Titrimetric Determination of Hexahydro-1,3,5-trinitro-<i>s</i>-triazine (RDX) and Octahydro-1,3,5,7-tetranitro-<i>s</i>-tetrazine (HMX) with Ferrous Sulfate

Simecek, Jaromir.

doi:10.1021/ac60170a032

Cited by 10 publications

(2 citation statements)

References 13 publications

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“…RDX and HMX were determined by titrimetric methods with ferrous sulfate. But the dependence of the amount of HNO 3 yielded from RDX on RDX concentration in 97.5% H 2 SO 4 and on the size of the RDX crystals are limiting this method (5) . A chromatographic (2) and an infrared method (1) have been described, but they are of limited use.…”

Section: Introductionmentioning

confidence: 99%

Determination of Binary Mixtures of Nitramines by aSpectrophotometric Method Using Partial Least SquaresMultivariate Calibration

Chaloosi

Gholamian

Zarei

2001

Propellants Explos. Pyrotech

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The UV‐absorption spectra of cyclo‐1,3,5‐trimethylene‐2,4,6‐trinitramine (RDX) and cyclo‐1,3,5,7‐tetramethylene‐2,4,6,8‐tetranitra mine (HMX) are strongly overlapping and do not allow their direct determination without previous separation by conventional methods. A partial least squares method (PLS) in a multicomponent analysis provides a sensitive and accurate technique for the analysis of complex mixtures with strong overlapping spectra. The experimental calibration matrix was designed with 15 samples. The concentration varied between 0.584 μg/ml and 10.220 μg/ml for HMX, and between 0.400 μg/ml and 8.000 μg/ml for RDX. The cross‐validation method was used to select the number of factors. To check the accuracy of the proposed method, the optimized model obtained by using PLS‐2 was applied to the determination of these compounds in industrial samples.

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Section: Introductionmentioning

confidence: 99%

Determination of Binary Mixtures of Nitramines by aSpectrophotometric Method Using Partial Least SquaresMultivariate Calibration

Chaloosi

Gholamian

Zarei

2001

Propellants Explos. Pyrotech

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“…Thus, nitrolysis of trans -3,7-diacetyl-5-(difluoramino)-9-oxa-3,7-diazabicyclo[3.3.1]nonan-1-ol produced an unprecedented nitrate ester of a hemiacetal, 5-(difluoramino)-3,7-dinitro-9-oxa-3,7-diazabicyclo[3.3.1]non-1-yl nitrate, which underwent slow spontaneous elimination of NO 2 after workup. Difluoramination of the nitro-protected diazocine under conventional conditions allowed the formation of desired nitramine 1 , but the yield was quite poor (∼1% in the last step) due to the known instability of nitramines in strong nonnitrating acids …”

Section: Introductionmentioning

confidence: 99%

Difluoramination of Heterocyclic Ketones: Control of Microbasicity

1998

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Difluoramination of a tetrahydro-1,5-diazocine-3,7(2H,6H)-dione to the corresponding 3,3,7,7-tetrakis(difluoramino)diazocine was achieved by a judicious choice of protecting group. Arenesulfonyl protecting groups for the diazocine nitrogens proved superior to acetyl during the slow disruption of the transannular bridge in 9-oxa-3,7-diazabicyclo[3.3.1]nonane intermediates by difluorosulfamic acid. While a 1,5-ditosyl derivative failed to proceed beyond the product of addition of difluoramine to one ketone carbonyl (hemiaminal 6), the use of 4-nitrobenzenesulfonyl as the protecting groups lowered the nitrogens' basicities below that of the oxygen site in the dione and intermediates, allowing the reaction to proceed to a gem-bis(difluoramino)diazocine product (11). A safer procedure for handling difluoramine is described.

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Semimicro spectrophotometric determination of RDX and HMX

Norwitz

Galan

1969

Microchemical Journal

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Titrimetric Determination of Hexahydro-1,3,5-trinitro-s-triazine (RDX) and Octahydro-1,3,5,7-tetranitro-s-tetrazine (HMX) with Ferrous Sulfate

Cited by 10 publications

References 13 publications

Determination of Binary Mixtures of Nitramines by aSpectrophotometric Method Using Partial Least SquaresMultivariate Calibration

Determination of Binary Mixtures of Nitramines by aSpectrophotometric Method Using Partial Least SquaresMultivariate Calibration

Difluoramination of Heterocyclic Ketones: Control of Microbasicity

Semimicro spectrophotometric determination of RDX and HMX

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