CN110095564A - A method of with titratable amine total in potentiometric determination 2-Propen-1-amine polymer with(chloromethyl)oxirane carbonate - Google Patents
A method of with titratable amine total in potentiometric determination 2-Propen-1-amine polymer with(chloromethyl)oxirane carbonate Download PDFInfo
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- CN110095564A CN110095564A CN201910438497.8A CN201910438497A CN110095564A CN 110095564 A CN110095564 A CN 110095564A CN 201910438497 A CN201910438497 A CN 201910438497A CN 110095564 A CN110095564 A CN 110095564A
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- titration
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
- G01N31/162—Determining the equivalent point by means of a discontinuity
- G01N31/164—Determining the equivalent point by means of a discontinuity by electrical or electrochemical means
Abstract
The invention discloses a kind of methods with titratable amine total in potentiometric determination 2-Propen-1-amine polymer with(chloromethyl)oxirane carbonate, it is related to chemical analysis technology field, determination step is as follows: taking this product about 1.0g, it is accurately weighed to be placed in titration cup, 1.0mol/L hydrochloric acid solution 13-17ml is added, adds water 30-40ml, stirring 30-50 minutes, according to potentiometric titration, using glass electrode, above-mentioned solution is determined with 1.0mol/L sodium hydroxide titration drop；Method constant-current titration jumping of the invention is obvious, and precision, accuracy meet the requirements, and compared with traditional acid base titration, has many advantages, such as high efficiency, easy to operate, easy grasp.
Description
Technical field
The present invention relates to chemical analysis technology fields, and in particular to a kind of in potentiometric determination 2-Propen-1-amine polymer with(chloromethyl)oxirane carbonate
The method of total titratable amine.
Background technique
2-Propen-1-amine polymer with(chloromethyl)oxirane carbonate is a kind of high molecular polymer that will not be rapidly absorbed by a human, it carries multiple amino, due to this product
Amino in molecule is weak base, and the titration jump of equivalent point will not be sharp, traditional to be judged reaction eventually according to acid-base indicator
The method error of point is larger.And potentiometric titrimeter is that the jumping of electrode potential is leaned on to indicate titration end-point, can effectively monitor drop
Determine terminal.The present invention is carefully designed titration parameters, can be worked as with effective monitoring etc. using highly sensitive autopotentiometric titrator
Point realizes total titratable amine measurement of this product.Experiment shows that constant-current titration jumping is obvious, and precision, accuracy meet the requirements, can
Effectively to measure the content of total titratable amine in 2-Propen-1-amine polymer with(chloromethyl)oxirane carbonate.
Summary of the invention
Since conventional acid base titration is unable to judge accurately the titration end-point of the total titratable amine of 2-Propen-1-amine polymer with(chloromethyl)oxirane carbonate, for this
One problem, the present invention provides a kind of method with titratable amine total in potentiometric determination 2-Propen-1-amine polymer with(chloromethyl)oxirane carbonate, the present invention
Purpose be to be realized by following technical proposals:
A method of with titratable amine content total in potentiometric determination 2-Propen-1-amine polymer with(chloromethyl)oxirane carbonate, which is characterized in that packet
Include following steps:
(1) 2-Propen-1-amine polymer with(chloromethyl)oxirane carbonate sample about 1.0g is taken, it is accurately weighed to be placed in titration cup；
(2) 1.0mol/L hydrochloric acid solution 15ml is measured with pipette precision, adds water 35ml, stirred 40 minutes；
(3) potentiometric titration is shone, titration parameters are set, model selection balances control model, and dE 0.2mV, dt are 1 second；
Threshold value is set as 4~6mV/mL；Equivalent point selects two, the control of the potential value of one of equivalent point 150mV~250mV it
Between, the potential value of another equivalent point controls between -250mV~-280mV；Using glass electrode, with 1.0mol/L hydrogen-oxygen
Change sodium titrating solution and titrates above-mentioned solution；
A kind of method with titratable amine content total in potentiometric determination 2-Propen-1-amine polymer with(chloromethyl)oxirane carbonate, feature exist
In the step (2) is middle to measure 1.0mol/L hydrochloric acid solution 17ml with pipette precision, adds water 35ml, stirs 40 minutes；
A kind of method with titratable amine content total in potentiometric determination 2-Propen-1-amine polymer with(chloromethyl)oxirane carbonate, feature exist
In model selection balances control model in the step (3), and dE 0.2mV, dt are 1 second, i.e. potential change control is in 0.2mV/
Under the premise of s, potentiometric titrimeter can be dripped into next drop；
A kind of method with titratable amine content total in potentiometric determination 2-Propen-1-amine polymer with(chloromethyl)oxirane carbonate, feature exist
In threshold value is set as 4~6mV/mL in the step (3)；
A kind of method with titratable amine content total in potentiometric determination 2-Propen-1-amine polymer with(chloromethyl)oxirane carbonate, feature exist
In, the step (3) is medium when point selection two, and the potential value of one of equivalent point controls between 150mV~250mV,
The potential value of another equivalent point controls between -250mV~-280mV.
A method of with titratable amine total in potentiometric determination 2-Propen-1-amine polymer with(chloromethyl)oxirane carbonate, experimentation is as follows:
One, experimental principle
Contain amino in this product molecular structure, amino exists in molecule with two kinds of kenels: free amine group and ammonium ion.First
Excessive hydrochloric acid is added into sample, so that the amino in all molecules is converted into ammonium ion, is then dripped with standard caustic soda solution
Fixed above-mentioned acid solution, it will there are two equivalence point of titration, when free acid complete neutralization generates first equivalent point；Ammonium ion
Complete neutralization generates second equivalent point when being converted into free amine group, amino consumption in difference, that is, sample molecule of two equivalent points
The amount of titrant；
Two, key instrument and reagent
Plum Teller T5 potentiometric titrimeter, METTLER TOLEDO electronic balance, METTLER TOLEDO DGi111-SC are multiple
Close Glass pH electrodes, 1mol/l sodium hydroxide titration liquid, 1mol/l hydrochloric acid solution
Three, the measurement of sample
(1) operation and calculating process
2-Propen-1-amine polymer with(chloromethyl)oxirane carbonate (calling this product in the following text) about 1.0g is taken, it is accurately weighed to be placed in titration cup, 1.0mol/L hydrochloric acid is added
Solution 15ml adds water 35ml, stirs 40 minutes, according to potentiometric titration, titration parameters are carefully arranged, and using glass electrode, uses
1.0mol/L sodium hydroxide titration drop determines above-mentioned solution.
X=[(V2-V1) × C]/W
Wherein: X is total titratable amine content (mmol/g)
V2 is the volume number (ml) that second equivalent point consumes titrating solution
V1 is the volume number (ml) that first equivalent point consumes titrating solution
C is the concentration (mol/L) of 1.0mol/L sodium hydroxide titration liquid
W is samples weighing (g), in terms of dry product
(2) repeated experiment
This product about 1.0g is taken, it is accurately weighed to be placed in titration cup, 1.0mol/L hydrochloric acid solution 15ml is added, adds water 35ml,
Stirring 40 minutes, according to potentiometric titration, is carefully arranged titration parameters, using glass electrode, with 1.0mol/L sodium hydroxide titration
Drop determines above-mentioned solution, repeats to titrate 6 parts of samples.As a result it see the table below.
Repeated experiment result
Conclusion: as seen from the above table, 6 parts of samples of replication, total titratable amine product average content is 12.23mmol/g, RSD
It is 0.49%, less than 2%, it is seen that this method repeatability is good.
(3) Intermediate precision is tested
According to " repetitive test method ", there are different analysis personnel in not same date, 6 parts of samples of replication investigate 12
The RSD of secondary measurement result.As a result it see the table below.
Precision test result
Conclusion: as seen from the above table, 12 parts of samples of replication, total titratable amine product average content is 12.23mmol/g,
RSD is 0.42%, less than 2%, it is seen that this method precision is good.
By adopting the above technical scheme, accurate the beneficial effects of the present invention are: method constant-current titration jumping of the invention is obvious
Degree, accuracy meet the requirements, and compared with traditional acid base titration, have many advantages, such as high efficiency, easy to operate, easy grasp.
Detailed description of the invention
Fig. 1: potential value E (mV) with titration volumes V (mV) variation tendency；As seen from the figure, potential value E (mV) with
The increase of titration volumes V (ml) and change, there are two equivalent points, respectively 2.961596ml and 14.061852ml；
Fig. 2: dE/dV (mV/mL) with titration volumes V (mL) variation tendency；As seen from the figure, dE/dV (mV/mL)
Change with the increase of titration volumes V (ml), there are two be present in the peak value of dE/dV (mV/mL) that is, respectively for equivalent point
For 2.961596ml, 14.061852ml.
Specific embodiment
The present invention described further below, but practical range of the invention is not limited.
Embodiment 1
(1) 2-Propen-1-amine polymer with(chloromethyl)oxirane carbonate (calling this product in the following text) about 1.0g is taken, it is accurately weighed to be placed in titration cup；
(2) 1.0mol/L hydrochloric acid solution 15ml is measured with pipette precision, adds water 35ml, stirred 40 minutes；
(3) potentiometric titration is shone, titration parameters are carefully set, using glass electrode, with 1.0mol/L sodium hydroxide titration
Drop determines above-mentioned solution.
(4) titration terminates, by the content that total titratable amine is calculated.
Embodiment 2
(1) this product about 1.0g is taken, it is accurately weighed to be placed in titration cup；
(2) 1.0mol/L hydrochloric acid solution 13ml is measured with pipette precision, adds water 35ml, stirred 40 minutes；
(3) potentiometric titration is shone, titration parameters are carefully set, using glass electrode, with 1.0mol/L sodium hydroxide titration
Drop determines above-mentioned solution.
(4) titration terminates, by the content that total titratable amine is calculated.
Embodiment 3
(1) this product about 1.0g is taken, it is accurately weighed to be placed in titration cup；
(2) 1.0mol/L hydrochloric acid solution 17ml is measured with pipette precision, adds water 35ml, stirred 40 minutes；
(3) potentiometric titration is shone, titration parameters are carefully set, using glass electrode, with 1.0mol/L sodium hydroxide titration
Drop determines above-mentioned solution.
(4) titration terminates, by the content that total titratable amine is calculated.
Embodiment 4
(1) this product about 1.0g is taken, it is accurately weighed to be placed in titration cup；
(2) 1.0mol/L hydrochloric acid solution 15ml is measured with pipette precision, adds water 35ml, stirred 30 minutes；
(3) potentiometric titration is shone, titration parameters are carefully set, using glass electrode, with 1.0mol/L sodium hydroxide titration
Drop determines above-mentioned solution.
(4) titration terminates, by the content that total titratable amine is calculated.
Embodiment 5
(1) this product about 1.0g is taken, it is accurately weighed to be placed in titration cup；
(2) 1.0mol/L hydrochloric acid solution 15ml is measured with pipette precision, adds water 35ml, stirred 50 minutes；
(3) potentiometric titration is shone, titration parameters are carefully set, using glass electrode, with 1.0mol/L sodium hydroxide titration
Drop determines above-mentioned solution.
(4) titration terminates, by the content that total titratable amine is calculated.
Embodiment 6
(1) this product about 1.0g is taken, it is accurately weighed to be placed in titration cup；
(2) 1.0mol/L hydrochloric acid solution 15ml is measured with pipette precision, adds water 30ml, stirred 40 minutes；
(3) potentiometric titration is shone, titration parameters are carefully set, using glass electrode, with 1.0mol/L sodium hydroxide titration
Drop determines above-mentioned solution.
Embodiment 7
(1) this product about 1.0g is taken, it is accurately weighed to be placed in titration cup；
(2) 1.0mol/L hydrochloric acid solution 15ml is measured with pipette precision, adds water 40ml, stirred 40 minutes；
(3) potentiometric titration is shone, titration parameters are carefully set, using glass electrode, with 1.0mol/L sodium hydroxide titration
Drop determines above-mentioned solution.
(4) titration terminates, by the content that total titratable amine is calculated.
Claims (5)
1. a kind of method with titratable amine content total in potentiometric determination 2-Propen-1-amine polymer with(chloromethyl)oxirane carbonate, which is characterized in that including
Following steps:
(1) 2-Propen-1-amine polymer with(chloromethyl)oxirane carbonate sample about 1.0g is taken, it is accurately weighed to be placed in titration cup；
(2) 1.0mol/L hydrochloric acid solution 13-17ml is measured with pipette precision, adds water 30-40ml, stirred 30-50 minutes；
(3) potentiometric titration is shone, titration parameters are set, model selection balances control model, and dE 0.2mV, dt are 1 second；Threshold value
It is set as 4~6mV/mL；Equivalent point selects two, and the potential value of one of equivalent point controls between 150mV~250mV, separately
The potential value of an outer equivalent point controls between -250mV~-280mV；Using glass electrode, with 1.0mol/L sodium hydroxide
Titrating solution titrates above-mentioned solution.
2. a kind of side with titratable amine content total in potentiometric determination 2-Propen-1-amine polymer with(chloromethyl)oxirane carbonate according to claim 1
Method, which is characterized in that measure 1.0mol/L hydrochloric acid solution 15ml with pipette precision in the step (2), add water 35ml, stir
40 minutes.
3. a kind of side with titratable amine content total in potentiometric determination 2-Propen-1-amine polymer with(chloromethyl)oxirane carbonate according to claim 1
Method, which is characterized in that model selection balances control model in the step (3), and dE 0.2mV, dt are 1 second, i.e. potential change
Under the premise of 0.2mV/s, potentiometric titrimeter can be dripped into next drop for control.
4. a kind of side with titratable amine content total in potentiometric determination 2-Propen-1-amine polymer with(chloromethyl)oxirane carbonate according to claim 1
Method, which is characterized in that threshold value is set as 4~6mV/mL in the step (3).
5. a kind of side with titratable amine content total in potentiometric determination 2-Propen-1-amine polymer with(chloromethyl)oxirane carbonate according to claim 1
Method, which is characterized in that the step (3) is medium when point selection two, the control of the potential value of one of equivalent point 150mV~
Between 250mV, the potential value of another equivalent point is controlled between -250mV~-280mV.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110726803A (en) * | 2019-11-01 | 2020-01-24 | 江苏扬农化工集团有限公司 | Method for determining amino value by automatic potentiometric titration |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110726803A (en) * | 2019-11-01 | 2020-01-24 | 江苏扬农化工集团有限公司 | Method for determining amino value by automatic potentiometric titration |
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Application publication date: 20190806 |