of sodium hydroxide; V represents the volume of standard solution of sodium hydroxide, ml; M represents the molal weight of sulfuric acid, g/mol; V0 represents the volume of copper iron sulfuric acid solution, ml.
The sulfuric acid solution of described cupric iron is 1ml; The specification of conical flask used is 250ml, and the addition of deionized water is 75 ~ 100ml, and the amount that adds potassium oxalate is 0.5g.
positive beneficial effect of the present invention (advantage):
The present invention adopts acid base titration method to measure the acidity of cupric iron sulfuric acid solution
,taking bromcresol green-methyl red mixed indicator as indicator, taking potassium oxalate as screening agent, can solve well terminal in original acid base detemination method and change unconspicuous problem, and solution does not have precipitation generation in titration process.The method titration end-point is easier to judgement, and the acidity of mensuration is more accurate.
In the present invention, because the pH of bromcresol green-methyl red End point indication is 5.0, when terminal, adopt the method for two standard solution of sodium hydroxide of excessive dropping, be conducive to the accuracy of acidity assaying.
In the solution that the present invention measures, whether the height of copper concentration of iron, and terminal colour is always bright green, and the terminal colour of mensuration is more wide in range to the requirement of copper concentration of iron in solution, and the applicability of the method is stronger.
Embodiment
For fully understanding the present invention, the present invention will be further described by the following examples, but do not represent any limitation of the invention, and Wen Zhongru is special instruction no, and percentage composition is wherein weight ratio.
embodiment mono-:an assay method for cupric iron sulfuric acid solution acidity, first calculates in solution acidity when copper iron ion content is 0g/L.
1, assay method
Pipette the sulfuric acid solution of 1ml cupric iron in 250ml conical flask, add 75ml ~ 100ml deionized water, add potassium oxalate 0.5g, shake up and make it abundant dissolving, add 6 ~ 10 bromcresol green-methyl red mixed indicators, use standard solution of sodium hydroxide titration, in titration process when sulfuric acid solution is when kermesinus becomes bottle green, add two after minim, be terminal.
2, instrument, reagent
Acid-base universal burette: 50ml; Conical flask: 250ml; Single graticule transfer pipet: 1ml;
NaOH: top grade is pure; Potassium oxalate: analyze pure; Bromcresol green-methyl red mixed indicator.
3, solution preparation
(1) standard solution of sodium hydroxide of 0.1mol/L;
(2) bromcresol green methyl red indicator: adopt three parts of A reagent and a B reagent to mix;
A reagent: wherein containing bromcresol green indicator 1g/L, all the other are 95%(quality) ethanolic solution;
B reagent: wherein containing methyl red indicator 2g/L, all the other are 95%(quality) ethanolic solution.
4, result is calculated:
,
In formula: W------represents acidity g/L;
The concentration mol/L of C-------standard solution of sodium hydroxide;
The volume of the standard solution of sodium hydroxide that V-------consumes, ml;
The molal weight of M-------sulfuric acid, g/mol;
V0------sample volume, ml.
Use respectively methyl red indicator and bromocresol green-methyl red indicator, solution acidity is measured; Solution terminal colour taking methyl red as indicator is as yellow, and the solution terminal colour taking bromcresol green-methyl red as indicator is bright green; Amount and the acidity value of the standard solution of sodium hydroxide consuming are as shown in table 1, and the pH value of deionized water is 6.65.Specifically in table 1.
As can be seen from Table 1, the acidity value that while measuring with different indicator the solution that copper iron content of the same race is 0g/L, the standard solution of sodium hydroxide of consumption is identical, measure is identical, and with the fixed terminal pH value of PH instrumentation too.
embodiment bis-:an assay method for cupric iron sulfuric acid solution acidity, when in solution to be measured: 0g/L < content of copper ion < 5g/L, when 0g/L < iron ion content < 5g/L;
1, assay method
Pipette the sulfuric acid solution of 1ml cupric iron in 250ml conical flask, add 75ml ~ 100ml deionized water, add potassium oxalate 0.5g, shake up and make it abundant dissolving, add 6 ~ 10 bromcresol green-methyl red mixed indicators, carry out titration with standard solution of sodium hydroxide, when sulfuric acid solution is when kermesinus becomes bottle green, add two after minim, be terminal.
2, instrument, reagent
Acid-base universal burette: 50ml; Conical flask: 250ml; Single graticule transfer pipet: 1ml;
NaOH: top grade is pure; Potassium oxalate: analyze pure; Bromcresol green-methyl red mixed indicator.
3, solution preparation
(1) standard solution of sodium hydroxide of 0.1mol/L;
(2) bromcresol green methyl red indicator: adopt three parts of A reagent and a B reagent to mix.
A reagent: wherein containing bromcresol green indicator 1g/L, all the other ethanolic solutions that are 95%;
B reagent: wherein containing methyl red indicator 2g/L, all the other ethanolic solutions that are 95%.
4, result is calculated:
In formula: W------represents acidity g/L;
The concentration mol/L of C-------standard solution of sodium hydroxide;
The volume of the standard solution of sodium hydroxide that V-------consumes, ml;
The molal weight of M-------sulfuric acid, g/mol;
V0------sample volume, ml.
Be indicator with methyl red and bromcresol green-methyl red respectively, solution acidity is measured; Solution terminal colour taking methyl red as indicator is as yellow, and the solution terminal colour taking bromcresol green methyl red as indicator is bright green; Amount and the acidity value of the standard solution of sodium hydroxide consuming are as shown in table 2, and the pH value of deionized water is 6.65.
As can be seen from Table 2, in the time that copper iron content in solution is greater than 0g/L and is less than 5g/L, can find out according to the pH value of the volume of consumption standard solution of sodium hydroxide, acidity value, terminal: during taking methyl red as indicator, when acidity assaying result is indicator than bromcresol green methyl red, measurement result is bigger than normal.The ferric ion here comprises divalence and ferric iron.
embodiment tri-:the assay method of cupric iron sulfuric acid solution acidity, method is identical with embodiment bis-, but solution difference to be measured used while mensuration: in solution to be measured when 0g/L < content of copper ion < 5g/L, iron ion content > 5g/L
Use respectively methyl red indicator and bromocresol green-methyl red indicator, the acidity of solution is measured; Solution taking methyl red as indicator has turbid phenomenon to produce, and solution terminal colour is yellow; Solution terminal colour taking bromcresol green-methyl red as indicator is bright green; Amount and the acidity value of the standard solution of sodium hydroxide consuming are as shown in table 3, and the pH value of deionized water is 6.65.
As can be seen from Table 3, when in solution when 0g/L < content of copper ion < 5g/L, iron ion content > 5g/L, can find out according to the volume, acidity value, the terminal pH value that consume standard solution of sodium hydroxide: during taking methyl red as indicator, when acidity assaying result is indicator than with bromcresol green-methyl red, measurement result is bigger than normal.
embodiment tetra-:the assay method of cupric iron sulfuric acid solution acidity, method is identical with embodiment bis-, solution difference to be measured used when mensuration: copper ion content of solution > 5g/L to be measured, 0g/L < iron ion content < 5g/L;
Use respectively methyl red indicator and bromocresol green-methyl red indicator, solution acidity is measured; Solution terminal colour taking methyl red as indicator is bright green, and the terminal colour taking bromcresol green-methyl red as indicator is bright green; Amount and the acidity value of the standard solution of sodium hydroxide consuming are as shown in table 4, and the pH value of deionized water is 6.65.
As can be seen from Table 4, in the time of copper ion content of solution > 5g/L, 0g/L < iron ion content < 5g/L, can find out according to the volume, acidity value, the whole pH value that consume standard solution of sodium hydroxide: during taking methyl red as indicator, when acidity assaying result is indicator than bromcresol green-methyl red, measurement result is bigger than normal.
embodiment five:the assay method of cupric iron sulfuric acid solution acidity, method is identical with embodiment bis-, but solution difference to be measured used while measuring: in solution to be measured, copper iron ion content is all greater than 5g/L:
Be indicator with methyl red and bromcresol green-methyl red respectively, solution acidity is measured; Taking methyl red as indicator, in solution, there is red muddy generation; Taking bromcresol green-methyl red as indicator, terminal colour is bright green, without turbid phenomenon; Amount and the acidity value of the standard solution of sodium hydroxide consuming are as shown in table 5, and deionized water pH value is 6.65.
As can be seen from Table 5, while measuring the identical solution of copper iron ion content differences, acidity with different indicator, according to the judgement of terminal pH value, higher as indicator measurement result taking methyl red, the measurement result deviation taking bromcresol green-methyl red as indicator is less.
Claims (4)
1. an assay method for cupric iron sulfuric acid solution acidity, is characterized in that: the method comprises the following steps:
Pipette the sulfuric acid solution of cupric iron in conical flask, add deionized water, then add appropriate potassium oxalate, shake up potassium oxalate is fully dissolved, drip 6 ~ 10 bromcresol green-methyl red mixed indicators, carry out titration with standard solution of sodium hydroxide; In titration process, when sulfuric acid solution is when kermesinus becomes bottle green, add two standard solution of sodium hydroxide after minim and be terminal; According to acid base titration formula, obtain the acidity of this cupric iron sulfuric acid solution.
2. assay method as claimed in claim 1, it is characterized in that: the consisting of of described bromcresol green-methyl red mixed indicator: the concentration of bromcresol green indicator is 1g/L, the concentration of methyl red indicator is 2g/L, the ethanolic solution that solvent for use is 95%, and the two volume ratio is 3:1; The concentration of described standard solution of sodium hydroxide is 0.1mol/L.
3. assay method as claimed in claim 1, is characterized in that: described acid base titration formula is
, in formula: W represents acidity g/L; C represents the concentration mol/L of standard solution of sodium hydroxide; V represents the volume of standard solution of sodium hydroxide, ml; M represents the molal weight of sulfuric acid, g/mol; V0 represents the volume of copper iron sulfuric acid solution, ml.
4. the assay method as described in claim 1-3 any one, is characterized in that: the sulfuric acid solution of described cupric iron is 1ml; The specification of conical flask used is 250ml, and the addition of deionized water is 75 ~ 100ml, and the amount that adds potassium oxalate is 0.5g.
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| CN104713876A (en) * | 2015-03-27 | 2015-06-17 | 山东海容电源材料有限公司 | Method for determining free oxalic acid in mono-oxalate lithium borate |
| CN107478489A (en) * | 2017-07-17 | 2017-12-15 | 呼伦贝尔驰宏矿业有限公司 | A kind of Rapid Volumetric Determination method of sulfate radical in high iron content, cupric oxygen leaching liquid |
| CN111551668A (en) * | 2020-05-08 | 2020-08-18 | 山东东岳高分子材料有限公司 | Method for measuring acid value content in perfluoropolyether |
| CN112526061A (en) * | 2020-11-26 | 2021-03-19 | 昆山金城试剂有限公司 | Purity detection method for electronic-grade reagent |
| CN113176256A (en) * | 2021-05-07 | 2021-07-27 | 金川集团镍盐有限公司 | Method for rapidly judging concentration of hydrogen ions in unknown nickel-containing solution |
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Cited By (5)
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| CN104713876A (en) * | 2015-03-27 | 2015-06-17 | 山东海容电源材料有限公司 | Method for determining free oxalic acid in mono-oxalate lithium borate |
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| CN111551668A (en) * | 2020-05-08 | 2020-08-18 | 山东东岳高分子材料有限公司 | Method for measuring acid value content in perfluoropolyether |
| CN112526061A (en) * | 2020-11-26 | 2021-03-19 | 昆山金城试剂有限公司 | Purity detection method for electronic-grade reagent |
| CN113176256A (en) * | 2021-05-07 | 2021-07-27 | 金川集团镍盐有限公司 | Method for rapidly judging concentration of hydrogen ions in unknown nickel-containing solution |
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