Statistical optimization for determination of trace amounts of RDX in matrix of HMX using GC-ECD

Abstract

1,3,5,7-Tetranitro-1,3,5,7-tetrazocane (HMX) is one of the most powerful military explosives that is produced by means of Bechmann method. Simultaneous, 1,3,5-rinitroperhydro-1,3,5-triazine (RDX) as a by-product is produced in this method that affect on the purity and sensitivity of HMX. Using a simple and fast technique is important for determination of trace amounts of RDX in the HMX matrix. The technique of gas chromatography-electron capture detector (GC-ECD) was proposed for these reasons. Because the presence of several parameters in the proposed technique, the experimental design methods of factorial and central composite were used for the experiments of screening and optimization, respectively. The parameters of oven programming, injection volume, injection temperature, carrier gas flow rate, and detector temperature were used in experiments of screening. The analysis of variance and Pareto plots showed that the injection temperature and carrier gas flow rate must be optimized among the parameters. After the screening and optimization of the studied parameters, the selected conditions were oven programming 10 °C min −1 , injection volume 1 μL, injection temperature 250 °C, carrier gas (N 2 ) flow rate 3 mL min −1 , and detector temperature 300 °C. The calibration curve and detection limit of the optimized method were 10-90 and 1.8 mg L −1 , respectively, of RDX in matrix of HMX. The relative standard deviation of the measurement was 1.89%. Finally, the RDX recovery percentages in HMX matrix in the three spiked samples were also calculated.

Design of experiment techniques for the optimization of chromatographic analysis conditions: A review

“…There is no doubt that more attention should be shown on the applications of DoE on these aspects. Some examples of DoE techniques applied for the development of analysis method in GC, TLC, and HSCCC are listed in Table 4 [111][112][113][114][115][116][117][118][119][120][121].…”

Quantitative analysis of CL‐20 explosive by smartphone‐based chemiluminescence method

“…On the other hand, the pollution of water and wastewater and finally soil is significant in the process of explosives production [1]. Various methods have been used to determine explosives purity and trace amounts in natural samples that can be referred to gas chromatography (GC) [2], mass spectroscopy (MS) [3], high-performance liquid chromatography (HPLC) [4], thin layer chromatography (TLC) [5], ion mobility spectrometer (IMS) [6], voltammetry [7], luminescence (photo and chemiluminescence), and so on.…”

Study on the Thermal Stability of Octogen and other Energetic Materials (RDX, TNT, NQ, PBT, TDI and HTPB)

“…Due to the high mechanical sensitivity of HMX, in order to improve its safety, HMX was often mixed with many cladding materials to promote the safety of explosives, and has been widely used in the field of mixed explosives or propellants. The literatures [19][20][21][22][23][24][25][26][27] explored the effects of RDX, TNT, aluminized hydrides, TKX-50, CL-20 and other substances on the thermal safety, isothermal kinetics, explosion performance, thermal decomposition mechanism, sensitivity and mechanical properties of HMX. It was found that the properties of HMX alteration significantly in their mixtures.…”