CN109580873A - A kind of measuring method of triamido guanidine nitrate purity - Google Patents
A kind of measuring method of triamido guanidine nitrate purity Download PDFInfo
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- CN109580873A CN109580873A CN201811614537.1A CN201811614537A CN109580873A CN 109580873 A CN109580873 A CN 109580873A CN 201811614537 A CN201811614537 A CN 201811614537A CN 109580873 A CN109580873 A CN 109580873A
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- solution
- guanidine nitrate
- triamido
- measuring method
- triamido guanidine
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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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
Abstract
The present invention discloses a kind of measuring method of triamido guanidine nitrate purity, it is the following steps are included: the 1) decomposition of triamido guanidine nitrate: with the acidity of sulfuric acid control solution, under certain acidity, using potassium bromate as oxidant, triamido guanidine nitrate oxygenolysis is generated into N2 and CO2；2) consume excessive potassium bromate: excessive potassium iodide being added into solution, in the dark in solution the oxidizing substance reaction generation elemental iodine stronger than elemental iodine；3) it titrates: the elemental iodine generated using the titration of 0.1mol/L sodium thiosulfate standard solution, while doing blank assay；4) purity of triamido nitric acid is calculated.The relative standard deviation of the purity for the triamido guanidine nitrate that the present invention measures is less than 0.5%.
Description
Technical field
The present invention relates to a kind of chemical products purity analysis technical fields, and in particular to a kind of triamido guanidine nitrate purity
Measuring method.
Background technique
Triamido guanidine nitrate (TAGN) is a kind of ionic compound, forms one due to the delocalization of electronics in cation
A big pi bond, improves the stability of molecule；The positive enthalpy of formation with higher；Nitrogen content height, carbohydrate content are low in molecule, more hold
Easily reach oxygen balance, gas production is big when combustion explosion, and it is a kind of important that product, which is mainly nitrogen gas and water and carbon dioxide gas,
Energetic material can be used as deoxidier and Shattering rate intermediate, it can also be used to rocket engine high energy smokeless propellant, gas hair
Raw agent and explosive additive.TAGN nitrogen content is high, and nitrogen exists in a manner of hydrazine, for propellant angle, in thermodynamics
On be advantageous；In addition, TAGN has good thermal stability, there is preferable compatibility with other components of propellant, using
Before can long term storage and never degenerate.
In the production and use process, synthesis and designer are highly desirable to the accurate purity of TAGN to instruct to synthesize and make
With.But in the prior art, the also no specific technical solution of the measuring method of purity accurate for triamido guanidine nitrate.
Summary of the invention
The purpose of the present invention is in view of the above shortcomings of the prior art, provide a kind of measurement side of triamido guanidine nitrate purity
Method, the measuring method is simple and easy, can carry out accurate quantitative analysis to the content of triamido guanidine nitrate.
Above-mentioned purpose of the invention is achieved through the following technical solutions:
A kind of measuring method of triamido guanidine nitrate purity comprising following steps:
1) decomposition of triamido guanidine nitrate: triamido guanidine nitrate sample is weighed, 250ml is settled to after dissolution, is quantitatively pipetted
Then 5.00ml sample is added excessive bromic acid potassium solution, reacts under certain acidity into conical flask, by triamido guanidine nitrate
Oxygenolysis generates N2And CO2, while obtaining solution A；
2) it consumes excessive potassium bromate: excessive potassium iodide being added into solution A and is reacted, solution B is obtained；
3) blank assay: will exist with bromic acid potassium solution same amount of in step 1) and with potassium iodide same amount of in step 2)
It is reacted under the conditions of certain acidity, obtains solution C；
4) it titrates: distinguishing titration solution B and solution C with sodium thiosulfate standard solution, starch indicator is added, titration is eventually
Solution is become colorless transparent by blue when point, records the volume V of the sodium thiosulfate standard solution of titration solution B consumption respectively1
With the volume V of the sodium thiosulfate standard solution of titration solution C consumption0；
5) the purity ω of triamido nitric acid.
The measuring method of triamido guanidine nitrate purity according to the present invention, in the step 1), the triamido
For the quality of guanidine nitrate sample between the range of 0.0001g-3.4792g, weighing need to be accurate to 0.1mg.
The concentration of the measuring method of triamido guanidine nitrate purity according to the present invention, the bromic acid potassium solution exists
Within the scope of 0.01mol/L-0.02mol/L.
The measuring method of triamido guanidine nitrate purity according to the present invention, in the step 1), the potassium bromate of addition
Molal quantity should control and pipetting 2 times of the molal quantity of the triamido guanidine nitrate into conical flask between 0.00083mol.
The measuring method of triamido guanidine nitrate purity according to the present invention in the step 1), is controlled molten with sulfuric acid
The acidity of liquid, addition acidity are c (1/2H2SO4The sulfuric acid of)=6mol/L, by the acidity c (H of solution+) control 3mol/L~
3.6mol/L。
The measuring method of triamido guanidine nitrate purity according to the present invention, the chemical reaction in the step 1) is such as
Under:
The measuring method of triamido guanidine nitrate purity according to the present invention, the chemical reaction in the step 2) is such as
Under:
BrO2-+5Br-+6H+=3Br2+3H2O
Br2+2I-=I2+2Br-。
The measuring method of triamido guanidine nitrate purity according to the present invention, in the step 4), the thiosulfuric acid
The concentration of sodium standard solution is 0.1mol/L.
The measuring method of triamido guanidine nitrate purity according to the present invention, in the step 4), in titration process,
When solution B and solution C by kermesinus take off be faint yellow when, add starch indicator, the chemical reaction of titration process is as follows:
2S2O3 2-+I2=S4O6 2-+2I-。
The measuring method of triamido guanidine nitrate purity according to the present invention, which is characterized in that in the step 5), root
The purity ω of triamido guanidine nitrate is calculated according to formula (1).
In formula:
The volume of the sodium thiosulfate standard solution of V0- titration solution C consumption, units/ml；
The volume of the sodium thiosulfate standard solution of V1- titration solution B consumption, units/ml；
The concentration of c- sodium thiosulfate standard solution, unit mol/L；
The molal weight of M- triamido guanidine nitrate, unit g/mol；
The quality of m- triamido guanidine nitrate sample, unit g.
Measuring method of the invention is simple and reliable, can carry out accurate quantitative analysis to the content of triamido guanidine nitrate, measurement
The relative standard deviation of the purity of triamido guanidine nitrate is less than 0.5%.
Specific embodiment
To keep the present invention easier to understand, elaborate below in conjunction with embodiment to the present invention.Following examples are only
To illustrative and not limiting technical solution of the present invention, repair according to actual needs not departing from any of spirit and scope of the invention
Change or refuse to replace, is intended to be within the scope of the claims of the invention.
Measuring method of the invention the following steps are included:
1) decomposition of triamido guanidine nitrate: accurately weighing sample, with water dissolution, is settled to 250ml, quantitatively pipettes 5.00ml
Sample is into 250ml conical flask；Excessive bromic acid potassium solution is added, adds the acidity c (H of sulfuric acid control solution+)=3mol/L~
3.6mol/L, close plug, adds aqueous to seal, and is stirred to react 10min, and triamido guanidine nitrate oxygenolysis is generated N2And CO2And solution A；
It chemically reacts as follows:
2) it consumes excessive potassium bromate: excessive potassium iodide being added into solution A, close plug adds aqueous to seal, and places in dark place anti-
5min is answered, following chemical reaction occurs, generates solution B；
BrO2-+5Br-+6H+=3Br2+3H2O
Br2+2I-=I2+2Br-。
3) blank assay: will exist with bromic acid potassium solution same amount of in step 1) and with potassium iodide same amount of in step 2)
It is reacted under the conditions of certain acidity, obtains solution C
4) titrate: distinguishing titration solution B and solution C using the sodium thiosulfate standard solution of 0.1mol/L, to solution by
Kermesinus takes off when being faint yellow, is separately added into 1ml starch indicator, and it is transparent that titration end-point is that solution is become colorless by blue；Point
Not Ji Lu titration solution B consumption sodium thiosulfate standard solution volume V1With the sodium thiosulfate mark of titration solution C consumption
The volume V of quasi- solution0；The chemical reaction of titration process is as follows:
2S2O3 2-+I2=S4O6 2-+2I-。
5) the purity ω of triamido guanidine nitrate is calculated according to formula (1).
In formula:
The volume of the sodium thiosulfate standard solution of V0- titration solution C consumption, units/ml；
The volume of the sodium thiosulfate standard solution of V1- titration solution B consumption, units/ml；
The concentration of c- sodium thiosulfate standard solution, unit mol/L；
The molal weight of M- triamido guanidine nitrate, unit g/mol；
The quality of m- triamido guanidine nitrate sample, unit g.
The arithmetic mean of instantaneous value being measured in parallel several times is as a result, relative error is no more than 0.5%.
Embodiment 1
The triamido guanidine nitrate sample 2.0122g that lot number is 201602 is weighed, constant volume is pipetted at 250ml aqueous solution
5.00ml sample solution is in 250mL conical flask, the accurate bromic acid potassium solution 35.00ml that 0.01667mol/L is added, after stirring
Sulfuric acid is added by the controlling pH of solution in c (H+)=3.2mol/L, close plug, adds aqueous to seal, and is stirred to react 10min, then plus
Enter 3g potassium iodide, close plug adds aqueous to seal, and reacts 5min in dark place, obtains solution B；Simultaneously by the potassium bromate of 0.01667mol/L
Solution 35.00ml and 3g potassium iodide is added in 250mL conical flask, and sulfuric acid is added by the controlling pH of solution in c (H+)=
3.2mol/L, close plug, adds aqueous to seal, and is stirred to react 5min in dark place and reacts 5min, obtains solution C.It is thio with 0.1mol/L
Sulfuric acid sodium standard solution titration solution B and solution C, when solution by kermesinus take off be faint yellow when, be separately added into 1ml starch instruction
Agent, titration end-point are become colorless for solution by blue transparent；The sodium thiosulfate standard solution of record titration solution B consumption respectively
Volume V1With the volume V of the sodium thiosulfate standard solution of titration solution C consumption0.Above-mentioned experiment repeats four groups.According to formula
(1) purity of triamido guanidine nitrate sample is calculated, the results are shown in Table 1.
Embodiment 2
The triamido guanidine nitrate sample 1.9583g that lot number is 201503 is weighed, other are counted with embodiment 1 according to formula (1)
The purity of triamido guanidine nitrate sample is calculated, the results are shown in Table 1.
Embodiment 3
Triamido guanidine nitrate coarse-grain 1# sample 2.2231g is weighed, other calculate triamido with embodiment 1, according to formula (1)
The purity of guanidine nitrate sample, the results are shown in Table 1.
Table 1
As it can be seen from table 1 can accurately measure the purity of triamido guanidine nitrate using method of the invention, and opposite
Standard deviation is lower than 0.5%.
The above, optimal specific embodiment only of the invention, but scope of protection of the present invention is not limited thereto,
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should be covered by the protection scope of the present invention.
The content that description in the present invention is not described in detail belongs to the well-known technique of professional and technical personnel in the field.
Claims (10)
1. a kind of measuring method of triamido guanidine nitrate purity comprising following steps:
1) decomposition of triamido guanidine nitrate: triamido guanidine nitrate sample is weighed, 250ml is settled to after dissolution, is quantitatively pipetted
Then 5.00ml sample is added excessive bromic acid potassium solution, reacts under certain acidity into conical flask, by triamido guanidine nitrate
Oxygenolysis generates N2And CO2, while obtaining solution A；
2) it consumes excessive potassium bromate: excessive potassium iodide being added into solution A and is reacted, solution B is obtained；
3) blank assay: will be with bromic acid potassium solution same amount of in step 1) and with potassium iodide same amount of in step 2) certain
It is reacted under acidity condition, obtains solution C；
4) it titrates: distinguishing titration solution B and solution C with sodium thiosulfate standard solution, be added starch indicator, when titration end-point
Solution become colorless by blue it is transparent, respectively record titration solution B consumption sodium thiosulfate standard solution volume V1 and drop
Determine the volume V0 of the sodium thiosulfate standard solution of solution C consumption；
5) the purity ω of triamido nitric acid.
2. the measuring method of triamido guanidine nitrate purity according to claim 1, which is characterized in that in the step 1),
For the quality of the triamido guanidine nitrate sample between the range of 0.0001g-3.4792g, weighing need to be accurate to 0.1mg.
3. the measuring method of triamido guanidine nitrate purity according to claim 1, which is characterized in that the bromic acid potassium solution
Concentration within the scope of 0.01mol/L-0.02mol/L.
4. the measuring method of triamido guanidine nitrate purity according to claim 1, which is characterized in that in the step 1),
The molal quantity of the potassium bromate of addition, which should control, is pipetting 2 times of the molal quantity of the triamido guanidine nitrate into conical flask extremely
Between 0.00083mol.
5. the measuring method of triamido guanidine nitrate purity according to claim 1, which is characterized in that in the step 1),
With the acidity of sulfuric acid control solution, addition acidity is c (1/2H2SO4The sulfuric acid of)=6mol/L, by the acidity c (H of solution+) control
In 3mol/L~3.6mol/L.
6. the measuring method of triamido guanidine nitrate purity according to claim 1, which is characterized in that in the step 1)
It chemically reacts as follows:
7. the measuring method of triamido guanidine nitrate purity according to claim 1, which is characterized in that in the step 2)
It chemically reacts as follows:
BrO2-+5Br-+6H+=3Br2+3H2O
Br2+2I-=I2+2Br-。
8. the measuring method of triamido guanidine nitrate purity according to claim 1, which is characterized in that in the step 4),
The concentration of the sodium thiosulfate standard solution is 0.1mol/L.
9. the measuring method of triamido guanidine nitrate purity according to claim 1, which is characterized in that in the step 4),
In titration process, when solution B and solution C by kermesinus take off be faint yellow when, add starch indicator, the change of titration process
It is as follows to learn reaction:
2S2O3 2-+I2=S4O6 2-+2I-。
10. a kind of measuring method of triamido guanidine nitrate purity according to claim 1 to 9, feature exist
In in the step 5), according to the purity ω of formula (1) calculating triamido guanidine nitrate:
In formula:
The volume of the sodium thiosulfate standard solution of V0- titration solution C consumption, units/ml；
The volume of the sodium thiosulfate standard solution of V1- titration solution B consumption, units/ml；
The concentration of c- sodium thiosulfate standard solution, unit mol/L；
The molal weight of M- triamido guanidine nitrate, unit g/mol；
The quality of m- triamido guanidine nitrate sample, unit g.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112326869A (en) * | 2020-09-25 | 2021-02-05 | 佛山市南海北沙制药有限公司 | Method for determining and identifying content of guanidine nitrate |
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