Improvement of extraction efficiency for spectrophotometric determination of NO3- and NO2- in Gunshot residues; An application for a shooting distance study

Thanakorn Pluangklang; Areerut Rimmai; Kanchana Sermsaeng; Sirinapa Noibungkha; Charoensak Lao-ngam; Laddawan Chonsalasin

doi:10.14456/nujst.2018.5

Authors

Thanakorn Pluangklang Chemistry Program, Faculty of Science and Technology, Nakhon Ratchasima Rajabhat University
Areerut Rimmai Police forensic Science Center 3, Royal Thai Police
Kanchana Sermsaeng Police forensic Science Center 3, Royal Thai Police
Sirinapa Noibungkha Police forensic Science Center 3, Royal Thai Police
Charoensak Lao-ngam Chemistry Program, Faculty of Science and Technology, Nakhon Ratchasima Rajabhat University
Laddawan Chonsalasin Chemistry Program, Faculty of Science and Technology, Nakhon Ratchasima Rajabhat University

DOI:

https://doi.org/10.14456/nujst.2018.5

Keywords:

Extraction, NO3- and NO2-, Gunshot residues

Abstract

This research studied parameters affecting the extraction efficiency of NO₃^-and NO₂^- from gunshot residue samples (GSRs). The spectrophotometric determination of NO₃^-and NO₂^- was carried out using the principle of a Griess reaction. For this work, both sampling and extraction parameters were investigated before selecting the optimal condition for a study of shooting distance. The results showed that a mixed solution of 1% Sulfanilamide and 1% N-(1-Naphthyl) ethylene diamine (NED) in 0.5 molL^-1 HCl (Griess reagent) and 30 min reaction time provided good sensitivity for the determination of NO₂^- at 540 nm. In the case of NO₃^-, 1% VCl₃ in Griess reagent was used to reduce NO₃^- to NO₂^- before analysis with the same principle. The optimal condition for a sampling procedure used 150 µL of room temperature deionized water per cotton brush swab for two replicated GSR collections. Samples were stored for 1 week before analysis could be carried out at 4 ^OC in a refrigerator or at room temperature without significantly different results. On the other hand, 4 mL of room temperature deionized water with and without ultrasonic extraction times of 5 or 30 min respectively were the selected parameters for NO₂^-and NO₃^- extraction from GSRs.
The proposed method could be applied completely for spectrophotometric determination of NO₃^-and NO₂^- in GSRs. The limits of detection (LOD) of NO₂^- and NO₂^- + NO₃^- were 0.27×10^-6 and 3.58×10^-6molL^-1 respectively with a relative standard deviation of the given slope. A wide linearity range between 2.17×10^-6to 217×10^-6molL^-1 was obtained and a percentage of recovery in the range of 96.24 – 102.32 and 98.04 – 105.96 for NO₃^- and NO₂^-was achieved, respectively. This method can be performed for determination of NO₃^- and NO₂^-content at a maximum 304.8 centimeter shooting distance. From these findings, the proposed sampling, extracting and determining methods for NO₃^-and NO₂^- in GSRs are highly sensitive, precise, robust, simple and inexpensive, with a short analysis time and provide a useful alternative procedure for analytical chemists or forensic scientists in their work.

Keywords:, , Gunshot residues

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