X-Ray Spectrographic Analysis of the 3-d Transition Metal Corrosion Products Using Potassium Bromide Disks

AbstractA technique has been developed for quantitative analysis of the major constituents in small samples (less than 0.1 g) of corrosion products found On various missile parts. The technique was developed primarily to aid in interpretation of X-ray diffraction patterns of multicomponent corrosion products. The corrosion sample is mixed with KBr and the mixture is pressed into a disk in the same fashion commonly used in infrared work. The Br Kβ1 line serves as an internal standard. Intensities of the element's Kα line and the internal standard are established by scanning through the appropriate Bragg angle and recording peak heights on a strip-chart recorder. A xenon-filled proportional detector and a pulse-height analyzer were used.The percent of an element is determined by references to calibration curves which relate intensity ratios to weight ratios for the 3-d transition metals. The oxides of the metals were used in the preparation of the calibration curves. The weight ratio vs. intensity ratio relationship is linear over the weight ratio range 0.01 to 0.11. Data were collected using an air path and a helium path; the higher intensity ratios obtained with, the helium path, and the dependence of intensity on atomic number are illustrated. A comparison is made between the intensity ratios in a KBr matrix and in a NaBr matrix. The technique developed requires about 15 min sample preparation time.

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'Copper and Bronze in Art' and the Search for Rare Corrosion Products

10.20944/preprints202103.0523.v1 ◽

2021 ◽

Author(s):

Gerhard Eggert

Keyword(s):

Corrosion Products ◽

Metal Corrosion ◽

Copper Corrosion ◽

X Ray Diffraction ◽

Pigment Synthesis ◽

X Ray ◽

Soda Glass ◽

Black Spots ◽

Cupric Hydroxide

Information taken from David A. Scott’s book “Copper and Bronze in Art” was crucial for research on copper corrosion products in Stuttgart. Examples discussed are the nature and variability of ‘Black Spots’ (aka ‘Brown Fuzzies’); cupric hydroxide by cleaning, patination, and pigment synthesis; the wondrous phenomenon of curly malachite; chalconatronite formed by contact to soda glass; the formation of copper formates by glass-induced metal corrosion; and synthesis and X-ray diffraction of basic copper acetates (‘verdigris’).

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Preparation, properties and structure of some intermediate nido- and arachno-monocarbaboranes

Collection of Czechoslovak Chemical Communications ◽

10.1135/cccc19812345 ◽

1981 ◽

Vol 46 (10) ◽

pp. 2345-2353 ◽

Cited By ~ 33

Author(s):

Karel Baše ◽

Bohumil Štíbr ◽

Jiří Dolanský ◽

Josef Duben

Keyword(s):

Transition Metal ◽

Metal Complexes ◽

Transition Metal Complexes ◽

Nmr Spectra ◽

Liquid Ammonia ◽

X Ray Diffraction ◽

X Ray ◽

H Nmr ◽

Starting Compound

The 6-N(CH3)3-6-CB9H11 carbaborane reacts with sodium in liquid ammonia with the formation of 6-CB9H12- which was used as a starting compound for preparing the 4-CB8H14, 9-L-6-CB9H13 (L = (CH3)2S, CH3CN and P(C6H5)3), 1-(η5-C5H5)-1,2-FeCB9H10-, and 2,3-(η5-C5H5)2-2,31-Co2CB9H10- carboranes. The 4-CB8H14 compound was dehydrogenated at 623 K to give 4-(7)-CB8H12 carborane. Base degradation of 6-N(CH3)3-6-CB9H11 in methanol resulted in the formation of 3,4-μ-N(CH3)3CH-B5H10. The structure of all compounds was proposed on the basis of their 11B and 1H NMR spectra and X-ray diffraction was used in the case of the transition metal complexes.

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Identification of corrosion products and 3D distribution in reinforced concrete using X-ray micro computed tomography

Construction and Building Materials ◽

10.1016/j.conbuildmat.2019.02.133 ◽

2019 ◽

Vol 207 ◽

pp. 304-315 ◽

Cited By ~ 6

Author(s):

Guohao Fang ◽

Weijian Ding ◽

Yuqing Liu ◽

Jianchao Zhang ◽

Feng Xing ◽

...

Keyword(s):

Computed Tomography ◽

Reinforced Concrete ◽

Corrosion Products ◽

Micro Computed Tomography ◽

X Ray

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Regiospezifische Insertion von [SCN]- und [SeCN]- in die S – C- bzw. Se– C-Bindung Übergangsmetall-koordinierter Thietane und SelenetaneRegiospecific Insertion of [SCN]- and [SeCN]- in the S–C- and Se–C-Bond of Transition-Metal-Coordinated Thietanes and Selenetanes

Zeitschrift für Naturforschung B ◽

10.1515/znb-1993-1121 ◽

1993 ◽

Vol 48 (11) ◽

pp. 1613-1620 ◽

Cited By ~ 5

Author(s):

Helmut Fischer ◽

Claudia Kalbas ◽

Carsten Troll ◽

Klaus H. Fluck

Keyword(s):

Nitrogen Atom ◽

Transition Metal ◽

Structure Analysis ◽

Trans Isomer ◽

X Ray ◽

Tungsten Complexes ◽

Membered Heterocycle

Pentacarbonyl(thietane)tungsten complexes react with thiocyanate, [SCN]-, and SiO2/H2O by insertion of the CN group into a S—C bond of the four-membered heterocycle, 1,3-migration of the pentacarbonyltungsten fragment and protonation of the nitrogen atom to give tungsten-coordinated thiazinthione complexes. Analogously, the reactions of a thietane tungsten complex with [SeCN]- and SiO2/H2O affords a thiazinselone complex. A selenazinthione complex is obtained from a selenetane complex and [SCN]- (+ SiO2/H2O). The insertions are regiospecific and stereoselective. The structure of the trans-isomer of a pentacarbonyl-(thiazinthione) complex has been established by X-ray structure analysis.

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