scholarly journals Conical Nanoindentation Allows Azimuthally Independent Hardness Determination in Geological and Biogenic Minerals

Materials ◽  
2019 ◽  
Vol 12 (10) ◽  
pp. 1630 ◽  
Author(s):  
Corinna F. Böhm ◽  
Patrick Feldner ◽  
Benoit Merle ◽  
Stephan E. Wolf
Keyword(s):  
Standard Deviation ◽  
Mechanical Performance ◽  
Azimuthal Dependence ◽  
Azimuthal Variation ◽  
Conical Indenter ◽  
Pile Up ◽  
Hardness Values

The remarkable mechanical performance of biominerals often relies on distinct crystallographic textures, which complicate the determination of the nanohardness from indentations with the standard non-rotational-symmetrical Berkovich punch. Due to the anisotropy of the biomineral to be probed, an azimuthal dependence of the hardness arises. This typically increases the standard deviation of the reported hardness values of biominerals and impedes comparison of hardness values across the literature and, as a result, across species. In this paper, we demonstrate that an azimuthally independent nanohardness determination can be achieved by using a conical indenter. It is also found that conical and Berkovich indentations yield slightly different hardness values because they result in different pile-up behaviors and because of technical limitations on the fabrication of perfectly equivalent geometries. For biogenic crystals, this deviation of hardness values between indenters is much lower than the azimuthal variation in non-rotational-symmetrical Berkovich indentations.

Effects of the substrate on the determination of hardness of thin films by the nanoscratch and nanoindentation techniques: A comparative study for the cases of soft film on hard substrate and hard film on soft substrate.

2003 ◽  
Vol 795 ◽  
Author(s):  
Noureddine Tayebi ◽  
Andreas A. Polycarpou ◽  
Thomas F. Conry
Keyword(s):  
Thin Films ◽  
Elastic Recovery ◽  
Hard Substrate ◽  
Substrate Effect ◽  
Soft Substrate ◽  
Substrate Interaction ◽  
Pile Up ◽  
Fused Quartz ◽  
Hardness Values

ABSTRACTHardness values of Au/Fused Quartz and SiO2/Al systems, which correspond to the cases of soft film on hard substrate and hard film on soft substrate, were measured using both the nanoindentation and nanoscratch techniques. The effect of substrate interaction on the measurement of hardness using the nanoscratch technique is found to be much less pronounced compared to that of the nanoindentation technique. Such reduction in substrate effect is attributed to the features used in the nanoscratch analysis: (a) direct imaging of residual profile allows for the effect of pile-up/sink-in to be considered, (b) lower normal loads applied as compared to the nanoindentation, (c) effect of elastic recovery of the plastically deformed surfaces is included in the nanoscratch analysis, whereas the nanoindentation analysis is based solely on the load-displacement data. Moreover, experiments with residual scratch depths as shallow as 3 nm are used to estimate hardness of thin films; a promising indication for the use of such technique in the measurements of ultra-thin films.

Anisotropy of Nanoindentation – a tool for the determination of nanocrystal orientation ?

2003 ◽  
Vol 779 ◽  
Author(s):  
David Christopher ◽  
Steven Kenny ◽  
Roger Smith ◽  
Asta Richter ◽  
Bodo Wolf ◽  
...  
Keyword(s):  
Crystal Surface ◽  
Scanning Force Microscopy ◽  
Depth Range ◽  
Dislocation Loops ◽  
Force Microscopy ◽  
Pile Up ◽  
Out Of Plane ◽  
Scanning Force ◽  
Dynamics Simulations

AbstractThe pile up patterns arising in nanoindentation are shown to be indicative of the sample crystal symmetry. To explain and interpret these patterns, complementary molecular dynamics simulations and experiments have been performed to determine the atomistic mechanisms of the nanoindentation process in single crystal Fe{110}. The simulations show that dislocation loops start from the tip and end on the crystal surface propagating outwards along the four in-plane <111> directions. These loops carry material away from the indenter and form bumps on the surface along these directions separated from the piled-up material around the indenter hole. Atoms also move in the two out-of-plane <111> directions causing propagation of subsurface defects and pile-up around the hole. This finding is confirmed by scanning force microscopy mapping of the imprint, the piling-up pattern proving a suitable indicator of the surface crystallography. Experimental force-depth curves over the depth range of a few nanometers do not appear smooth and show distinct pop-ins. On the sub-nanometer scale these pop-ins are also visible in the simulation curves and occur as a result of the initiation of the dislocation loops from the tip.

An Automated Procedure for the Determination of Ammonia in Tobacco

1972 ◽  
Vol 6 (4) ◽  
Author(s):  
P.F. Collins ◽  
W.W. Lawrence ◽  
J.F. Williams
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Distillation Method ◽  
Relative Standard ◽  
Tobacco Sample ◽  
Automated Determination

AbstractA procedure for the automated determination of ammonia in tobacco has been developed. Ammonia is extracted from the ground tobacco sample with water and is determined with a Technicon Auto Analyser system which employs separation of the ammonia through volatilization followed by colourimetry using the phenate-hypochlorite reaction. The procedure has been applied to a variety of tobaccos containing from 0.02 to 0.5 % ammonia with an overall relative standard deviation of 2 %. The accuracy of the procedure as judged by recovery tests and by comparison to a manual distillation method is considered adequate

Determination of alcohols in mixtures by 19F NMR spectroscopy using hexefluoroacetone reagent

1982 ◽  
Vol 47 (7) ◽  
pp. 1973-1978 ◽  
Author(s):  
Jiří Karhan ◽  
Zbyněk Ksandr ◽  
Jiřina Vlková ◽  
Věra Špatná
Keyword(s):  
Standard Deviation ◽  
Nmr Spectroscopy ◽  
Standard Method ◽  
Internal Standard ◽  
Internal Standard Method ◽  
Concentration Region ◽  
Experimental Conditions ◽  
Curve Method ◽  
Sample Preparation Procedure

The determination of alcohols by 19F NMR spectroscopy making use of their reaction with hexafluoroacetone giving rise to hemiacetals was studied on butanols. The calibration curve method and the internal standard method were used and the results were mutually compared. The effects of some experimental conditions, viz. the sample preparation procedure, concentration, spectrometer setting, and electronic integration, were investigated; the conditions, particularly the concentrations, proved to have a statistically significant effect on the results of determination. For the internal standard method, the standard deviation was 0.061 in the concentration region 0.032-0.74 mol l-1. The method was applied to a determination of alcohols in the distillation residue from an oxo synthesis.

scholarly journals Observing UT1-UTC with VGOS

2021 ◽  
Vol 73 (1) ◽  
Author(s):  
Rüdiger Haas ◽  
Eskil Varenius ◽  
Saho Matsumoto ◽  
Matthias Schartner
Keyword(s):  
Standard Deviation ◽  
Reference Frame ◽  
Earth Rotation ◽  
Space Observatory ◽  
International Earth Rotation ◽  
Onsala Space Observatory ◽  
X Band ◽  
First Results

AbstractWe present first results for the determination of UT1-UTC using the VLBI Global Observing System (VGOS). During December 2019 through February 2020, a series of 1 h long observing sessions were performed using the VGOS stations at Ishioka in Japan and the Onsala twin telescopes in Sweden. These VGOS-B sessions were observed simultaneously to standard legacy S/X-band Intensive sessions. The VGOS-B data were correlated, post-correlation processed, and analysed at the Onsala Space Observatory. The derived UT1-UTC results were compared to corresponding results from standard legacy S/X-band Intensive sessions (INT1/INT2), as well as to the final values of the International Earth Rotation and Reference Frame Service (IERS), provided in IERS Bulletin B. The VGOS-B series achieves 3–4 times lower formal uncertainties for the UT1-UTC results than standard legacy S/X-band INT series. The RMS agreement w.r.t. to IERS Bulletin B is slightly better for the VGOS-B results than for the simultaneously observed legacy S/X-band INT1 results, and the VGOS-B results have a small bias only with the smallest remaining standard deviation.

scholarly journals Indirect and Direct Determination of the Casein Content of Milk by Kjeldahl Nitrogen Analysis: Collaborative Study

1998 ◽  
Vol 81 (4) ◽  
pp. 763-774 ◽  
Author(s):  
Joanna M Lynch ◽  
David M Barbano ◽  
J Richard Fleming
Keyword(s):  
Standard Deviation ◽  
Nitrogen Content ◽  
Relative Standard Deviation ◽  
Collaborative Study ◽  
Direct Determination ◽  
Raw Milk ◽  
Method Performance ◽  
Relative Standard ◽  
Milk Casein

Abstract The classic method for determination of milk casein is based on precipitation of casein at pH 4.6. Precipitated milk casein is removed by filtration and the nitrogen content of either the precipitate (direct casein method) or filtrate (noncasein nitrogen; NCN) is determined by Kjeldahl analysis. For the indirect casein method, milk total nitrogen (TN; Method 991.20) is also determined and casein is calculated as TN minus NCN. Ten laboratories tested 9 pairs of blind duplicate raw milk materials with a casein range of 2.42- 3.05℅ by both the direct and indirect casein methods. Statistical performance expressed in protein equivalents (nitrogen ⨯ 6.38) with invalid and outlier data removed was as follows: NCN method (wt%), mean = 0.762, sr = 0.010, SR = 0.016, repeatability relative standard deviation (RSDr) = 1.287℅, reproducibility relative standard deviation (RSDR) = 2.146%; indirect casein method (wt℅), mean = 2.585, repeatability = 0.015, reproducibility = 0.022, RSDr = 0.560℅, RSDR = 0.841; direct casein method (wt℅), mean = 2.575, sr = 0.015, sR = 0.025, RSDr = 0.597℅, RSDR = 0.988℅. Method performance was acceptable and comparable to similar Kjeldahl methods for determining nitrogen content of milk (Methods 991.20, 991.21,991.22, 991.23). The direct casein, indirect casein, and noncasein nitrogen methods have been adopted by AOAC INTERNATIONAL.

Quantitative Determination of some Carbonate Minerals in Greenschist Facies Meta-volcanic Rocks

1972 ◽  
Vol 9 (1) ◽  
pp. 36-42 ◽  
Author(s):  
Calvert C. Bristol
Keyword(s):  
Standard Deviation ◽  
Quantitative Determination ◽  
Volcanic Rocks ◽  
Internal Standard ◽  
Greenschist Facies ◽  
Carbonate Mineral ◽  
Mineral Contents ◽  
X Ray ◽  
Fine Grained

X-ray powder diffraction methods, successful in quantitative determination of silicate minerals in fine-grained rocks, have been applied to the determination of calcite, dolomite, and magnesite in greenschist facies meta-volcanic rocks. Internal standard graphs employing two standards (NaCl and Mo) have been determined.Carbonate mineral modes (calcite and dolomite) for 6 greenschist facies meta-volcanic rocks obtained by the X-ray powder method have been compared to normative carbonate mineral contents calculated for the same rocks. This comparison showed a maximum variation of 7.7 wt.% between the X-ray modes and the normative carbonate mineral contents of the rocks. Maximum standard deviation for the X-ray modes of these rocks was equivalent to 4.4 wt.%.

scholarly journals The Influence of Manufacturing Parameters on the Mechanical Behaviour of PLA and ABS Pieces Manufactured by FDM: A Comparative Analysis

Materials ◽  
2018 ◽  
Vol 11 (8) ◽  
pp. 1333 ◽  
Author(s):  
Adrián Rodríguez-Panes ◽  
Juan Claver ◽  
Ana Camacho
Keyword(s):  
Tensile Strength ◽  
Mechanical Behaviour ◽  
Mechanical Performance ◽  
Acrylonitrile Butadiene Styrene ◽  
Polymer Materials ◽  
Fused Deposition Modelling ◽  
Fused Deposition ◽  
Layer Orientation ◽  
Lower Variability

This paper presents a comparative study of the tensile mechanical behaviour of pieces produced using the Fused Deposition Modelling (FDM) additive manufacturing technique with respect to the two types of thermoplastic material most widely used in this technique: polylactide (PLA) and acrylonitrile butadiene styrene (ABS). The aim of this study is to compare the effect of layer height, infill density, and layer orientation on the mechanical performance of PLA and ABS test specimens. The variables under study here are tensile yield stress, tensile strength, nominal strain at break, and modulus of elasticity. The results obtained with ABS show a lower variability than those obtained with PLA. In general, the infill percentage is the manufacturing parameter of greatest influence on the results, although the effect is more noticeable in PLA than in ABS. The test specimens manufactured using PLA perform more rigidly and they are found to have greater tensile strength than ABS. The bond between layers in PLA turns out to be extremely strong and is, therefore, highly suitable for use in additive technologies. The methodology proposed is a reference of interest in studies involving the determination of mechanical properties of polymer materials manufactured using these technologies.

Determination of Nitrate in Water by HPLC

2013 ◽  
Vol 448-453 ◽  
pp. 406-408
Author(s):  
Jing Liu ◽  
Xiao Na Ji ◽  
Qing Kai Ren ◽  
Sheng Shu Ai ◽  
Li Jun Wan ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Recovery Rate ◽  
High Performance ◽  
Separation Efficiency ◽  
Fast Analysis ◽  
Relative Standard

We established a method fordetermination of nitrate in water by High Performance Liquid Chromatography(HPLC). The sample was analysed by HPLC-ADA and was quantitated by externalstandard method after being simply processed. This methd has the advantages ofhigh separation efficiency and fast analysis. The experiment result showed thatthe linearly dependent coefficient was0.994, the recovery rate was between 98.7%～105.7%,the relative standard deviation（RSD）wasless than 2.1 %, and the lowest detectable limit is 0.01ng (S/N=1.6).

scholarly journals Determination of Sodium Cromoglycate by a New Kinetic Spectrophotometric Method in Biological Samples

2013 ◽  
Vol 2013 ◽  
pp. 1-5
Author(s):  
Mohsen Keyvanfard ◽  
Khadijeh Alizad ◽  
Razieh Shakeri
Keyword(s):  
Standard Deviation ◽  
Sodium Cromoglycate ◽  
Spectrophotometric Method ◽  
Calibration Curve ◽  
Biological Samples ◽  
Limit Of Detection ◽  
Micellar Medium ◽  
Relative Standard ◽  
Kinetic Spectrophotometric

A new kinetic spectrophotometric method is described for the determination of ultratrace amounts of sodium cromoglycate (SCG). The method based on catalytic action of SCG on the oxidation of amaranth with periodate in acidic and micellar medium. The reaction was monitored spectrophotometrically by measuring the decrease in absorbance of the amaranth at 518 nm, for the first 4 min from initiation of the reaction. Calibration curve was linear in the range of 4.0−36.0 ng mL−1SCG. The limit of detection is 2.7 ng mL−1SCG. The relative standard deviation (RSD) for ten replicate analyses of 12, 20, and 28 ng mL−1SCG was 0.40%, 0.32%, and 0.53%, respectively. The proposed method was used for the determination of SCG in biological samples.

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