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Precise assay of TATB by the determination of total amino and nitro functional groups
Author(s) -
Rigdon L. P.,
Stephens F. B.,
Harrar J. E.
Publication year - 1983
Publication title -
propellants, explosives, pyrotechnics
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.56
H-Index - 65
eISSN - 1521-4087
pISSN - 0721-3115
DOI - 10.1002/prep.830080607
Subject(s) - tatb , chemistry , nitro , electrolyte , coulometry , chromatography , dissolution , saturated calomel electrode , nuclear chemistry , inorganic chemistry , electrode , electrochemistry , organic chemistry , working electrode , explosive material , alkyl , detonation
Methods have been developed for the precise assay of the explosive l,3,5‐triamino‐2,4,6‐trinitrobenzene (TATB) using procedures that quantitatively measure total nitro and/or total amino functional groups. The method for the determination of total nitro groups is based on the dissolution of TATB in DMSO‐NaOH, electrolytic reduction of ‐NO 2 to ‐NH 2 , and measurement by controlled‐potential coulometry. The reduction is carried out at a mercury pool electrode at −0.60 V versus standard calomel electrode (SCE) in a supporting electrolyte 1 M in H 3 PO 4 and 3 M in HClO 4 . Background corrections are low, and samples containing 0.1 mg to 2 mg of TATB per ml can be analyzed with a precision and accuracy of 0.25% to 0.5%. The method for determining total amino groups is based on the conversion of ‐NH 2 to NH 3 in a Kjeldahl‐type apparatus. The sample does not require an acid digestion step. The ‐ NH 2 groups are readily converted to NH 3 and distilled from a solution of NaOH and dimethylsulfoxide (DMSO). Individual samples of 120 mg‐170 mg of TATB can be conveniently assayed for amino groups with an accuracy and precision of about 0.25%.