CA2113558C - Detection of explosive and narcotics by low power large sample volume nuclear quadrupole resonance (nqr) - Google Patents

Detection of explosive and narcotics by low power large sample volume nuclear quadrupole resonance (nqr)

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Publication number
CA2113558C
CA2113558C CA 2113558 CA2113558A CA2113558C CA 2113558 C CA2113558 C CA 2113558C CA 2113558 CA2113558 CA 2113558 CA 2113558 A CA2113558 A CA 2113558A CA 2113558 C CA2113558 C CA 2113558C
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Prior art keywords
coil
specimen
strength
magnetic field
train
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Expired - Lifetime
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CA 2113558
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French (fr)
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CA2113558A1 (en
Inventor
Michael L. Buess
Allen N. Garroway
Joel B. Miller
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US Department of Navy
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US Department of Navy
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Priority claimed from US07/730,722 external-priority patent/US5233300A/en
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Publication of CA2113558C publication Critical patent/CA2113558C/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01RMEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R33/00Arrangements or instruments for measuring magnetic variables
    • G01R33/20Arrangements or instruments for measuring magnetic variables involving magnetic resonance
    • G01R33/44Arrangements or instruments for measuring magnetic variables involving magnetic resonance using nuclear magnetic resonance [NMR]
    • G01R33/441Nuclear Quadrupole Resonance [NQR] Spectroscopy and Imaging

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Geophysics And Detection Of Objects (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)

Abstract

The sensitive detection of explosives and narcotics by nuclear quadrupole resona nce (NQR) is performed at low rf power by assuring that the rf field strength is larger than the local magnetic field. Additionally, it has been recognized that signal-to-noise ratio of a signal induced by a specimen of fixed size decrease b y only the square root of the coil size. Thus, rather than scaling power linearly with coil size, as conventionally done to maintain the sa me rf field intensity, the power needs only be increased by the square root of the increased coil size to assure maintenance of the same signal to noise ratio. This technique permits the use of larger coils than previously used. The invention is useful fo r both volume coils and surface coils.

Description

W093/02~5 2 1 1 3 5 S S PCT/US92/03117 .,~. 1 DETECTION OF EXPLOSIVE AND NARCOTICS BY LOW POWER LARGE
5 SAMPLE VOLUME NUCLEAR QUADRUPOLE RESONANCE (NQR) Background of the Invention Field of the Invention The present invention is directed generally to a method and an improved system for detecting nitrogenous explosives or narcotics by nuclear quadrupole resonance (NQR), and more specifically, to a lower power method for detecting those materials.
Description of the Prior Art In order to limit the unrestricted flow of explosives and narcotics, it is desired to detect sub-kilogram quantities of those materials in monitoring stations. Most military explosives and narcotics share common features: they are crystalline solids containing nitrogen. Presently, the explosive detections system and methods cannot reliably detect sub-kilogram quantities of military explosives against a background of more benign materials. In conventional vapor-based systems, dynamites and contaminated explosives may be detected. However, military explosives such as hexhydro-1,3,5-trinitro-s-triazene (commonly referred to as RDX and 2,2-bis[(nitroxy)methyl]-1,3-propanediol, dinitrate (commonly referred to as PETN) are not reliably detected by the conventional vapor base systems especially when countermeasures are taken to reduce the effluent vapor and particles. Thermal neutron systems, which are 14N detectors, can detect relevant quantities of explosives. Unfortunately, conventional thermal neutron analysis systems frequently alarm on nitrogen-containing plastics. High false alarm rates are produced for inspected bags containing a few bomb equivalents of nitrogen in a benign form since the conventional thermal neutron analysis systems are sensitive only to the nuclear cross sections and not to any details of the particular chemical SUBSTITUTE SHEET

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environment of the ~etecte~l nitrogen nuclear. Hence the false alarm rate is inherently high, even with some spatial discrimination. Also, nuclear magnetic resonance (NMR) has been considered for ~etecting explosives. Because a large magnetic field is conventionally required for NMR, m~gn~tically recorded data would be undesirable altered and other m~gnPti7~kle 5 materials could be damaged. Furthermore, the conventional non-vapor methods and systems are not suitable for inspect*ng people.
Buess et al., U.S. Patent 5,206,592, DETECTION OF EXPLOS~VES BY NUCLEAR
QUADRUPOLE RESONANCE, discloses a method and system for NQR detection of explosives. Recited advantages of NQR for explosives detection are:
(i) Specificity: the NQR resonant frequency of a quadrupolar nucleus in a crystalline solid is quite well-defined. Most explosives of interest conta*n nitrogen and are crystalline solids. Most nitrogen found in the contents of airline bags is in a polymeric form, with associated broad, weaker NQR resonances and generally at frequencies other than the characteristic frequencies of the explosive. NQR is sensitive to the rllemir~l structure, rather 15 than just the nuclear cross-section, as in the thermal neutron analysis approaches. For NQR, false alarms from other nitrogenous materials will be far less of a problem than in nuclear-based detection techniques.
(ii) Sensitivity: though NQR is not a very sensitive spectroscopy, the parent disclosure describes techniques to make the response more sensitive to the des*ed explosive 20 and less sensitive to interfering signals. Sensitivity is a function of coil geometry and coil size.
The invention described in the parent disclosure has demonstrated sensitivity to detect the equivalent of subkilogram qu~ntiti~s of explosive near a brief case-sized m.o~n-lerline coil and substantially less explosives in a small solenoidal coil of 25 mm ~ m~ter in a few seconds.

2113~58 W093/0236~ PCT/US92/03117 ,.. .
(iii) Localization: one of the novel features of the NRL approach is to localize the transmitting field and the receiver by a specialized surface coil, never previously used for NQR. One type of surface coil, the 'meanderline' coil, localizes the sensitive inspection region to a well-defined region. Furthermore, the electrical and magnetic fields of the meanderline coil fall off very rapidly with distance, so that a person can be scanned by an NQR
detector without depositing substantial rf power into the body.

Summary of the Invention It is an object of the present invention to safely detect small quantities of nitrogenous explosives and narcotics within a large volume of material to be searched using low power techniques.
It is another object of the present invention to provide a system for detecting nitrogenous explosives and narcotics by nuclear quadrupole resonance over a large volume, at low power, less intense rf fields.
These and other objects are achieved by recognizing that the strength of the applied rf field need only be at least equal to the strength of the local magnetic field due to dipole-dipole interactions. A corollary of this principle is that the signal-to-noise ratio of a signal induced by a specimen of fixed size decreases by only the square root of the coil size, and using this recognition in the detection of explosives and narcotics by NQR. Thus, rather than scaling power linearly with coil size, as conventionally done to maintain the same rf field intensity, the power can be increased significantly less. Specifically, the power need only be increased by the square root of the increased coil size to assure maintenance of the same signal to noise ratio. This approach permits the use of larger coils than previously used.
The approach is useful for both volume coils and surface coils.
For example, a more conventional approach would require an rf peak power of about 6 MW for a 300 liter inspection volume. In contrast we have achieved detection with power SUBSllrlul~: SHEET

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levels of 400 watts. A 5 watt meanderline coil NQR explosives detector is feasible for use on people: the prior approach would have necessitated about a peak power of about 30 kW.

Detailed Des~ lion of the Preferred El.ll,odi~ents The technique utilized according to the present invention is pure nuclear quadrupolar resonance as taught in the previously mentioned Buess et al. patent application. Excitation and detection may be ~clroll,led by any means known in the art, for example, a surface coil, such 10 as a m~n~erline coil or a more conventional 'volume' coil such as a cylindrical or rectangular solenoid, a toroid, or a Helmholtz coil. Pure NQR is typically performed in zero magnetic field: no magnet is required.
As taught in the parent Buess et al. patent application, the specimen is irradiated with a train of radio-frequency (rf) pulses whose frequency has been chosen to be near to the known 15 14N NQR frequency of the explosive or narcotic. For example, RDX has resonance lines near 1.8, 3.4 and 5.2 MHz, while PETN's NQR resonances are near 0.4, 0.5, and 0.9 MHz. Any irradiation sequence useful in NQR processes may be used according to the present invention.
One prerclled irradiation sequence is the strong off-resonance comb (SORC), in which the pulse separations are less than the spin-spin relaxation time T2, producing about one-half of the 20 equilibrium magnetization after every pulse.
Conventionally, intense rf magnetic fields are used to excite the NQR lines and generation of such intense fields requires substantial rf power with associated possibility of depositing unacceptable amounts of power into the scanned objects . Power deposition can have unfortunate consequences for sc~nning of baggage and small cargo, wherein at some suitably ~'' 4a 2 ~ ~ 3 5 ~
high power level, damage to electronics may occur by over voltage or local heating through electrostatic coupling of the electric field or inductive coupling to the m~n~tic ~'''' .

W093/02365 2 1 1 3 5 ~ 8 PCT/US92/03117 field. For scanning people, rf power deposition, primarily by eddy current loss, can pose a problem at these frequencies (1-5 MHz). A detailed discussion of the effects of rf power and field strength values on articles and persons and the acceptable levels of exposure to rf energy is unnecessary here and beyond the scope of this disclosure. It is sufficient to state that an advantage of the present approach that average and peak rf power levels can be reduced by orders of magnitude below those used in prior practice.
An rf field strength of B1 applied near the resonance frequency nutates the spins (for a spin I=l nucleus) through an angle of 2yB1tw, where y is the magnetogyric ratio of the nuclear spin and t~ is the pulse width. For a fixed nutation angle, an intense pulse has a shorter duration and, correspondingly, excites a broader region of the spectrum.
Conventionally, one excites the NQR resonance with a pulse sufficiently long to cause the spins to nutate through about 119~, giving a maximum magnetization. On commercial NQR
spectrometers in a laboratory setting, the pulses required to obtain 119~ tip angle typically have widths of 20-50 ~s and cover a bandwidth 1/t~ of 50-20 kHz. The rf field strength B1 used in such cases is therefore 10-25 gauss.
As part of the present invention, it was recognized that the magnitude of the rf field strength need only be larger or equal to the magnitude of the local magnetic field strength due to dipole-dipole contributions. Hence the necessary rf field strength B1mjn is of the order of l/yT2 where T2 is the spin-spin relaxation time due to dipolar decoupling. Therefore, for example, the strong off resonance comb excitation will work quite satisfactorily at such low rf intensity. For RDX-based explosives, the present invention has successfully utilized rf fields as low as 0.7 G (0.07 mT). (The width of the 14N NQR
line is also partly determined by inhomogeneous interactions due to distribution of the quadrupolar coupling constants, induced by strain, impurities and variations in temperature.
Such an inhomogeneous contribution to the width is not as important as the homogeneous contribution from the dipole-dipole coupling.) SUBSTITUTE SHEET

211335~

6 ~
Therefore, although the prior art applies an rf field of a strength that is at least 100 times greater in magnitude than that of the local magnetic field, the present invention achieves successful NQR detection of nitrogenous explosives and narcotics by using a rf field strength to local field strength ratio of from 1 or about 1 to about 50, preferably as close as possible to 1. Typically, a ratio of about 2 to about 30, more typically a ratio of about 2 to about 20, and most typically a ratio of about 2 to about 10 is used.
A second, related aspect of the present invention is the use of large volume sample coils: since only rather modest rf field strengths are required, a fixed rf power can irradiate a much larger volume by the present method. In a coil of effective volume V and quality factor Q, a pulse of power P
creates a rf field strength B1 proportional to (PQ/Vvo)1/2, where vO is the carrier frequency. By the principle of reciprocity, the signal-to-noise ratio obtainable from a given amount of sample will scale with the strength of B1 per unit current.
Hence, provided there is sufficient power to irradiate the NQR
line, a specimen of fixed size will induce a signal which scales as (coil volume)~1/2. For example the penalty in signal-to-noise ratio increasing coil volume by a factor of 15000 on comparing a 20 cm3 coil to a 300 liter coil volume is about 120.
Thus, according to the present invention, one can irradiate, for example, a volume of about 300 liters and detect significant quantities of explosive in a reasonably short time with an rf peak power of 400 watts, the same peak power conventionally employed on a small 20 cm3 coil system. If one followed the more prior art approach of maintaining the same rf field intensity B~, one would need to scale the power linearly with coil volume, necessitating an rf peak power of 6 MW for the 300 liter system, in contrast to the 400 watts used according to the present invention. In the present invention, the scaling of peak power with size can be significantly less than linear.
As the NQR transitions are induced by rf pulses, discussion so far has centered on the pulse or peak power which creates the (peak) rf magnetic field intensity. Peak power SUBSTITUTE SHEET

2113~
W093/02365 PCI~/US92/03117 r dictates not only the necessary power requirement of the rf transmitter, but also determines the peak voltages induced in the specimen. One must also be concerned with average power which also places some requirements on the rf transmitter and also determines the maximum power which is deposited into the scanned object. (It must be noted that most of the rf energy is dissipated in the coil by resistive losses, with only a fraction dissipated in the specimen through dielectric or eddy current losses. Furthermore, where power dissipation in the specimen may be a problem, there are other well-known rf shielding techniques which can reduce the fraction of the rf power actually dissipated in the specimen.) To appreciate the advantages of the present invention, consider scaling up the coil volume while keeping the rf peak power essentially fixed.
For simplicity of argument, keep the nutation angle about the same in the large volume coil as in the small coil. Hence the rf pulse length will need to be increased in direct proportion to (coil volume) 1/2, and so the average power will increase by that same factor, provided the same pulse spacing is maintained. That is, the scaling of average power with size can be significantly less than linear, and in particular, may be between as low as proportionate to the square root of coil volume without significantly decreasing the signal to noise ratio. In the SORC sequence a typical rf pulse duty factor with short pulses spaced closer than the spin-spin relaxation time T2 might be 0.2% for a small volume coil. To maintain the same nutation angle and the same spacing between pulses, a duty cycle of about 25~ is then required for the 300 liter coil.
For operating conditions with a peak power of 400 w, the average power dissipated in the small coil would be 0.8 W and, by the present invention, only 100 W in the 300 liter coil, far less than the 6 kW average power which would be dictated by maintaining the large rf magnetic field in the large sample coil.
While the above description has focused on "volume coils", for the sake of simplicity, other types of coils, such as the circular surface coil, the pancake coil, the meanderline and other variants, may be successfully used in conjunction with the principles of the present invention.
SUBSTITUTE SHEET

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8 w The improvement offered by the present invention to that disclosed in the parent patent application is that very large sample volumes can be inspected for explosives or narcotics by NQR, without a proportional increase in peak power or average power levels. In practice, suitcase-sized sample volumes can be inspected at rather modest peak and average rf power levels.
Furthermore, this approach makes feasible the examination of people by large surface coils, such as the meanderline, or even 'volume' coils such as a solenoid, as indicated below.
Obviously, many modifications and variations of the present invention are possible in light of the above teachings.
It is therefore to be understood that, within the scope of the appended claims, the invention may be practiced otherwise than as specifically described.

SUBSTITUTE SHEET

Claims (18)

Claims What is claimed is:
1. A method for detecting a class of explosives and narcotics containing nitrogen in a specimen by nuclear quadrupole resonance, comprising the steps of:
(a) generating a train of radio frequency pulses having a predetermined frequency;
(b) transmitting said train of radio frequency pulses to a coil;
(c) irradiating the specimen with an rf field of predetermined strength in response to said train of radio frequency pulses transmitted to said coil at said step (b), said specimen having a local magnetic field due to dipole-dipole contributions;
(d) detecting an integrated nitrogen signal in response to irradiating the specimen at said step (c);
(e) receiving said integrated nitrogen signal detected at said step (d);
(f) comparing said integrated nitrogen signal to a predetermined threshold value; and (g) signalling when said integrated nitrogen signal exceeds said predetermined threshold value;
wherein the strength of said predetermined rf field and said local magnetic field is at a ratio of about 1:1 to about 50:1.
2. The method of claim 1, wherein the ratio of the strength of said magnetic field to the strength of said local field is about 1:1 to about 30:1.
3. The method of claim 2, wherein the ratio of the strength of said magnetic field to the strength of said local field is about 1:1 to about 20:1.
4. The method of claim 3, wherein the ratio of the strength of said magnetic field to the strength of said local field is about 2:1 to about 20:1.
5. The method of claim 3, wherein the ratio of the strength of said magnetic field to the strength of said local field is about 1:1 to about 10:1.
6. The method of claim 5, wherein the ratio of the strength of said magnetic field to the strength of said local field is about 2:1 to about 10:1.
7. A method according to Claim 1, wherein said step (a) generates said predetermined frequency of said train of radio frequency pulses to be near to a 14N NQR frequency of the type of explosive or narcotic to be detected.
8. A method according to Claim 1, wherein said step (a) generates said train of radio frequency pulses comprising a strong off-resonance comb of radio frequency pulses.
9. A method according to claim 1, wherein said coil is a meanderline surface coil for detecting the class of explosives and narcotics in the specimen at predetermined areas.
10. A method according to claim 1, wherein said coil comprises a localized coil for detecting the class of explosives and narcotics in the specimen at predetermined regions.
11. A method according to Claim 1, wherein said coil comprises a solenoidal coil for detecting the class of explosives and narcotics in the entire specimen.
12. A method according to Claim 1, wherein said coil comprises a toroidal coil for detecting the class of explosives and narcotics in the specimen at predetermined regions.
13. In a system for detecting a class of explosives and narcotics containing nitrogen in a specimen by nuclear quadrupole resonance, said system including:
a first coil of predetermined size for irradiating the specimen with a train of radio frequency pulses of predetermined average power and frequency and detecting an integrated nitrogen signal in response to irradiating the specimen;
pulse generating means for generating said train of radio frequency pulses;
coupling means for transmitting said train of radio frequency pulses to said first coil and receiving said integrated nitrogen signal from said first coil;
comparing means for comparing said integrated nitrogen signal to a predetermined threshold value; and an alarm for signalling when said integrated nitrogen signal exceeds said predetermined threshold value;
the improvement wherein a second coil of a predetermined size larger than said first coil is substituted for said first coil, and said pulse-generating means is adapted so that the predetermined average power of said train of rf pulses generated thereby causes said first coil to irradiate said specimen with a train of rf pulses of an average power increased with respect to the predetermined average power irradiated by said first coil significantly less than in direct proportion to the linear increase in volume of said second coil with respect to said first coil.
14. The system of claim 9, wherein said pulse-generating means is adapted so that the predetermined average power of said train of rf pulses generated thereby causes said first coil to irradiate said specimen with a train of rf pulses of a average power increased with respect to the predetermined average power irradiated by said first coil in direct proportion to about the square root of the increase in coil volume.
15. A system for detecting a class of explosives and narcotics containing nitrogen in a specimen having a local magnetic field due to dipole-dipole contributions, by nuclear quadrupole resonance, said system including:
a coil of predetermined size for irradiating the specimen with a train of radio frequency pulses of predetermined frequency and detecting an integrated nitrogen signal in response to irradiating the specimen;
pulse generating means for generating said train of radio frequency pulses;
coupling means for transmitting said train of radio frequency pulses to said coil and receiving said integrated nitrogen signal from said coil;
comparing means for comparing said integrated nitrogen signal to a predetermined threshold value; and an alarm for signalling when said integrated nitrogen signal exceeds said predetermined threshold value;
wherein said pulse-generating means causes said coil to irradiate said specimen with an rf field having a strength which is from about equal to the strength of the local magnetic field of said sample up to about 50 times the strength of the local magnetic field of the specimen.
16. The system of claim 15, wherein said pulse-generating means causes said coil to irradiate said specimen with an rf field having a strength which is from about equal to the strength of the local magnetic field of said sample up to about 30 times the strength of the local magnetic field of the specimen.
17. The system of claim 16, wherein said pulse-generating means causes said coil to irradiate said specimen with an rf field having a strength which is from about equal to the strength of the local magnetic field of said sample up to about 20 times the strength of the local magnetic field of the specimen.
18. The system of claim 17, wherein said pulse-generating means causes said coil to irradiate said specimen with an rf field having a strength which is from about equal to the strength of the local magnetic field of said sample up to about 10 times the strength of the local magnetic field of the specimen.
CA 2113558 1991-07-16 1992-04-24 Detection of explosive and narcotics by low power large sample volume nuclear quadrupole resonance (nqr) Expired - Lifetime CA2113558C (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US07/730,722 US5233300A (en) 1991-05-23 1991-07-16 Detection of explosive and narcotics by low power large sample volume nuclear quadrupole resonance (NQR)
US730,722 1991-07-16

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CA2113558A1 CA2113558A1 (en) 1993-02-04
CA2113558C true CA2113558C (en) 1999-03-23

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GB9319875D0 (en) * 1993-09-27 1994-03-09 British Tech Group Apparatus for and methods of nuclear resonance testing
US5608321A (en) * 1995-12-28 1997-03-04 The United States Of America As Represented By The Secretary Of The Navy Method and apparatus for detecting target species having quadropolar muclei by stochastic nuclear quadrupole resonance
WO2011093429A1 (en) * 2010-01-29 2011-08-04 財団法人北九州産業学術推進機構 Method for manufacturing highly sensitive atmosphere sensor, highly sensitive atmosphere sensor, and method for sensing substance using the highly sensitive atmosphere sensor

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US4166972A (en) * 1977-10-05 1979-09-04 Southwest Research Institute NMR discrimination apparatus and method therefor
US4296378A (en) * 1979-04-05 1981-10-20 Southwest Research Institute Apparatus providing enhanced detection of specimens in inhomogeneous fields
US4514691A (en) * 1983-04-15 1985-04-30 Southwest Research Institute Baggage inspection apparatus and method for determining presences of explosives
GB8701695D0 (en) * 1987-01-27 1987-03-04 Smith J A S Detecting compounds
WO1990004169A1 (en) * 1988-10-07 1990-04-19 Hitachi, Ltd. Method and apparatus for detecting particular substance

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EP0746774A4 (en) 1994-03-30
WO1993002365A1 (en) 1993-02-04
JP2002509601A (en) 2002-03-26
EP0746774A1 (en) 1996-12-11
CA2113558A1 (en) 1993-02-04

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