作者は感謝してXRPD測定を行うため女史クリスティーヌ・ステファニーを認めます。マリアンシューフとレベッカKuiter（美術の州立アカデミーとデザインシュツットガルト）が（ 図7）タイルの写真のために認められています。

<ol><li><a target="_blank" href="http://scholar.google.com/scholar?hl=en&safe=off&q=%22The+interface+between+science+and+conservation%2C+Occacional+Paper+116%22">The interface between science and conservation, Occacional Paper 116</a>. Bradley, S. M. , British Museum. London. (1997).</li>
<li><a target="_blank" href="http://scholar.google.com/scholar?hl=en&safe=off&q=%22Powder+Diffraction%3ATheory+and+Practice%22">Powder Diffraction:Theory and Practice</a>. Dinnebier, R. E., Billinge, S. J. L. , 1st edition, Royal Society of Chemistry. (2008).</li>
<li>Debye, P., Scherrer, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Interferenzen+an+regellos+orientierten+Teilchen+im+Roentgenlicht%5BTitle%5D)+AND+%22Phys.+Zeit%22%5BJournal%5D)">Interferenzen an regellos orientierten Teilchen im Roentgenlicht.</a> Phys. Zeit. 17, 277-283 (1916).</li>
<li>Hull, A. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((A+New+Method+of+X-Ray+Crystal+Analysis%5BTitle%5D)+AND+%22Phys.+Rev%22%5BJournal%5D)">A New Method of X-Ray Crystal Analysis.</a> Phys. Rev. 10 (6), 661-696 (1917).</li>
<li>Rietveld, H. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((A+profile+refinement+method+for+nuclear+and+magnetic+structures%5BTitle%5D)+AND+%22J.+Appl.+Cryst%22%5BJournal%5D)">A profile refinement method for nuclear and magnetic structures.</a> J. Appl. Cryst. 2, 65-71 (1969).</li>
<li>Oszlanyi, G., Suto, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Ab+initio+structure+solution+by+charge+flipping%5BTitle%5D)+AND+%22Acta+Crystallogr.+Sect.+A%22%5BJournal%5D)">Ab initio structure solution by charge flipping.</a> Acta Crystallogr. Sect. A. 60 (2), 134-141 (2004).</li>
<li>Newsam, J. M., Deem, M. W., Freeman, C. M. Direct Space Methods of Structure Solution from Powder Diffraction Data. <a target="_blank" href="http://scholar.google.com/scholar?hl=en&safe=off&q=author%3aNewsam%2C+JM+%22NIST+Special+Publication+864%3A+Accuracy+in+Powder+Diffraction+II%3A+Proceedings+of+the+International+Conference+May+26-29%2C+1992%22">NIST Special Publication 864: Accuracy in Powder Diffraction II: Proceedings of the International Conference May 26-29, 1992</a>. Prince, E., Stalick, J. K. , NIST - United States Department of Commerce. Gaithersburg. 80-91 (1992).</li>
<li>Dinnebier, R. E., Runčevski, T., Fischer, A., Eggert, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Solid-State+Structure+of+a+Degradation+Product+Frequently+Observed+on+Historic+Metal+Objects%5BTitle%5D)+AND+%22Inorg.+Chem%22%5BJournal%5D)">Solid-State Structure of a Degradation Product Frequently Observed on Historic Metal Objects.</a> Inorg. Chem. 54 (6), 2638-2642 (2015).</li>
<li>Wahlberg, N., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Crystal+Structure+of+Thecotrichite%2C+an+Efflorescent+Salt+on+Calcareous+Objects+Stored+in+Wooden+Cabinets%5BTitle%5D)+AND+%22Cryst.+Growth+Des%22%5BJournal%5D)">Crystal Structure of Thecotrichite, an Efflorescent Salt on Calcareous Objects Stored in Wooden Cabinets.</a> Cryst. Growth Des. 15 (6), 2795-2800 (2015).</li>
<li>Eggert, G., Fischer, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Gef%C3%A4hrliche+Nachbarschaft%3A+Durch+Glas+induzierte+Metallkorrosion+an+Museums-Exponaten+-+Das+GIMME-Projekt%5BTitle%5D)+AND+%22Restauro%22%5BJournal%5D)">Gefährliche Nachbarschaft: Durch Glas induzierte Metallkorrosion an Museums-Exponaten - Das GIMME-Projekt.</a> Restauro. 1, 38-43 (2012).</li>
<li><a target="_blank" href="http://scholar.google.com/scholar?hl=en&safe=off&q=%22TOPAS+%28current+version+5.0%29%22">TOPAS (current version 5.0)</a>. , Bruker AXS Inc. Madison, Wisconsin, USA. 
 <a target="_blank" href="https://www.bruker.com/products/x-ray-diffraction-and-elemental-analysis/x-ray-diffraction/xrd-software/topas.html">https://www.bruker.com/products/x-ray-diffraction-and-elemental-analysis/x-ray-diffraction/xrd-software/topas.html</a> (2015).</li>
<li>Coelho, A. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Indexing+of+powder+diffraction+patterns+by+iterative+use+of+singular+value+decomposition%5BTitle%5D)+AND+%22J.+Appl.+Crystallogr%22%5BJournal%5D)">Indexing of powder diffraction patterns by iterative use of singular value decomposition.</a> J. Appl. Crystallogr. 36 (1), 86-95 (2003).</li>
<li><a target="_blank" href="http://scholar.google.com/scholar?hl=en&safe=off&q=%22International+Tables+for+Crystallography+Volume+A%3A+Space-group+symmetry%22">International Tables for Crystallography Volume A: Space-group symmetry</a>. , (2006).</li>
<li>Pawley, G. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Unit-cell+refinement+from+powder+diffraction+scans%5BTitle%5D)+AND+%22J.+Appl.+Crystallogr%22%5BJournal%5D)">Unit-cell refinement from powder diffraction scans.</a> J. Appl. Crystallogr. 14, 357-361 (1981).</li>
<li>Cheary, R. W., Coelho, A. A., Cline, J. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Fundamental+Parameters+Line+Profile+Fitting+in+Laboratory+Diffractometers%5BTitle%5D)+AND+%22J.+Res.+Natl.+Inst.+Stand.+Technol%22%5BJournal%5D)">Fundamental Parameters Line Profile Fitting in Laboratory Diffractometers.</a> J. Res. Natl. Inst. Stand. Technol. 109 (1), 1-25 (2004).</li>
<li>Karle, J., Hauptman, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((A+theory+of+phase+determination+for+the+four+types+of+non-centrosymmetric+space+groups+1P222%2C+2P22%2C+3P12%2C+3P22%5BTitle%5D)+AND+%22Acta+Crystallogr%22%5BJournal%5D)">A theory of phase determination for the four types of non-centrosymmetric space groups 1P222, 2P22, 3P12, 3P22.</a> Acta Crystallogr. 9, 635-651 (1956).</li>
<li>Coelho, A. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Whole-profile+structure+solution+from+powder+diffraction+data+using+simulated+annealing%5BTitle%5D)+AND+%22J.+Appl.+Crystallogr%22%5BJournal%5D)">Whole-profile structure solution from powder diffraction data using simulated annealing.</a> J. Appl. Crystallogr. 33 (3), 899-908 (2000).</li>
<li>Macrae, C. F., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Mercury%3A+visualization+and+analysis+of+crystal+structures%5BTitle%5D)+AND+%22J.+Appl.+Crystallogr%22%5BJournal%5D)">Mercury: visualization and analysis of crystal structures.</a> J. Appl. Crystallogr. 39 (3), 453-457 (2006).</li>
<li><a target="_blank" href="http://scholar.google.com/scholar?hl=en&safe=off&q=%22Modern+Diffraction+Methods%22">Modern Diffraction Methods</a>. Mittemeijer, E. J., Welzel, U. , Wiley-VCH Verlag GmbH. (2012).</li>
</ol>

The authors have nothing to disclose.

XRPD is a suitable technique for conservation research as it is non-destructive, fast and easy-to-use. XRPD data can be used in routine qualitative analysis, owing to the fact that the powder pattern is a fingerprint signature to the corresponding crystal structure. The biggest advantage of XRPD over other analytic techniques is the ability of performing simultaneous qualitative and quantitative analysis of crystalline constituents in mixtures by using the Rietveld refinement method5. Moreover, the presence of amorphous content can be detected and its amount estimated. However, this procedure requires knowledge on every crystal structure present in the mixture that is a subject to investigation. 
To apply the method of XRPD routinely for structure determination to conservation science, several critical boundary conditions for the laboratory powder diffractometer must be fulfilled: 1.) To avoid preferred orientation in powder samples, transmission or even better Debye-Scherrer geometry must be used. 2.) Laboratory powder diffractometers should be equipped with a primary beam monochromator to ensure strict monochromatization and a position sensitive strip detector for high intensity (= good counting statistics) and high resolution. This particular type of instrument leads to sharp peak profiles which can be adequately described by few fundamental parameters being of great benefit for the separation of overlapping reflections. 
Indexing of the powder pattern which is often regarded as the bottleneck in the structure determination process should be done with exhaustive methods like "singular value decomposition", which is also insensitive to small amounts of impurities. Due to the strongly reduced information content of a powder pattern as compared to a single crystal data set, a sophisticated combination of direct and reciprocal space structure determination algorithms is needed for a high success rate. The combination of charge flipping, simulated annealing and difference-Fourier analysis has been proven to be among the most promising approaches. Providing that the material under investigation is reasonably crystalline, crystal structures with 20-25 structural parameters can nowadays been solved almost routinely from powder diffraction data if the procedure described above is used. It can be expected that this limit can be pushed to much more complex crystal structures with the advent of better instrumentation, the use of synchrotron radiation, and even more sophisticated structure determination algorithms.
Even after 250 (!) years of conservation research and 100 years of crystal structure analysis, there are still many crystalline corrosion products on artifacts of unknown exact composition and structure. This is mainly due to the unavailability of naturally or synthetically grown single crystals of suitable size. XRPD data analysis as described here can overcome this restriction since powder samples are amenable to investigation. A quantum leap forward in Conservation Science as well as in other fields!

保存科学は、成果物の保存に科学的な（しばしば化学）メソッドを適用します。 （？：どのようにそれはその時に行われた「技術的な美術史」）とその崩壊経路の適切な保全治療法を開発するための前提条件としてこれは人工物の生産の調査を含んでいます。しばしば、これらの研究は、炭酸塩、ギおよび酢酸塩などの有機金属塩を扱います。それらのいくつかが意図的に適切な化合物（ 例えば、酢）を使用して製造されている、他のものは大気中（屋内の大気汚染から二酸化炭素またはカルボニル化合物）1を劣化反応に由来します。実際の問題として、これらの腐食防止材料の多くの結晶構造はまだ不明です。幾何学的構造の知識がより良い生産と崩壊反応を理解し、混合物の場合には完全な定量分析を可能にするために、保存科学をするのに役立ちますので、これは、不幸な事実です。 関心のある材料は、十分な大きさと品質の単結晶を形成することを条件として、単結晶回折結晶構造を決意するための選択方法です。これらの境界条件が満たされない場合、粉末回折最も近い代替物です。単結晶回折に比べて粉末回折の最大の欠点は、（ベクトル散乱）相互D -ベクトルD *の配向情報の損失にあります。換言すれば、単一の回折スポットの強度は、球体の表面上に塗抹されています。これは、粉末パターンの一次元2θ軸上に三次元回折（=逆数）空間の投影と考えることができます。結果として、異なる方向が、同じまたは類似の長さのベクトルを散乱、それが困難または不可能にさえ、これらの反射2（Fを分離すること系統的または偶然重なっigure 1）。これはまた、その初期の発明にもかかわらず、粉末回折は、わずか4年第1単結晶実験3,4の後、半世紀以上も相同定および定量化のために主に使用された主な理由です。それにもかかわらず、簡単に図2から推論することができるように粉末パターンの情報量が膨大である。実際の課題は、しかしながら、ルーチンの方法で可能な限り多くの情報を明らかにすることです。 この目標に向けた重要なステップは、疑いなく、粉末回折データから結晶構造精密化のための局所最適化技術を発明1969年5でヒューゴリートフェルトのアイデアでした。従って、この方法は、アカウントに本質的にピークの重なりを取って、単一の強度を絞り込むが、複雑さを増すのモデルに対する全体の粉末パターンはありません。その時から、粉末回折法を用いて、科学者は、もはやデータ解析bに限定されませんでしたyの方法は、単結晶調査のために開発されました。数年リートベルト法を発明した後、 第一原理構造決定のための粉末回折法の力が認められました。この方法は、まだルーチンとみなすことはできないが、より多くの複雑な結晶構造を決定するために、今日では、ほとんどすべての自然科学の枝やエンジニアリング用粉末回折。最後の十年の中では、実験室での粉末回折計の新世代は、高解像度、高エネルギー、高強度を提供する設計されました。高いエネルギーが吸収を戦うながら、よりよい解決はすぐに優れたピーク分離につながります。基本的な物理パラメータに基づいて、より優れたピークプロファイルの説明（ 図3）の利点は、より詳細な構造の調査を可能にするブラッグ反射のより正確な強度です。ドメインサイズとmicrostraなどの近代的な機器やソフトウェアであっても微細構造のパラメータを持ちます日常的に粉末回折データから推定されます。 粉末回折データから結晶構造を決意するためのすべてのアルゴリズムは、単一のピーク強度は、全粉末パターンまたは両方の組み合わせを使用します。従来の単結晶逆空間技術は、多くの場合、利用可能な観察と構造パラメータとの間の好ましくない比に失敗します。この状況は、シミュレーテッドアニーリング技術7（ 図5）が最も顕著な代表される「電荷フリッピング」技術6（ 図4）と直接空間での大域的最適化手法の開発、の導入により劇的に変化しました。具体的には、構造決意プロセスに化学的知識の導入は、剛体または結合長に関わる分子化合物の既知の接続を使用して強く必要なパラメータの数を減少させる角度。換言すれば、内すべての単一原子のための3つの位置パラメータの代わりには、原子のグループの自由の唯一の外部（および内部数）度を決定する必要があります。これは、粉末法単結晶分析に真の選択肢になる構造の複雑さのこの減少です。 著者8,9の二つの先駆的な事例は、粉末回折データを用いて複雑な腐食生成物の複雑な結晶構造を解決することが可能であることを証明しました。他のアプローチに比べ結晶学的研究の優位性は、両方の場合で報告式を解く結晶構造を考慮した後に修正しなければならなかったという事実によって特に示されました。 博物館での調査中の両方の材料の発生は、木製のキャビネットに自分のストレージに関連するか、またはカルボニル汚染物質の他の供給源にさらされています。調査中の第1の材料は、水酸化ナトリウム、ギ酸銅、水酸化酸化ヒドラましたTE、銅4のNa 4 O美術館のコレクションにソーダガラス/銅合金複合体の歴史的なオブジェクト（ 例えば、エナメル）上に形成さ（HCOO）8（OH）2∙4H 2 O（サンプル1）、ホルムアルデヒド及びギ酸にさらさなどの木製収納キャビネット、接着剤、から。この劣化現象は最近、「ガラス誘発される金属腐食」10として特徴付けられています。第二のケーススタディ、thecotrichite、カルシウム3（CH 3 COO）3 Clで（NO 3）2∙6H 2 O（サンプル2）については、選ばれました。 Thecotrichiteは、オーク材のキャビネットやディスプレイケースに格納されているタイルや石灰岩の博物館のオブジェクト、上の針状微結晶を形成頻繁に観察風化塩です。この場合、木は人工物からの可溶性塩化物及び硝酸塩と反応して酢酸のソースとして機能します。 次のテキストの一部、構造dの個々のステップで保存科学から腐食生成物に適用される粉末回折データを用いeterminationプロセスが詳細に示されています。

<table><tbody><tr><td>Stadi-P&amp;nbsp;</td><td>Stoe &amp;amp; Cie GmbH</td><td></td><td>Powder Diffractometer</td></tr><tr><td>Mythen 1-K (450 &amp;mu;m)</td><td>Dectris Ltd.</td><td></td><td>Position Sensitive Detector</td></tr><tr><td>Mark tube borosilicate glass No. 50, 0.5 mm diameter</td><td>Hilgenberg GmbH</td><td>4007605</td><td>Low absorbing capillaries</td></tr><tr><td>Topas 5.0</td><td>Bruker AXS Advanced X-ray Solutions GmbH</td><td></td><td>Powder Diffraction Evaluation Software</td></tr></tbody></table>

x-ray powder diffraction in conservation science: towards routine crystal structure determination of corrosion products on heritage art objects

実験室の高分解能X線粉末回折（XRPD）を使用して歴史的な美術品の結晶構造決意及び腐食生成物の改良プロセスは、2つのケーススタディを介して詳細に示されています。 調査中の第1の材料は、水酸化ナトリウム、ギ酸銅、水酸化酸化物水和物、銅4のNa 4 O（HCOO）ソーダガラス/銅合金複合体の歴史的なオブジェクト（ 例えば 、エナメル）上に形成さ8（OH）2∙4H 2 O（サンプル1）でした博物館のホルムアルデヒドと木製収納キャビネットから放出されたギ酸にさらさコレクション、接着剤などでこの劣化現象は最近、「ガラス誘発される金属の腐食」として特徴付けられています。 第二のケーススタディ、thecotrichite、カルシウム3（CH 3 COO）3 Clで（NO 3）2∙6H 2 O（サンプル2）については、風化している、選ばれました塩は、木製キャビネットやディスプレイケースに格納されているタイルや石灰岩オブジェクトの針状微結晶を形成します。この場合、木は人工物またはその環境からの可溶性塩化物及び硝酸塩と反応して酢酸のソースとして機能します。 幾何学的構造の知識は、より良い生産と崩壊反応を理解し、混合物の頻繁な場合には、完全な定量分析を可能にするために、保存科学をするのに役立ちます。

Watch this Scientific Journal Video about X-ray Powder Diffraction in Conservation Science: Towards Routine Crystal Structure Determination of Corrosion Products on Heritage Art Objects at JoVE.com

X-ray Powder Diffraction in Conservation Science: Towards Routine Crystal Structure Determination of Corrosion Products on Heritage Art Objects

Modern high resolution X-ray powder diffraction (XRPD) in the laboratory is used as an efficient tool to determine crystal structures of long-known corrosion products on historic objects.

保存科学における粉末X線回折：遺産アートオブジェクトに対する腐食製品のルーチンの結晶構造の決意に向けて

The crystal structure determination and refinement process of corrosion products on historic art objects using laboratory high-resolution X-ray powder ...

x-ray-powder-diffraction-conservation-science-towards-routine-crystal

Nanyang Technological University

Research

JoVE Journal

Chemistry

16.1K ビュー.  Max-Planck-Institute for Solid State Research. Modern high resolution X-ray powder diffraction (XRPD) in the laboratory is used as an efficient tool to determine crystal structures of long-known corrosion products on historic objects.

ビデオ: X-ray Powder Diffraction in Conservation Science: Towards Routine Crystal Structure Determination of Corrosion Products on Heritage Art Objects

Synthesis and Microdiffraction at Extreme Pressures and Temperatures

High pressure compounds and polymorphs are investigated for a broad range of purposes such as determine structures and processes of deep planetary interiors, design materials with novel properties, understand the mechanical behavior of materials exposed to very high stresses as in explosions or impacts. Synthesis and structural analysis of materials at extreme conditions of pressure and temperature entails remarkable technical challenges. In the laser heated diamond anvil cell (LH-DAC), very high pressure is generated between the tips of two opposing diamond anvils forced against each other; focused infrared laser beams, shined through the diamonds, allow to reach very high temperatures on samples absorbing the laser radiation. When the LH-DAC is installed in a synchrotron beamline that provides extremely brilliant x-ray radiation, the structure of materials under extreme conditions can be probed in situ. LH-DAC samples, although very small, can show highly variable grain size, phase and chemical composition. In order to obtain the high resolution structural analysis and the most comprehensive characterization of a sample, we collect diffraction data in 2D grids and combine powder, single crystal and multigrain diffraction techniques. Representative results obtained in the synthesis of a new iron oxide, Fe4O5 1 will be shown.

The laser heated diamond anvil cell combined with synchrotron micro-diffraction techniques allows researchers to explore the nature and properties of new phases of matter at extreme pressure and temperature (PT) conditions. Heterogeneous samples can be characterized in situ under high pressure by 2D mapping and combined powder, single-crystal and multigrain diffraction approaches.

エクストリーム圧力と温度での合成とMicrodiffraction

High pressure compounds and polymorphs are investigated for a broad range of purposes such as determine structures and processes of deep planetary ...

工学

High Pressure Single Crystal Diffraction at PX^2

In this report we describe detailed procedures for carrying out single crystal X-ray diffraction experiments with a diamond anvil cell (DAC) at the GSECARS 13-BM-C beamline at the Advanced Photon Source. The DAC program at 13-BM-C is part of the Partnership for Extreme Xtallography (PX^2) project. BX-90 type DACs with conical-type diamond anvils and backing plates are recommended for these experiments. The sample chamber should be loaded with noble gas to maintain a hydrostatic pressure environment. The sample is aligned to the rotation center of the diffraction goniometer. The MARCCD area detector is calibrated with a powder diffraction pattern from LaB6. The sample diffraction peaks are analyzed with the ATREX software program, and are then indexed with the RSV software program. RSV is used to refine the UB matrix of the single crystal, and with this information and the peak prediction function, more diffraction peaks can be located. Representative single crystal diffraction data from an omphacite (Ca0.51Na0.48)(Mg0.44Al0.44Fe2+0.14Fe3+0.02)Si2O6 sample were collected. Analysis of the data gave a monoclinic lattice with P2/n space group at 0.35 GPa, and the lattice parameters were found to be: a = 9.496 &#177;0.006 &#197;, b = 8.761 &#177;0.004 &#197;, c = 5.248 &#177;0.001 &#197;, &#946; = 105.06 &#177;0.03&#186;, &#945; = &#947; = 90&#186;.

In this report, we describe detailed procedures for carrying out single crystal X-ray diffraction experiments with a diamond anvil cell at the GSECARS 13-BM-C beamline at the Advanced Photon Source. ATREX and RSV programs are used to analyze the data.

PX ^ 2の高圧単結晶回折

In this report we describe detailed procedures for carrying out single crystal X-ray diffraction experiments with a diamond anvil cell (DAC) at the ...

化学

Reliable Mechanochemistry: Protocols for Reproducible Outcomes of Neat and Liquid Assisted Ball-mill Grinding Experiments

The equilibrium outcomes of ball mill grinding can dramatically change as a function of even tiny variations in the experimental conditions such as the presence of very small amounts of added solvent. To reproducibly and accurately capture this sensitivity, the experimentalist needs to carefully consider every single factor that can affect the ball mill grinding reaction under investigation, from ensuring the grinding jars are clean and dry before use, to accurately adding the stoichiometry of the starting materials, to validating that the delivery of solvent volume is accurate, to ensuring that the interaction between the solvent and the powder is well understood and, if necessary, a specific soaking time is added to the procedure. Preliminary kinetic studies are essential to determine the necessary milling time to achieve equilibrium. Only then can exquisite phase composition curves be obtained as a function of the solvent concentration under ball mill liquid assisted grinding (LAG). By using strict and careful procedures analogous to the ones here presented, such milling equilibrium curves can be obtained for virtually all milling systems. The system we use to demonstrate these procedures is a disulfide exchange reaction starting from the equimolar mixture of two homodimers to obtain at equilibrium quantitative heterodimer. The latter is formed by ball mill grinding as two different polymorphs, Form A and Form B. The ratio R = [Form B] / ([Form A] + [Form B]) at milling equilibrium depends on the nature and concentration of the solvent in the milling jar.

We present detailed procedures to produce experimental equilibrium curves of the phase composition as a function of solvent concentration in a solid state system under milling conditions.

信頼性の高いメカノケミストリー: ニートや液体の再現可能な成果のためのプロトコル支援ボールミル粉砕実験

The equilibrium outcomes of ball mill grinding can dramatically change as a function of even tiny variations in the experimental conditions such as the ...

Microfluidic Chips for In Situ Crystal X-ray Diffraction and In Situ Dynamic Light Scattering for Serial Crystallography

This protocol describes fabricating microfluidic devices with low X-ray background optimized for goniometer based fixed target serial crystallography. The devices are patterned from epoxy glue using soft lithography and are suitable for in situ X-ray diffraction experiments at room temperature. The sample wells are lidded on both sides with polymeric polyimide foil windows that allow diffraction data collection with low X-ray background. This fabrication method is undemanding and inexpensive. After the sourcing of a SU-8 master wafer, all fabrication can be completed outside of a cleanroom in a typical research lab environment. The chip design and fabrication protocol utilize capillary valving to microfluidically split an aqueous reaction into defined nanoliter sized droplets. This loading mechanism avoids the sample loss from channel dead-volume and can easily be performed manually without using pumps or other equipment for fluid actuation. We describe how isolated nanoliter sized drops of protein solution can be monitored in situ by dynamic light scattering to control protein crystal nucleation and growth. After suitable crystals are grown, complete X-ray diffraction datasets can be collected using goniometer based in situ fixed target serial X-ray crystallography at room temperature. The protocol provides custom scripts to process diffraction datasets using a suite of software tools to solve and refine the protein crystal structure. This approach avoids the artefacts possibly induced during cryo-preservation or manual crystal handling in conventional crystallography experiments. We present and compare three protein structures that were solved using small crystals with dimensions of approximately 10-20 &#181;m grown in chip. By crystallizing and diffracting in situ, handling and hence mechanical disturbances of fragile crystals is minimized. The protocol details how to fabricate a custom X-ray transparent microfluidic chip suitable for in situ serial crystallography. As almost every crystal can be used for diffraction data collection, these microfluidic chips are a very efficient crystal delivery method.

Microfluidic Chips for In Situ Crystal X-ray Diffraction and In Situ Dynamic Light Scattering for Serial Crystallography

This protocol describes in detail how to fabricate and operate microfluidic devices for X-ray diffraction data collection at room temperature. Additionally, it describes how to monitor protein crystallization by dynamic light scattering and how to process and analyze obtained diffraction data.

シリアル結晶の結晶 x 線回折その場その場での動的光散乱のためのマイクロ流体チップ

This protocol describes fabricating microfluidic devices with low X-ray background optimized for goniometer based fixed target serial crystallography. The ...

Synchrotron X-ray Microdiffraction and Fluorescence Imaging of Mineral and Rock Samples

In this report, we describe a detailed procedure for acquiring and processing&#160;x-ray microfluorescence (&#956;XRF), and Laue and powder microdiffraction two-dimensional (2D) maps at beamline 12.3.2 of the Advanced Light Source (ALS), Lawrence Berkeley National Laboratory. Measurements can be performed on any sample that is less than 10 cm x 10 cm x 5 cm, with a flat exposed surface. The experimental geometry is calibrated using standard materials (elemental standards for XRF, and crystalline samples such as Si, quartz, or Al2O3 for diffraction). Samples are aligned to the focal point of the x-ray microbeam, and raster scans are performed, where each pixel of a map corresponds to one measurement, e.g., one XRF spectrum or one diffraction pattern. The data are then processed using the in-house developed software XMAS, which outputs text files, where each row corresponds to a pixel position. Representative data from moissanite and an olive snail shell are presented to demonstrate data quality, collection, and analysis strategies.

We describe a beamline setup meant to carry out rapid two-dimensional x-ray fluorescence and x-ray microdiffraction mapping of single crystal or powder samples using either Laue (polychromatic radiation) or powder (monochromatic radiation) diffraction. The resulting maps give information about strain, orientation, phase distribution, and plastic deformation.

・鉱物及び岩石試料の蛍光を放射光 x 線回折

In this report, we describe a detailed procedure for acquiring and processing&#160;x-ray microfluorescence (&#956;XRF), and Laue and powder ...

ホスホネート基幹細胞の合成と発見:ソルボサーマルアプローチ

Discovery and Synthesis Optimization of Isoreticular Al(III) Phosphonate-Based Metal-Organic Framework Compounds Using High-Throughput Methods

High-throughput (HT) methods are an important tool for the fast and efficient screening of synthesis parameters and the discovery of new materials. This manuscript describes the synthesis of metal-organic frameworks (MOFs) from solution using an HT reactor system, resulting in the discovery of various phosphonate-based MOFs of the composition [Al2H12-x(PMP)3]Clx&#8729;6H2O (H4PMP = N,N &#39;-piperazine bis(methylenephosphonic acid)) for x = 4, 6, denoted as Al-CAU-60-xHCl, containing trivalent aluminum ions. This was accomplished under solvothermal reaction conditions by systematically screening the impact of the molar ratio of the linker to the metal and the pH of the reaction mixture on the product formation. The protocol for the HT investigation includes six steps: a) synthesis planning (DOE = design of&#160;experiment) within the HT methodology, b) dosing and working with in-house developed HT reactors, c) solvothermal synthesis, d) synthesis workup using in-house developed filtration blocks, e) characterization by HT powder X-ray diffraction, and f) evaluation of the data. The HT methodology was first used to study the influence of acidity on the product formation, leading to the discovery of Al-CAU-60&#8729;xHCl (x = 4 or 6).

著者スポットライト:微多孔質材料化学における発見の加速 

The targeted synthesis of new metal-organic frameworks (MOFs) is difficult, and their discovery depends on the knowledge and creativity of the chemist. High-throughput methods allow complex synthetic parameter fields to be explored quickly and efficiently, accelerating the process of finding crystalline compounds and identifying synthetic and structural trends.

ハイスループット法を用いた等網状Al(III)ホスホネート系金属有機骨格化合物の発見と合成最適化

High-throughput (HT) methods are an important tool for the fast and efficient screening of synthesis parameters and the discovery of new materials. This ...

X-ray Diffraction

Source: Faisal Alamgir, School of Materials Science and Engineering, Georgia Institute of Technology, Atlanta, GA
X-ray diffraction (XRD) is a technique used in materials science for determining the atomic and molecular structure of a material. This is done by irradiating a sample of the material with incident X-rays and then measuring the intensities and scattering angles of the X-rays that are scattered by the material. The intensity of the scattered X-rays are plotted as a function of the scattering angle, and the structure of the material is determined from the analysis of the location, in angle, and the intensities of scattered intensity peaks. Beyond being able to measure the average positions of the atoms in the crystal, information on how the actual structure deviates from the ideal one, resulting for example from internal stress or from defects, can be determined.
The diffraction of the X-rays, that is central to the XRD method, is a subset of the general X-ray scattering phenomena. XRD, which is generally used to mean can wide-angle X-ray diffraction (WAXD), falls under several methods that use the elastically scattered X-ray waves. Other elastic scattering based X-ray techniques include small angle X-ray scattering (SAXS), where the X-rays are incident on the sample over the small angular range of 0.1-100 typically). SAXS measures structural correlations of the scale of several nanometers or larger (such as crystal superstructures), and X-ray reflectivity that measures the thickness, roughness, and density of thin films. WAXD covers an angular range beyond 100.

X-Ray Diffraction for Determining Atomic and Molecular Structure

X線回折

Source: Faisal Alamgir, School of Materials Science and Engineering, Georgia Institute of Technology, Atlanta, GA
X-ray diffraction (XRD) is a technique ...

Education

JoVE Science Education

材料工学

X-ray Fluorescence (XRF)

Source: Laboratory of Dr. Lydia Finney &#8212; Argonne National Laboratory
X-ray fluorescence is an induced, emitted radiation that can be used to generate spectroscopic information. X-ray fluorescence microscopy is a non-destructive imaging technique that uses the induced fluorescence emission of metals to identify and quantify their spatial distribution.

保存科学における粉末X線回折：遺産アートオブジェクトに対する腐食製品のルーチンの結晶構造の決意に向けて

要約

さらに動画を探す

エクストリーム圧力と温度での合成とMicrodiffraction

PX ^ 2の高圧単結晶回折

信頼性の高いメカノケミストリー: ニートや液体の再現可能な成果のためのプロトコル支援ボールミル粉砕実験

シリアル結晶の結晶 x 線回折その場その場での動的光散乱のためのマイクロ流体チップ

・鉱物及び岩石試料の蛍光を放射光 x 線回折

ハイスループット法を用いた等網状Al(III)ホスホネート系金属有機骨格化合物の発見と合成最適化

ハイスループット法を用いた等網状Al(III)ホスホネート系金属有機骨格化合物の発見と合成最適化

ハイスループット法を用いた等網状Al(III)ホスホネート系金属有機骨格化合物の発見と合成最適化

X線回折

蛍光 x 線 (XRF)