CN109828082A - A kind of quantitative detecting method of desulfurization alcoholic lye neutral and alkali ingredient - Google Patents
A kind of quantitative detecting method of desulfurization alcoholic lye neutral and alkali ingredient Download PDFInfo
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Abstract
The invention belongs to chemical analysis fields, more particularly to a kind of quantitative detecting method of desulfurization alcoholic lye neutral and alkali ingredient, method includes the following steps: a) mixing desulfurization alcoholic lye with ALIZARIN YELLOW GG-thymol blue indicator, blue is become from green with the color of titration with hydrochloric acid to solution；B) it will mix by the solution of step a) titration with formaldehyde and phenolphthalein indicator, be become colorless with the color of titration with hydrochloric acid to solution by red；C) it will be mixed by the solution of step b) titration with bromocresol green-methyl red mixed indicator, kermesinus is become from green with the color of titration with hydrochloric acid to solution；D) according to step a)~c) each step titrate consumed by hydrochloric acid content, the content of each alkaline components in the desulfurization alcoholic lye is calculated.Method provided by the invention carries out stepwise titration to desulfurization alcoholic lye using a variety of indicator, realizes the quantitative detection to the alkaline components in desulfurization alcoholic lye, most authentic and valid data can be provided for operator.
Description
Technical field
The invention belongs to chemical analysis field more particularly to a kind of quantitative detection sides of desulfurization alcoholic lye neutral and alkali ingredient
Method.
Background technique
Desulfurization alcoholic lye is the alkali wash water that cycle uses during liquefied gas or demercaptaning for gasoline, due to during mercaptan
A variety of chemical reactions can constantly occur for the NaOH contained in alkali wash water, therefore will lead to the ingredient of desulfurization alcoholic lye in use process
Middle change it is complex.
During removal of mercaptans, the changes of contents of each alkaline components can cause significantly the effect of removal of mercaptans in desulfurization alcoholic lye
It influences, therefore the concrete content of each alkaline components in used desulfurization alcoholic lye is periodically surveyed during removal of mercaptans
It surely is very necessary.But traditional acid-base titration is only applicable to the OH in measurement desulfurization alcoholic lye-Concentration can not measure de-
The content of each specific alkaline components in mercaptan lye.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of quantitative detecting method of desulfurization alcoholic lye neutral and alkali ingredient,
Method provided by the invention can carry out quantitative detection to the alkaline components in desulfurization alcoholic lye.
The present invention provides a kind of quantitative detecting methods of desulfurization alcoholic lye neutral and alkali ingredient, comprising the following steps:
A) desulfurization alcoholic lye is mixed with ALIZARIN YELLOW GG-thymol blue indicator, with the color of titration with hydrochloric acid to solution
Blue is become from green, is denoted as the first titration end-point；
The ingredient of the desulfurization alcoholic lye includes NaOH, Na2S, NaHS and Na2CO3One of or it is a variety of；
B) it will be mixed by the solution of step a) titration with formaldehyde and phenolphthalein indicator, with the color of titration with hydrochloric acid to solution
It is become colorless by red, is denoted as the second titration end-point；
C) it will be mixed by the solution of step b) titration with bromocresol green-methyl red mixed indicator, extremely with titration with hydrochloric acid
The color of solution becomes kermesinus from green, is denoted as third titration end-point；
D) according to step a)~c) each step titrate consumed by hydrochloric acid content, each alkali in the desulfurization alcoholic lye is calculated
The content of property ingredient.
Preferably, the alkaline components of the desulfurization alcoholic lye are by NaOH, Na2S and Na2CO3Composition；
The content of NaOH is calculated according to formula (1) in the desulfurization alcoholic lye:
W1=(V1-V2+V3) × cM/ (m × 1000) × 100%............................. (1)；
In formula (1): the mass concentration of W1 expression NaOH；V1It indicates to be titrated to consumed by the first titration end-point in step a)
Hydrochloric acid volume；V2It indicates to be titrated to hydrochloric acid volume consumed by the second titration end-point in step b)；V3It indicates to be titrated in step c)
Hydrochloric acid volume consumed by third titration end-point；C indicates to titrate the molar concentration of hydrochloric acid used；The molal weight of M expression NaOH；
The quality of m expression desulfurization alcoholic lye；
Na in the desulfurization alcoholic lye2The content of S is calculated according to formula (2):
W2=(V2-V3) × cM/ (m × 1000) × 100%....................... (2)；
In formula (2): W2 indicates Na2The mass concentration of S；V2It indicates to be titrated to consumed by the second titration end-point in step b)
Hydrochloric acid volume；V3It indicates to be titrated to hydrochloric acid volume consumed by third titration end-point in step c)；C indicates to titrate hydrochloric acid used
Molar concentration；M indicates Na2The molal weight of S；The quality of m expression desulfurization alcoholic lye；
Na in the desulfurization alcoholic lye2CO3Content according to formula (3) calculate:
W3=V3× cM/ (m × 1000) × 100%........................ (3)；
In formula (3): W3 indicates Na2CO3Mass concentration；V3Indicate that being titrated to third titration end-point in step c) is consumed
Hydrochloric acid volume；C indicates to titrate the molar concentration of hydrochloric acid used；M indicates Na2CO3Molal weight；M indicates desulfurization alcoholic lye
Quality.
Preferably, the alkaline components of the desulfurization alcoholic lye are by NaOH and Na2CO3Composition；
The content of NaOH is calculated according to formula (4) in the desulfurization alcoholic lye:
W4=V1× cM/ (m × 1000) × 100%............................ (4)；
In formula (4): the mass concentration of W4 expression NaOH；V1It indicates to be titrated to consumed by the first titration end-point in step a)
Hydrochloric acid volume；C indicates to titrate the molar concentration of hydrochloric acid used；The molal weight of M expression NaOH；The matter of m expression desulfurization alcoholic lye
Amount；
Na in the desulfurization alcoholic lye2CO3Content according to formula (5) calculate:
W5=V2× cM/ (m × 1000) × 100%................................ (5)；
In formula (5): W5 indicates Na2CO3Mass concentration；V2Indicate that being titrated to the second titration end-point in step b) is consumed
Hydrochloric acid volume；C indicates to titrate the molar concentration of hydrochloric acid used；M indicates Na2CO3Molal weight；M indicates desulfurization alcoholic lye
Quality.
Preferably, the alkaline components of the desulfurization alcoholic lye are by Na2S, NaHS and Na2CO3Composition:
Na in the desulfurization alcoholic lye2The content of S is calculated according to formula (6):
W6=V1× cM/ (m × 1000) × 100%................. (6)；
In formula (6): W6 indicates Na2The mass concentration of S；V1It indicates to be titrated to consumed by the first titration end-point in step a)
Hydrochloric acid volume；C indicates to titrate the molar concentration of hydrochloric acid used；M indicates Na2The molal weight of S；The matter of m expression desulfurization alcoholic lye
Amount；
Na in the desulfurization alcoholic lye2CO3Content according to formula (7) calculate:
W7=V3× cM/ (m × 1000) × 100%........................ (7)；
In formula (7): W7 indicates Na2CO3Mass concentration；V3Indicate that being titrated to third titration end-point in step c) is consumed
Hydrochloric acid volume；C indicates to titrate the molar concentration of hydrochloric acid used；The molal weight of M expression NaOH；M indicates desulfurization alcoholic lye
Quality；
The content of NaHS is calculated according to formula (8) in the desulfurization alcoholic lye:
W8=(V2-V1-V3) × cM/ (m × 1000) × 100%............................... (8)；
In formula (8): the mass concentration of W8 expression NaHS；V1It indicates to be titrated to consumed by the first titration end-point in step a)
Hydrochloric acid volume；V2It indicates to be titrated to hydrochloric acid volume consumed by the second titration end-point in step b)；V3It indicates to be titrated in step c)
Hydrochloric acid volume consumed by third titration end-point；C indicates to titrate the molar concentration of hydrochloric acid used；The molal weight of M expression NaHS；
The quality of m expression desulfurization alcoholic lye.
Preferably, in step a), the pH value of first titration end-point is 9.5~10.5.
Preferably, in step a), the pH value of first titration end-point is 10.
Preferably, in step b), the pH value of second titration end-point is 7.5~8.5.
Preferably, in step b), the pH value of second titration end-point is 8.1.
Preferably, in step c), the pH value of the third titration end-point is 4.5~5.5.
Preferably, in step c), the pH value of the third titration end-point is 4.9.
Compared with prior art, the present invention provides a kind of quantitative detecting methods of desulfurization alcoholic lye neutral and alkali ingredient.This
Detection method includes the following steps for invention offer: a) desulfurization alcoholic lye is mixed with ALIZARIN YELLOW GG-thymol blue indicator,
Blue is become from green with the color of titration with hydrochloric acid to solution, is denoted as the first titration end-point；The desulfurization alcoholic lye at subpackage
Include NaOH, Na2S, NaHS and Na2CO3One of or it is a variety of；B) will refer to by the solution of step a) titration with formaldehyde and phenolphthalein
Show that agent mixes, is become colorless with the color of titration with hydrochloric acid to solution by red, be denoted as the second titration end-point；C) step b) will be passed through
The solution of titration is mixed with bromocresol green-methyl red mixed indicator, becomes dark from green with the color of titration with hydrochloric acid to solution
Red is denoted as third titration end-point；D) according to step a)~c) each step titrate consumed by hydrochloric acid content, be calculated described de-
The content of each alkaline components in mercaptan lye.Method provided by the invention carries out substep to desulfurization alcoholic lye using a variety of indicator
Titration, and the content that each alkaline components in desulfurization alcoholic lye have been calculated in consumed hydrochloric acid content is titrated according to each step, it is real
The quantitative detection to the alkaline components in desulfurization alcoholic lye is showed, most authentic and valid data can be provided for operator.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
The present invention provides a kind of quantitative detecting methods of desulfurization alcoholic lye neutral and alkali ingredient, comprising the following steps:
A) desulfurization alcoholic lye is mixed with ALIZARIN YELLOW GG-thymol blue indicator, with the color of titration with hydrochloric acid to solution
Blue is become from green, is denoted as the first titration end-point；
The ingredient of the desulfurization alcoholic lye includes NaOH, Na2S, NaHS and Na2CO3One of or it is a variety of；
B) it will be mixed by the solution of step a) titration with formaldehyde and phenolphthalein indicator, with the color of titration with hydrochloric acid to solution
It is become colorless by red, is denoted as the second titration end-point；
C) it will be mixed by the solution of step b) titration with bromocresol green-methyl red mixed indicator, extremely with titration with hydrochloric acid
The color of solution becomes kermesinus from green, is denoted as third titration end-point；
D) according to step a)~c) each step titrate consumed by hydrochloric acid content, each alkali in the desulfurization alcoholic lye is calculated
The content of property ingredient.
In method provided by the invention, desulfurization alcoholic lye is mixed with ALIZARIN YELLOW GG-thymol blue indicator first.
Wherein, the ingredient of the desulfurization alcoholic lye includes NaOH, Na2S, NaHS and Na2CO3One of or it is a variety of；The alizarin yellow
GG- thymol blue indicator can be prepared in accordance with the following methods:
I) ALIZARIN YELLOW GG and ethanol solution are mixed, obtains solution A；
Ii) thymol blue and ethanol solution are mixed, obtain solution B；
Iii) solution A and solution B are mixed, obtain ALIZARIN YELLOW GG-thymol blue indicator.
In the preparation method of above-mentioned ALIZARIN YELLOW GG-thymol blue indicator provided by the invention, step i) and step
Ii) there is no sequencing.In step i), the concentration of the ethanol solution is preferably 40~60wt%, more preferably 50wt%；Institute
The amount ratio for stating ALIZARIN YELLOW GG and ethanol solution is preferably 0.1g:(50~200) mL, more preferably 0.1g:100mL.Step ii)
In, the concentration of the ethanol solution is preferably 40~60wt%, more preferably 50wt%；The thymol blue and ethanol solution
Amount ratio be preferably 0.1g:(50~200) mL, more preferably 0.1g:100mL.Step iii) in, the solution A and solution B
Volume ratio be preferably (10~50): 20, more preferably 30:20.
In method provided by the invention, after desulfurization alcoholic lye is mixed with ALIZARIN YELLOW GG-thymol blue indicator, obtain
The solution of green becomes blue with the color of titration with hydrochloric acid to solution later, is denoted as the first titration end-point.Wherein, described first
The pH value of titration end-point is preferably 9.5~10.5, and more preferably 10.
In method provided by the invention, after solution is titrated to the first titration end-point, by after titration solution and formaldehyde and
Phenolphthalein indicator mixing.Wherein, the concentration of the formaldehyde is preferably 30~45wt%, more preferably 36~38wt%；The phenol
The concentration of phthalein indicator is preferably 5~15g/L, more preferably 10g/L；The amount ratio of the formaldehyde and phenolphthalein indicator is preferably
10mL:(1~5) drop, more preferably 10mL:2 drop.After solution after titration is mixed with formaldehyde and phenolphthalein indicator, red is obtained
Solution, become colorless later with the color of titration with hydrochloric acid to solution, be denoted as the second titration end-point.Wherein, second titration
The pH value of terminal is preferably 7.5~8.5, and more preferably 8.1.
In method provided by the invention, after solution is titrated to the second titration end-point, by the solution and bromine cresols after titration
Green-methyl red mixed indicator mixing.Wherein, the bromocresol green-methyl red mixed indicator can match in accordance with the following methods
System:
I) bromocresol green and ethyl alcohol are mixed, obtain solution A；
II) methyl red and ethyl alcohol are mixed, obtain solution B；
III) solution A and solution B are mixed, obtain bromocresol green-methyl red mixed indicator.
In the preparation method of above-mentioned bromocresol green-methyl red mixed indicator provided by the invention, step I) and step
II) there is no sequencing.Step I) in, the amount ratio of the bromocresol green and ethyl alcohol is preferably 0.01g:(50~200) mL, more
Preferably 0.01g:100mL.Step II) in, the amount ratio of the methyl red and ethyl alcohol is preferably 0.02g:(50~200) mL,
More preferably 0.02g:100mL.Step III) in, the volume ratio of the solution A and solution B is preferably (10~50): 20, it is more excellent
It is selected as 30:20.
In method provided by the invention, after the solution after titration is mixed with bromocresol green-methyl red mixed indicator, obtain
To the solution of green, becomes kermesinus with the color of titration with hydrochloric acid to solution later, be denoted as third titration end-point.Wherein, described
The pH value of third titration end-point is preferably 4.5~5.5, and more preferably 4.9.
In method provided by the invention, after completing above-mentioned three steps titration, consumed hydrochloric acid content is titrated according to each step,
The content of each alkaline components in the desulfurization alcoholic lye is calculated.
In one embodiment provided by the invention, three steps titration concentration of hydrochloric acid used is identical, the desulfurization alcoholic lye
In the contents of each alkaline components under type such as can be used be calculated:
A) when the alkaline components of the desulfurization alcoholic lye are by NaOH, Na2S and Na2CO3When composition；
The content of NaOH is calculated according to formula (1) in the desulfurization alcoholic lye:
W1=(V1-V2+V3) × cM/ (m × 1000) × 100%............................. (1)；
In formula (1): W1 indicates the mass concentration of NaOH, unit %；V1It indicates to be titrated to the first titration end in step a)
Hydrochloric acid volume, unit mL consumed by point；V2It indicates to be titrated to hydrochloric acid volume consumed by the second titration end-point in step b),
Unit is mL；V3It indicates to be titrated to hydrochloric acid volume consumed by third titration end-point, unit mL in step c)；C indicates titration
The molar concentration of hydrochloric acid used, unit mol/L；M indicates the molal weight of NaOH, unit g/mol；M indicates removal of mercaptans alkali
The quality of liquid, unit g；
Na in the desulfurization alcoholic lye2The content of S is calculated according to formula (2):
W2=(V2-V3) × cM/ (m × 1000) × 100%....................... (2)；
In formula (2): W2 indicates Na2The mass concentration of S, unit %；V2It indicates to be titrated to the second titration end-point in step b)
Consumed hydrochloric acid volume, unit mL；V3It indicates to be titrated to hydrochloric acid volume consumed by third titration end-point in step c), it is single
Position is mL；C indicates to titrate the molar concentration of hydrochloric acid used, unit mol/L；M indicates Na2The molal weight of S, unit g/
mol；M indicates the quality of desulfurization alcoholic lye, unit g；
Na in the desulfurization alcoholic lye2CO3Content according to formula (3) calculate:
W3=V3× cM/ (m × 1000) × 100%........................ (3)；
In formula (3): W3 indicates Na2CO3Mass concentration, unit %；V3It indicates to be titrated to third titration in step c) eventually
Hydrochloric acid volume, unit mL consumed by point；C indicates to titrate the molar concentration of hydrochloric acid used, unit mol/L；M is indicated
Na2CO3Molal weight, unit g/mol；M indicates the quality of desulfurization alcoholic lye, unit g.
B) when the alkaline components of the desulfurization alcoholic lye are by NaOH and Na2CO3When composition；
The content of NaOH is calculated according to formula (4) in the desulfurization alcoholic lye:
W4=V1× cM/ (m × 1000) × 100%............................ (4)；
In formula (4): W4 indicates the mass concentration of NaOH, unit %；V1It indicates to be titrated to the first titration end in step a)
Hydrochloric acid volume, unit mL consumed by point；C indicates to titrate the molar concentration of hydrochloric acid used, unit mol/L；M indicates NaOH
Molal weight, unit g/mol；M indicates the quality of desulfurization alcoholic lye, unit g；
Na in the desulfurization alcoholic lye2CO3Content according to formula (5) calculate:
W5=V2× cM/ (m × 1000) × 100%................................ (5)；
In formula (5): W5 indicates Na2CO3Mass concentration, unit %；V2It indicates to be titrated to the second titration end in step b)
Hydrochloric acid volume, unit mL consumed by point；C indicates to titrate the molar concentration of hydrochloric acid used, unit mol/L；M is indicated
Na2CO3Molal weight, unit g/mol；M indicates the quality of desulfurization alcoholic lye, unit g.
C) when the alkaline components of the desulfurization alcoholic lye are by Na2S, NaHS and Na2CO3When composition:
Na in the desulfurization alcoholic lye2The content of S is calculated according to formula (6):
W6=V1× cM/ (m × 1000) × 100%................. (6)；
In formula (6): W6 indicates Na2The mass concentration of S, unit %；V1It indicates to be titrated to the first titration end-point in step a)
Consumed hydrochloric acid volume, unit mL；C indicates to titrate the molar concentration of hydrochloric acid used, unit mol/L；M indicates Na2S's
Molal weight, unit g/mol；M indicates the quality of desulfurization alcoholic lye, unit g；
Na in the desulfurization alcoholic lye2CO3Content according to formula (7) calculate:
W7=V3× cM/ (m × 1000) × 100%........................ (7)；
In formula (7): W7 indicates Na2CO3Mass concentration；V3Indicate that being titrated to third titration end-point in step c) is consumed
Hydrochloric acid volume；C indicates to titrate the molar concentration of hydrochloric acid used；The molal weight of M expression NaOH；M indicates desulfurization alcoholic lye
Quality；
The content of NaHS is calculated according to formula (8) in the desulfurization alcoholic lye:
W8=(V2-V1-V3) × cM/ (m × 1000) × 100%............................... (8)；
In formula (8): W8 indicates the mass concentration of NaHS, unit %；V1It indicates to be titrated to the first titration end in step a)
Hydrochloric acid volume, unit mL consumed by point；V2It indicates to be titrated to hydrochloric acid volume consumed by the second titration end-point in step b),
Unit is mL；V3It indicates to be titrated to hydrochloric acid volume consumed by third titration end-point, unit mL in step c)；C indicates titration
The molar concentration of hydrochloric acid used, unit mol/L；M indicates the molal weight of NaHS, unit g/mol；M indicates removal of mercaptans alkali
The quality of liquid, unit g.
Method provided by the invention carries out stepwise titration to desulfurization alcoholic lye using a variety of indicator, and is dripped according to each step
The content of each alkaline components in desulfurization alcoholic lye has been calculated in hydrochloric acid content consumed by fixed, realizes in desulfurization alcoholic lye
The quantitative detection of alkaline components can provide most authentic and valid data for operator.
For the sake of becoming apparent from, it is described in detail below by following embodiment.
In following embodiments of the invention, used reagent situation is as follows:
Formaldehyde: 36~38wt% is filtered with preceding with Medium speed filter paper, and with phenolphthalein indicator, sodium hydroxide solution is added dropwise in micro-
It is red.
Hydrochloric Standard Titration: 0.5mol/L.
ALIZARIN YELLOW GG-thymol blue mixed indicator: 0.1g ALIZARIN YELLOW GG a) is dissolved in the ethyl alcohol of 100mL50wt%
In, obtain solution A；B) 0.1g thymol blue is dissolved in the ethyl alcohol of 100mL 50wt%, obtains solution B；C) take 30mL's
Solution A and the mixing of the solution B of 20mL.
Phenolphthalein indicator: 10g/L.
Bromocresol green-methyl red mixed indicator: a) 0.01g bromocresol green is dissolved in 100mL ethyl alcohol, obtains solution A；
B) 0.02g methyl red is dissolved in 100mL ethyl alcohol, obtains solution B, (c) take the solution A of 30mL and the solution B mixing of 20mL.
Sodium hydroxide: analysis is pure.
Embodiment 1
Simulation desulfurization alcoholic lye is prepared, the content of NaOH is 4.00wt%, Na in the simulation desulfurization alcoholic lye2S's contains
Amount is 1.97wt%, Na2CO3Content be 2.62wt%.Quantitative inspection is carried out using the simulation desulfurization alcoholic lye as solution to be measured
It surveys, detailed process includes:
2mL solution to be measured is pipetted, quality is accurately weighed.It is placed in 100mL beaker, adds 75mL distilled water, add 6 drop alizarin yellows
GG- thymol blue indicator, is titrated with Hydrochloric Standard Titration, and solution becomes blue from green, and the as first titration is eventually
Point, pH value of solution=10.0, write down the volume V of standard titration solution consumed by titrating at this time1(V1=5mL).This step titration process
In, it Quick shaking to move conical flask, is slowly dropped into Hydrochloric Standard Titration, rate of titration is about 60 drops/min.
10mL formaldehyde and 2 drop phenolphthalein indicators are added, continues to be titrated with Hydrochloric Standard Titration, solution colour is by red
Color becomes colorless, as the second titration end-point, at this time pH value of solution=8.1, writes down the body of standard titration solution consumed by titrating
Product V2(V2=2mL).
3 drop bromocresol greens-methyl red mixed indicator is added, continues to be titrated with Hydrochloric Standard Titration, solution face
Color becomes kermesinus, as third titration end-point from green, and pH value of solution=4.9 are terminal at this time, writes down mark consumed by titration
The volume V of quasi- titration solution3(V3=1mL).
The content of NaOH in desulfurization alcoholic lye is calculated according to formula (1):
W1=(V1-V2+V3) × cM/ (m × 1000) × 100%
=(5-2+1) × 0.5 × 40/ (2 × 1000) × 100%
=4%.
Na in desulfurization alcoholic lye is calculated according to formula (2)2The content of S:
W2=(V2-V3) × cM/ (m × 1000) × 100%
=(2-1) × 0.5 × 78/ (2 × 1000) × 100%
=1.95%.
Na in desulfurization alcoholic lye is calculated according to (3)2CO3Content:
W3=V3× cM/ (m × 1000) × 100%
=1 × 0.5 × 106/ (2 × 1000) × 100%
=2.65%.
Embodiment 2
Simulation desulfurization alcoholic lye is prepared, the content of NaOH is 6.00wt%, Na in the simulation desulfurization alcoholic lye2CO3Contain
Amount is 4.00wt%.Quantitative detection is carried out using the simulation desulfurization alcoholic lye as solution to be measured, detailed process includes:
2mL solution to be measured is pipetted, quality is accurately weighed.It is placed in 100mL beaker, adds 75mL distilled water, add 6 drop alizarin yellows
GG- thymol blue indicator, is titrated with Hydrochloric Standard Titration, and solution becomes blue from green, and the as first titration is eventually
Point, pH value of solution=10.0, write down the volume V of standard titration solution consumed by titrating at this time1(V1=6mL).This step titration process
In, it Quick shaking to move conical flask, is slowly dropped into Hydrochloric Standard Titration, rate of titration is about 60 drops/min.
10mL formaldehyde and 2 drop phenolphthalein indicators are added, continues to be titrated with Hydrochloric Standard Titration, solution colour is by red
Color becomes colorless, as the second titration end-point, at this time pH value of solution=8.1, writes down the body of standard titration solution consumed by titrating
Product V2(V2=1.5mL).
3 drop bromocresol greens-methyl red mixed indicator is added, continues to be titrated with Hydrochloric Standard Titration, solution face
Color becomes kermesinus, as third titration end-point from green, and pH value of solution=4.9 are terminal at this time, writes down mark consumed by titration
The volume V of quasi- titration solution3(V3=2mL).
The content of NaOH in desulfurization alcoholic lye is calculated according to formula (4):
W4=V1× cM/ (m × 1000) × 100%
=6 × 0.5 × 40/ (2 × 1000) × 100%
=6%.
Na in desulfurization alcoholic lye is calculated according to formula (5)2CO3Content:
W5=V2× cM/ (m × 1000) × 100%
=1.5 × 0.5 × 106/ (2 × 1000) × 100%
=3.975%.
Embodiment 3
Prepare simulation desulfurization alcoholic lye, Na in the simulation desulfurization alcoholic lye2The content of S is 3.92wt%, Na2CO3Contain
Amount is 5.35wt%, and the content of NaHS is 0.70wt%.Quantitative inspection is carried out using the simulation desulfurization alcoholic lye as solution to be measured
It surveys, detailed process includes:
2mL solution to be measured is pipetted, quality is accurately weighed.It is placed in 100mL beaker, adds 75mL distilled water, add 6 drop alizarin yellows
GG- thymol blue indicator, is titrated with Hydrochloric Standard Titration, and solution becomes blue from green, and the as first titration is eventually
Point, pH value of solution=10.0, write down the volume V of standard titration solution consumed by titrating at this time1(V1=2mL).This step titration process
In, it Quick shaking to move conical flask, is slowly dropped into Hydrochloric Standard Titration, rate of titration is about 60 drops/min.
10mL formaldehyde and 2 drop phenolphthalein indicators are added, continues to be titrated with Hydrochloric Standard Titration, solution colour is by red
Color becomes colorless, as the second titration end-point, at this time pH value of solution=8.1, writes down the body of standard titration solution consumed by titrating
Product V2(V2=4.5mL).
3 drop bromocresol greens-methyl red mixed indicator is added, continues to be titrated with Hydrochloric Standard Titration, solution face
Color becomes kermesinus, as third titration end-point from green, and pH value of solution=4.9 are terminal at this time, writes down mark consumed by titration
The volume V of quasi- titration solution3(V3=2mL).
Na in desulfurization alcoholic lye is calculated according to formula (6)2The content of S:
W6=V1× cM/ (m × 1000) × 100%
=2 × 0.5 × 78/ (2 × 1000) × 100%
=3.9%.
Na in desulfurization alcoholic lye is calculated according to formula (7)2CO3Content:
W7=V3× cM/ (m × 1000) × 100%
=2 × 0.5 × 106/ (2 × 1000) × 100%
=5.3%.
The content of NaHS in desulfurization alcoholic lye is calculated according to formula (8):
W8=(V2-V1-V3) × cM/ (m × 1000) × 100%
=(4.5-2-2) × 0.5 × 56/ (2 × 1000) × 100%
=0.7%.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of quantitative detecting method of desulfurization alcoholic lye neutral and alkali ingredient, comprising the following steps:
A) desulfurization alcoholic lye is mixed with ALIZARIN YELLOW GG-thymol blue indicator, with the color of titration with hydrochloric acid to solution by green
Discoloration is blue, is denoted as the first titration end-point；
The ingredient of the desulfurization alcoholic lye includes NaOH, Na2S, NaHS and Na2CO3One of or it is a variety of；
B) it will be mixed by the solution of step a) titration with formaldehyde and phenolphthalein indicator, with the color of titration with hydrochloric acid to solution by red
Color becomes colorless, and is denoted as the second titration end-point；
C) it will be mixed by the solution of step b) titration with bromocresol green-methyl red mixed indicator, with titration with hydrochloric acid to solution
Color kermesinus is become from green, be denoted as third titration end-point；
D) according to step a)~c) each step titrate consumed by hydrochloric acid content, be calculated in the desulfurization alcoholic lye each alkalinity at
The content divided.
2. quantitative detecting method according to claim 1, which is characterized in that the alkaline components of the desulfurization alcoholic lye by
NaOH、Na2S and Na2CO3Composition；
The content of NaOH is calculated according to formula (1) in the desulfurization alcoholic lye:
W1=(V1-V2+V3) × cM/ (m × 1000) × 100%............................. (1)；
In formula (1): the mass concentration of W1 expression NaOH；V1It indicates to be titrated to hydrochloric acid consumed by the first titration end-point in step a)
Volume；V2It indicates to be titrated to hydrochloric acid volume consumed by the second titration end-point in step b)；V3It indicates to be titrated to third in step c)
Hydrochloric acid volume consumed by titration end-point；C indicates to titrate the molar concentration of hydrochloric acid used；The molal weight of M expression NaOH；M table
Show the quality of desulfurization alcoholic lye；
Na in the desulfurization alcoholic lye2The content of S is calculated according to formula (2):
W2=(V2-V3) × cM/ (m × 1000) × 100%....................... (2)；
In formula (2): W2 indicates Na2The mass concentration of S；V2It indicates to be titrated to hydrochloric acid consumed by the second titration end-point in step b)
Volume；V3It indicates to be titrated to hydrochloric acid volume consumed by third titration end-point in step c)；C indicates to titrate mole of hydrochloric acid used
Concentration；M indicates Na2The molal weight of S；The quality of m expression desulfurization alcoholic lye；
Na in the desulfurization alcoholic lye2CO3Content according to formula (3) calculate:
W3=V3× cM/ (m × 1000) × 100%........................ (3)；
In formula (3): W3 indicates Na2CO3Mass concentration；V3It indicates to be titrated to salt consumed by third titration end-point in step c)
Sour volume；C indicates to titrate the molar concentration of hydrochloric acid used；M indicates Na2CO3Molal weight；The matter of m expression desulfurization alcoholic lye
Amount.
3. quantitative detecting method according to claim 1, which is characterized in that the alkaline components of the desulfurization alcoholic lye by
NaOH and Na2CO3Composition；
The content of NaOH is calculated according to formula (4) in the desulfurization alcoholic lye:
W4=V1× cM/ (m × 1000) × 100%............................ (4)；
In formula (4): the mass concentration of W4 expression NaOH；V1It indicates to be titrated to hydrochloric acid consumed by the first titration end-point in step a)
Volume；C indicates to titrate the molar concentration of hydrochloric acid used；The molal weight of M expression NaOH；The quality of m expression desulfurization alcoholic lye；
Na in the desulfurization alcoholic lye2CO3Content according to formula (5) calculate:
W5=V2× cM/ (m × 1000) × 100%................................ (5)；
In formula (5): W5 indicates Na2CO3Mass concentration；V2It indicates to be titrated to salt consumed by the second titration end-point in step b)
Sour volume；C indicates to titrate the molar concentration of hydrochloric acid used；M indicates Na2CO3Molal weight；The matter of m expression desulfurization alcoholic lye
Amount.
4. quantitative detecting method according to claim 1, which is characterized in that the alkaline components of the desulfurization alcoholic lye by
Na2S, NaHS and Na2CO3Composition:
Na in the desulfurization alcoholic lye2The content of S is calculated according to formula (6):
W6=V1× cM/ (m × 1000) × 100%................. (6)；
In formula (6): W6 indicates Na2The mass concentration of S；V1It indicates to be titrated to hydrochloric acid consumed by the first titration end-point in step a)
Volume；C indicates to titrate the molar concentration of hydrochloric acid used；M indicates Na2The molal weight of S；The quality of m expression desulfurization alcoholic lye；
Na in the desulfurization alcoholic lye2CO3Content according to formula (7) calculate:
W7=V3× cM/ (m × 1000) × 100%........................ (7)；
In formula (7): W7 indicates Na2CO3Mass concentration；V3It indicates to be titrated to salt consumed by third titration end-point in step c)
Sour volume；C indicates to titrate the molar concentration of hydrochloric acid used；The molal weight of M expression NaOH；The quality of m expression desulfurization alcoholic lye；
The content of NaHS is calculated according to formula (8) in the desulfurization alcoholic lye:
W8=(V2-V1-V3) × cM/ (m × 1000) × 100%................................ (8)；
In formula (8): the mass concentration of W8 expression NaHS；V1It indicates to be titrated to hydrochloric acid consumed by the first titration end-point in step a)
Volume；V2It indicates to be titrated to hydrochloric acid volume consumed by the second titration end-point in step b)；V3It indicates to be titrated to third in step c)
Hydrochloric acid volume consumed by titration end-point；C indicates to titrate the molar concentration of hydrochloric acid used；The molal weight of M expression NaHS；M table
Show the quality of desulfurization alcoholic lye.
5. quantitative detecting method according to claim 1, which is characterized in that in step a), first titration end-point
PH value is 9.5~10.5.
6. quantitative detecting method according to claim 5, which is characterized in that in step a), first titration end-point
PH value is 10.
7. quantitative detecting method according to claim 1, which is characterized in that in step b), second titration end-point
PH value is 7.5~8.5.
8. quantitative detecting method according to claim 7, which is characterized in that in step b), second titration end-point
PH value is 8.1.
9. quantitative detecting method according to claim 1, which is characterized in that in step c), the third titration end-point
PH value is 4.5~5.5.
10. quantitative detecting method according to claim 9, which is characterized in that in step c), the third titration end-point
PH value is 4.9.
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