Radio-frequency μSR experiments at the ISIS pulsed muon facility

This paper explores the use of pulsed radio-frequency (RF) techniques to remove the frequency limitations imposed on conventional transverse muon spin rotation (μSR) experiments at a pulsed muon source by the finite muon pulse width. The implementation of the 90° pulse technique is demonstrated by observing the free precession signal of diamagnetic muons implanted in polythene, the change in signal amplitude as a function of RF pulse length is plotted and the precise condition for a 90° pulse determined. The technique is evaluated by comparing measurements made using conventional spin rotation experiments to those employing pulsed RF methods. The potential for applying standard NMR multiple-pulse methods to the μSR experiment is considered and the use of two-pulse RF sequences (90° _x ?τ?90° _x and 90° _x ?τ?180° _x ) to form a muon spin echo demonstrated.     

Large angle spin-echo imaging

A study was undertaken to assess the use of excitation flip angles greater than 90° for T₁ weighted spin-echo (SE) imaging with a single 180° refocusing pulse and short TR values. Theoretical predictions of signal intensity for SE images with excitation pulse angles of 90–180° were calculated based on the Bloch equations and then measured experimentally from MR images of MnCl₂ phantoms of various concentrations. Liver signal-to-noise ratios (SNR) and liver-spleen contrast-to-noise ratios (CNR) were measured from breathhold MR images of the upper abdomen in 16 patients using 90 and 110° excitation flip angles. The theoretical predictions showed significant improvements in SNR with excitation flip angles >90°, which were more pronounced at small TR values. The phantom studies showed reasonably good agreement with the theoretical predictions in correlating the excitation pulse angle with signal intensity. In the human imaging studies, the 110° excitation pulse angle resulted in a 7.4% (p < .01) increase in liver SNR and an 8.2% (p = .2) increase in liver-spleen CNR compared to the 90° pulse angle at TR = 275 ms. Increased signal intensity resulting from the use of large flip angle excitation pulses with a single echo SE pulse sequence was predicted and confirmed experimentally in phantoms and humans.     

Measurement of multiplet intensities and noble gas-broadened line widths in the V3-fundamental of methane

Integrated intensity data at 300°K for J-multiplets between P(11)and R(11) in the _{V3-fundamental of ¹²CH4} are presented, along with the intensity of the entire Q-branch, which also encompasses the Q-branch of the _{V3-fundamental of ¹³CH4}. These data, together with theoretical estimates for the intensities of J-multiplets of J > 11, sum up to a value of S_band= 284±14cm^?2atm^?1 at 300°K. This results is in excellent agreement with most of the previously published values for this parameter. Within experimental error, the intensities of the J-multiplets in the _{V3-fundamental do not seem to exhibit the strong anamolies that were characteristic of lines in the 2V3}-band.Line widths have been measured at 100°K, 130°K, 190°K, 250°K, and 300°K for R(0), R(1), and R(2) broadened by He, Ne and Ar. The temperature dependence of the line width is discussed for the three cases of broadening. In neon broadening at 300°K, the ‘effective mean line widths’ for multiplets R(3) through R(11) have also been obtained experimentally; their J-dependence is interpreted using Gordon's theory of line shapes in multiplet spectra.     

In vivo lactate editing in single voxel proton spectroscopy and proton spectroscopic imaging by homonuclear polarisation transfer

Volume-selective lactate editing has been performed successfully in vitro and in vivo in the brain on a clinical scanner using a PRESS-based single voxel ¹H spectroscopy and a ¹H spectroscopic imaging sequence. The PRESS sequence was made sensitive to homonuclear polarisation by replacing the standard 180° refocusing pulses with 90° pulses. Two acquisitions were made at a total echo time around 2/J (J is the coupling constant for CH and CH₃ spins in lactate ≈7 Hz) whose individual echo times differed by 5.5 ms. Subtraction of one signal from the other yielded the lactate resonance alone. The technique is an effective method of separating the overlapping signals of lactate and lipids. Furthermore this editing method can be performed without state of the art MRI scanner hardware.     

Angular correlation study of levels in 16C

Angular correlation measurements using the ¹⁴C(t, pγ)¹⁶C reaction result in the following spin assignments to levels in ¹⁶C: E_x = 1.766 MeV, J = 2; E_x = 3.980 MeV, J = 2; E_x = 4.083 MeV, J = 3; E_x = 4.138 MeV, J = 4.     

Selective Detection of 1H NMR Resonances of 13CHn Groups Using Two-Dimensional Maximum-Quantum Correlation Spectroscopy

Methods for editing spectra based upon maximum-quantum filtering in two-dimensional ¹H NMR are presented (MAXY NMR). Separation of ¹H resonances from ¹³CH, ¹³CH₂, and ¹³CH₃ groups is demonstrated, using the coherence of the attached natural-abundance ¹³C spin. Two-dimensional correlation pulse sequences based on J connectivity (MAXY-COSY), total J connectivity (MAXY-TOCSY), and NOE and exchange processes (MAXY-NOESY) are given and exemplified using dexamethasone as a model compound. In addition, an improved form of a ¹³CH₂ only COSY spectrum (gem-COSY) is shown, and the application of z magnetic-field gradients is demonstrated as an alternative to phase cycling. The approach should have utility in the assignment of complex ¹H NMR spectra which arise from peptides or complex mixtures such as biofluids.     

Spin waves in MnO; from 4°K to temperatures close to TN

Spin waves have been measured in MnO by inelastic scattering of neutrons from 4 °K to a temperature 0·25 °K below T_N. The 4 °K spectrum is interpreted in the frame of linear spin wave theory with effective exchange integrals J₁^? = 0·321 meV, J₁⁺ = 0·424 meV, J₂¹ = 0·446 meV and a phenomenological parameter for anisotropy D₁ = 0·059 meV. The effect of the actual dipole-dipole Hamiltonian is shown to give a priori a very good account of the lifting of the degeneracy of spin waves near the Brillouin zone center. The Bloch model for interacting spin waves and theories based on Green function approximations have been adapted to the MnO case, in order to compute the main properties (mean magnetization of a sublattice, anisotropic deformation, extra isotropic contraction and magnon spectrum) at many temperatures. Comparison of these with experimental results tends to favour a generalized Callen renormalization model, which gives an overall fit from 4 °K, to temperalures close to T_N.     

On the role of experimental imperfections in constructing 1H spin diffusion NMR plots for domain size measurements

We discuss the precision of 1D chemical-shift-based ¹H spin diffusion NMR experiments as well as straightforward experimental protocols for reducing errors. The ¹H spin diffusion NMR experiments described herein are useful for samples that contain components with significant spectral overlap in the ¹H NMR spectrum and also for samples of small mass (<1 mg). We show that even in samples that display little spectral contrast, domain sizes can be determined to a relatively high degree of certainty if common experimental variability is accounted for and known. In particular, one should (1) measure flip angles to high precision (≈±1° flip angle), (2) establish a metric for phase transients to ensure their repeatability, (3) establish a reliable spectral deconvolution procedure to ascertain the deconvolved spectra of the neat components in the composite or blend spin diffusion spectrum, and (4) when possible, perform 1D chemical-shift-based ¹H spin diffusion experiments with zero total integral to partially correct for errors and uncertainties if these requirements cannot fully be implemented. We show that minimizing the degree of phase transients is not a requirement for reliable domain size measurement, but their repeatability is essential, as is knowing their contribution to the spectral offset (i.e. the J₁ coefficient). When performing experiments with zero total integral in the spin diffusion NMR spectrum with carefully measured flip angles and known phase transient effects, the largest contribution to error arises from an uncertainty in the component lineshapes which can be as high as 7%. This uncertainty can be reduced considerably if the component lineshapes deconvolved from the composite or blend spin diffusion spectra adequately match previously acquired pure component spectra.     

Electromagnetic transition strengths in 24Na

Mean lifetimes, excitation energies and branching ratios of ²⁴Na states, populated in the ²³Na(d, p)²⁴Na reaction have been measured. Gamma-ray spectra were measured at three angles in coincidence with proton groups at θ_p = 169°. Mean lifetimes obtained from DSA are (excitation energy in keV, lifetime in fs): 563, > 1000; 1341, 95 ± 30; 1344, 38 ± 11; 1346, > 1500; 1512, 38 ± 11; 1846, 260 ± 50; 1885, 36 ± 9; 2513, 15 ± 7; 2563, < 25; 2904, 50 ± 15; 2978, < 25; 3216, 22 ± 8; 3372, 19 ± 5. For higher levels up to 4207 keV upper limits of 30 fs were set. In combination with earlier work the following unique spin(-parity) assignments could be made: J^π(1846) = 2⁺, J(2513) = 3, J^π(3745) = 3^?. A new level at E_x = 3681.7 ± 0.6 keV is reported.     

Non-collinear spin arrangements in NiZn ferrites studied by the Mössbauer effect

Samples of the nickel-zinc ferrite series Ni_xZn_1-xFe₂O₄ with x = 0.15, 0.20, and 0.25 have been studied by the Mössbauer-effect technique at liquid helium temperature using longitudinal magnetic fields of 16kOe. The hyperfine fields at ⁵⁷Fe nuclei in A and B sites have been determined. Canted spin structures associated with Fe³⁺ ions are observed for all samples. Spectra were fitted using a localized canting model. The ratio of intrasublattice to intersublattice exchange constants resulting in the best fit is J_BB/J_AB = 0.130±0.005.     

Anomalous pulse angle dependence of the single and double quantum echoes in a photoinduced spin-correlated coupled radical pair

In this work the response of a spin-correlated coupled radical pair to the sequence flash-t-P _ζ-τ-P _2ζ-T is investigated. For the theoretical analysis, the density operator formalism is used. Analytical expressions are derived for the electron spin single (SQ ESE) and double-quantum echoes (DQ ESE) as a function of pulse flip angle and singlet-triplet mixing angle. To illustrate the theoretical results, computer simulations are presented. In the limit of weak coupling, the “out-of-phase” SQ ESE is shown to be of a pure two-spin order having the maximal amplitude for the flip angle of 65.9°. The echo following the Hahn sequence vanishes in the same limit. This confirms the theoretical result already presented in the literature. However, the more general analysis shows that outside the weak coupling approximation the Hahn echo is of purely one-spin order, whereas the echo following the flash-t-P _ζ-τ-P _2ζ-t sequence has its maximal amplitude for the flip angle of 75° and the singlet-triplet mixing angle of 27°. The “in-phase” single- and double-quantum echoes are shown to vanish due to averaging out, within the electron spin resonance spectrometer deadtime, of contributions modulated with the sum and difference of the zero-quantum beat frequency and the frequency due to the spin-spin interaction within the pair. The calculated out-of-phase DQ ESE signal is inverted with respect to the out-of-phase SQ ESE and has only the half of its amplitude. The DQ ESE vanishes for the Hahn sequence. The echo has maximal amplitude in the weak-coupling limit for the flip angle of 65.9°. In contradiction to the analytical result previously published, the out-of-phase DQ ESE does not vanish for long τ and large zero-quantum-beat frequency.     

Radiative decay ofJ/ψ into γ π+ π−

The radiative decayJ/ψ → γ π⁺ π^? has been studied using the 8.6 millionJ/ψ produced in the DM2 experiment at the DCIe ⁺e^? storage rings at Orsay. The π⁺ π^? mass spectrum shows a cleanf ₂ (1270) signal, and the possible presence of two other states at thef ₂ (1720) andf ₄ (2030) masses. For thef ₂ (1270), the branching ratio BR(J/ψ →γf)xBR(f→π⁺ π^?) is measured to be (7.50±0.30±1.12)×10^?4, and the spin analysis prefers theJ=2 assignment, with helicity parametersx=0.83±0.06 andy=0.01±0.06. The existence of higher mass states is discussed.     

Study of antiferromagnetic phenomenon for oxo-bridged iron (III) dimers in model molecules of methemerythrin

By introducing the covalent effect into the Girerd–Journaux–Kahn's magnetic theory a more general magnetic exchange formula for describing transition-metal ion pairs in covalent complex molecules has been established. By this formula and by the use of our double-slater-type-function (DSF) calculation procedure the relationship between the magnetic exchange coupling parameter J and the covalent factor N has been studied. It is shown that for the oxo-bridged Fe(III) dimer there exists a nearly linear relation between J and N, and that the stronger is the covalent effect the stronger is the antiferromagnetic coupling interaction. It is also shown that in a series of model molecules of methemerythrin derivatives, such as in (FeSalen)₂O·2py, FeSalenCl·(CH₃NO₂)_x, enH₂[(FeHEDTA)₂O]·6H₂O, Na₄[(FeHEDTA)₂O]·12H₂O, [(Fe(terpy))₂O](NO₃)₄·H₂O and Fe(terpy)Cl₃, there are about 40% antiferromagnetic contributions that arise from the covalent effect, and that the theoretical values J=−95.5 to −100.7 cm⁻¹ are in good agreement with the experimental findings J=−90 to −105 cm⁻¹ for those model molecules.     

A microscopic analysis of moments of inertia

A microscopic analysis of moments of inertia is performed within the cranked Nilsson model. Special emphasis is put on the second-derivative moment of inertia, J⁽²⁾. Contributions to this from changes of rotational frequency and deformation are separately discussed. A simple expression for the latter is derived and it is for a studied series of Yb isotopes usually found to contribute with less than 10% to the total J⁽²⁾ value. J⁽¹⁾, J⁽²⁾ and J_rigid are calculated as functions of spin at the appropriate equilibrium deformations for the even-even nuclei ^160–176Yb. Variations of J⁽²⁾ with particle number and spin are discussed. Relations between J⁽²⁾ and the deformation are studied in detail, especially in connection with the super-backbending.     

Photovoltaic structures using AgSb(S x Se1−x )2 thin films as absorber

Photovoltaic structures were prepared using AgSb(S _x Se_1?x )₂ as absorber and CdS as window layer at various conditions via a hybrid technique of chemical bath deposition and thermal evaporation followed by heat treatments. Silver antimony sulfo selenide thin films [AgSb(S _x Se_1?x )₂] were prepared by heating multilayers of sequentially deposited Sb₂S₃/Ag dipped in Na₂SeSO₃ solution, glass/Sb₂S₃/Ag/Se. For this, Sb₂S₃ thin films were deposited from a chemical bath containing SbCl₃ and Na₂S₂O₃. Then, Ag thin films were thermally evaporated on glass/Sb₂S₃, followed by selenization by dipping in an acidic solution of Na₂SeSO₃. The duration of dipping was varied as 3, 4 and 5 h. Two different heat treatments, one at 350 °C for 20 min in vacuum followed by a post-heat treatment at 325 °C for 2 h in Ar, and the other at 350 °C for 1 h in Ar, were applied to the multilayers of different configurations. X-ray diffraction results showed the formation of AgSb(S _x Se_1?x )₂ thin films as the primary phase and AgSb(S,Se)₂ and Sb₂S₃ as secondary phases. Morphology and elemental detection were done by scanning electron microscopy and energy dispersive X-ray analysis. X-ray photoelectron spectroscopic studies showed the depthwise composition of the films. Optical properties were determined by UV–vis–IR transmittance and reflection spectral analysis. AgSb(S _x Se_1?x )₂ formed at different conditions was incorporated in PV structures glass/FTO/CdS/AgSb(S _x Se_1?x )₂/C/Ag. Chemically deposited post-annealed CdS thin films of various thicknesses were used as window layer. J–V characteristics of the cells were measured under dark and AM1.5 illumination. Analysis of the J–V characteristics resulted in the best solar cell parameters of V _oc = 520 mV, J _sc = 9.70 mA cm^?2, FF = 0.50 and η = 2.7 %.     

Spins in 23Na from 25Mg(d, α)

The ²⁵Mg(d, α)²³Na reaction has been investigated at bombarding energies of 12.07,11.82 and 11.57 MeV. Angular distributions are approximately symmetric about 90° and for states of known J^π angle-integrated cross sections $\text{σ}$ averaged over bombarding energy, are roughly proportional to $\text{2J + 1:}\text{σ}\text{/(2J + 1) = 25±4 μ}\text{b}$. Measured cross sections for other states, up to E_x = 7.9 MeV, have been used to place limits on J.     

New aspects of the rotational model in25Mg

Spin assignments have been made to the²⁵Mg levels in theE _x=5–6 MeV region fromγ-ray angular distributions measured in the²²Ne(α, n y) reaction atE _α=8.0 and 8.8 MeV and fromp-γ angular correlations measured in the²⁴Mg(d, p γ) reaction atE _d=6 MeV. Unique spin assignments ofJ=7/2, 5/2, 5/2, and 9/2 could be made to the levels atE _x=5005, 5511, 5851, and 5967 keV, respectively. Ambigious assignments have been made to the levels atE _x=5245, 5524, 5785, 6032 keV (J=11/2, 7/2), 5455 keVJ=13/2, 9/2), and 5738 keV (J=3/2, 5/2). The present data confirm previous assignments ofJ=1/2 to the levels atE _x=5108 and 5466 keV, respectively. Lifetime estimates have been obtained, using the Doppler-shift attenuation method, for the levels atE _x=5245 keV (τ=30–60 fs), 5785 keV (τ=50–100 fs), 5967 keV (τ=50–100 fs), and 5455 keV (τ>1ps). All other levels in theE _x=5–6 MeV region haveτ<60 fs. A breakdown of theK-selection rule has been observed in theγ-decay of some high spin states, indicating a deviation from the strong coupling model.     

Magnetic susceptibility of (CH3NH3)2FeCl3Br: An example of a canted spin system

Magnetic susceptibility of (CH₃NH₃)₂FeCl₃Br is measured in the temperature range 80–200°K. A sharp peak characteristic of a spin canted system is found at T_N(H=0)=98° K. Magnetic field dependence of the susceptibility and the effect of the halide ion size on the canted spin is discussed.     

Methyl isocyanate: An analysis of the low-J rotational spectrum using the quasi-symmetric top molecule approach

The low-J rotational spectrum of methyl isocyanate (CH₃NCO) has been analyzed in terms of the quasi-symmetric top molecule model, accounting explicitly for the large-amplitude CNC bending motion, and internal and overall rotation. An assignment of 25 J = 1 ← 0 and 2 ← 1 rotational transitions arising from the various CNC bending and torsional states is proposed. The molecule is found to be a nearly freely internally rotating quasi-symmetric top, with a barrier to linearity of the CNCO skeleton of 1049 cm^?1 and an equilibrium CNC valence angle of 140.2°.