CN104215740B - A kind of acidity assaying method of cupric ferrum sulfuric acid solution - Google Patents
A kind of acidity assaying method of cupric ferrum sulfuric acid solution Download PDFInfo
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- CN104215740B CN104215740B CN201410494670.3A CN201410494670A CN104215740B CN 104215740 B CN104215740 B CN 104215740B CN 201410494670 A CN201410494670 A CN 201410494670A CN 104215740 B CN104215740 B CN 104215740B
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 64
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 93
- 239000000243 solution Substances 0.000 claims abstract description 77
- 239000012086 standard solution Substances 0.000 claims abstract description 28
- MKNQNPYGAQGARI-UHFFFAOYSA-N 4-(bromomethyl)phenol Chemical compound OC1=CC=C(CBr)C=C1 MKNQNPYGAQGARI-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000003556 assay Methods 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- IRXRGVFLQOSHOH-UHFFFAOYSA-L dipotassium;oxalate Chemical compound [K+].[K+].[O-]C(=O)C([O-])=O IRXRGVFLQOSHOH-UHFFFAOYSA-L 0.000 claims abstract description 11
- 238000002479 acid--base titration Methods 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 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 9
- 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 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 239000001117 sulphuric acid Substances 0.000 claims description 4
- ABEWDFYANWOMJE-UHFFFAOYSA-N oxalic acid;potassium Chemical compound [K].OC(=O)C(O)=O ABEWDFYANWOMJE-UHFFFAOYSA-N 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 2
- 235000011149 sulphuric acid Nutrition 0.000 claims description 2
- 238000004448 titration Methods 0.000 abstract description 11
- 239000002253 acid Substances 0.000 abstract description 4
- 238000001556 precipitation Methods 0.000 abstract description 2
- CEQFOVLGLXCDCX-UHFFFAOYSA-N 2-[[4-(dimethylamino)phenyl]diazenyl]benzoic acid Chemical compound C1=CC(N(C)C)=CC=C1N=NC1=CC=CC=C1C(O)=O CEQFOVLGLXCDCX-UHFFFAOYSA-N 0.000 description 14
- 239000003153 chemical reaction reagent Substances 0.000 description 10
- -1 copper iron ion Chemical class 0.000 description 9
- 229910052742 iron Inorganic materials 0.000 description 9
- 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
- 239000002585 base Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000003513 alkali Substances 0.000 description 2
- IYRDVAUFQZOLSB-UHFFFAOYSA-N copper iron Chemical compound [Fe].[Cu] IYRDVAUFQZOLSB-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- QTWJRLJHJPIABL-UHFFFAOYSA-N 2-methylphenol;3-methylphenol;4-methylphenol Chemical compound CC1=CC=C(O)C=C1.CC1=CC=CC(O)=C1.CC1=CC=CC=C1O QTWJRLJHJPIABL-UHFFFAOYSA-N 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 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
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 229930003836 cresol Natural products 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 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 compound [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The present invention relates to the assay method of a kind of cupric ferrum sulfuric acid solution acidity.The method includes that the sulfuric acid solution pipetting cupric ferrum, in conical flask, adds deionized water, is subsequently adding appropriate potassium oxalate, shakes up and make potassium oxalate fully dissolve, drip 6 ~ 10 bromocresol green-methyl red mixed indicators, titrate with standard solution of sodium hydroxide；In titration process when sulfuric acid solution is become bottle green from kermesinus, it is terminal after amount two standard solution of sodium hydroxide of dropping；According to acid base titration formula, obtain the acidity of this cupric ferrum sulfuric acid solution.The present invention can solve terminal in original acid base detemination method well and change unconspicuous problem, and solution does not have precipitation generation in titration process；Titration end-point is easier to judge, the acidity of mensuration is more accurate.
Description
Technical field
The present invention relates to a kind of acidity assaying method, particularly relate to the mensuration side of a kind of cupric ferrum sulfuric acid solution acidity
Method.
Background technology
Acidity assaying is chemical engineering experiment and operation conventional when producing, current acidity assaying with C.I. 13020. as indicator,
Use and standard alkali solution is added dropwise in acid solution, utilize soda acid methyl red indicator to carry out titration end-point judgement, record
The standard alkali solution volume finally consumed, calculates the acid-base value of solution finally according to relevant formula.
Mensuration for cupric ferrum sulfuric acid solution acidity, it would however also be possible to employ above method.The problem that presently, there are is, when molten
When in liquid, ferrum copper content is less, copper is sheltered by potassium oxalate, and solution colour change first becomes yellow from redness, then becomes bright green,
Often change inconspicuous during by yellow to bright green；When iron content is bigger, make indicator with C.I. 13020., use sodium hydroxide standard
Solution titrates, and terminal colour is become yellow from redness, and produces a large amount of yellow mercury oxide, and this phenomena impair endpoint is finally made
Become the acidity error calculated according to formula bigger.
Summary of the invention
The technical problem to be solved in the present invention: be difficult to sentence for titration end-point during acidity assaying in solution prior art
The problem that break, mensuration acidity is inaccurate etc. exists, it is provided that a kind of titration end-point is prone to judgement, mensuration acidity accurate cupric ferrum
The assay method of sulfuric acid solution acidity.
Technical scheme:
The assay method of a kind of cupric ferrum sulfuric acid solution acidity, comprises the following steps:
Pipette the sulfuric acid solution of cupric ferrum in conical flask, add deionized water, be subsequently adding appropriate potassium oxalate, shake up and make
Potassium oxalate fully dissolves, and drips 6 ~ 10 bromocresol green-C.I. 13020. mixed indicators, carries out dripping with standard solution of sodium hydroxide
Fixed；In titration process when sulfuric acid solution is become bottle green from kermesinus, after amount two standard solution of sodium hydroxide of dropping i.e.
For terminal；According to acid base titration formula, obtain the acidity of this cupric ferrum sulfuric acid solution.
Consisting of of described bromocresol green-C.I. 13020. mixed indicator: the concentration of bromocresol green indicator is 1g/L, methyl
The concentration of red indicator is 2g/L, and solvent for use is the ethanol solution of 95%, and the two volume ratio is 3:1；Described sodium hydroxide standard
The concentration of solution is 0.1mol/L.
Described acid base titration formula is, in formula: W represents acidity g/L；C represents that sodium hydroxide standard is molten
Concentration mol/L of liquid；V represents the volume of standard solution of sodium hydroxide, ml；M represents the molal weight of sulphuric acid, g/mol；V0 represents
The volume of copper ferrum sulfuric acid solution, ml.
The sulfuric acid solution of described cupric ferrum is 1ml；The specification of conical flask used is 250ml, and the addition of deionized water is
75 ~ 100ml, the amount adding potassium oxalate is 0.5g.
The positive beneficial effect (advantage) of the present invention:
The present invention uses acid base titration method to measure the acidity of cupric ferrum sulfuric acid solution, with bromocresol green-C.I. 13020. mixing
Indicator is indicator, with potassium oxalate as screening agent, can solve terminal change in original acid base detemination method well inconspicuous
Problem, and in titration process solution do not have precipitation produce.The method titration end-point is easier to judge, the acidity of mensuration
More accurate.
The present invention is 5.0 due to the pH of bromocresol green-C.I. 13020. End point indication, during terminal, uses excess two hydrogen of dropping
The accuracy of the method for sodium oxide standard solution, beneficially 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, the terminal of mensuration
Color is more wide in range to the requirement of copper concentration of iron in solution, and the suitability of the method is stronger.
Detailed description of the invention
For fully understanding the present invention, the present invention will be further described by the following examples, it is not intended that to this
Any restriction of invention, Wen Zhongru no special instruction, percentage composition therein is weight ratio.
Embodiment one: the assay method of a kind of cupric ferrum sulfuric acid solution acidity, first calculating copper iron ion content in solution is
Acidity during 0g/L.
1, assay method
Pipette the sulfuric acid solution of 1ml cupric ferrum in 250ml conical flask, add 75ml ~ 100ml deionized water, add oxalic acid
Potassium 0.5g, shakes up and is allowed to fully dissolve, and adds 6 ~ 10 bromocresol green-C.I. 13020. mixed indicators, uses standard solution of sodium hydroxide
Titration, in titration process when sulfuric acid solution is become bottle green from kermesinus, after amount dropping two, is terminal.
2, instrument, reagent
Acid-base universal burette: 50ml；Conical flask: 250ml；Single graticule pipet: 1ml；
Sodium hydroxide: top grade is pure；Potassium oxalate: analytical pure；Bromocresol green-C.I. 13020. mixed indicator.
3, prepared by solution
(1) standard solution of sodium hydroxide of 0.1mol/L；
(2) bromocresol green methyl red indicator: use three parts of A reagent and a B reagent mixing；
A reagent: wherein indicator 1g/L Han bromocresol green, remaining is 95%(mass) ethanol solution；
B reagent: the wherein 2g/L Han methyl red indicator, remaining is 95%(mass) ethanol solution.
4, result calculates:,
In formula: W------represents acidity g/L；
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-------sulphuric acid, g/mol；
V0------sample volume, ml.
Respectively with methyl red indicator and bromocresol green-methyl red indicator, solution acidity is measured；With C.I. 13020.
Solution terminal colour for indicator is yellow, and the solution terminal colour with bromocresol green-C.I. 13020. as indicator is as bright green；
The amount of the standard solution of sodium hydroxide consumed and acidity value are as shown in table 1, and the pH value of deionized water is 6.65.Specifically it is shown in Table 1.
As can be seen from Table 1, when measuring, by different indicators, the solution that copper iron content of the same race is 0g/L, the hydroxide of consumption
Sodium standard solution acidity value identical, that measure is identical, and with the terminal pH value of PH meter mensuration too.
Embodiment two: the assay method of a kind of cupric ferrum sulfuric acid solution acidity, when in solution to be measured: 0g/L ＜ copper ion contains
During amount ＜ 5g/L, 0g/L ＜ iron ion content ＜ 5g/L；
1, assay method
Pipette the sulfuric acid solution of 1ml cupric ferrum in 250ml conical flask, add 75ml ~ 100ml deionized water, add oxalic acid
Potassium 0.5g, shakes up and is allowed to fully dissolve, and adds 6 ~ 10 bromocresol green-C.I. 13020. mixed indicators, uses standard solution of sodium hydroxide
Titrate, when sulfuric acid solution is become bottle green from kermesinus, after amount dropping two, be terminal.
2, instrument, reagent
Acid-base universal burette: 50ml；Conical flask: 250ml；Single graticule pipet: 1ml；
Sodium hydroxide: top grade is pure；Potassium oxalate: analytical pure；Bromocresol green-C.I. 13020. mixed indicator.
3, prepared by solution
(1) standard solution of sodium hydroxide of 0.1mol/L；
(2) bromocresol green methyl red indicator: use three parts of A reagent and a B reagent mixing.
A reagent: wherein indicator 1g/L Han bromocresol green, remaining is the ethanol solution of 95%；
B reagent: the wherein 2g/L Han methyl red indicator, remaining is the ethanol solution of 95%.
4, result calculates:
In formula: W------represents acidity g/L；
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-------sulphuric acid, g/mol；
V0------sample volume, ml.
It is indicator with C.I. 13020. and bromocresol green-C.I. 13020. respectively, solution acidity is measured；With C.I. 13020. for referring to
The solution terminal colour showing agent is yellow, and the solution terminal colour with bromocresol green C.I. 13020. as indicator is as bright green；Consume
The amount of standard solution of sodium hydroxide and acidity value as shown in table 2, the pH value of deionized water is 6.65.
As can be seen from Table 2, when in solution, copper iron content is less than 5g/L more than 0g/L, according to consuming sodium hydroxide standard
The volume of solution, acidity value, terminal pH value it can be seen that during with C.I. 13020. for indicator, acidity assaying result is than bromine cresol
When green C.I. 13020. is indicator, measurement result is bigger than normal.Here iron ion includes bivalence and ferric iron.
Embodiment three: the assay method of cupric ferrum sulfuric acid solution acidity, method is identical with embodiment two, but used when measuring
Solution to be measured is different: in solution to be measured when 0g/L ＜ content of copper ion ＜ 5g/L, iron ion content ＞ 5g/L,
Respectively with methyl red indicator and bromocresol green-methyl red indicator, the acidity of solution is measured；With methyl
The red solution for indicator has turbid phenomenon to produce, and solution terminal colour is yellow；With bromocresol green-C.I. 13020. as indicator
Solution terminal colour be bright green；The amount of the standard solution of sodium hydroxide consumed and acidity value are as shown in table 3, deionized water
PH value is 6.65.
As can be seen from Table 3, as 0g/L ＜ content of copper ion ＜ 5g/L, iron ion content ＞ 5g/L in solution, according to
Consume the volume of standard solution of sodium hydroxide, acidity value, terminal pH value it can be seen that during with C.I. 13020. for indicator, acidity is surveyed
Determining result ratio when being indicator with bromocresol green-C.I. 13020., measurement result is bigger than normal.
Embodiment four: the assay method of cupric ferrum sulfuric acid solution acidity, method is identical with embodiment two, used during mensuration
Solution to be measured is different: copper ion content of solution ＞ 5g/L to be measured, 0g/L ＜ iron ion content ＜ 5g/L；
Respectively with methyl red indicator and bromocresol green-methyl red indicator, solution acidity is measured；With C.I. 13020.
Solution terminal colour for indicator is bright green, and the terminal colour with bromocresol green-C.I. 13020. as indicator is as bright green；Disappear
The amount of the standard solution of sodium hydroxide of consumption and acidity value are as shown in table 4, and the pH value of deionized water is 6.65.
As can be seen from Table 4, as copper ion content of solution ＞ 5g/L, 0g/L ＜ iron ion content ＜ 5g/L, according to
Consume the volume of standard solution of sodium hydroxide, acidity value, whole pH value it can be seen that during with C.I. 13020. for indicator, acidity assaying
When result is indicator than bromocresol green-C.I. 13020., measurement result is bigger than normal.
Embodiment five: the assay method of cupric ferrum sulfuric acid solution acidity, method is identical with embodiment two, but used when measuring
Solution to be measured different: in solution to be measured, copper iron ion content is both greater than 5g/L:
It is indicator with C.I. 13020. and bromocresol green-C.I. 13020. respectively, solution acidity is measured；With C.I. 13020. for referring to
Show agent, solution has red muddy generation；With bromocresol green-C.I. 13020. as indicator, terminal colour is bright green, without muddy existing
As；The amount of the standard solution of sodium hydroxide consumed and acidity value are as shown in table 5, and deionized water pH value is 6.65.
As can be seen from Table 5, when measuring, by different indicators, the solution that copper iron ion content is different, acidity is identical, according to
Terminal pH value judges, higher with C.I. 13020. for indicator measurement result, the measurement result with bromocresol green-C.I. 13020. as indicator
Deviation is less.
Claims (2)
1. an assay method for cupric ferrum sulfuric acid solution acidity, is characterized in that: the method comprises the following steps:
Pipette the sulfuric acid solution of cupric ferrum in conical flask, add deionized water, be subsequently adding appropriate potassium oxalate, shake up and make oxalic acid
Potassium fully dissolves, and drips 6～10 bromocresol green-C.I. 13020. mixed indicators, titrates with standard solution of sodium hydroxide；Drip
During Ding when sulfuric acid solution is become bottle green from kermesinus, it is end after amount two standard solution of sodium hydroxide of dropping
Point；According to acid base titration formula, obtain the acidity of this cupric ferrum sulfuric acid solution；The sulfuric acid solution of described cupric ferrum is 1ml；Used
The specification of conical flask is 250ml, and the addition of deionized water is 75～100ml, and the amount adding potassium oxalate is 0.5g；Bromocresol green
The concentration of indicator is 1g/L, and the concentration of methyl red indicator is 2g/L, and solvent for use is the ethanol solution of 95%, the two volume
Ratio is 3:1；The concentration of described standard solution of sodium hydroxide is 0.1mol/L.
2. assay method as claimed in claim 1, is characterized in that: described acid base titration formula isIn formula: W
Represent acidity g/L；C represents concentration mol/L of standard solution of sodium hydroxide；V represents the volume of standard solution of sodium hydroxide, ml；M
Represent the molal weight of sulphuric acid, g/mol；V0 represents the volume of copper ferrum sulfuric acid solution, ml.
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| CN104713876B (en) * | 2015-03-27 | 2017-09-01 | 山东海容电源材料有限公司 | The assay method of free oxalic acid in a kind of single Lithium bis (oxalate) 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 |
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