CN116087375A - Guanidine nitrate quantitative analysis method - Google Patents

Guanidine nitrate quantitative analysis method Download PDF

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CN116087375A
CN116087375A CN202111303700.4A CN202111303700A CN116087375A CN 116087375 A CN116087375 A CN 116087375A CN 202111303700 A CN202111303700 A CN 202111303700A CN 116087375 A CN116087375 A CN 116087375A
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guanidine nitrate
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sodium hydroxide
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徐平
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Nantong Tendenci Chemical Co Ltd
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    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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Abstract

The invention provides a guanidine nitrate quantitative analysis method, which comprises the following steps: the sample is detected by a liquid chromatograph-ultraviolet detector (HPLC-UV), and is quantitatively analyzed by a chromatographic column ODS-3C 18, and the main peak content is calculated. Weighing a proper amount of sample, adding water for dissolution, adding phenolphthalein for titration by using sodium hydroxide, detecting the content of free nitric acid, continuously adding neutral formaldehyde solution into the sample, and detecting the content of free ammonium nitrate by titration by using sodium hydroxide standard solution. And finally subtracting the contents of free nitric acid and free ammonium nitrate from the main content, and calculating to obtain the guanidine nitrate content. The method is simple, quick and high in accuracy.

Description

Guanidine nitrate quantitative analysis method
Technical Field
The invention relates to a guanidine nitrate quantitative analysis method, and belongs to the technical field of analytical chemistry.
Background
Guanidine nitrate is an important pharmaceutical intermediate with the molecular formula of CH 5 N 3 ·HNO 3 . As a white granular solid. Guanidine nitrate is soluble in water and alcohol, insoluble in acetone, benzene and diethyl ether. The method is mainly used for synthesizing sulfa drugs such as sulfamidine, and the like, is also used for manufacturing raw materials of explosives, photographic materials and disinfectants, and can be used as an analysis reagent for detecting guanidine salts in complex acid.
In the existing standard analysis method of guanidine nitrate, the content cannot be analyzed by a precipitation method due to the purchase problem of picric acid reagent. As a raw material in the production process of the nitro guanidine, the technical quality guarantee cannot be provided for the production process due to the uncertainty of the content.
Disclosure of Invention
The invention aims to solve the problems existing in the use process of the conventional guanidine nitrate, and provides a quantitative analysis method of guanidine nitrate with small error.
The technical solution of the invention is as follows: the guanidine nitrate quantitative analysis method specifically comprises the following steps:
1) Separating and detecting the sample by a liquid chromatograph with an ultraviolet detector, quantitatively analyzing by a chromatographic column, and calculating the main content of guanidine nitrate according to a liquid chromatogram; the liquid chromatography detection conditions were as follows: the model of the chromatographic column is ODS-3C 18, and the specification is 4.0mm (id) multiplied by 150mm; mobile phase: methanol and water in a volume ratio of 5:95, and 3 drops of phosphoric acid are added dropwise; wavelength: 210nm; flow rate: 0.8ml/min; sensitivity: 0.05AUFS; sample injection amount: 50uL;
2) Weighing a proper amount of sample, adding water for dissolution, adding phenolphthalein for titration by sodium hydroxide, and detecting the content of free nitric acid; continuously adding neutral formaldehyde solution into the sample, titrating with sodium hydroxide standard solution, and detecting the content of free ammonium nitrate; and finally, subtracting the content of free nitric acid and free ammonium nitrate from the main content of guanidine nitrate calculated in the step 1), and calculating to obtain the content of guanidine nitrate.
Further, the measuring steps of the liquid chromatograph in the step 1) are specifically as follows:
1) Standard solution preparation: weighing guanidine nitrate standard sample in a container, adding mobile phase to a constant volume, and shaking to obtain standard solution;
2) Sample solution preparation: weighing a sample in a container, adding a mobile phase to a constant volume, and shaking uniformly to obtain a sample solution;
3) Sample injection analysis: continuously injecting two-needle standard solution into liquid chromatograph, injecting standard solution and sample solution into liquid chromatograph after the peak area error of the liquid chromatogram of the two-needle standard solution is less than 1%, measuring by liquid chromatograph to form liquid chromatogram, recording peak area values generated by the standard solution and the sample solution respectively
4) And (3) calculating results: the guanidine nitrate content was calculated as follows:
Figure 72964DEST_PATH_IMAGE002
wherein: m1 represents the weight of the guanidine nitrate standard sample, and the unit is g; m2 represents the weight of the guanidine nitrate sample in g; a1 represents the peak area of guanidine nitrate standard; a represents the peak area of a guanidine nitrate sample 2; p represents the percent purity of guanidine nitrate standard.
Further, the specific steps for calculating the guanidine nitrate content in the step 2) are as follows:
1) Weighing a certain amount of sample, adding water, dissolving, shaking, adding phenolphthalein indicator, titrating with sodium hydroxide until the end point is pink, keeping the end point for 30S unchanged, adding neutral formaldehyde, standing for 5min, titrating with sodium hydroxide until the end point is pink, and keeping the end point for 30S unchanged; the concentration of the phenolphthalein indicator is 1g/L; the concentration of the sodium hydroxide standard solution is 0.05mol/L; the volume concentration of the formaldehyde solution is 37%, and the formaldehyde solution is neutral;
2) And (3) calculating results: the formula for calculating the guanidine nitrate content X% is as follows:
X2%=V1C×0.063×100/m
X3%=V2C×0.08×100/m
X%=X1-X2-X3
wherein: v1 represents the volume of sodium hydroxide solution consumed in mL when analyzing free nitric acid; v2 represents the volume of sodium hydroxide standard solution consumed in mL when analyzing free ammonium nitrate; c represents the molar concentration of a sodium hydroxide standard solution, and the unit is mol/L; m represents the mass of the sample, and the unit is g;0.063 and 0.08 represent conversion coefficients. X1 represents the main content of guanidine nitrate obtained by liquid phase analysis; x2 represents the percentage of free nitric acid; x3 represents the percentage of free ammonium nitrate.
Compared with the prior art, the method is simple, quick and high in accuracy.
Drawings
FIG. 1 is a liquid chromatogram of a sample in example 1 of the present invention.
FIG. 2 is a liquid chromatogram of a sample in example 2 of the present invention.
FIG. 3 is a liquid chromatogram of the sample in example 3 of the present invention.
Detailed Description
The technical scheme of the invention is further described below according to a plurality of embodiments. In the description of the present specification, the contents of each example means that a specific technical feature described in connection therewith is included in at least one embodiment of the present invention. In this specification, a schematic representation of an embodiment does not necessarily refer to the same implementation or example. Furthermore, the particular features described may be combined in any suitable manner in any one or more embodiments or examples.
Example 1
1) Preparing a sodium hydroxide standard solution: preparing a sodium hydroxide standard titration solution with the concentration of 0.05mol/L according to GB/T601-2002;
2) Preparation of phenolphthalein indicator: 0.1g of phenolphthalein is taken and dissolved in 10-30mL of 95% ethanol, and then diluted to 100mL by ethanol;
3) Preparing neutral formaldehyde: dissolving 50mL of formaldehyde in 50mL of water, shaking uniformly, adding 3 drops of phenolphthalein indicator, and adjusting to be neutral by using a sodium hydroxide standard solution;
4) Liquid chromatography detection:
instrument: LC-20A has a UV detector; chromatographic column: ODS-3C 18 column, 4.0mm (id). Times.150 mm; mobile phase: methanol + water = 5 +95 plus 3 drops of phosphoric acid; wavelength: 210nm; flow rate: 0.8ml/min; sensitivity: 0.05AUFS; sample injection amount: 50ul;
the measuring step comprises the following steps:
A. preparing a standard sample: weighing 0.05g guanidine nitrate standard sample, fixing the volume by mobile phase in a 100ml volumetric flask, transferring 3ml of the solution to a 50ml volumetric flask, and shaking uniformly;
B. sample preparation: 0.05g (guanidine nitrate content about 90%) was weighed and treated as above;
C. sample injection analysis: continuously feeding two needles of standard samples, and after the area error is less than 1%, sampling according to the sequence of the standard samples, the samples and the standard samples;
D. result calculation
Figure 458946DEST_PATH_IMAGE002
Wherein: m is m 1 -the weight of guanidine nitrate standard sample in g;
m 2 -represents the weight of the guanidine nitrate sample in g;
A 1 -representing the peak area of guanidine nitrate standard;
A 2 peak area of guanidine nitrate sample;
p-represents the purity of guanidine nitrate standard,%;
FIG. 1 is a liquid chromatogram of quantitative analysis of a sample;
5) The method for measuring the content of the free nitric acid and the free ammonium nitrate comprises the following specific steps:
A. weighing 2g of sample in a container, adding water, dissolving, shaking uniformly, adding phenolphthalein indicator, titrating with sodium hydroxide until the end point is pink, keeping the end point unchanged for 30S, adding neutral formaldehyde, standing for 5min, titrating with sodium hydroxide until the end point is pink, and keeping the end point unchanged for 30S;
B. result calculation
The content is calculated by the following formula:
X2%=V 1 C×0.063×100/m
X3%=V 2 C×0.08×100/m
wherein: v (V) 1 -the volume of sodium hydroxide solution consumed in analysing the free nitric acid in mL;
V 2 -the volume of sodium hydroxide standard solution consumed in analysing the free ammonium nitrate in mL;
c, the molar concentration of the sodium hydroxide standard solution is expressed in mol/L;
m-the mass of the sample in g;
0.063, 0.08-conversion coefficient.
The guanidine nitrate content was finally calculated to be 90.52%.
Example 2
1) Preparing a sodium hydroxide standard solution: preparing a sodium hydroxide standard titration solution with the concentration of 0.05mol/L according to GB/T601-2002;
2) Preparation of phenolphthalein indicator: 0.1g of phenolphthalein is taken and dissolved in 10-30mL of 95% ethanol, and then diluted to 100mL by ethanol;
3) Preparing neutral formaldehyde: dissolving 50mL of formaldehyde in 50mL of water, shaking uniformly, adding 3 drops of phenolphthalein indicator, and adjusting to be neutral by using a sodium hydroxide standard solution;
4) Liquid chromatography detection:
instrument: LC-20A has a UV detector; chromatographic column: ODS-3C 18 column, 4.0mm (id). Times.150 mm; mobile phase: methanol + water = 5 +95 plus 3 drops of phosphoric acid; wavelength: 210nm; flow rate: 0.8ml/min; sensitivity: 0.05AUFS; sample injection amount: 50ul;
the measuring step comprises the following steps:
A. preparing a standard sample: weighing 0.05g guanidine nitrate standard sample, fixing the volume by mobile phase in a 100ml volumetric flask, transferring 3ml of the solution to a 50ml volumetric flask, and shaking uniformly;
B. sample preparation: 0.05g (guanidine nitrate content about 90%) was weighed and treated as above;
C. sample injection analysis: continuously feeding two needles of standard samples, and after the area error is less than 1%, sampling according to the sequence of the standard samples, the samples and the standard samples;
D. result calculation
Figure 832158DEST_PATH_IMAGE002
Wherein: m is m 1 -the weight of guanidine nitrate standard sample in g;
m 2 -represents the weight of the guanidine nitrate sample in g;
A 1 -representing the peak area of guanidine nitrate standard;
A 2 peak area of guanidine nitrate sample;
p-represents the purity of guanidine nitrate standard,%;
FIG. 2 is a liquid chromatogram of quantitative analysis of a sample;
5) The method for measuring the content of the free nitric acid and the free ammonium nitrate comprises the following specific steps:
A. weighing 2g of sample in a container, adding water, dissolving, shaking uniformly, adding phenolphthalein indicator, titrating with sodium hydroxide until the end point is pink, keeping the end point unchanged for 30S, adding neutral formaldehyde, standing for 5min, titrating with sodium hydroxide until the end point is pink, and keeping the end point unchanged for 30S;
B. result calculation
The content is calculated by the following formula:
X2%=V 1 C×0.063×100/m
X3%=V 2 C×0.08×100/m
wherein: v (V) 1 -the volume of sodium hydroxide solution consumed in analysing the free nitric acid in mL;
V 2 -the volume of sodium hydroxide standard solution consumed in analysing the free ammonium nitrate in mL;
c, the molar concentration of the sodium hydroxide standard solution is expressed in mol/L;
m-the mass of the sample in g;
0.063, 0.08-conversion coefficient.
The guanidine nitrate content was finally calculated to be 90.56%.
Example 3
1) Preparing a sodium hydroxide standard solution: with reference to GB/T601-2002, a standard titration solution of 0.05mol/L sodium hydroxide is prepared.
2) Preparation of phenolphthalein indicator: 0.1g of phenolphthalein was dissolved in 10-30mL of 95% ethanol and diluted with ethanol to 100mL.
3) Preparing neutral formaldehyde: 50mL of formaldehyde is taken and dissolved in 50mL of water, the mixture is shaken well, 3 drops of phenolphthalein indicator are added, and the mixture is neutralized by using a sodium hydroxide standard solution.
4) Liquid chromatography detection:
instrument: LC-20A has a UV detector; chromatographic column: ODS-3C 18 column, 4.0mm (id). Times.150 mm; mobile phase: methanol + water = 5 +95 plus 3 drops of phosphoric acid; wavelength: 210nm; flow rate: 0.8ml/min; sensitivity: 0.05AUFS; sample injection amount: 50ul.
The measuring step comprises the following steps:
A. preparing a standard sample: weighing 0.05g guanidine nitrate standard sample, fixing the volume by mobile phase in a 100ml volumetric flask, transferring 3ml of the solution to a 50ml volumetric flask, and shaking uniformly;
B. sample preparation: 0.05g (guanidine nitrate content about 90%) was weighed and treated as above;
C. sample injection analysis: continuously feeding two needles of standard samples, and after the area error is less than 1%, sampling according to the sequence of the standard samples, the samples and the standard samples;
D. result calculation
Figure 430630DEST_PATH_IMAGE002
Wherein: m is m 1 -the weight of guanidine nitrate standard sample in g;
m 2 -represents the weight of the guanidine nitrate sample in g;
A 1 -representing the peak area of guanidine nitrate standard;
A 2 peak area of guanidine nitrate sample;
p-represents the purity of guanidine nitrate standard,%;
FIG. 3 is a liquid chromatogram of quantitative analysis of a sample;
5) The method for measuring the content of the free nitric acid and the free ammonium nitrate comprises the following specific steps:
A. weighing 2g of sample in a container, adding water, dissolving, shaking uniformly, adding phenolphthalein indicator, titrating with sodium hydroxide until the end point is pink, keeping the end point unchanged for 30S, adding neutral formaldehyde, standing for 5min, titrating with sodium hydroxide until the end point is pink, and keeping the end point unchanged for 30S;
B. result calculation
The content is calculated by the following formula:
X2%=V 1 C×0.063×100/m
X3%=V 2 C×0.08×100/m
wherein: v (V) 1 -the volume of sodium hydroxide solution consumed in analysing the free nitric acid in mL;
V 2 -the volume of sodium hydroxide standard solution consumed in analysing the free ammonium nitrate in mL;
c, the molar concentration of the sodium hydroxide standard solution is expressed in mol/L;
m-the mass of the sample in g;
0.063, 0.08-conversion coefficient.
The guanidine nitrate content was finally calculated to be 90.66%.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.

Claims (9)

1. The guanidine nitrate quantitative analysis method is characterized by comprising the following steps of:
1) Separating and detecting the sample by a liquid chromatograph with an ultraviolet detector, quantitatively analyzing by a chromatographic column, and calculating the main content of guanidine nitrate according to a liquid chromatogram;
2) Weighing a proper amount of sample, adding water for dissolution, adding phenolphthalein for titration by sodium hydroxide, and detecting the content of free nitric acid; continuously adding neutral formaldehyde solution into the sample, titrating with sodium hydroxide standard solution, and detecting the content of free ammonium nitrate; and finally, subtracting the content of free nitric acid and free ammonium nitrate from the main content of guanidine nitrate calculated in the step 1), and calculating to obtain the content of guanidine nitrate.
2. The method for quantitative analysis of guanidine nitrate according to claim 1, wherein: the liquid chromatography detection conditions in the step 1) are as follows: mobile phase: methanol and water; wavelength: 210nm; flow rate: 0.8ml/min; sensitivity: 0.05AUFS; sample injection amount: 50uL.
3. The method for quantitative analysis of guanidine nitrate according to claim 2, wherein: the liquid chromatograph adopts a chromatographic column model of ODS-3C 18 with the specification of 4.0mm (id) multiplied by 150mm.
4. The method for quantitative analysis of guanidine nitrate according to claim 2, wherein: the volume ratio of methanol to water in the mobile phase is 5:95, and 3 drops of phosphoric acid were added dropwise.
5. The method for quantitative analysis of guanidine nitrate according to claim 1, wherein: the measuring steps of the liquid chromatograph in the step 1) are specifically as follows:
1) Standard solution preparation: weighing guanidine nitrate standard sample in a container, adding mobile phase to a constant volume, and shaking to obtain standard solution;
2) Sample solution preparation: weighing a sample in a container, adding a mobile phase to a constant volume, and shaking uniformly to obtain a sample solution;
3) Sample injection analysis: continuously injecting two-needle standard solution into liquid chromatograph, injecting standard solution and sample solution into liquid chromatograph after the peak area error of the liquid chromatogram of the two-needle standard solution is less than 1%, measuring by liquid chromatograph to form liquid chromatogram, recording peak area values generated by the standard solution and the sample solution respectively
4) And (3) calculating results: the guanidine nitrate content was calculated as follows:
Figure DEST_PATH_IMAGE001
wherein: m is m 1 The weight of the guanidine nitrate standard sample is expressed in g; m is m 2 The weight of the guanidine nitrate sample is expressed in g; a is that 1 Represents the peak area of guanidine nitrate standard; a represents 2 Peak area of guanidine nitrate sample; p represents the percent purity of guanidine nitrate standard.
6. The method for quantitative analysis of guanidine nitrate according to claim 1, wherein: the specific steps for calculating the guanidine nitrate content in the step 2) are as follows:
1) Weighing a certain amount of sample, adding water, dissolving, shaking, adding phenolphthalein indicator, titrating with sodium hydroxide until the end point is pink, keeping the end point for 30S unchanged, adding neutral formaldehyde, standing for 5min, titrating with sodium hydroxide until the end point is pink, and keeping the end point for 30S unchanged;
2) And (3) calculating results: the formula for calculating the guanidine nitrate content X% is as follows:
X2%=V 1 C×0.063×100/m
X3%=V 2 C×0.08×100/m
X%=X1-X2-X3
wherein: v (V) 1 Representation analysisWhen free nitric acid, the volume of sodium hydroxide solution is consumed, and the unit is mL; v (V) 2 The unit of the volume of the sodium hydroxide standard solution consumed in the analysis of free ammonium nitrate is mL; c represents the molar concentration of a sodium hydroxide standard solution, and the unit is mol/L; m represents the mass of the sample, and the unit is g;0.063, 0.08 represents a conversion coefficient;
x1 represents the main content of guanidine nitrate obtained by liquid phase analysis; x2 represents the percentage of free nitric acid; x3 represents the percentage of free ammonium nitrate.
7. The method for quantitative analysis of guanidine nitrate according to claim 6, wherein: the concentration of the phenolphthalein indicator is 1g/L.
8. The method for quantitative analysis of guanidine nitrate according to claim 6, wherein: the concentration of the sodium hydroxide standard solution is 0.05mol/L.
9. The method for quantitative analysis of guanidine nitrate according to claim 6, wherein: the formaldehyde solution has a volume concentration of 37% and is neutral.
CN202111303700.4A 2021-11-05 2021-11-05 Guanidine nitrate quantitative analysis method Pending CN116087375A (en)

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