behavior

JoVE行動学は、人間や動物の行動を理解するための観察および実験手法を公開しています。このセクションには、内外の刺激に対する遺伝的原因と生理学的反応を分析する方法と、関係する脳領域を調べる方法が含まれています。

行動学

biochemistry

JoVE生化学は、生体分子（タンパク質、核酸、炭水化物、脂質、代謝物など）の構造と機能、および生物学的プロセス中に起こるそれらの相互作用と変換についての理解を深める方法を出版しています。

生化学

bioengineering

JoVE生物工学は、物理学と生命科学を融合して基本的な生物学的プロセスと機能を理解する方法と技術を出版しています。このセクションでは、病気の測定、診断、治療を改善するための物理科学的ツールとアプローチについても特集します。

生物工学

biology

JoVE生物学は、細胞生物学、分子生物学、生命体生物学の分野で使用される方法を出版しています。これは、標準的な技法の新しいアプリケーションから、生物の基本的な生物学的機能を理解することを目的とした新規のアプローチにまで及びます。

生物学

cancer research

JoVEがん研究は、がん生物学の研究で使用される技術を出版しています。このセクションでは、発がん、薬剤耐性のメカニズム、診断、転移、革新的な治療法に取り組む研究方法論を取り上げます。

がん研究

chemistry

JoVE化学は、分析化学、有機化学、高分子化学、物理化学、無機化学など、幅広い分野の方法を出版しています。このセクションには、高度なまたはユニークなアプリケーション向けの材料および低分子の設計・調整も含まれています。

化学

developmental biology

JoVE発生生物学では、分子、細胞、組織、器官、および生物全体のレベルにおける、試験管内および/または生体内での生物発生を研究するのに使用される方法と技術を出版しています。

発生生物学

engineering

JoVE工学では、工学と応用物理学で利用される方法と技術を出版しています。方法には、機械、電気、化学のエンジニア、物理学者、材料科学者からの寄稿が含まれます。

工学

environment

JoVE環境学は、地球のプロセスと生態系を研究し、環境問題に対処するための研究方法と技術を出版しています。このセクションでは、農業および食品科学だけでなく、幅広い学際的な環境研究分野からの実験室およびフィールドベースの方法を取り上げます。

環境学

genetics

JoVE遺伝学は、ゲノミクス、遺伝子発現、遺伝子工学、後生遺伝学など、遺伝学のすべての分野（すべての生物）に取り組む方法を出版しています。このセクションでは、塩基配列決定技術とその応用の進歩についても特に取り上げます。

遺伝学

immunology and infection

JoVE免疫学と感染では、病原体に対する生物学的反応、感染に対する免疫反応、基本的な微生物学、および感染性微生物に対する新しい治療法を評価するための方法と技術を出版しています。

免疫・感染学

medicine

JoVE医学では、生物医学研究方法と臨床応用を出版しています。このセクションでは、疾患の動物モデル、医療処置、手術、患者のケーススタディ、および臨床試験の方法論について説明します。

医学

neuroscience

JoVE神経科学では、脳と神経系の構造、機能、生理学、および病態生理学を研究するための方法を出版しています。このセクションには、神経疾患および神経障害の潜在的な治療基盤と外科技術も含まれています。

神経科学

jove journal

JoVE Journal

科学ビデオジャーナル。査読された論文。学際的。

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Research

2D NMR: Heteronuclear Single-Quantum Correlation Spectroscopy (HSQC)

Heteronuclear single-quantum correlation spectroscopy (HSQC) is a 2D NMR technique that reveals one-bond correlations between hydrogen and a heteronucleus. The HSQC experiment is similar to the heteronuclear correlation experiment (HETCOR) but is more sensitive. In the HSQC spectrum, the proton chemical shift is plotted on the horizontal F2 axis, while the 13C chemical shift is plotted on the vertical F1 axis. The corresponding proton and 13C spectra are also shown. The HSQC contour plot does not have any diagonal peaks. All the cross-peaks indicate the protons directly attached to each carbon in a molecule. Similar to the COSY spectrum, imaginary lines are drawn in horizontal and vertical directions to identify the correlated peaks.
For example, the HSQC spectrum of 2-chlorobutane has a carbon signal at 11 ppm that can be assigned to the shielded methyl group and correlated to the proton multiplet at 1.01 ppm. The carbon signal at 24.8 ppm arises from the deshielded methyl group, which correlates to the proton multiplet at 1.52 ppm. Similarly, the methylene carbon signal at 33.3 ppm and methine carbon signal at 60.4 ppm correlate to the multiplets at 1.72 and 3.96 ppm, respectively.&#160; HSQC is a very useful technique for structurally elucidating complex molecules and is routinely used in protein NMR studies.

Heteronuclear single-quantum correlation spectroscopy (HSQC) is a 2D NMR technique that reveals one-bond correlations between hydrogen and a ...

2D NMR: Overview of Heteronuclear Correlation Techniques

Heteronuclear correlation spectroscopy is an analytical technique that investigates the coupling between different types of nuclei, often a proton and an X-nucleus, such as carbon-13 or nitrogen-15. This method is commonly used in nuclear magnetic resonance (NMR) spectroscopy to gain insights into complex chemical compounds&#39; structural and compositional aspects. A typical heteronuclear correlation spectrum displays X-nucleus chemical shifts on one axis and a proton spectrum on the other axis. Cross-peaks reveal the connection between specific protons and X-nuclei.
The main heteronuclear correlation experiments include HETCOR, HSQC, HMQC, and HMBC. HSQC, HMQC, and HMBC record the proton spectrum, whereas the X-nucleus spectrum is recorded by standard heteronuclear correlation spectroscopy or HETCOR. The HETCOR-HMQC-HSQC group of experiments cannot detect X-nuclei without an attached proton. HETCOR is used when ultrahigh peak resolution is required along the X-nucleus axis.
The heteronuclear single quantum correlation technique, or HSQC, investigates proton-to-X-nucleus single bond correlations. In an HSQC experiment, polarization is transferred from a proton nucleus to a neighboring X-nucleus and then back to the proton nucleus. The signal from the proton nuclei is then recorded. HSQC generates a spectrum like that of heteronuclear multiple-quantum correlation spectroscopy or HMQC but uses a different suppression method, providing better X-nucleus resolution along the axis.
Heteronuclear multiple-bond correlation, or HMBC, is a proton-detected experiment, like HMQC but with a longer initial delay time. This experiment is used to observe long-range proton to X-nucleus connectivity separated by 2-3 bonds, with some experiments going out to 4 or 5 bonds. In an HMBC experiment, direct one-bond correlations are suppressed as part of the sequence. The spectra of HMBC give rise to cross peaks that correlate which protons are coupled to what other specific X-nucleus is more than one bond away. The gradient HMBC (gHMBC) pulse sequence offers better suppression of interfering signals, making it particularly useful for analyzing complex molecules with overlapping signals.

Heteronuclear correlation spectroscopy is an analytical technique that investigates the coupling between different types of nuclei, often a proton and an ...

2D NMR: Homonuclear Correlation Spectroscopy (COSY)

Homonuclear correlation spectroscopy, or COSY, is a 2-dimensional NMR technique that provides information about coupled protons. Typically, the geminal and vicinal coupling are observed. For example, consider the COSY spectrum of ethyl acetate, where its 1D proton NMR spectrum is plotted along the vertical and horizontal axes with their corresponding chemical shift scale. Three spots on the diagonal corresponding to the three peaks in the 1D proton spectrum are called diagonal peaks. The COSY spectrum is symmetric about the diagonal, with signals above and below the diagonal called cross-peaks or off-diagonal peaks. An imaginary line is drawn from diagonal peaks parallel to the horizontal axis, leading to a cross peak. A vertical line is then drawn from the same cross peak towards the diagonal peak to correlate the peaks. The off-diagonal peaks correlating the multiplets at 1.25 and 4.2 ppm indicate that the methyl protons are coupled to the methylene protons. The signal at 2 ppm is not associated with cross-peaks because the protons are not involved in homonuclear coupling. A COSY spectrum is useful when overlapping multiplets complicate the corresponding 1D spectrum.

Homonuclear correlation spectroscopy, or COSY, is a 2-dimensional NMR technique that provides information about coupled protons. Typically, the geminal ...

Insensitive Nuclei Enhanced by Polarization Transfer (INEPT)

Insensitive Nuclei Enhanced by Polarization Transfer (INEPT) is an advanced Nuclear Magnetic Resonance (NMR) technique specifically designed to detect and enhance the signals of low-abundance nuclei, such as carbon-13 and nitrogen-15, in small molecules. The fundamental principle behind INEPT is the transfer of polarization from a more abundant and highly polarizable nucleus, typically hydrogen-1, to the low-abundance nucleus of interest. This process effectively boosts the NMR signal of the low-abundance nuclei, making them more easily detectable.
The INEPT technique involves a series of carefully timed radiofrequency (RF) pulses applied to the sample. These RF pulses excite the more abundant nuclei, causing them to align their spins in a specific manner. Through the process of spin coupling, the polarization of the more abundant nuclei is then transferred to the low-abundance nuclei. As a result, the NMR signal of these low-abundance nuclei is significantly enhanced, allowing for a more detailed analysis of the molecular structure.
Various pulse sequences have been developed to improve the observability of these low-abundance nuclei when coupled to a high-receptivity nucleus. The INEPT pulse sequence combines a spin echo and selective population inversion, which includes 90&#176; and 180&#176; pulses on the high-sensitivity (the I spins) and low-sensitivity nuclei (the S spins), respectively. Coupling-constant-based delays between pulses facilitate magnetization transfer through space or bond interactions. Additional RF pulses and delays invert the low-gamma magnetization, producing an observable NMR signal. The net result is an enhanced NMR signal from low-gamma nuclei that would otherwise be challenging to detect.
Various pulse sequences have been developed to improve the detection of low-abundance nuclei when coupled with high-receptivity nuclei such as protons. The INEPT sequence yields enhanced signals for insensitive nuclei, with half of the CH group producing negative peaks and the other half positive peaks. This pattern allows for discrimination between different types of carbon-hydrogen bonds within the molecule.
Decoupling methods can be employed to enhance sensitivity and resolution in distinguishing various carbon-hydrogen bonds, making INEPT an invaluable tool in the chemical and pharmaceutical industries.

Insensitive Nuclei Enhanced by Polarization Transfer (INEPT) is an advanced Nuclear Magnetic Resonance (NMR) technique specifically designed to detect and ...

Two-Dimensional (2D) NMR: Overview

The 1D NMR spectrum of large and complex molecules like natural products has complicated splitting patterns and overlapping signals, which can be easily interpreted using 2-dimensional (2D) NMR. Unlike 1D NMR, 2D NMR has two frequency axes that provide the coupling information between the nucleus A and nucleus B in a molecule. The process from which 2D spectra are obtained has four steps.
The first step is the preparation period, during which nucleus A is excited with a radiofrequency pulse. The second step is the evolution or wait period t1, which is incremented systematically, and no data is observed during this period. The next step is the mixing period, in which a second radiofrequency pulse is introduced, which transfers the magnetization to the spins of nucleus B. In the last step, the magnetization of nuclear spins from B is detected during the acquisition time t2 for each t1. Time domains t1 and t2 are Fourier transformed into frequency domains f1 and f2, and these correspond to two dimensions of 2D spectra, while the third dimension is the intensity. In 2D experiments, coupling between the same kind of nucleus is called homonuclear 2D experiments, whereas coupling between two types of nucleus is called heteronuclear 2D experiments. 2D spectra can be displayed as stacked or contour plots. When presented as stacked plots, 2D spectra are difficult to interpret. The contour plot is the horizontal cross-section of a stacked plot where the size of the circles shows the signal intensity. Its interpretation is straightforward and it is preferred for data analysis.

The 1D NMR spectrum of large and complex molecules like natural products has complicated splitting patterns and overlapping signals, which can be easily ...

2D NMR: Overview of Homonuclear Correlation Techniques

Homonuclear correlation spectroscopy (COSY) is a powerful technique used in Nuclear Magnetic Resonance (NMR) spectroscopy to study the correlations between nuclei of the same type within a molecule. It provides information about scalar couplings between adjacent nuclei, which helps determine connectivity and structural information. There are several COSY variants, each with its unique strengths and experimental parameters.
COSY90 is the standard two-dimensional (2D) COSY experiment that utilizes a second 90-degree pulse to achieve high sensitivity and resolution. It excels in analyzing small to medium-sized molecules and provides information on directly coupled protons. COSY45, similar to COSY90, uses 45-degree pulses instead of 90-degree pulses. This results in reduced sensitivity but improved resolution.
Long-range COSY (LR-COSY) extends the COSY experiment to detect scalar couplings between nuclei further apart in the molecule. It achieves this by combining multiple pulse sequences and magnetization transfers.
Relayed COSY is a variant of COSY that adds extra pulses to the standard pulse sequence to produce cross-peaks between cross-peaks, showing specific molecular connections hidden by overlapping signals.
TOCSY (Total Correlation Spectroscopy), also known as HOHAHA (Homonuclear Hartmann-Hahn Spectroscopy), reveals all through-bond connectivity between all coupled nuclei. TOCSY is especially useful for analyzing molecules with overlapping signals and complex coupling patterns.
NOESY (Nuclear Overhauser Effect Spectroscopy) measures the nuclear overhauser effect, which arises from dipole-dipole interactions between nuclei. It provides information about spatial proximity and can be used to determine the three-dimensional structure of a molecule.
ROESY (Rotating-frame Overhauser Enhancement Spectroscopy) is similar to NOESY but employs a different mechanism to obtain through-space correlations. It provides information about spatial proximity and is particularly useful for studying molecules with weak NOE signals.
In conclusion, choosing a COSY variant depends on the molecule or reaction under investigation and the desired information. The right COSY variant can be determined based on molecular size, coupling complexity, and the need for spatial or long-range connectivity data.

Homonuclear correlation spectroscopy (COSY) is a powerful technique used in Nuclear Magnetic Resonance (NMR) spectroscopy to study the correlations ...

Double Resonance Techniques: Overview

Double resonance techniques in Nuclear Magnetic Resonance (NMR) spectroscopy involve the simultaneous application of two different frequencies or radiofrequency pulses to manipulate and observe two distinct nuclear spins. One important application of double resonance is spin decoupling, which selectively suppresses coupling with one type of nucleus while observing the NMR signal from another nucleus, simplifying the spectrum and enhancing resolution.
Spin decoupling is usually achieved by irradiating the sample atoms with a suitable radio frequency (rf) pulse sequence, effectively eliminating all the coupling with one nuclide. This simplifies the observed spectrum, making it easier to analyze and understand the relationships between different nuclei.
Double resonance experiments can be classified as heteronuclear or homonuclear, depending on whether the two sets of nuclei are of different isotopes or the same isotope, respectively. They can also be selective or nonselective, depending on whether the irradiating frequency covers only a portion or all of the resonance frequencies.
In nonselective heteronuclear decoupling, samples are exposed to an appropriate radiofrequency range to remove all coupling with one nuclide. However, increased external field strengths necessitate more powerful irradiation across broader frequency ranges. In certain instruments, continuous irradiation creates enough heat to cause damage to thermally sensitive samples.
To overcome these problems, modern methods using a series of pulses and exact timing delays, like J-modulated spin echo pulse sequences, can be employed to eliminate or adjust coupling effects within the spectrum.
For example, the attached proton transfer (APT) experiment applies a J-modulated spin echo pulse sequence to focus on the phase of detected carbon signals. Carbon atoms attached to an even number of protons exhibit positive signals in the spectrum, while those bonded to an odd number of protons appear as negative signals.
It utilizes a combination of a 180&#176; proton pulse and broadband decoupling to simplify spectral interpretation and assign multiplicities. The 180&#176; pulse is applied to the protons during the APT experiment. Its role is to refocus the spin coupling evolution that naturally occurs due to interactions between protons and carbons.
Specifically, after the 90&#176; pulse creates transverse magnetization, the 180&#176; pulse ensures that the effects of coupling are frozen during the initial period where the decoupler is turned off. This means the chemical shifts evolve only during the time 1/J&#8203; (the coupling constant period) after the first 180&#176; pulse.
By carefully timing this pulse sequence, the experiment isolates carbon multiplicities by utilizing the J-coupling between carbons and their attached protons. After the coupling evolution period (1/J&#8203;), broadband decoupling is turned on. This removes the J-coupling signals, collapsing multiplets into single peaks for each carbon resonance.
The decoupling ensures that carbon signals are free of splitting, allowing for a clear differentiation of signals based on phase (positive or negative) rather than splitting patterns.
The APT technique selectively enhances carbon signals, providing valuable information about carbon-proton connectivity, the number of attached hydrogen atoms, and the overall molecular structure.

Double resonance techniques in Nuclear Magnetic Resonance (NMR) spectroscopy involve the simultaneous application of two different frequencies or ...

&sup1;H NMR of Labile Protons:  Deuterium (&sup2;H) Substitution

This lesson illustrates the role of deuterium substitution in simplifying the NMR spectrum of compounds comprising labile protons. One method employed is the use of deuterium. Amongst the three isotopes of hydrogen, deuterium (2H) has a nucleus composed of one proton and one neutron. When the D2O solvent is added to a pure dry ethanol solution, its labile proton is substituted with deuterium.
<img alt="Figure1" src="/files/ftp_upload/12280/12280-PT_Figure_1.svg" style="text-align: center; height: 700px;" />
Figure 1. The comparison of the proton NMR spectra of pure dry ethanol and the same in D2O solvent.
The signals from deuterium are not observed in a proton NMR spectrum, as deuterium&#8211;proton coupling is negligible, and no spin-spin splitting occurs between them. As shown in Figure 1, the NMR spectra of pure ethanol and ethanol in deuterium, the disappearance of the triplet in the latter, confirms that it corresponds to the labile &#8211;OH proton. Furthermore, the methylene protons that initially showed up as a multiplet transform to a quartet, proving that the multiplet is due to the coupling with the &#8211;OH proton and the methyl protons.

This lesson illustrates the role of deuterium substitution in simplifying the NMR spectrum of compounds comprising labile protons. One method employed is ...

Nuclear Overhauser Enhancement (NOE)

Irradiation of a spin-active nucleus causes an increase or decrease in the signal intensity of neighboring nuclei that are not necessarily chemically bonded or involved in J-coupling. &#160;This phenomenon, called the Nuclear Overhauser Enhancement (NOE), results from through-space interactions between the nuclear spins. The NOE effect decreases with increasing internuclear distance and is generally not observed beyond 4 angstroms. In NOE, dipole-dipole interactions between neighboring spin-active nuclei result in the transfer of nuclear spin polarization. These interactions can cause an increase or decrease in the signal intensity, which results in a positive or negative NOE, respectively.
NOE can be applied to improve the signal intensity of less sensitive nuclei such as carbon-13. Proton-decoupled carbon-13 spectra show a positive NOE effect, where the carbon signal intensities are substantially increased compared to those in proton-coupled spectra.
Targeted irradiation of specific nuclei can also reveal through-space proximity, which helps confirm stereochemistry and verify spectral peak assignments. The NOE effect is also applied in 2D NMR experiments, such as Nuclear Overhauser Effect Spectroscopy (NOESY), to determine the 3D structure of proteins.

Irradiation of a spin-active nucleus causes an increase or decrease in the signal intensity of neighboring nuclei that are not necessarily chemically ...

&sup1;H NMR of Labile Protons: Temporal Resolution

Protons bonded to heteroatoms such as nitrogen and oxygen exhibit a range of chemical shift values. This is due to the varying degree of hydrogen bonding between the proton and the heteroatom in other molecules. The extent of hydrogen bonding affects the electron density around the proton, thereby giving different chemical shift values for the protons in the proton NMR spectrum.
The &#8211;OH proton in alcohols typically appears in the range of &#948; 2 to 5 ppm but can vary depending on the specific alcohol and conditions. This &#8211;OH proton undergoes rapid proton exchange with other molecules and is referred to as a labile proton. So, the exact &#948; value of the &#8211;OH proton and the spin-spin coupling involving the &#8211;OH proton and the other protons in the alcohol depends on the rate of the &#8211;OH proton exchange. The proton exchange rate, in turn, depends on multiple factors, including the purity of the alcohol sample, temperature, and solvent.
<img alt="Figure1" src="/files/ftp_upload/12279/12279-PT_Figure_1.svg" style="text-align: center; height: 350px;" />
Figure 1. The triplet of a &#8211;OH proton in the proton NMR spectrum of neat ethanol.
For example, the &#8211;OH proton exchange in a pure dry ethanol sample is very slow on the NMR time scale, giving enough time for the spin-spin coupling. Consequently, as depicted in Figure 1, the proton NMR spectrum of pure dry ethanol shows a triplet for the &#8211;OH proton due to the spin-spin coupling with adjacent methylene protons. The methylene protons are seen as a multiplet due to the coupling with the &#8211;OH proton and the methyl protons.
The presence of trace amounts of an acid or base increases the proton exchange rate. The proton exchange becomes rapid, and the NMR spectrometer only records an average of all the possible environments for the &#8211;OH proton.
<img alt="Figure2" src="/files/ftp_upload/12279/12279-PT_Figure_2.svg" style="text-align: center; height: 325px;" />
Figure 2. The broad singlet of a &#8211;OH proton in the proton NMR spectrum of neat ethanol.
As a result, as recorded in Figure 2, the &#8211;OH proton exhibits a broad singlet. The protons from the adjacent methylene group present a quartet where the splitting is caused only by the adjoining methyl group.

Protons bonded to heteroatoms such as nitrogen and oxygen exhibit a range of chemical shift values. This is due to the varying degree of hydrogen bonding ...

&sup1;H NMR of Conformationally Flexible Molecules: Variable-Temperature NMR

The axial and equatorial protons in cyclohexane can be distinguished by performing a variable-temperature NMR experiment. In this process, except for one proton, the remaining eleven protons are replaced by deuterium. The deuterium substitution avoids the possible peak splitting caused by the spin-spin coupling between the adjacent protons. The remaining proton flips between the axial and equatorial positions.
<img alt="Figure1" src="/files/ftp_upload/13016/13016-PT_Figure_1.svg" style="text-align: center; height: 480px;" />
Figure 1. The temperature-dependent proton NMR spectra of cyclohexane.
Figure 1 depicts the proton NMR spectrum of the deuterium substituted sample, recorded at various temperatures. At room temperature, the rapid ring flipping of cyclohexane results in a single sharp peak. As the temperature is lowered to &#8722;60&#176;C, the rate of chair-chair interconversion reduces, resulting in the broadening of the peak.
Further lowering of the temperature broadens the peak, forming a saddle that splits into two peaks. On reaching a temperature lower than &#8722;89&#176;C, two sharp, well-resolved peaks corresponding to the equatorial and axial protons are formed. The peaks corresponding to the equatorial and axial protons occur at &#948; 1.62 and 1.14, respectively. At such low temperatures, the rate of chair-chair interconversion is reduced significantly, enabling the detection of the two distinct sets of protons on the NMR time scale.

The axial and equatorial protons in cyclohexane can be distinguished by performing a variable-temperature NMR experiment. In this process, except for one ...

&sup1;H NMR of Conformationally Flexible Molecules: Temporal Resolution

At room temperature, the chair conformer of cyclohexane undergoes rapid ring flipping between two equivalent chair conformers at a rate of approximately 105 times per second. These two chair conformers are in equilibrium. The rapid ring flipping results in the interconversion of the axial proton to an equatorial proton and an equatorial to the axial proton. Such interconversions are too rapid and cannot be detected on the NMR timescale. Hence, the NMR spectrometer cannot distinguish between the axial and equatorial protons, resulting in a single peak at &#948; 1.4.
Similarly, NMR averages all the conformations of any molecule with rapid conformational equilibria. For example, the CH3 protons in bromoethane have a single resonance and coupling constant for splitting by the CH2 protons due to the rapid internal rotation of the carbon-carbon bond. Lastly, besides conformational equilibria, the time-averaging effect of NMR spectroscopy is also observed in some chemical reactions.

At room temperature, the chair conformer of cyclohexane undergoes rapid ring flipping between two equivalent chair conformers at a rate of approximately ...

Mass Spectrometry: Carboxylic Acid, Ester, and Amide Fragmentation

The fragmentation patterns observed for compounds such as carboxylic acids, esters, and amides in the mass spectra include &#9082;-cleavage and McLafferty rearrangement. Fragmentation by &#9082;-cleavage preferentially occurs at the carbon-carbon bond at the &#9082;-position next to the carboxylic group to generate a neutral radical and a cation. Long chain compounds with hydrogen at their &#947;-carbon undergo McLafferty rearrangement to give a radical cation and a neutral alkene.
For example, the fragmentation of butyramide is demonstrated in Figure 1. The molecular ion peak of butyramide, which contains one nitrogen atom, shows an odd mass-to-charge ratio of 87. Fragmentation of butyramide molecular ion by &#9082;-cleavage produces a cation at a mass-to-charge ratio 44. In addition to &#9082;-cleavage, butyramide molecular ion also undergoes fragmentation via McLafferty rearrangement. The base peak at the mass-to-charge ratio 59 arises due to McLafferty rearrangement.
<img alt="Figure1" src="/files/ftp_upload/13051/13051_PT_Figure_1.svg" style="text-align: center; height: 250px;" />

The fragmentation patterns observed for compounds such as carboxylic acids, esters, and amides in the mass spectra include &#9082;-cleavage and McLafferty ...

Chemical Ionization (CI) Mass Spectrometry

The molecular ion peak of a molecule in the mass spectrum provides vital information for molecular identification. However, conventional electron impact ionization can lead to the rapid dissociation of some molecular ions before they reach the detector. A milder ionization method is required to increase the lifetime of such ionized analyte molecules. Chemical ionization (CI) is a gas-phase protonation reaction useful for mass-analyzing analyte molecules that are easily protonated to yield the corresponding conjugate acid. In this process, the sample is mixed with an excess reagent gas, which ensures the electron impact occurs primarily on the reagent gas. The charged species formed from the reagent protonates the analyte molecule, producing a relatively stable protonated analyte (conjugate acid) compared to the molecular ion. This results in an M+1 peak in the mass spectrum. The conjugate acid may then undergo fragmentation that generates additional signals.
For example, the CI of di-sec-butyl ether in methane gas illustrates this process. When the ether is mixed with excess methane gas as a reagent, electron impact occurs on methane rather than the ether. The resulting methane radical cation can react with another methane molecule to generate a methane radical and a methanium ion. The methanium ion is a source of gas-phase protons, which can protonate the ether to form its conjugate acid. The sequential reactions during the chemical ionization of di-sec-butyl ether are depicted in Figure 1.
<img alt="Figure1" src="/files/ftp_upload/12300/12300_PT_Figure_1.svg" style="text-align: center; height: 175px;" />
Figure 1: Chemical ionization of di-sec-butyl ether methane mixture.
This conjugate acid of the ether (m/z = 131) is relatively more stable than the molecular ion (m/z = 130) of ether formed via the conventional electron impact ionization. In the traditional route, the molecular ion undergoes fragmentation via &#945; cleavage, giving a signal at m/z = 101. Figure 2 illustrates the reactions that occur during electron impact ionization directly on di-sec-butyl ether.
<img alt="Figure2" src="/files/ftp_upload/12300/12300_PT_Figure_2.svg" style="text-align: center; height: 175px;" />
Figure 2: Electron impact ionization of di-sec-butyl ether and fragmentation of the molecular ion.
So, the mass spectra of di-sec-butyl ether ionized via CI feature an M+1 peak at m/z = 131. On the other hand, mass spectra of di-sec-butyl ether ionized via electron impact ionization do not show any peak at the m/z value of its molecular weight. Figures 3a and 3b show the mass spectra of di-sec-butyl ether ionized via the electron impact and chemical ionization methods, respectively.
<img alt="Figure3" src="/files/ftp_upload/12300/12300_PT_Figure_3.svg" style="text-align: center; height: 225px;" />
Figure 3:&#160;a) No m/z = 130 peak is visible in the mass spectrum obtained via electron impact ionization of di-sec-butyl ether. b) The m/z = 131 peak is clearly visible in the mass spectrum obtained via chemical ionization of di-sec-butyl ether.

The molecular ion peak of a molecule in the mass spectrum provides vital information for molecular identification. However, conventional electron impact ...

Mass Spectrometry: Alkyl Halide Fragmentation

Chlorine isotopes exist as 35Cl and 37Cl in a 3:1 ratio, while bromine isotopes exist as 79Br and 81Br in a 1:1 ratio. The mass spectrum of alkyl halides typically produces two distinct molecular ion peaks, the molecular ion peak, [M], and the molecular ion plus two, [M + 2] peak. The relative heights of these two peaks are proportional to the isotopic abundance ratios of the halide. For example, 2&#8208;chloropropane and 1&#8208;bromopropane display two peaks with relative peak heights in a 3:1 and 1:1 ratio, respectively.
Alkyl halides typically lose a non-bonding electron from the halogen to form molecular ions. The base peak results from the heterolytic cleavage of the carbon&#8211;halogen bond, where the bonding electrons go to the most electronegative atom, forming a cation and halogen atom. Interestingly, the &#9082;-cleavage is observed only in alkyl chlorides, not alkyl bromides. In alkyl chlorides, the&#160; C&#8211;Cl and C&#8211;C bonds exhibit similar strengths, while in alkyl bromides, the C&#8211;Br bond is weaker than the C&#8211;C bond. Consequently, the alkyl chlorides form a stable cation, where the positive charge is shared between the two atoms.
While less commonly discussed, fluoroalkanes and iodoalkanes exhibit unique fragmentation behavior. Fluoroalkanes, due to the strength of the C&#8211;F bond and the presence of only one isotope (19F), show limited fragmentation and lack isotopic peaks. Iodoalkanes, with their weak C&#8211;I bond and a single isotope (127I), predominantly fragment by losing iodine, resulting in simpler spectra with less isotopic splitting.

Chlorine isotopes exist as 35Cl and 37Cl in a 3:1 ratio, while bromine isotopes exist as 79Br and 81Br in a 1:1 ratio. The mass spectrum of alkyl halides ...

Electrospray Ionization (ESI) Mass Spectrometry

Higher molecular weight biomolecules are nonvolatile compounds that may decompose before ionizing or vaporizing during mass analysis with conventional electron impact ionization methods. Accordingly, electrospray ionization (ESI) is the favored method for vaporizing and ionizing biomolecules as it circumvents rapid fragmentation and enables the recording of mass signals for the entire biomolecule.
ESI utilizes electrical energy to transfer ions from the liquid phase of the sample into the gaseous phase. The analyte biomolecule is premixed with an ionic liquid&#8212;a nonmolecular compound serving as the ionization source. The solution is sprayed through a high-voltage capillary to generate a fine aerosol. The voltage difference applied between the capillary and the entrance of the analysis chamber causes the movement of charged droplets toward the analysis chamber. The ionic liquid from the aerosol evaporates during this movement, leaving behind a variably protonated or ionized analyte molecule. These charged species are detected in the mass spectrum at an m/z value equivalent to the sum of the analyte molecule&#39;s molecular mass and the ions&#39; molecular weight from the ionic liquid associated with the analyte molecule.
The position of mass signals varies depending on the type of cations present in the ionic liquid. For example, the presence of sodium ions in the ionic liquid leads to an (M+23) peak in the mass spectra, while the presence of a proton results in an (M+1) peak.

Higher molecular weight biomolecules are nonvolatile compounds that may decompose before ionizing or vaporizing during mass analysis with conventional ...

Matrix-Assisted Laser Desorption Ionization (MALDI)

Matrix-assisted laser desorption ionization (MALDI) is a powerful analytical technique used in mass spectrometry. It enables the identification and characterization of various biomolecules, including proteins, peptides, nucleic acids, and carbohydrates. MALDI spectrometry is widely employed in biological and medical research, as well as in fields like pharmacology and biochemistry.
The analyte of interest, a biomolecule or a mixture of biomolecules, is mixed with a suitable matrix material. The matrix is usually an organic compound, such as a small organic acid or a crystalline substance, that facilitates ionization. This analyte-matrix mixture is then deposited onto a target surface, inserted into the mass spectrometer, and dried. During drying, the matrix forms small crystals that incorporate the analyte molecules within their structure.
Once the sample is prepared, a pulsed laser is directed onto the target surface. The matrix molecules absorb the laser beam energy, causing them to heat up and vaporize rapidly. This process is known as laser desorption. As the matrix molecules vaporize, they carry the embedded analyte molecules. The vaporized analyte molecules become ionized through a process called proton transfer. The proton transfer occurs between the matrix and the analyte molecule. The matrix molecule donates a proton to the analyte molecule, resulting in the formation of protonated ions. The analyte ions are then accelerated by an electric field and further separated based on their mass-to-charge ratio in a time-of-flight mass analyzer.
The mass spectrum obtained from MALDI spectrometry provides valuable information about the mass and relative abundance of the analyzed biomolecules.

Matrix-assisted laser desorption ionization (MALDI) is a powerful analytical technique used in mass spectrometry. It enables the identification and ...

Mass Spectrometry: Aldehyde and Ketone Fragmentation

In mass spectrometry, the fragmentation of aliphatic aldehydes and ketones generally occurs through three key mechanisms: &#945;-cleavage, inductive cleavage, and the McLafferty rearrangement.
<ol>
	<li>&#945;-Cleavage 
	&#945;-Cleavage is a common fragmentation in carbonyl compounds where the bond adjacent to the carbonyl group is broken. This process produces an alkyl radical and an acylium cation, which is often detected in the mass spectrum due to its stability.</li>
	<li>Inductive Cleavage 
	In inductive cleavage, fragmentation yields an acyl radical and an alkyl cation. This occurs when electrons are drawn toward the carbonyl, weakening adjacent bonds and resulting in a distinctive fragmentation pattern. For example, in the mass spectrum of 5-methyl-2-hexanone, inductive cleavage produces an alkyl cation at a mass-to-charge (m/z) ratio of 71.</li>
	<li>McLafferty Rearrangement 
	The McLafferty rearrangement is a specific fragmentation pattern for carbonyl compounds with &#947;-hydrogen (hydrogen on the third carbon from the carbonyl group). The molecule undergoes a six-membered cyclic transition in this rearrangement, yielding a radical cation and a neutral alkene. For 5-methyl-2-hexanone, this rearrangement results in a peak at m/z 58.</li>
</ol>
Example: Fragmentation of 5-methyl-2-hexanone 
In the mass spectrum of 5-methyl-2-hexanone, the molecular ion undergoes these fragmentation patterns:
<ol style="list-style-type: circle;">
	<li>Inductive cleavage produces an alkyl cation at m/z 71.</li>
	<li>&#945;-Cleavage results in the base peak at m/z 43.</li>
	<li>McLafferty rearrangement creates a distinct peak at m/z 58.</li>
</ol>
An additional diagnostic feature in aldehydes is the M&#8722;1 peak, which arises due to the &#945;-cleavage of the aldehyde proton. In mass spectrometric analysis, this peak can help identify aldehydes, specifically among other carbonyl compounds.
Understanding these fragmentation pathways is crucial for interpreting mass spectra, particularly in identifying functional groups and distinguishing between similar compounds.

In mass spectrometry, the fragmentation of aliphatic aldehydes and ketones generally occurs through three key mechanisms: &#945;-cleavage, inductive ...

Mass Spectrometry: Alcohol Fragmentation

Alcohols (R-OH) ionize to lose one non-bonded electron from the oxygen atom, forming molecular ions. Due to their tendency to fragment rapidly, the intensity of the molecular ion peak in the mass spectrum is weak or sometimes absent. The fragmentation patterns for alcohols occur in two ways, i.e. &#9082;-cleavage and dehydration. During &#9082;-cleavage, the bond at the &#9082;-position adjacent to the hydroxyl group cleaves to give a resonance-stabilized cation and a radical. However, intramolecular dehydration involves losing a water molecule from an alcohol, forming an alkene cation, which shows a peak at M&#8722;18. Consider the fragmentation of butanol as shown below. &#9082;-cleavage produces a base peak at a mass-to-charge ratio of 31. In the case of dehydration, the fragmentation forms an alkene radical cation at a mass-to-charge ratio of 56.
<img alt="Figure1" src="/files/ftp_upload/13046/13046-PT_Figure_1.svg" style="text-align: center; height: 175px;" />

Alcohols (R-OH) ionize to lose one non-bonded electron from the oxygen atom, forming molecular ions. Due to their tendency to fragment rapidly, the ...

Mass Spectrometry: Amine Fragmentation

Amines can be identified using mass spectroscopy based on their characteristic fragmentation patterns. The molecular ions of amines undergo fragmentation via &#9082;-cleavage. The &#9082;-cleavage of the carbon-carbon bonds in amines generates an alkyl radical and resonance-stabilized nitrogen-containing cation.
In amines, the number of nitrogen atoms affects the mass of the molecular ion, which is described by the nitrogen rule of mass spectrometry. This rule states that a compound containing a single or an odd number of nitrogen atoms produces a molecular ion with an odd molecular weight, while a compound with no or an even number of nitrogen atoms generates a molecular ion with an even molecular weight.
For example, the mass spectrum of 3-methyl-1-butanamine, which contains one nitrogen atom, displays a molecular ion having an odd mass-to-charge ratio of 87. Fragmentation of this molecular ion via &#9082;-cleavage produces a base peak, which features a mass signal at a mass-to-charge ratio of 30, corresponding with the loss of the 2-methyl propyl radical.
Similarly, the fragmentation of triethylamine via &#9082;-cleavage generates a cation at a mass-to-charge ratio of 86. The molecular ion peak shows an odd mass-to-charge ratio of 101, as shown below.
<img alt="Figure1" src="/files/ftp_upload/13048/13048_PT_Figure_1.svg" style="text-align: center; height: 105px;" />

Amines can be identified using mass spectroscopy based on their characteristic fragmentation patterns. The molecular ions of amines undergo fragmentation ...

Mass Spectrometry: Cycloalkene Fragmentation

The molecular ions of cycloalkenes undergo fragmentation via a retro-Diels&#8211;Alder reaction.

The reaction proceeds via the cleavage of two carbon-carbon bonds in the cycloalkene to yield ethene. The remaining part of the cycloalkene structure is a dienyl radical cation with a molecular weight of 28 u lower than the molecular ion. This fragmentation pathway is similar to the fragmentation of cycloalkanes releasing ethene, differing only in the resultant radical cation. An alkyl species forms from the cycloalkane, whereas a dienyl species originates from the cycloalkene.

Retro-Diels&#8211;Alder reactions of cycloalkenes are also similar to the McLafferty-rearrangement-type fragmentation observed in acyclic alkenes with hydrogen on the &#947; carbon. In both cases, cleavage occurs at two positions, yielding an ethene molecule and an alkenyl species. In acyclic alkenes, the cleavage occurs at one carbon-carbon bond and a carbon-hydrogen bond, along with rearranging hydrogen from one carbon to another. In cyclic alkenes, cleavage occurs at two carbon&#8211;carbon bonds without any atomic rearrangement. Figure 1 depicts the fragmentation of cyclohexene via a retro-Diels&#8211;Alder reaction.
<img alt="Figure1" src="/files/ftp_upload/13044/13044-PT_Figure_1.svg" style="text-align: center; height: 90px;" />
Figure 1: Fragmentation of cyclohexene via a retro-Diels&#8211;Alder reaction.
In addition to the retro-Diels&#8211;Alder reaction, branched cycloalkenes exhibit fragmentation via cleavage of the side chain to form a cycloalkene cation. For example, the fragmentation of 1-methyl-1-cyclohexene via a retro-Diels&#8211;Alder reaction and side-chain cleavage are shown in Figure 2.
<img alt="Figure2" src="/files/ftp_upload/13044/13044-PT_Figure_2.svg" style="text-align: center; height: 225px;" />
Figure 2: Fragmentation of 1-methyl-1-cyclohexene via (top) a retro-Diels&#8211;Alder reaction; (bottom) side-chain cleavage.
The corresponding signals of the isoprenyl radical cation and the cyclohexenyl cation are evident in the mass spectrum of 1-methyl-1-cyclohexene shown in Figure 3.
<img alt="Figure3" src="/files/ftp_upload/13044/13044-PT_Figure_3.svg" style="text-align: center; height: 250px;" />
Figure 3: Mass spectrum of 1-methyl-1-cyclohexene.

The molecular ions of cycloalkenes undergo fragmentation via a retro-Diels&#8211;Alder reaction.

The reaction proceeds via the cleavage of two ...

Mass Spectrometry: Alkyne Fragmentation

The fragmentation of alkynes preferentially occurs at the carbon&#8211;carbon bond between the &#945; and &#946; carbon of the alkyne bond to generate a 3-propynyl cation (or propargyl cation). In terminal alkynes, there is the only type of fragmentation that yields the 3-propynyl cation. The unsubstituted 3-propynyl cation exhibits a peak at a mass-to-charge ratio of 39. In internal alkynes, the 3-propynyl cation is substituted. For example, 2-pentyne fragments into methyl-substituted 3-propynyl cation, which subsequently features as a mass signal at the mass-to-charge ratio of 56. The 3-propynyl cation is resonance-stabilized, and the corresponding mass signal is intense in the mass spectrum of alkynes. Figure 1 shows the fragmentation of 1-pentyne into an ethyl radical and a resonance stabilized 3-propynyl cation.
<img alt="Figure1" src="/files/ftp_upload/13045/13045-PT_Figure_1.svg" style="text-align: center; height: 115px;" />
Figure 1: Fragmentation of 1-pentyne molecular ion to yield the 3-propynyl cation.
Another fragmentation pathway observed in terminal alkynes is the loss of hydrogen from the terminal sp carbon. This results in a mass signal with a mass-to-charge ratio of one unit less than the molecular ion. This M&#8211;1 peak is very intense and becomes the base peak in the mass spectra of many alkynes, so it can be used to identify alkynes.
<img alt="Figure2" src="/files/ftp_upload/13045/13045-PT_Figure_2.svg" style="text-align: center; height: 275px;" />
Figure 2: The mass spectrum of 1-pentyne.

The fragmentation of alkynes preferentially occurs at the carbon&#8211;carbon bond between the &#945; and &#946; carbon of the alkyne bond to generate a ...

Mass Spectrometry: Aromatic Compound Fragmentation

Upon ionization, aromatic compounds generate a molecular ion that is observed as a prominent peak in their mass spectra. For example, the molecular ion peak for benzene appears at a mass-to-charge ratio of 78, while toluene is observed at a mass-to-charge ratio of 92. The molecular ion benzene is highly stable and does not readily undergo further fragmentation due to the significant amount of energy required to disrupt the aromatic stability of the benzene ring. In contrast, the molecular ion of alkyl&#8208;substituted benzenes, such as toluene, can undergo fragmentation by losing a hydrogen atom, forming a benzylic carbocation. This carbocation can rearrange to form the resonance-stabilized tropylium cation, which appears in the mass spectra as a strong peak. In the case of toluene, this strong peak is observed at a mass-to-charge ratio of 91.

Upon ionization, aromatic compounds generate a molecular ion that is observed as a prominent peak in their mass spectra. For example, the molecular ion ...

Mass Spectrometry: Long-Chain Alkane Fragmentation

The molecular ions of linear alkanes prefer to fragment at the carbon-carbon bond away from the end of the chain since the cleavage of an inner bond creates a stable carbocation and a stable radical. Consequently, the mass signals of linear alkanes feature intense peaks in the middle of the mass-to-charge ratio plot with weaker peaks on either end. The fragmentation of each carbon-carbon bond with the release of a methyl group in each splitting leads to prominent peaks in the mass spectra separated by 14 u. Smaller mass signals near each prominent peak result arise from secondary fragmentation at the carbon-hydrogen bond.
For example, consider the fragmentation pattern of n-hexane shown in Figure 1 and the corresponding mass spectra in Figure 2.
<img alt="Figure1" src="/files/ftp_upload/12299/12299-PT_Figure_1.svg" style="text-align: center; height: 500px;" />
Figure 1: Fragmentation of n-hexane molecular ion.
<img alt="Figure2" src="/files/ftp_upload/12299/12299-PT_Figure_2.svg" style="text-align: center; height: 275px;" />
Figure 2: Mass spectrum of n-hexane.
The signals at a mass-to-charge ratio of 71, 57, 43, 29, and 15 indicate that the cleavage can occur at all carbon-carbon bonds in the molecule. However, the relative abundance of these peaks varies. The difference between molecular ion signal and signal at 71 indicates the separation of methyl groups (M.W. = 15 u) group from molecular ions. Further release of a CH2 group from that fragment (M.W. = 14 u) results in a signal at 57. The signals at 43, 29, and 15 are due to the subsequent releases of CH2 groups. The abundance of signals at 15 and 71 is minimal due to the least probability for the formation of unstable methyl carbocation or a methyl radical, respectively. The base peak at 43 indicates the most preferred fragmentation, which yields a pair of stable carbocation and radical.

The molecular ions of linear alkanes prefer to fragment at the carbon-carbon bond away from the end of the chain since the cleavage of an inner bond ...

Aerodynamic Performance of a Model Aircraft: The DC-6B

Source: Jose Roberto Moreto and Xiaofeng Liu, Department of Aerospace Engineering, San Diego State University, San Diego, CA
The low-speed wind tunnel is a valuable tool to study aircraft aerodynamic characteristics and evaluate aircraft performance and stability. Using a scale model of a DC-6B aircraft that has a removable tail and a 6-component external aerodynamic force balance, we can measure the lift coefficient (CL), drag coefficient (CD), pitching moment coefficient (CM), and yaw moment coefficient (CN) of the model airplane with and without its tail and evaluate the effect of the tail on aerodynamic efficiency, longitudinal stability and directional stability.
In this demonstration, airplane aerodynamic characteristics and flight performance and stability are analyzed using the aerodynamic force balance measurement method. This method is widely used in aerospace industries and research labs for aircraft and rocket development. Here, a model DC-6B airplane is analyzed at different flow conditions and configurations, and its behavior is analyzed when it is subjected to sudden changes.

Forces at a Non-zero Windspeed in the DC-6B Model Aircraft

模型航空機の空力性能:DC-6B

Source: Jose Roberto Moreto and Xiaofeng Liu, Department of Aerospace Engineering, San Diego State University, San Diego, CA
The low-speed wind tunnel is ...

Propeller Characterization: Variations in Pitch, Diameter, and Blade Number on Performance

Source: Shreyas Narsipur, Mechanical and Aerospace Engineering, North Carolina State University, Raleigh, NC
A propeller is a twisted airfoil, where the angle of the chord changes with respect to the location, along the radial station, as shown in Figure 1. Propellers are widely used in aircraft and watercraft propulsion systems thereby necessitating detailed characterizations of propellers to design high performance vehicles.
<img src="/files/ftp_upload/10460/10460fig1.jpg" />
Figure 1. Chord, thickness, and pitch at a radial station.
One of the defining characteristics of a propeller is the pitch/twist. The pitch of the propeller, generally given in units of length, is the theoretical distance the propeller will travel through the air in one single revolution. However, due to the drag force on the aircraft and the propeller, the propeller never travels its theoretical distance. The actual distance travelled is referred to as the effective pitch of the propeller, and the difference between the theoretical or geometric pitch and the effective pitch is referred to as propeller slip, as illustrated in Figure 2.
<img src="/files/ftp_upload/10460/10460fig2.jpg" />
Figure 2. Representation of pitch and slip.
In this demonstration, seven propellers are characterized using a propeller test rig in a subsonic wind tunnel. This is followed by a detailed parametric study to analyze the effects of variations in pitch, diameter, and number of blades on propeller performance.

Propeller Characterization: Pitch, Diameter and Blade Number

プロペラの特性評価:性能のピッチ、直径、ブレード数の変動

Source: Shreyas Narsipur, Mechanical and Aerospace Engineering, North Carolina State University, Raleigh, NC
A propeller is a twisted airfoil, where the ...

Airfoil Behavior: Pressure Distribution over a Clark Y-14 Wing

Source: David Guo, College of Engineering, Technology, and Aeronautics (CETA), Southern New Hampshire University (SNHU), Manchester, New Hampshire
An airfoil is a 2-dimensional wing section that represents critical wing performance characteristics. The pressure distribution and lift coefficient are important parameters that characterize the behavior of airfoils. The pressure distribution is directly related to the lift generated by airfoils. A Clark Y-14 airfoil, which is used in this demonstration, has a thickness of 14% and is flat on the lower surface from 30% of chord length to the back.
Here we will demonstrate how the pressure distribution around an airfoil is measured using a wind tunnel. A Clark Y-14 airfoil model with 19 pressure ports is used to collect pressure data, which is used to estimate the lift coefficient.

翼挙動:クラークY-14翼上の圧力分布

Source: David Guo, College of Engineering, Technology, and Aeronautics (CETA), Southern New Hampshire University (SNHU), Manchester, New Hampshire
An ...

Clark Y-14 Wing Performance: Deployment of High-lift Devices (Flaps and Slats)

Source: David Guo, College of Engineering, Technology, and Aeronautics (CETA), Southern New Hampshire University (SNHU), Manchester, New Hampshire
A wing is the major lift-generating apparatus in an airplane. Wing performance can be further enhanced by deploying high-lift devices, such as flaps (at the trailing edge) and slats (at the leading edge) during takeoff or landing.
In this experiment, a wind tunnel is utilized to generate certain airspeeds, and a Clark Y-14 wing with a flap and slat is used to collect and calculate data, such as the lift, drag and pitching moment coefficient. A Clark Y-14 airfoil is shown in Figure 1 and has a thickness of 14% and is flat on the lower surface from 30% of the chord to the back. Here, wind tunnel testing is used to demonstrate how the aerodynamic performance of a Clark Y-14 wing is affected by high-lift devices, such as flaps and slats.
<img src="/files/ftp_upload/10454/10454fig1.jpg" />
Figure 1. Clark Y-14 airfoil profile.

Clark Y-14 Wing Performance: Deployment of High-lift Devices

クラークY-14ウィング性能:ハイリフトデバイス(フラップとスラット)の展開

Source: David Guo, College of Engineering, Technology, and Aeronautics (CETA), Southern New Hampshire University (SNHU), Manchester, New Hampshire
A wing ...

Turbulence Sphere Method: Evaluating Wind Tunnel Flow Quality

Source: Jose Roberto Moreto and Xiaofeng Liu, Department of Aerospace Engineering, San Diego State University, San Diego, CA
Wind tunnel tests are useful in the design of vehicles and structures that are subjected to airflow during their use. Wind tunnel data are generated by applying a controlled air flow to a model of the object being studied. The test model usually has a similar geometry but is a smaller scale compared to the full-sized object. To ensure accurate and useful data is collected during low speed wind tunnel tests, there must be a dynamic similarity of the Reynolds number between the tunnel flow field over the testing model and the actual flow field over the full-sized object.
In this demonstration, wind tunnel flow over a smooth sphere with well-defined flow characteristics will be analyzed. Because the sphere has well-defined flow characteristics, the turbulence factor for the wind tunnel, which correlates the effective Reynolds number to the test Reynolds number, can be determined, as well as the free-stream turbulence intensity of the wind tunnel.

Turbulence Measurements at Varying Air Speeds

乱流球法:風洞流量の評価

Source: Jose Roberto Moreto and Xiaofeng Liu, Department of Aerospace Engineering, San Diego State University, San Diego, CA
Wind tunnel tests are useful ...

Cross Cylindrical Flow: Measuring Pressure Distribution and Estimating Drag Coefficients

Source: David Guo, College of Engineering, Technology, and Aeronautics (CETA), Southern New Hampshire University (SNHU), Manchester, New Hampshire
The pressure distributions and drag estimations for cross cylindrical flow have been investigated for centuries. By ideal inviscid potential flow theory, the pressure distribution around a cylinder is vertically symmetric. The pressure distribution upstream and downstream of the cylinder is also symmetric, which results in a zero-net drag force. However, experimental results yield very different flow patterns, pressure distributions and drag coefficients. This is because the ideal inviscid potential theory assumes irrotational flow, meaning viscosity is not considered or taken into account when determining the flow pattern. This differs significantly from reality.
In this demonstration, a wind tunnel is utilized to generate a specified airspeed, and a cylinder with 24 ports of pressure is used to collect pressure distribution data. This demonstration illustrates how the pressure of a real fluid flowing around a circular cylinder differs from predicted results based on the potential flow of an idealized fluid. The drag coefficient will also be estimated and compared to the predicted value.

Cross Cylindrical Flow: Pressure Distribution &amp; Drag Coefficients

円筒形のクロスフロー:圧力分布の測定とドラッグ係数の推定

Source: David Guo, College of Engineering, Technology, and Aeronautics (CETA), Southern New Hampshire University (SNHU), Manchester, New Hampshire
The ...

Nozzle Analysis: Variations in Mach Number and Pressure Along a Converging and a Converging-diverging Nozzle

Source: Shreyas Narsipur, Mechanical and Aerospace Engineering, North Carolina State University, Raleigh, NC
A nozzle is a device that is commonly used to accelerate or decelerate flow by virtue of its varying cross-section. Nozzles are widely used in aerospace propulsion systems. In rockets, propellant that is ejected from the chamber is accelerated through a nozzle to create a reaction force that propels the system. In jet engines, a nozzle is used to transform energy from a high-pressure source into kinetic energy of the exhaust to produce thrust. The isentropic model along the nozzle is sufficient for a first-order analysis as the flow in a nozzle is very rapid (and thus adiabatic to a first approximation) with very little frictional loses (because the flow is nearly one-dimensional with a favorable pressure gradient, except if shock waves form and nozzles are relatively short).
In this experiment, two types of nozzles are mounted on a nozzle test rig, and a pressure flow is created using a compressed air source. The nozzles are run for different back-pressure settings to analyze the internal flow in the nozzles under varying flow conditions, identify the various flow regimes, and compare the data to theoretical predictions.

Nozzle Analysis: Mach Number and Converging-diverging Nozzle

ノズル解析:収束と収束発散ノズルに沿ったマッハ数と圧力の変動

Source: Shreyas Narsipur, Mechanical and Aerospace Engineering, North Carolina State University, Raleigh, NC
A nozzle is a device that is commonly used to ...

Schlieren Imaging: A Technique to Visualize Supersonic Flow Features

Source: Jose Roberto Moreto, Jaime Dorado, and Xiaofeng Liu, Department of Aerospace Engineering, San Diego State University, San Diego, CA
Military jet fighters and projectiles can fly at incredible speeds that exceed the speed of sound, which means they are traveling at a supersonic speed. The speed of sound is the speed at which a sound wave propagates through a medium, which is 343 m/s. Mach numbers are used to gauge the flight speed of an object relative to the speed of sound.
An object traveling at the speed of sound would have a Mach number of 1.0, whereas an object traveling faster than the speed of sound has a Mach number greater than 1.0. The compressibility effects of air must be accounted for when traveling at such speeds. A flow is considered compressible when the Mach number is greater than 0.3. In this demonstration, Mach 2.0 supersonic flow over a cone will be analyzed by visualizing the formation of shock waves and compression waves in compressible flow using a Schlieren system.

Schlieren Imaging: Visualization of Supersonic Flow Features

シュリーレンイメージング:超音速流機能を可視化する技術

Source: Jose Roberto Moreto, Jaime Dorado, and Xiaofeng Liu, Department of Aerospace Engineering, San Diego State University, San Diego, CA
Military jet ...

Flow Visualization in a Water Tunnel: Observing the Leading-edge Vortex Over a Delta Wing

Source: Jose Roberto Moreto, Gustaaf Jacobs and Xiaofeng Liu, Department of Aerospace Engineering, San Diego State University, San Diego, California
The delta wing, shown in Figure 1D, is a popular design in high-speed airplanes due to its superb performance in transonic and supersonic flight regimes. This type of wing has a small aspect ratio and high sweep angle, which reduces drag at high subsonic, transonic and supersonic flight regimes. The aspect ratio is defined as the wing span divided by the average chord <img align="middle" src="/files/ftp_upload/10459/10459eq1a.jpg" />.
An important advantage of the delta wing is its high stall angle. The stall of a delta wing is delayed compared to the stall of a high aspect ratio wing. This is because the lift of a delta wing is enhanced by the leading-edge vortex over the wing.
An effective way to observe this vortex flow phenomenon and study the vortex breakdown in a delta wing is by visualizing the flow in a water tunnel. By injecting dye in the flow surrounding a model from dye ports on the leading-edge, the vortex development and breakdown can be observed and its position measured. The data can also be used to estimate the stall angle.
<img src="/files/ftp_upload/10459/10459fig1.jpg" />
Figure 1. Typical wing planform shapes: A) Rectangular, with constant chord along span, B) elliptical, C) tapered, with variable chord along the span, and D) delta wing, an aft-swept wing with zero taper ratio.

Flow in a Water Tunnel: Leading-edge Vortex over a Delta Wing

水洞における流れの可視化:デルタウィング上の最先端渦の観察

Source: Jose Roberto Moreto, Gustaaf Jacobs and Xiaofeng Liu, Department of Aerospace Engineering, San Diego State University, San Diego, California
The ...

Surface Dye Flow Visualization: A Qualitative Method to Observe Streakline Patterns in Supersonic Flow

Flow visualization around or on a body is an important tool in aerodynamics research. It provides a method to qualitatively and quantitatively study flow structure, and it also helps researchers theorize and verify fluid flow behavior. Flow visualization can be divided into two categories: off-the-surface visualization and surface flow visualization. Off-the-surface flow visualization techniques involve determining the flow characteristics around the body of interest. They include but are not restricted to particle image velocimetry (PIV), Schlieren imaging, and smoke flow visualization. These techniques can provide qualitative as well as quantitative data on the flow around a body. However, these techniques are generally expensive and difficult to set-up. Surface flow visualization techniques, on the other hand, involve coating the body of interest with a dye to study flow on the surface. These techniques, which are more invasive in practice, include dye flow visualization and, more recently, use pressure-sensitive paint, which gives a detailed image of the flow on the body&#39;s surface. This allows researchers to visualize different flow features, including laminar bubbles, boundary layer transitions, and flow separation. Dye flow visualization, the technique of interest in the current experiment, provides a qualitative picture of the surface flow and is one of the simplest and most cost-effective surface flow visualization methods, specifically for visualizing gaseous flows on a body.
In this experiment, the surface flow behavior on six bodies are studied in supersonic flow. The streakline patterns are obtained using the dye flow visualization technique, and the flow paths, degree of flow attachment and separation, and location and type of shocks are identified and studied from the flow images.

Surface Dye Flow: Streakline Patterns in Supersonic Flow

表面染料フロー可視化:超音速流のストリークラインパターンを観察する定性的方法

Flow visualization around or on a body is an important tool in aerodynamics research. It provides a method to qualitatively and quantitatively study flow ...

Pitot-static Tube: A Device to Measure Air Flow Speed

Source: David Guo, College of Engineering, Technology, and Aeronautics (CETA), Southern New Hampshire University (SNHU), Manchester, New Hampshire
A Pitot-static tube is widely used for measuring unknown speeds in air flow, for example, it is used to measure airplane airspeed. By Bernoulli's principle, airspeed is directly related to variations in pressure. Therefore, the Pitot-static tube senses the stagnation pressure and static pressure. It is connected to a manometer or pressure transducer to obtain pressure readings, which allows airspeed prediction.
In this experiment, a wind tunnel is utilized to generate certain airspeeds, which is compared against Pitot-static tube predictions. The sensitivity of the Pitot-static tube due to misalignment with respect to flow direction is also investigated. This experiment will demonstrate how air flow speed is measured using a Pitot-static tube. The goal will be to predict the air flow speed based on the pressure measurements obtained.

ピトースタティックチューブ:空気の流速を測定する装置

Source: David Guo, College of Engineering, Technology, and Aeronautics (CETA), Southern New Hampshire University (SNHU), Manchester, New Hampshire
A ...

Constant Temperature Anemometry: A Tool to Study Turbulent Boundary Layer Flow

Source: Xiaofeng Liu, Jose Roberto Moreto, and Jaime Dorado, Department of Aerospace Engineering, San Diego State University, San Diego, California
A boundary layer is a thin flow region immediately adjacent to the surface of a solid body immersed in flow field. In this region, viscous effects, such as the viscous shear stress, dominate, and the flow is retarded due to the influence of friction between the fluid and the solid surface. Outside of the boundary layer, the flow is inviscid, i.e., there is no dissipative effects due to friction, thermal conduction or mass diffusion.
The boundary layer concept was introduced by Ludwig Prandtl in 1904, which enables significant simplification to the Navier-Stokes (NS) equation for the treatment of flow over a solid body. Inside the boundary layer, the NS equation is reduced to the boundary layer equation, while outside of the boundary layer, the flow can be described by the Euler equation, which is a simplified version of the NS equation.
<img src="/files/ftp_upload/10455/10455fig1a.jpg" />
Figure 1. Boundary layer development over a flat plate.
The simplest case for boundary layer development occurs on a flat plate at zero angle of incidence. When considering boundary layer development on a flat plate, the velocity outside of the boundary layer is constant so that the pressure gradient along the wall is considered to be zero.
The boundary layer, which naturally develops on a solid body surface, typically undergoes the following stages: first, the laminar boundary layer state; second, the transition state, and third, the turbulent boundary layer state. Each state has its own law(s) describing the flow structure of the boundary layer.
The research into the development and structure of boundary layer is of great importance for both theoretical study and practical applications. For example, boundary layer theory is the basis for calculating the skin friction drag on ships, aircraft and the blades of turbomachines. Skin friction drag is created on the body surface within the boundary layer and is due to the viscous shear stress exerted on the surface through fluid particles in direct contact with it. The skin friction is proportional to the fluid viscosity and the local velocity gradient on the surface in the surface normal direction. Skin friction drag is present on the entire surface, thus it becomes significant over large areas, such as an airplane wing. Additionally, turbulent fluid flow creates more skin friction drag. The macro-turbulent fluid motion enhances the momentum transfer within the boundary layer by bringing fluid particles with high momentum down to the surface.
This demonstration focuses on the turbulent boundary layer over a flat plate, in which the flow is irregular, such as in mixing or eddying, and the fluctuations are superimposed on the mean flow. Thus, the velocity at any point in a turbulent boundary layer is a function of time. In this demonstration, constant temperature hot-wire anemometry, or CTA, will be used to conduct a boundary layer survey. Then, the Clauser chart method will be used to calculate the skin friction coefficient in a turbulent boundary layer.

Constant Temperature Anemometry: Turbulent Boundary Layer Flow Study

一定温度麻酔:乱流境界層の流れを研究するツール

Source: Xiaofeng Liu, Jose Roberto Moreto, and Jaime Dorado, Department of Aerospace Engineering, San Diego State University, San Diego, California
A ...

Pressure Transducer: Calibration Using a Pitot-static Tube

Source: Shreyas Narsipur, Mechanical and Aerospace Engineering, North Carolina State University, Raleigh, NC
Fluid pressure is an important flow characteristic that is required to determine the aerodynamics of a system. One of the oldest and still existing pressure measurement systems is the manometer due to its accuracy and simplicity of operation. The manometer is generally a U-shaped glass tube that is partially filled with liquid, as shown in Figure 1. The U-tube manometer requires no calibration because it does not have any moving parts, and its measurements are functions of gravity and the liquid&#39;s density. Therefore, the manometer is a simple and accurate measurement system.
<img src="/files/ftp_upload/10467/10467fig1.jpg" /> 
Figure 1. Schematic of a U-tube manometer.
Real-time pressure measurements are obtained in aircraft by connecting the stagnation and static pressure ports of a pitot-static probe, a device that is commonly used to measure fluid flow pressure, to the ports of a pressure measurement device. This allows pilots to obtain existing flight conditions and to warn them if any changes to the flight conditions occur. While manometers provide very accurate pressure readings, they are inherently bulky. A more realistic solution is needed to measure aircraft pressures, as one of the primary design objectives is to keep the overall aircraft weight as low as possible. Today, electromechanical pressure transducers, which convert the applied pressure to an electric signal, are widely used for pressure sensing applications on aircraft because they are small, lightweight, and can be placed almost anywhere in the airframe. The above characteristics not only help reduce weight but also reduce the amount of tubing required to connect the pitot-static probe to the transducer, thereby decreasing the data response time. Additionally, in experimental aircraft flight testing, miniature pressure transducers come in handy as they allow researchers to maximize pressure data collection without significantly adding to the weight of the aircraft. While different types of pressure transducers with varying measurement techniques exist, one of the more common types of transducer is the capacitive pressure transducer. As transducers are capable of only sending signals in terms of voltage and current, calibration of the transducer is required to relate the strength of a particular signal to the pressure that causes the transducer to generate the signal. The final curve fit that relates the transducer current or voltage to a physical measurement, in our case pressure, is commonly referred to as the transducer calibration curve.
In this experiment, a pitot-static probe is placed in a subsonic wind tunnel with the stagnation and static pressure ports connected to the total and static ports of both the U-tube manometer and the pressure transducer. The wind tunnel is then run at different dynamic pressure settings, and the corresponding pressure reading from the U-tube manometer, and current readings produced by the transducer are recorded. This data is then used to generate calibration curves for the pressure transducer.

Calibration of Pressure Transducer Using a Pitot-static Tube

圧力トランスデューサ:ピトースタティックチューブを用いてキャリブレーション

Source: Shreyas Narsipur, Mechanical and Aerospace Engineering, North Carolina State University, Raleigh, NC
Fluid pressure is an important flow ...

Real-time Flight Control: Embedded Sensor Calibration and Data Acquisition

Source: Ella M. Atkins, Department of Aerospace Engineering, University of Michigan, Ann Arbor, MI
Overview
Autopilot allows aircraft to be stabilized using data collected from onboard sensors that measure the aircraft&#8217;s orientation, angular velocity, and airspeed. These quantities can be adjusted by the autopilot so that the aircraft automatically follows a flight plan from launch (takeoff) through recovery (landing). Similar sensor data is collected to control all types of aircraft, from large fixed-wing commercial transport aircraft to small-scale multiple-rotor helicopters, such as the quadcopter with four thruster units.
With inertial position and velocity captured by a sensor such as the Global Positioning System (GPS), the autopilot real-time flight control system enables a multicopter or fixed-wing aircraft to stabilize its attitude and airspeed to follow a prescribed trajectory. Sensor integration, calibration, data acquisition, and signal filtering are prerequisites for experiments in flight control.
Here we describe a sensor suite that provides the necessary data for flight control. Signal interfaces and data acquisition on two different embedded computer platforms are described, and sensor calibration is summarized. Single-channel moving average and median filters are applied to each data channel to reduce high-frequency signal noise and eliminate outliers.
In this experiment, data acquisition and sensor calibration for real-time flight control is demonstrated. Several published papers have described the principles of sensor data collection and control, and they have recently focused on sensors for small unmanned aerial vehicles (UAVs) [1-3].

Real-time Flight Control: Embedded Sensor Calibration

リアルタイムフライトコントロール:埋め込みセンサーキャリブレーションとデータ取得

Source: Ella M. Atkins, Department of Aerospace Engineering, University of Michigan, Ann Arbor, MI
Overview
Autopilot allows aircraft to be stabilized ...

Multicopter Aerodynamics: Characterizing Thrust on a Hexacopter

Source: Prashin Sharma and Ella M. Atkins, Department of Aerospace Engineering, University of Michigan, Ann Arbor, MI
Multicopters are becoming popular for a variety of hobby and commercial applications. They are commonly available as quadcopter (four thrusters), hexacopter (six thrusters), and octocopter (eight thrusters) configurations. Here, we describe an experimental process to characterize the multicopter performance. A modular small hexacopter platform providing propulsion unit redundancy is tested. The individual static motor thrust is determined using a dynamometer and varying propeller and input commands. This static thrust is then represented as a function of motor RPM, where the RPM is determined from motor power and control input. The hexacopter is then mounted on a load cell test stand in a 5&#8217; x 7&#8217; low-speed recirculating wind tunnel, and its aerodynamic lift and drag force components were characterized during flight at varying motor signals, free-stream flow speed, and angle of attack.

A hexacopter was selected for this study because of its resilience to motor (propulsion unit) failure, as reported in Clothier1. Along with redundancy in the propulsion system, the selection of high-reliability components is also required for safe flight, particularly for missions over-populated regions. In Ampatis2, the authors discuss the optimal selection of multicopter parts, such as motors, blades, batteries, and electronic speed controllers. Similar research has also been reported in Bershadsky3, which focuses on the proper selection of a propeller system to satisfy mission requirements. Along with redundancy and reliability of components, understanding vehicle performance is also essential to assure flight envelope limits are respected and to select the most efficient design.

Characterizing Thrust on Hexacopter: Dynamometer Experiment

マルチコプターエアロダイナミクス:ヘキサコプター上の推力の特徴付け

Source: Prashin Sharma and Ella M. Atkins, Department of Aerospace Engineering, University of Michigan, Ann Arbor, MI
Multicopters are becoming popular ...

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