CN102141537B - Analysis method of sulfate radicals in sulfate and thiosulfate mixture - Google Patents

Analysis method of sulfate radicals in sulfate and thiosulfate mixture Download PDF

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CN102141537B
CN102141537B CN 201010575740 CN201010575740A CN102141537B CN 102141537 B CN102141537 B CN 102141537B CN 201010575740 CN201010575740 CN 201010575740 CN 201010575740 A CN201010575740 A CN 201010575740A CN 102141537 B CN102141537 B CN 102141537B
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sulfate
dithizone
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赵汝鸣
王波
罗文新
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China Haohua Dalian Research and Design Institute of Chemical Industry Coltd
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Abstract

The invention belongs to the field of chemical analysis and relates to an analysis method of sulfate radicals in a sulfate and thiosulfate mixture. The method provided by the invention comprises the following steps: a) preparing and calibrating a lead nitrate standard solution, preparing an ethanol aqueous solution of lead nitrate, shifting the sulfate radical standard solution with known volume and concentration, using the aqueous solution added with ethanol as a medium, adjusting the pH value to be 4-5, inserting a lead ion-selective electrode and a silver-silver chloride electrode, carrying out automatic potentiometric titration by utilizing the lead nitrate standard solution and computing the concentration of the lead nitrate standard solution; and b) measuring the content of the thiosulfate by directly utilizing iodine standard solution titration to analyze the sulfate radicals, using the aqueous solution added with the ethanol into the solution to be measured as the medium, adjusting the pH value to be 4-5, inserting the lead ion-selective electrode and the silver-silver chloride electrode, carrying out the automatic potentiometric titration by utilizing the lead nitrate standard solution and measuring the total content of the sulfate and the thiosulfate, thereby computing the content of the sulfate radicals.

Description

The analytical approach of sulfate radical in sulfate and the thiosulfate mixture
Technical field
The invention belongs to chemical analysis field, relate to the analytical approach of sulfate radical in sulfate and the thiosulfate mixture.
Background technology
The analytical approach that sulfate is commonly used has the chromatography of ions, gravimetry, photometry, kemet agent EDTA titrimetry and the benzidine hydrochloride precipitation method etc.If be mixed with thiosulfate in the sulfate, thiosulfate will disturb the mensuration of sulfate.The chromatography of ions can be measured sulfate radical and the thiosulfate anion in the potpourri simultaneously, though that method is disturbed is little, specificity is strong, because instrument and equipment is expensive, operating conditions is higher, common laboratory is difficult to popularization and application; Gravimetry, photometry, kemet agent EDTA titrimetry and the benzidine hydrochloride precipitation method etc. all need the thiosulfate decomposition is removed, thereby measuring process are increased because interference phenomenon is serious, and prolong analysis time.The present invention does not need the thiosulfate decomposition is removed when measuring, and has reduced measuring process, has shortened analysis time, has improved efficient.
Summary of the invention
The invention provides the analytical approach of sulfate radical in a kind of sulfate and the thiosulfate mixture.
The principle of the invention is to adopt iodimetric titration namely directly with iodine standard solution titration determination thiosulfuric acid salt content, and sulfate and thiosulfate total content are measured in potentiometric titration, thereby measure sulfate radical content.Because lead sulfate and lead thiosulfate solubleness in aqueous medium are larger, potentiometric titration should carry out reducing the solubleness of lead salt under the condition that adds non-aqueous solvent, make titration end-point that larger potential break be arranged, the present invention adopts be in solution to be measured, add ethanol aqueous solution as medium, titrant is the ethanol water of plumbi nitras.
The analytical approach of sulfate radical in sulfate and the thiosulfate mixture, the method comprises the steps:
A) Dithizone preparation and demarcation:
Take by weighing the 2.3g plumbi nitras, with a small amount of water-soluble solution, add 1mL1: 1 plumbi nitras, use 40-60% ethanolic solution A constant volume to 1L.
With pipette, pipette the sulfate radical standard liquid that 5mL concentration is 0.01041mol/L, be placed in the 100mL beaker, add again 60-70% ethanolic solution B 40mL, put into one piece of stirrer, be placed on magnetic stirrer, with the salpeter solution of 1mol/L, regulating pH value is 4～5, insert Lead Ion-selective Electrode and silver-silver chloride electrode, under at the uniform velocity stirring, with Dithizone, carry out automatic potentiometric titration, the Dithizone volume Vc that equivalent point consumes, according to formula 1, calculate Dithizone concentration
C ( PbN O 3 , mol / L ) = 0.05205 Vc - - - ( 1 )
In the top formula:
Vc: the Dithizone volume numerical value (unit is mL) of consumption
B) analysis of sulfate radical
Take by weighing sulfate and thiosulfate mixture M (accurately to 0.0002) g, the dissolving constant volume is diluted with water to scale in the 500mL volumetric flask, shake up, and obtains the solution first.
Pipette 20mL solution first with transfer pipet, place the 250mL conical flask, add 10mL acetic acid-sodium acetate buffer solution (PH ≈ 6), the 1.0g potassium iodide is used the iodine standard solution titration, during nearly terminal point, add 1mL～2mL starch indicator solution, continue to be titrated to solution and be blue, colour-fast in the 30s, be terminal point, the iodine standard solution volume V that consumes 1
Pipette 20mL solution first with transfer pipet, place the 100mL volumetric flask, be diluted with water to scale, shake up, obtain solution second.Pipette 5mL solution second with transfer pipet, place the 100mL beaker, add again 60-70% ethanolic solution B 40mL, put into one piece of stirrer, place on the magnetic stirrer, regulating pH value with the salpeter solution of 1mol/L is 4～5, inserts Lead Ion-selective Electrode and silver-silver chloride electrode, under at the uniform velocity stirring, carry out automatic potentiometric titration with Dithizone, the Dithizone volume V that equivalent point consumes 2,
Calculate the sulfate radical mass percentage concentration according to formula 2,
W ( S O 4 2 - ) = ( V 2 × N 2 × 20 - V 1 × N 1 ) × B M × 40 × 100 - - - ( 2 )
In the top formula:
W: sulfate radical mass percentage concentration numerical value represents with %;
V 1: the iodine standard solution volume numerical value (unit is mL) of consumption;
N 1: the concentration of the amount of substance of iodine standard solution
Figure GSB00000972977400022
Numerical value (unit is mol/L);
V 2: the Dithizone volume numerical value (unit is mL) of consumption;
N 2: the concentration C (PbNO of the amount of substance of Dithizone 3) numerical value (unit is mol/L);
M: the quality numerical value of sample sulfate and thiosulfate mixture (unit is g);
B: the molal weight of sulfate radical (96.06g/mol)
Ethanolic solution (%) is percent by volume.
Preferred ethanolic solution A concentration is 50% in the said method, and ethanolic solution B concentration is 70%,
Preferred said method comprises the steps:
A) Dithizone preparation and demarcation:
Take by weighing the 2.3g plumbi nitras, with a small amount of water-soluble solution, add 1mL1: 1 plumbi nitras, with 50% ethanolic solution constant volume to 1L.
With pipette, pipette the sulfate radical standard liquid that 5mL concentration is 0.01041mol/L, be placed in the 100mL beaker, add again 70% ethanolic solution 40mL, put into one piece of stirrer, be placed on magnetic stirrer, with the salpeter solution of 1mol/L, regulating pH value is 4～5, insert Lead Ion-selective Electrode and silver-silver chloride electrode, under at the uniform velocity stirring, with Dithizone, carry out automatic potentiometric titration, the Dithizone volume Vc that equivalent point consumes, according to formula 1, calculate Dithizone concentration
C ( PbN O 3 , mol / L ) = 0.05205 Vc - - - ( 1 )
In the top formula:
Vc: the Dithizone volume numerical value (unit is mL) of consumption
B) analysis of sulfate radical
Take by weighing sulfate and thiosulfate mixture M (accurately to 0.0002) g, the dissolving constant volume is diluted with water to scale in the 500mL volumetric flask, shake up, and obtains the solution first.
Pipette 20mL solution first with transfer pipet, place the 250mL conical flask, add 10mL acetic acid-sodium acetate buffer solution (PH ≈ 6), the 1.0g potassium iodide is used the iodine standard solution titration, during nearly terminal point, add 1mL～2mL starch indicator solution, continue to be titrated to solution and be blue, colour-fast in the 30s, be terminal point, the iodine standard solution volume V that consumes 1
Pipette 20mL solution first with transfer pipet, place the 100mL volumetric flask, be diluted with water to scale, shake up, obtain solution second.Pipette 5mL solution second with transfer pipet, place the 100mL beaker, add again 70% ethanolic solution 40mL, put into one piece of stirrer, place on the magnetic stirrer, regulating pH value with the salpeter solution of 1mol/L is 4～5, inserts Lead Ion-selective Electrode and silver-silver chloride electrode, under at the uniform velocity stirring, carry out automatic potentiometric titration with Dithizone, the Dithizone volume V that equivalent point consumes 2,
Raw materials usedly in the method for the present invention all can buy from market.
The excellence of the analytical approach of sulfate radical point is that the result is accurate in sulfate of the present invention and the thiosulfate mixture, and analysis simple to operate is quick, can accurate instruction production.
In the gas sweetening process, sulfate and thiosulfate association are normally arranged in the absorption liquid, the sulfate radical of measuring wherein fast and accurately has great importance to production, the present invention does not need the thiosulfate decomposition is removed when measuring, reduced measuring process, shorten analysis time, improved efficient.Therefore the present invention plays an important role to measuring the desulfurization liquid absorption element.
Description of drawings
The preparation of Fig. 1 Dithizone and the titration curve of demarcating
The titration curve of the analysis of sulfate radical among Fig. 2 embodiment 1
The titration curve of the analysis of sulfate radical among Fig. 3 embodiment 2
Embodiment
In order to understand the present invention, the below further specifies the present invention with embodiment, but does not limit the present invention.
The Preparation Example of the compounds of this invention
Embodiment 1:
A) Dithizone preparation and demarcation
Take by weighing the 2.4072g plumbi nitras, with a small amount of water-soluble solution, add 1mL1: 1 plumbi nitras, with 50% ethanolic solution constant volume to 1L.
Transfer pipet pipettes the sulfate radical standard solution that 5mL concentration is 0.01041mol/L, place the 100mL beaker, add again 70% ethanolic solution 40ml, put into one piece of stirrer, place on the magnetic stirrer, regulating pH value with the salpeter solution of 1mol/L is 4～5, insert 305 type Lead Ion-selective Electrodes and 851 type silver-silver chloride electrodes, under at the uniform velocity stirring, carry out automatic potentiometric titration with Dithizone, the Dithizone volume 7.174mL that equivalent point consumes, titration curve is seen Fig. 1.
Calculate Dithizone concentration, C (PbNO according to above-mentioned formula 1 3)=0.007255mol/L.
B) analysis of sulfate radical
Take by weighing sulfate and thiosulfate mixture 4.8151g, the dissolving constant volume is diluted with water to scale in the 500mL volumetric flask, shake up, and obtains the solution first.
Pipette 20mL solution first with transfer pipet, place the 250mL conical flask, add 10mL acetic acid-sodium acetate buffer solution (PH ≈ 6), the 1.0g potassium iodide is used iodine standard solution
Figure GSB00000972977400041
Titration during nearly terminal point, adds 1mL～2mL starch indicator solution, continues to be titrated to solution and is blue, and is colour-fast in the 30s, is terminal point, the iodine standard solution volume 10.35ml that consumes.
Pipette 20mL solution first with transfer pipet, place the 100mL volumetric flask, be diluted with water to scale, shake up, obtain solution second.Pipette 5mL solution second with transfer pipet, place the 100mL beaker, add again 70% ethanolic solution 40mL, put into one piece of stirrer, place on the magnetic stirrer, regulating pH value with the salpeter solution of 1mol/L is 4～5, insert 305 type Lead Ion-selective Electrodes and 851 type silver-silver chloride electrodes, under at the uniform velocity stirring, carry out automatic potentiometric titration with Dithizone, the Dithizone volume 7.961mL that equivalent point consumes, titration curve is seen Fig. 2.
Calculate sulfate radical mass percentage concentration W (SO according to above-mentioned formula 2 4 2-)=15.41%
Embodiment 2:
A) Dithizone preparation and demarcation
With embodiment 1.
B) analysis of sulfate radical
Take by weighing sulfate and thiosulfate mixture 3.8681g, the dissolving constant volume is diluted with water to scale in the 500mL volumetric flask, shake up, and obtains the solution first.
Pipette 20mL solution first with transfer pipet, place the 250mL conical flask, add 10mL acetic acid-sodium acetate buffer solution (PH ≈ 6), the 1.0g potassium iodide is used iodine standard solution
Figure GSB00000972977400042
Titration during nearly terminal point, adds 1mL～2mL starch indicator solution, continues to be titrated to solution and is blue, and is colour-fast in the 30s, is terminal point, the iodine standard solution volume 3.10ml that consumes.
Pipette 20mL solution first with transfer pipet, place the 100mL volumetric flask, be diluted with water to scale, shake up, obtain solution second.Pipette 5mL solution second with transfer pipet, place the 100mL beaker, add again 70% ethanolic solution 40mL, put into one piece of stirrer, place on the magnetic stirrer, regulating pH value with the salpeter solution of 1mol/L is 4～5, insert 305 type Lead Ion-selective Electrodes and 851 type silver-silver chloride electrodes, under at the uniform velocity stirring, carry out automatic potentiometric titration with Dithizone, the Dithizone volume 7.786mL that equivalent point consumes, titration curve is seen Fig. 3.
Calculate sulfate radical mass percentage concentration W (SO according to above-mentioned formula 2 4 2-)=54.40%.
The inventive method is described by specific embodiment.Those skilled in the art can use for reference the links such as content appropriate change raw material of the present invention, process conditions and realize corresponding other purpose, its relevant change does not all break away from content of the present invention, all similar replacements and change will become apparent to those skilled in the art that and all be deemed to be included within the scope of the present invention.

Claims (1)

1. the analytical approach of sulfate radical in a sulfate and the thiosulfate mixture, the method comprises the steps:
A) Dithizone preparation and demarcation:
Take by weighing the 2.3g plumbi nitras, with a small amount of water-soluble solution, add 1mL1: 1 salpeter solution, with 40-60% ethanolic solution A constant volume to 1L, pipette the sulfate radical standard solution that 5mL concentration is 0.01041mol/L with transfer pipet, place the 100mL beaker, add again 60-70% ethanolic solution B 40mL, put into one piece of stirrer, place on the magnetic stirrer, regulate pH value to 4～5 with the salpeter solution of 1mol/L, insert Lead Ion-selective Electrode and silver-silver chloride electrode, carry out automatic potentiometric titration with Dithizone under at the uniform velocity stirring, the Dithizone volume Vc that equivalent point consumes calculates Dithizone concentration according to formula 1;
C ( PbN O 3 , mol / L ) = 0.05205 Vc - - - ( 1 )
In the top formula:
Vc: the Dithizone volume numerical value that equivalent point consumes, unit is mL;
B) analysis of sulfate radical
Take by weighing sulfate and thiosulfate mixture 0.0002g, the dissolving constant volume is diluted with water to scale in the 500mL volumetric flask, shake up, and obtains the solution first;
Pipette 20mL solution first with transfer pipet, place the 250mL conical flask, add 10mL PH ≈ 6 acetic acid-sodium acetate buffer solution, the 1.0g potassium iodide is used the iodine standard solution titration, during nearly terminal point, add 1mL～2mL starch indicator solution, continue to be titrated to solution and be blue, colour-fast in the 30s, be terminal point, the iodine standard solution volume V that consumes 1
Pipette 20mL solution first with transfer pipet, place the 100mL volumetric flask, be diluted with water to scale, shake up, obtain solution second, pipette 5mL solution second with transfer pipet, place the 100mL beaker, add again 60-70% ethanolic solution B 40mL, put into one piece of stirrer, place on the magnetic stirrer, salpeter solution with 1mol/L is regulated pH value to 4～5, insert Lead Ion-selective Electrode and silver-silver chloride electrode, under at the uniform velocity stirring, carry out automatic potentiometric titration with Dithizone, the Dithizone volume V that equivalent point consumes 2
Calculate the sulfate radical mass percentage concentration according to formula 2,
W ( S O 4 2 - ) = ( V 2 × N 2 × 20 - V 1 × N 1 ) × B M × 40 × 100 - - - ( 2 )
In the top formula:
W: the sulfate radical mass percentage concentration, numerical value represents with %;
V 1: the iodine standard solution volume numerical value of consumption, unit is mL;
N 1: the concentration of the amount of substance of iodine standard solution Numerical value, unit are mol/L;
V 2: the Dithizone volume numerical value that equivalent point consumes, unit is mL;
N 2: the concentration C (PbNO of the amount of substance of Dithizone 3) numerical value, unit is mol/L;
M: the quality numerical value of sample sulfate and thiosulfate mixture, unit are g;
B: the molal weight of sulfate radical, 96.06g/mol;
Ethanolic solution is percent by volume.
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CN105954341A (en) * 2016-04-26 2016-09-21 中国冶金地质总局山东局测试中心 Method for continuous analysis determination of calcium oxide and magnesium oxide in limestone
CN107167552A (en) * 2016-08-31 2017-09-15 北京彤程创展科技有限公司 A kind of method for determining sulfur content in rubber and rubber product
CN109324094B (en) * 2018-11-05 2020-12-01 西安热工研究院有限公司 Method for detecting sulfate radical content by conductivity titration
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