Nuclear quadrupole resonance of explosives: Simultaneous detection of RDX and PETN in semtex

We have used nuclear quadrupole resonance (NQR) for the detection of¹⁴N in explosives and introduce a new method for the simultaneous detection of the explosives cyclotrimethylene trinitramine (RDX) and pentaerythritol tetranitrate (PETN). We have developed an interleaved pulse sequence, which provides efficient excitation of both RDX and PETN, to drive a solenoid coil that is doubly resonant at 3.41 and 0.89 MHz (suitable resonant frequencies of RDX and PETN, respectively). The excitation of RDX and PETN is carried out alternately within the pulse sequence via frequency hops in the spectrometer; no electronic switching is required to alternately returne the doubly resonant probe to the resonant frequency of each material. The signals from RDX and PETN, which are separated by about 2.52 MHz, are brought into the same audio window by mixing with a suitable intermediate frequency. We have tested the doubly resonant probe and interleaved pulse sequence on plastic formulations of RDX and PETN, on their own (PE-4 and Detasheet respectively) and as a mixture in Semtex.     

利用核四极矩共振技术探测炸药

介绍了用核四极矩共振的原理进行爆炸危险物品检测的方法及实验测试系统. 该系统运用特殊的激励信号来激发被检测样品中所含的特殊元素¹⁴N（炸药的主要成分）,使其产生核四极矩共振,并产生辐射,从而达到检测的目的. 由于该辐射信号的能量非常小(10 nV量级）,在通常的环境中很难检测该信号, 这就对此弱信号的检测和提取提出了很高的要求. 本测试系统使用了一系列有效的组合激励信号及弱信号采集、处理技术,在通常环境中成功地检测到了RDX（黑索金）信号.     

NQR炸药探测系统中射频线圈的设计研究

基于核四极矩共振(Nuclear Quadrupole Resonance, NQR)炸药探测原理,对探测系统中拾取信号的关键部件射频线圈进行了优化设计,并确定了小型螺线管型线圈的直径、长度和匝数. 试验测试表明,此线圈射频场均匀性好、信噪比大、灵敏度高,可以快速准确探测到NQR信号,验证了线圈设计理论的有效性和制作方法的可行性. 该设计方法对提高隐藏炸药探测的准确率以及不同试验条件下射频线圈的设计具有重要意义.     

A study of continuous-wave two-frequency NQR

A simple continuous-wave parallel to pulse version of a multifrequency nuclear quadrupole resonance (NQR) device was constructed and tested: two orthogonal radio-frequency (RF) fields were applied simultaneously at two suitable frequencies to a multilevel quadrupole probe (I⋝1). A modified superregenerative NQR oscillator-detector (SRO) was utilized. An additional coil and RF source were used to irradiate the sample at the second frequency. After tuning the SRO to a chosen NQR line, the signal proportional to the population difference of the corresponding pair of energy levels was monitored. When another suitable transition was saturated simultaneously, sharing one level with the monitored line, the corresponding population change was also reflected in the first signal intensity change. The phenomenon was examined for Sb nuclei in Sb₂S₃ powder at room temperature.     

Factors affecting the NQR line width in nitramine explosives

A number of factors associated with crystal quality contribute to the nuclear quadrupole resonance (NQR) line width. Imperfections such as dislocations, voids, strain and impurities can be electrical sources that distort the electric field gradient at nearby quadrupolar nuclei and broaden the observed NQR line. We measured the¹⁴N NQR line widths in powdered samples of the nitramine explosives hexahydro-1,3,5-trinitro-s-triazine (RDX), octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX) and 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane and show correlations with sample purity, particle size distribution and density. Cast plastic-bonded explosives containing either RDX or HMX were also studied and their line widths compared with those of the powdered samples.     

核四极共振隐藏炸药探测信息库设计

利用核四极共振(Nuclear Quadrupole Resonance, 简称NQR)技术探测炸药时,实验复杂,参数繁多. 原子核参数、脉冲参数、环境参数等各参数对炸药共振频率及探测信噪比都有不同程度的影响. 针对长期以来国内外一直没有统一的炸药信息库,测试数据无法有效记录和管理的现象,在全面分析各参数与共振频率之间关系的基础上,设计并实现了隐藏炸药探测信息库. 该信息库能有效的收集和记录炸药参数信息,为今后炸药测试数据的统计分析提供统一规范的数据支持.      

Feedback optimization of pulse width in the SORC sequence.

A method for increasing the signal-to-noise ratio (SNR) of nuclear quadrupole resonance (NQR) measurements by automatically adjusting a pulse parameter in real-time is presented. This approach is useful in situations where the optimal pulse parameters cannot be chosen beforehand due to lack of knowledge regarding the system. For example, NQR provides a means for detecting explosives by revealing the presence of (14)N. In this particular application, the distance between the search coil and the explosive, as well as the temperature of the explosive, is unknown. As a result, a fixed set of pulse parameters will not yield the largest SNR for all possible search applications. This paper describes a feedback algorithm that uses measurements of the NQR signal to automatically adjust the pulse width in the strong off-resonant comb sequence to maximize the SNR of the NQR measurement. Experimental results obtained using a sample of sodium nitrite are presented.     

Effect of <Superscript>14</Superscript>N Nucleus Capture in Nuclear Quadrupole Resonance at Small Relaxation Parameters

Experiments on detecting induction signals of nuclear quadrupole resonance (NQR) on ¹⁴N nuclei in hexahydro-1,3,5-trinitro-s-triazine C₃H₆N₆O₆ (RDX) with preliminary changed population densities of NQR energy levels upon exposure to a saturating pulse are described. It is demonstrated that this actually causes the induction signal amplitude to change; however, complete saturation of the transition cannot be reached because of the NQR relaxation time. It is also demonstrated that the results of calculations without regard for the relaxation processes in RDX lack experimental support. Experimental data demonstrate the feasibility of application of the methods of preliminary change of the population densities (by pumping) for multifrequency experiments in NQR and explosive detection.__________Translated from Izvestiya Vysshikh Uchebnykh Zavedenii, Fizika, No. 4, pp. 49–52, April, 2005.     

NQR Characteristics of an RDX Plastic Explosives Simulant

For reliable detection of explosives, a combination of methods integrated within a single measurement platform may increase detection performance. However, the efficient field testing of such measurement platforms requires the use of inexplosive simulants that are detectable by a wide range of methods. Physical parameters such as simulant density, elemental composition and crystalline structure must closely match those of the target explosive. The highly discriminating bulk detection characteristics of nuclear quadrupole resonance (NQR) especially constrain simulant design. This paper describes the development of an inexplosive RDX simulant suited to a wide range of measurement methods, including NQR. Measurements are presented that confirm an RDX NQR response from the simulant. The potential use of the simulant for field testing a prototype handheld NQR-based RDX detector is analyzed. Only modest changes in prototype operation during field testing would be required to account for the use of simulant rather than real explosive.     

New Methods for Detection of 14N NQR Frequencies

Nitrogen atoms are present in a number of solid explosives and illicit substances. The nuclear quadrupole resonance (NQR) spectra and spin?Clattice relaxation of the nitrogen atomic nucleus ¹⁴N can be used to characterize these compounds and to distinguish between possible crystal polymorphs. After the characteristic ¹⁴N NQR frequencies and spin?Clattice relaxation rates in a compound are determined, NQR can be used to detect this compounds and, in case of crystal polymorphs, also to determine the method of preparation. The ¹⁴N NQR frequencies and spin?Clattice relaxation rates are measured either by pulse NQR or by nuclear quadrupole double resonance (NQDR) based on magnetic field cycling. Here, we discuss several ¹H?C¹⁴N NQDR techniques which can be used to measure the ¹⁴N NQR frequencies and spin?Clattice relaxation rates under various experimental conditions. Some characteristic applications of these techniques are presented and discussed in details.     

Nuclear Quadrupole Interactions in Nuclear Quadrupole Resonance Detection of Energetic and Controlled Materials: Theoretical Study

There has been a growing interest in nuclear quadrupole resonance (NQR) techniques useful for the detection of explosives and drugs in solid state systems. This paper uses the first-principles one-electron Hartree?CFock theoretical method to study the nuclear quadrupole interaction parameters e ² qQ and ?? for the ¹⁴N nuclei in the explosives RDX and ??-HMX as well as the drugs cocaine and heroin. It has been found in our earlier published investigations reviewed here that there is very good agreement for our calculated e ² qQ and ?? for ¹⁴N, for all these four systems, and experiment. We also present our unpublished theoretical results for cocaine with an HCl molecule attached. We successfully explain quantitatively the drastic decrease in e ² qQ in going to cocaine-HCl from cocaine-free base as well as the observed substantial increase in ?? and discuss the implications of these dramatic changes for NQR detection in general.     

<Superscript>14</Superscript>N Nuclear Quadrupole Resonance Study of Polymorphism in Trinitrotoluene Samples Obtained from Old Ordnances

The field application of a ¹⁴N nuclear quadrupole resonance (NQR) detector needed for the detection of different explosives, including trinitrotoluene (TNT), requires the examination of the distribution of ¹⁴N NQR lines stemming from the monoclinic and/or orthorhombic modifications of TNT, as well as from a mixture of both. In this work, 30 different TNT samples up to 70 years old were measured. The main result of this study is that the measured ¹⁴N NQR spectrum is strongly influenced by the environmental conditions to which the explosive was subject during its history.     

Application of the Wavelet Transform for Detecting Signals of Nuclear Quadrupole Resonance

In the present study, the wavelet transform is used to increase the signal-to-noise ratio of nuclear quadrupole resonance (NQR) signals in the direct pulse method. The efficiency of the wavelet and Fourier transforms used for detecting the NQR signal component is compared. The signal consists of noise, magnetoacoustic and piezoelectric signals, noise from external sources, and NQR signal. Signals from ¹⁴ N nuclei in hexahydro-1,3,5-trinitro-s-triazine C₃H₆N₆O₆ (RDX) are investigated at a temperature of 298 K.__________Translated from Izvestiya Vysshikh Uchebnykh Zavedenii, Fizika, No. 1, pp. 47–50, January, 2005.     

一种改进的微弱NQR信号检测算法

核四极矩共振（NQR）是一种固态射频谱分析技术,可用于检测高危险爆炸物. 然而NQR信号本身非常弱,并且易受线圈的热噪声和外部射频干扰的影响,低信噪比限制了NQR的实际应用. 该文提出一种改进的微弱NQR信号检测算法. 首先利用Hankel矩阵方式下奇异值分解的方法,有效地抑制射频干扰和噪声,并将NQR信号分离出来. 然后提出了一种基于MUSIC谱估计的非线性最小二乘检测器,它既保证了高的频率分辨率,又大大降低了运算量. 仿真数据和实测数据结果表明该算法的有效性.     

The two-frequency nuclear quadrupole resonance for explosives detection

The two-frequency nuclear quadrupole resonance (NQR) of¹⁴N nuclei is described for purposes of explosives detection. Two applications are known: two-frequency NQR for increasing the signal intensity, two-frequency NQR for improved reliability of explosives detection. The two-frequency experiments were carried out in hexahydro-1,3,5-trinitro-s-triazine C₃H₆N₆O₆ and sodium nitrite NaNO₂ as a substitute for octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocycine C₄H₈N₈O₈. The two-frequency sequences for NQR are proposed for increasing the amplitude of NQR signal and improvement of detection condition.     

Temperature dependence of17O and14N NQR frequencies in commercial TNT

The temperature dependence of the¹⁷O nuclear quadrupole resonance (NQR) frequencies has been measured in commercial trinitrotoluene by highly sensitive nuclear quadrupole double resonance techniques. The¹⁴N NQR frequencies have been measured in the same sample for comparison. In contrast to the¹⁴N quadrupole coupling constant, the¹⁷O quadrupole constant increases with increasing temperature.     

Application of the spherical tensor method for Two-Frequency pure NQR of spinI=1 nuclei

The results of a theoretical investigation of two-frequency excitation in pure nuclear quadrupole resonance (NQR) for a spinI=1 nucleus with a nonaxial elecric field gradient are presented. The multipole tensor operator technique is used for the treatment of the one- and two-frequency pulse excitations. The results are applied to the characterization of the two-frequency signal of nitrogen¹⁴N nuclei. The experiments on sodium nitrite, NaNO₂, confirm the presence of additional (two-frequency) echo in the NQR signal. The effect of resonance offsets on two-frequency NQR is also considered.     

Circularly Polarized RF Magnetic Fields for Spin-1 NQR

The low sensitivity of nuclear quadrupole resonance (NQR) of powders is due, in part, to the inability to efficiently excite and detect nuclei at all crystal orientations. Here we describe the use of circularly polarized RF magnetic fields for excitation followed by detection of the resultant circular RF magnetization in I=1 NQR to increase the fraction of nuclei excited and detected. We show that the technique can greatly improve the effective RF field homogeneity and increase the largest signal amplitude by a factor of 1.72. In favorable cases, the resulting circularly polarized NQR signal can be separated from linearly polarized magnetoacoustic and piezoelectric ringing artifacts that occur in some NQR materials detection applications.     

相位可控的核四极矩共振激励脉冲发生器设计

在核四极矩共振（NQR）领域,射频激励脉冲信号的优劣对NQR响应信号有重要影响.针对常规方法中射频激励脉冲参数不可控的问题,本文基于32位闪存微型控制器STM32和直接数字频率合成（DDS）芯片AD9910设计了一种相位可控激励脉冲发生器.采用STM32控制AD9910产生波形参数（脉冲宽度、脉冲间隔、脉冲个数和共振频率等）可控的射频激励脉冲,利用LabVIEW软件平台设计脉冲参数设置界面,并建立计算机与微控制器通信,实现波形参数的精确优化控制.实验结果表明,该方法实现了相位可控的NQR激励脉冲序列,可为后续NQR信号检测提供有效激励源.     

Improving N nuclear quadrupole resonance detection of trinitrotoluene using off-resonance effects

The off-resonance dependence of the amplitudes of the six dominant ¹⁴N nuclear quadrupole resonance (NQR) lines in commercial polymorphic trinitrotoluene (TNT) sample were experimentally determined for a wide range of experimental parameters when irradiated with the spin-lock spin-echo (SLSE) pulse sequence. We find that the amplitudes off-resonance dependence follows a sinc-like function with an additional modulation due to the spacing between the RF pulses. This dependence can be very well modeled with expressions we have derived for a single site ¹⁴N NQR in paranitrotoluene (PNT). The results can be immediately used for the reduction of the number of free parameters used in the robust signal processing models for the TNT NQR detectors.