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Determination method of monoaminoguanidine nitrate and diaminoguanidine nitrate content

A guanidine nitrate and determination method technology, applied in the fields of chemistry and chromatographic analysis, can solve problems such as inability to obtain target component standard samples, and achieve the effects of being easy to popularize and use, widely used in instruments, and accurate in detection results

Active Publication Date: 2022-04-12
HUBEI INST OF AEROSPACE CHEMOTECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to overcome the deficiencies in the prior art, the present inventor has carried out testing method research, has provided a kind of content assay method of MAGN and DAGN in measuring TAGN, and it can avoid impurity interference and can't obtain the problem of target component standard sample, effectively Improve the accuracy and stability of sample test results and reduce data processing errors

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  • Determination method of monoaminoguanidine nitrate and diaminoguanidine nitrate content
  • Determination method of monoaminoguanidine nitrate and diaminoguanidine nitrate content

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Step 1. Preparation of test sample solution: Weigh 0.0416g of TAGN sample raw material, dissolve it in a 100mL volumetric flask, dissolve it with ultrapure water and sonicate for 30min, and wait until the sample solution is completely clear and transparent, let it stand to constant volume. Form the sample solution to be tested, and its concentration is respectively 4.16×10 -4 g / mL, filtered through a 0.22μm pore needle filter.

[0036]Step 2, determine the detection conditions: the sample solution is determined by ion chromatography, and the chromatographic separation conditions are: IonPac CS12A cation exchange analysis column, the inner diameter of the particles is 5 μm, the inner diameter of the chromatographic column is 3 mm, and the column length is 150 mm. IonPac CG12A guard column 4×50mm. Methanesulfonic acid eluent, the concentration is 20mMol, the column temperature is 35°C, the flow rate is 0.8mL / min, the injection volume is 25μL, the conductivity detector, t...

Embodiment 2

[0042] Step 1, prepare test sample solution: Weigh 7 parts of TAGN sample raw materials, and the prepared concentration is 4.16×10 -4 g / mL, 4.07×10 -4 g / mL, 5.19×10 -4 g / mL, 3.25×10 -4 g / mL, 4.21×10 -4 g / mL, 6.17×10 -4 g / mL, 6.25×10 -4 g / mL sample solution, dissolved in ultrapure water and sonicated for 30 minutes, after the sample solution is completely clear and transparent, let stand to constant volume. Filter with a needle filter head with a pore size of 0.22 μm.

[0043] Step 2, determine the detection conditions: the sample solution is determined by ion chromatography, and the chromatographic separation conditions are: IonPac CS12A cation exchange analysis column, the inner diameter of the particles is 5 μm, the inner diameter of the chromatographic column is 3 mm, and the column length is 150 mm. IonPac CG12A guard column 4×50mm. Methanesulfonic acid eluent, the concentration is 50mMol, the column temperature is 35°C, the flow rate is 1.2mL / min, the injection vol...

Embodiment 3

[0051] Step 1. Preparation of test sample solution: Weigh 0.0416g of TAGN sample raw material, dissolve it in a 100mL volumetric flask, dissolve it with ultrapure water and sonicate for 30min, and wait until the sample solution is completely clear and transparent, let it stand to constant volume. The solution to be tested is formed, and its concentration is 4.16×10 -4 g / mL, filtered through a 0.22μm pore needle filter.

[0052] Step 2, determine the detection conditions: the sample solution is determined by ion chromatography, and the chromatographic separation conditions are: IonPac CS12A cation exchange analysis column, the inner diameter of the particles is 5 μm, the inner diameter of the chromatographic column is 3 mm, and the column length is 150 mm. IonPac CG12A guard column 4×50mm. Methanesulfonic acid eluent, the concentration is 20mMol, the column temperature is 35°C, the flow rate is 0.8mL / min, the injection volume is 25μL, the conductivity detector, the test curren...

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Abstract

The invention provides a method for determining the content of monoaminoguanidine nitrate and diaminoguanidine nitrate, comprising: preparing a detection sample solution: fully dissolving a sample containing triaminoguanidine nitrate TAGN with water to form a detection sample solution; Conditions: Use an ion chromatography system, use a cation exchange analytical column for component separation, column temperature 20-40°C, methanesulfonic acid as eluent, flow rate 0.8-1.2mL / min, injection volume 5-25μL, use Conductivity detector; content determination: test under determined detection conditions, separate and obtain monoaminoguanidinium ions, diaminoguanidinium ions and triaminoguanidinium ions, and quantify by external standard method, and obtain monoaminoguanidine after conversion Content of nitrate MAGN and diaminoguanidine nitrate DAGN. The invention realizes the determination of the content of MAGN and DAGN in TAGN, has the advantages of good repeatability of detection data, accurate and reliable data processing, and provides technical support for controlling the quality of TAGN products.

Description

technical field [0001] The invention relates to the field of chromatographic analysis in the chemical field, in particular to a method for determining the content of monoaminoguanidine nitrate (MAGN) and diaminoguanidine nitrate (DAGN) in triaminoguanidine nitrate (TAGN). Background technique [0002] Triaminoguanidine nitrate TAGN is an important gas generating agent raw material, and impurities such as monoaminoguanidine nitrate MAGN and diaminoguanidine nitrate DAGN in triaminoguanidine nitrate TAGN may seriously affect the product quality of the gas generating agent ( Ao Guojun, Liu Zhenhua, Zhang Tonglai, Yang Li, Zhang Jianguo. Research Progress of Triaminoguanidine Series Energetic Compounds [J]. Energetic Materials, 2008, 16(4): 450-457.). Therefore, it is necessary to control the purity of TAGN and the content of impurities such as MAGN and DAGN. Although the chemical analysis method, carbon, hydrogen, oxygen and nitrogen element analysis method and melting point d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/60G01N30/64G01N30/96
CPCG01N30/02G01N30/06G01N30/60G01N30/64G01N30/96G01N2030/645G01N2030/047
Inventor 聂海英韦雪梅刘治国赵华丽刘梦梅鹏程安百强徐娜郭滢媛
Owner HUBEI INST OF AEROSPACE CHEMOTECHNOLOGY