Quantitative analysis method for ammonium dinitramide in ammonium dinitramide aqueous solution or solid
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A technique for ammonium dinitramide and quantitative analysis, applied in the field of quantitative analysis of ammonium dinitramide
Inactive Publication Date: 2021-05-25
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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[0004] The quantitative detection methods of ADN include empirical density method, UV ultraviolet spectrophotometer method, ion chromatography, etc., but the above
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Embodiment 1
[0057] The method of step 1 was adopted: chromatographic column AS-22; column temperature 30°C; suppressor model AMMS 3004mm; conductivity detector. The sample volume for each injection was 25 μL.
[0058] Gradient elution, the eluent flow rate is 1.20mL / min; eluent A: 4.5mmol Na 2 CO 3 +1.4mmol NaHCO 3 Aqueous solution; eluent B: acetonitrile (chromatographically pure); ion chromatography gradient elution detection procedure is:
[0059] Initial stage: from 0 min to 12 min, pass 100% eluent A;
[0060] Intermediate stage: from the 12th minute to the 22nd minute, start to pass 70% V / V eluent A+30% V / V eluent B;
[0061] The next stage: after the end of the intermediate stage: through 100% eluent A; the measurement program stops after 35 minutes;
[0062] Carry out nitrate, sulfate radical standard curve drawing by above ion chromatographic conditions, concrete data is as shown in table 1, and the standard curve figure and standard curve regression equation of nitrate and ...
Embodiment 2
[0083] Using the same nitrate and sulfate standard curves and regression equations as in Example 1, the concentrations prepared by the mixed acid nitration method are respectively estimated to be about 3 kinds of ADN sample solutions of 10wt%, 20wt% and 40wt% according to the above-mentioned measurement conditions. Test, the assay results of nitrate and sulfate are shown in Table 7 and Table 8 respectively.
[0086] Table 8 Sulfate concentration determination result
[0087]
[0088]
[0089] As in Example 1, the detected metal ion content was extremely low, so it was ignored.
[0090] Weigh a certain amount of ADN sample solution, add 10mL neutral formaldehyde solution, let stand for 5 minutes, add 1 drop of phenolphthalein indicator, titrate with 0.1011mol / L sodium hydroxide standard solution, titrate the solution to pink as the titration end point, record Consumed volume of sodium hydroxide, whil...
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Abstract
The invention discloses a quantitative analysis method for the content of ADN in an ammonium dinitramide (ADN, NH4N (NO2) 2) aqueous solution or solid. The method includes: detecting the content of sulfate radical (SO4 < 2->) and nitrate radical (NO3 <->) impurities in the ADN sample through an ion chromatography method; detecting the content of metal ions (K < + >, Na < + >, Ca < 2 + > and Mg < 2 + >) in the sample through an ICP method; detecting the content of total ammonium ions (NH4 +) in the sample by a formaldehyde-acid-base titration method; and calculating the content of dinitramide ions (N (NO2) 2-) in the sample according to the balance of anions and cations in the solution. If N (NO2) 2-anions correspond to NH4 + cations, calculating the content of ADN in the sample. The method effectively avoids the problem that no commercially available ADN standard sample is available for quantitative detection, initiates an analysis method capable of accurately quantifying the ADN component in the ADN sample without the ADN standard sample, and can effectively meet the quantitative detection requirement of the ADN content in the ADN product.
Description
technical field [0001] The invention relates to a quantitative analysis method of ammonium dinitramide in aqueous solution and ammonium dinitramide in solid. It is mainly used for quantitative analysis and detection of ADN content in ADN aqueous solution and ADN solid product. Background technique [0002] Ammonium dinitramide is a new type of high-energy ionic liquid energy material, which has the advantages of high energy, stable and rapid decomposition, complete combustion without residue, clean exhaust, large gas generation, low signal characteristics and non-toxicity. It can be used as a green propulsion material in the auxiliary power field of civil aerospace and aviation to meet its non-toxic application requirements. At the same time, it can be used as a material for gas generators, ionic liquid explosives, solid explosives, low-signature high-energy oxidants, and synthetic raw materials for other high-energy ionic liquids, and has high application value. [0003] ...
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IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/047G01N2030/8859
Inventor 丛伟民王晓东王雅彬夏连根张万生
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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