CN112326869A - Method for determining and identifying content of guanidine nitrate - Google Patents
Method for determining and identifying content of guanidine nitrate Download PDFInfo
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- CN112326869A CN112326869A CN202011020919.9A CN202011020919A CN112326869A CN 112326869 A CN112326869 A CN 112326869A CN 202011020919 A CN202011020919 A CN 202011020919A CN 112326869 A CN112326869 A CN 112326869A
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Abstract
The invention discloses a method for measuring and identifying the content of guanidine nitrate, which comprises the following steps: s1, carrying out a nitrate group identification test and a guanidine group identification test on a sample; s2, measuring the content of ammonium nitrate in the sample, and S3, measuring the content of guanidine nitrate in the sample. According to the guanidine nitrate determination method, the condition that guanidine nitrate does not exist in the sample is eliminated by performing the nitrate group identification test and the guanidine group identification test on the sample, so that the subsequent content test result is prevented from being interfered, and the result accuracy is higher. When the tested sample does not contain guanidine or nitrate, the test can be ended in advance without subsequent test steps, so that the process can be saved and the efficiency can be improved. In addition, the testing method does not need picric acid, and the adopted testing reagents are common laboratory reagents, so that the threshold of the reagents is low, and the method is convenient to popularize and use.
Description
Technical Field
The invention relates to the technical field of chemical analysis, in particular to a method for determining and identifying the content of guanidine nitrate.
Background
Guanidine nitrate is used as a pharmaceutical raw material and is widely applied to the synthesis of sulfa drugs, antibacterial synergists TMP and DVD. In order to ensure that the produced guanidine nitrate really and reliably meets the target substance and meets the quality standard requirement, a guanidine nitrate identification and inspection method is established, the key raw material guanidine nitrate in the production process is analyzed and identified, and the obtained product is ensured to be the raw material guanidine nitrate meeting the quality standard. At present, the content of guanidine nitrate is measured by adopting a picric acid gravimetric method, and picric acid is one of explosives, is toxic, mainly causes skin injury and has strong irritation. Through friction and vibration, violent explosion is easy to occur, and the material has strong oxidizing property and can react violently with combustible substances and reducing agents to generate combustion explosion. When purchasing picric acid, a purchasing unit has procedures of purchasing explosive articles, registering, purchasing storage quality, then recording in a public security bureau, and a seller has procedures of distribution and transportation, so that the purchasing process of picric acid is very complicated. Meanwhile, in the industrial standard of industrial guanidine nitrate, the method for measuring the guanidine nitrate content by a picric acid method takes about 5-6 hours for detection, has long detection period and is not beneficial to the control of the production process.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for determining and identifying the content of guanidine nitrate, which does not need to rely on picric acid for determination and has safe and reliable determination process and accurate result.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a method for measuring and identifying the content of guanidine nitrate comprises the following steps:
s1, carrying out a nitrate group identification test and a guanidine group identification test on a sample, and when the test result shows that the nitrate group and the guanidine group exist in the sample at the same time, determining that the guanidine nitrate exists in the sample, and continuously testing the sample; when the test result shows that the nitrate and the guanidine do not coexist in the sample, the test conclusion is that the sample contains no guanidine nitrate;
s2, measuring the content of ammonium nitrate in the sample, and weighing G1Adding water to the sample, heating to dissolve the sample, cooling to room temperature, then dropwise adding a phenolphthalein indicator, titrating the solution by using 0.1mol/L sodium hydroxide titration solution until the solution is reddish, then adding a neutral formaldehyde solution, uniformly mixing, standing for 3-5 minutes, titrating the solution by using 0.1mol/L sodium hydroxide titration solution until the solution is reddish, keeping the color of the solution unchanged after 1-2 minutes, and recording the consumption volume V of the sodium hydroxide titration solution after the titration is finished;
calculating the mass percent of ammonium nitrate in the sample
Wherein V is the volume of sodium hydroxide titration solution consumed by the test sample for the second time, and the unit of the volume is ml; c is the molar concentration of sodium hydroxide titration solution (0.1mol/L), and the unit mol/L; g1Unit of (d) is g; w is the weight loss percentage of the sample after drying;
s3, measuring the content of guanidine nitrate in the sample:
test group: weighing the weight G2Adding glacial acetic acid to the sample to dissolve the sample, cooling the sample to room temperature, dropwise adding a crystal violet indicator, titrating the solution by using perchloric acid standard titration solution until the solution turns yellow, and recording the consumption volume V of the perchloric acid titration solution1；
Control group: taking glacial acetic acid with the same volume of the test group, dropwise adding a crystal violet indicator, titrating with perchloric acid standard titration solution until the solution turns yellow, and recording the consumption volume V of the perchloric acid titration solution0；
Calculating the mass percent of guanidine nitrate in the sample
Wherein, V1In units of ml, V0The unit of (A) is ml; g2Unit of (d) is g; w is the percent loss on drying of the sample; m1Is the corrected concentration of perchloric acid titration solution (0.1mol/L), mol/L; when the measured room temperature is different from the calibrated room temperature (| T)1-T0| is not less than 2 ℃), the concentration is corrected according to the following formula:
wherein M is0The standard concentration of perchloric acid titration solution (0.1mol/L) is unit mol/L; t is1Room temperature in the measurement, T0Room temperature for calibrationIn units of ℃.
Preferably, after the sample is dissolved by adding water, adding sulfuric acid, mixing, cooling to room temperature, and adding ferrous sulfate test solution; if the solution delaminates and the interface appears brown, the sample contains nitrate groups.
Preferably, in step S1, the guanidino differential test comprises the following steps: and (3) adding water to the sample for dissolving, adding an alpha-naphthol test solution for mixing, and then adding a sodium hypobromite test solution, wherein if the solution turns red, the sample contains guanidyl.
Preferably, the preparation process of the ferrous sulfate test solution is as follows: taking 8g of ferrous sulfate crystals, and adding 100ml of newly boiled cold water for dissolving to obtain the ferrous sulfate crystal.
Preferably, the preparation process of the alpha-naphthol test solution is as follows: taking 10.5ml of 15% alpha-naphthol ethanol solution, slowly adding 6.5ml of sulfuric acid, uniformly mixing, then adding 40.5ml of ethanol and 4ml of water, and uniformly mixing to obtain the alpha-naphthol ethanol solution.
Preferably, the preparation process of the sodium hypobromite test solution is as follows: taking 20g of sodium hydroxide, adding 75ml of water for dissolving, adding 5ml of bromine, and adding water for diluting to 100 ml.
The invention has the beneficial effects that: according to the guanidine nitrate determination method, the condition that guanidine nitrate does not exist in the sample is eliminated by performing the nitrate group identification test and the guanidine group identification test on the sample, so that the subsequent content test result is prevented from being interfered, and the result accuracy is higher. When the tested sample does not contain guanidine or nitrate, the test can be ended in advance without subsequent test steps, so that the process can be saved and the efficiency can be improved. In addition, the testing method does not need picric acid, and the adopted testing reagents are common laboratory reagents, so that the threshold of the reagents is low, and the method is convenient to popularize and use.
Detailed Description
The claimed solution of the present invention will now be described in further detail with reference to examples.
A method for measuring and identifying the content of guanidine nitrate comprises the following steps:
s1, carrying out a nitrate group identification test and a guanidine group identification test on a sample.
In this example, the nitrate-based discrimination test comprises the following steps: a sample (0.5 g) is dissolved in 10ml of water to obtain a test solution. Taking 1ml of test solution, placing the test solution in a test tube, adding 1ml of sulfuric acid, carefully mixing, cooling, adding 0.5ml of ferrous sulfate test solution along the wall of the test tube, and if the solution is layered and the joint interface is brown, the sample contains a nitrate group. Wherein the preparation process of the ferrous sulfate test solution comprises the following steps: taking 8g of ferrous sulfate crystals, and adding 100ml of newly boiled cold water for dissolving to obtain the ferrous sulfate crystal.
In this example, the guanidino differential test comprises the following steps: a sample (0.5 g) is dissolved in 10ml of water to obtain a test solution. Taking 1ml of test solution, adding 0.5ml of alpha-naphthol test solution, mixing, adding 0.5ml of sodium hypobromite test solution, and if the solution becomes red, the sample contains guanidyl. The preparation process of the alpha-naphthol test solution comprises the following steps: taking 10.5ml of 15% alpha-naphthol ethanol solution, slowly adding 6.5ml of sulfuric acid, uniformly mixing, then adding 40.5ml of ethanol and 4ml of water, and uniformly mixing to obtain the alpha-naphthol ethanol solution. The preparation process of the sodium hypobromite test solution comprises the following steps: taking 20g of sodium hydroxide, adding 75ml of water for dissolving, adding 5ml of bromine, and adding water for diluting to 100 ml. When the test result shows that the nitrate and the guanidine exist in the sample at the same time, the test conclusion is that the guanidine nitrate exists in the sample, and the sample continues to be tested; when the test result shows that no nitrate group and guanidine group coexist in the sample, the test result shows that no guanidine nitrate exists in the sample.
S2, measuring the content of ammonium nitrate in the sample: weighing the weight G1The sample was placed in a 250ml Erlenmeyer flask and dissolved by adding 100ml of water under heating, in this example G1The concentration is 2.0g, the concentration is accurate to 0.0001g, 2 drops of phenolphthalein indicator are dripped after the solution is cooled to room temperature, the solution is titrated by 0.1mol/L sodium hydroxide titration solution until the solution is reddish, then neutral formaldehyde solution is added, the solution is placed for 3 to 5 minutes after being uniformly mixed, the solution is titrated by 0.1mol/L sodium hydroxide titration solution until the solution is reddish, the color does not disappear after 1 to 2 minutes, the titration is finished, and the consumption volume V of the sodium hydroxide titration solution is recorded;
calculating the mass percent of ammonium nitrate in the sample:
wherein V is the volume of sodium hydroxide titration solution consumed by the second titration test sample, and the unit of the volume is ml; c is the molar concentration of sodium hydroxide titration solution (0.1mol/L), and the unit mol/L; g1Unit of (d) is g; w is the weight loss percentage of the sample after drying;
s3, measuring the content of guanidine nitrate in the sample:
test group: weighing the weight G2Into a 100ml conical flask with a stopper, G in this example2Is 0.1g, is accurate to 0.0001g, then is added with glacial acetic acid 30ml, is heated to be dissolved, is cooled to room temperature and is added with 3 drops of crystal violet indicator dropwise, then is titrated by perchloric acid standard titration liquid until the solution becomes yellow, and the consumption volume V of the perchloric acid titration liquid is recorded1；
Control group: taking glacial acetic acid with the same volume of the test group, dropwise adding a crystal violet indicator, titrating with perchloric acid standard titration solution until the solution turns yellow, and recording the consumption volume V of the perchloric acid titration solution0；
Calculating the mass percent of guanidine nitrate in the sample:
wherein, V1In units of ml, V0The unit of (A) is ml; g2Unit of (d) is g; w is the percent loss on drying of the sample; m1Is the corrected concentration of perchloric acid titration solution (0.1mol/L), mol/L; when the measured room temperature is different from the calibrated room temperature (| T)1-T0| is not less than 2 ℃), the concentration is corrected according to the following formula:
wherein M is0The standard concentration of perchloric acid titration solution (0.1mol/L) is unit mol/L; t is1Room temperature in the measurement, T0Room temperature, unit c, as calibrated.
The test method in this example is now compared with the prior art method for measuring the guanidine nitrate content (HG 3269-1989-T). The comparison method is to use three different samples to respectively test by adopting the method of the embodiment and the method of the prior art, and the test results are as follows:
| sample (I) | Examples | HG3269-1989-T |
| A | 95.4％ | 95.6％ |
| B | 95.2％ | 95.3％ |
| C | 95.5％ | 95.8％ |
The results show that the deviation of the detection method adopted by the invention on the content determination result of guanidine nitrate from the prior art is small, which can show that the detection method of the invention has accurate and reliable results.
The above-described embodiments are merely preferred embodiments of the present invention, which is not intended to limit the present invention in any way. Those skilled in the art can make many changes and modifications to the disclosed embodiments, or modify equivalent embodiments to practice the disclosed embodiments, without departing from the scope of the disclosed embodiments. Therefore, equivalent variations made according to the idea of the present invention should be covered within the protection scope of the present invention without departing from the contents of the technical solution of the present invention.
Claims (6)
1. The method for measuring and identifying the content of guanidine nitrate is characterized by comprising the following steps:
s1, carrying out a nitrate group identification test and a guanidine group identification test on a sample, and when the test result shows that the nitrate group and the guanidine group exist in the sample at the same time, determining that the guanidine nitrate exists in the sample, and continuously testing the sample; when the test result shows that the nitrate and the guanidine do not coexist in the sample, the test conclusion is that the sample contains no guanidine nitrate;
s2, measuring the content of ammonium nitrate in the sample, and weighing G1Adding water to the sample, heating to dissolve the sample, cooling to room temperature, then dropwise adding a phenolphthalein indicator, titrating the solution by using 0.1mol/L sodium hydroxide titration solution until the solution is reddish, then adding a neutral formaldehyde solution, uniformly mixing, standing for 3-5 minutes, titrating the solution by using 0.1mol/L sodium hydroxide titration solution until the solution is reddish, keeping the color of the solution unchanged after 1-2 minutes, and recording the consumption volume V of the sodium hydroxide titration solution after the titration is finished; (ii) a
Calculating the mass percent of ammonium nitrate in the sample
Wherein V is the volume of sodium hydroxide titration solution consumed by the second titration test sample, and the unit of the volume is ml; c is the molar concentration of sodium hydroxide titration solution (0.1mol/L), and the unit mol/L; g1Unit of (d) is g; w is the weight loss percentage of the sample after drying;
s3, measuring the content of guanidine nitrate in the sample:
test group: weighing the weight G2Adding glacial acetic acid to the sample to dissolve the sample, cooling the sample to room temperature, dropwise adding a crystal violet indicator, titrating the solution by using perchloric acid standard titration solution until the solution turns yellow, and recording the consumption volume V of the perchloric acid titration solution1；
Control group: taking glacial acetic acid with the same volume of the test group, dropwise adding a crystal violet indicator, titrating with perchloric acid standard titration solution until the solution turns yellow, and recording the consumption volume V of the perchloric acid titration solution0；
Calculating the mass percent of guanidine nitrate in the sample
Wherein, V1In units of ml, V0The unit of (A) is ml; g2Unit of (d) is g; w is the percent loss on drying of the sample;
M1is the corrected concentration of perchloric acid titration solution (0.1mol/L), mol/L; when the measured room temperature is different from the calibrated room temperature (| T)1-T0| is not less than 2 ℃), the concentration is corrected according to the following formula:
wherein M is0The standard concentration of perchloric acid titration solution (0.1mol/L) is unit mol/L; t is1Room temperature in the measurement, T0Room temperature, unit c, as calibrated.
2. The method for determining the content of guanidine nitrate according to claim 1, wherein: in step S1, the nitrate-based discrimination test includes the following steps: adding water to a sample for dissolving, adding sulfuric acid for mixing, cooling to room temperature, and adding a ferrous sulfate test solution; if the solution delaminates and the interface appears brown, the sample contains nitrate groups.
3. The method for determining the content of guanidine nitrate according to claim 1, wherein: in step S1, the guanidino differential test includes the following steps: and (3) adding water to the sample for dissolving, adding an alpha-naphthol test solution for mixing, and then adding a sodium hypobromite test solution, wherein if the solution turns red, the sample contains guanidyl.
4. The method for determining the content of guanidine nitrate according to claim 2, wherein: the preparation process of the ferrous sulfate test solution comprises the following steps: taking 8g of ferrous sulfate crystals, and adding 100ml of newly boiled cold water for dissolving to obtain the ferrous sulfate crystal.
5. The method for determining the content of guanidine nitrate according to claim 3, wherein: the preparation process of the alpha-naphthol test solution comprises the following steps: taking 10.5ml of 15% alpha-naphthol ethanol solution, slowly adding 6.5ml of sulfuric acid, uniformly mixing, then adding 40.5ml of ethanol and 4ml of water, and uniformly mixing to obtain the alpha-naphthol ethanol solution.
6. The method for determining the content of guanidine nitrate according to claim 3, wherein: the preparation process of the sodium hypobromite test solution comprises the following steps: taking 20g of sodium hydroxide, adding 75ml of water for dissolving, adding 5ml of bromine, and adding water for diluting to 100 ml.
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| CN103439215A (en) * | 2013-08-28 | 2013-12-11 | 南通天泽化工有限公司 | Quick detecting method for guanidine nitrate content |
| CN109580873A (en) * | 2018-12-27 | 2019-04-05 | 湖北航天化学技术研究所 | A kind of measuring method of triamido guanidine nitrate purity |
| CN111189827A (en) * | 2020-01-19 | 2020-05-22 | 佛山市南海北沙制药有限公司 | Detection method for identifying refined aldehyde |
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