Accurate determination of inorganic ions in water-soluble particulate matter by coupling high efficiency diffusion and filtration techniques

1986 ◽  
Vol 17 (3) ◽  
pp. 582 ◽  
Author(s):  
F. De Santis ◽  
V. Di Palo ◽  
C. Perrino
2003 ◽  
Vol 90 (1) ◽  
pp. 41-52 ◽  
Author(s):  
Seppo Ahvenjärvi ◽  
Aila Vanhatalo ◽  
Kevin J. Shingfield ◽  
Pekka Huhtanen

Four studies were conducted to compare the effect of four indigestible markers (LiCoEDTA, Yb-acetate, Cr-mordanted straw and indigestible neutral-detergent fibre (INDF)) and three marker systems on the flow of digesta entering the omasal canal of lactating dairy cows. Samples of digesta aspirated from the omasal canal were pooled and separated using filtration and high-speed centrifugation into three fractions defined as the liquid phase, small particulate and large particulate matter. Co was primarily associated with the liquid phase, Yb was concentrated in small particulate matter, whilst Cr and INDF were associated with large particles. Digesta flow was calculated based on single markers or using the reconstitution system based on combinations of two (Co + Yb, Co + Cr and Co + INDF) or three markers (Co + Yb + Cr and Co + Yb + INDF). Use of single markers resulted in large differences between estimates of organic matter (OM) flow entering the omasal canal suggesting that samples were not representative of true digesta. Digesta appeared to consist of at least three phases that tended to separate during sampling. OM was concentrated in particulate matter, whilst the liquid phase consisted mainly of volatile fatty acids and inorganic matter. Yb was intimately associated with nitrogenous compounds, whereas Cr and INDF were concentrated in fibrous material. Current data indicated that marker systems based on Yb in combination with Cr or INDF are required for the accurate determination of OM, N and neutral-detergent fibre flow. In cases where the flow of water-soluble nutrients entering the omasal canal is also required, the marker system should also include Co.


2020 ◽  
Vol 26 (2) ◽  
pp. 240-246 ◽  
Author(s):  
Kevin G. Field ◽  
Benjamin P. Eftink ◽  
Chad M. Parish ◽  
Stuart A. Maloy

AbstractComplex material systems in which microstructure and microchemistry are nonuniformly dispersed require three-dimensional (3D) rendering(s) to provide an accurate determination of the physio-chemical nature of the system. Current scanning transmission electron microscope (STEM)-based tomography techniques enable 3D visualization but can be time-consuming, so only select systems or regions are analyzed in this manner. Here, it is presented that through high-efficiency multidimensional STEM acquisition and reconstruction, complex point cloud-like microstructural features can quickly and effectively be reconstructed in 3D. The proposed set of techniques is demonstrated, analyzed, and verified for a high-chromium steel with heterogeneously situated features induced using high-energy neutron bombardment.


1966 ◽  
Vol 33 (1) ◽  
pp. 51-64 ◽  
Author(s):  
L. W. Phipps ◽  
F. H. S. Newbould

SummaryA technique for determining the concentration of leucocytes in cow's milk is described which is more rapid and accurate as well as much less tedious than conventional microscope methods. The leucocytes are isolated from the fat globules of comparable size by a novel centrifuging procedure. Sizing of the leucocytes with a Coulter electronic counter shows that their volumes range from about 45 to 1770 µm3but a partially overlapping distribution of other particulate matter prevents the accurate determination of the total number of cells present. The numbers counted in truncated leucocyte distributions, however, correlate linearly with total cell counts determined with an improved microscope method up to 6 × 106cells/ml of milk.


Author(s):  
Abookleesh L Frage , Almrhag M. Omar , Zatout M. Massoud

Headspace solid phase microextraction, fundamental& principle with its application on the determination of various pesticides are reviewed in this article. Pesticides extraction as a sample preparation step prior to subsequent analysis is aimed to achieve a reliable and accurate determination of this contaminants residue in food. Fast and high efficiency extraction process with free solvent consumption and overall cost is achieved through headspace solid phase micro extraction. HSPME is an equilibrium process which depends on the physio-chemical properties of the analyte to be extracted. Sample preparation and extraction condition such as fiber coating, temperature, time etc, have a direct impact on the extraction efficiency and sensitivity of headspace technique.


2012 ◽  
Vol 12 (10) ◽  
pp. 27367-27393
Author(s):  
S. Canepari ◽  
C. Farao ◽  
E. Marconi ◽  
C. Giovannelli ◽  
C. Perrino

Abstract. This paper describes the optimization and validation of a new simple method for the quantitative determination of water in atmospheric particulate matter (PM). The analyses are performed by using a coulometric Karl-Fisher system equipped with a controlled heating device; different water contributions are separated by the application of an optimized thermal ramp (three heating steps: 50–120 °C, 120–180 °C, 180–250 °C). The analytical performance of the method was verified by using standard materials containing 5.55% and 1% by weight of water. The recovery was greater than 95%; the detection limit was about 20 μg. The method was then applied to NIST reference materials (NIST1649a, urban particulate matter) and to real PM10 samples collected in different geographical areas. In all cases the repeatability was satisfactory (10–15%). When analyzing the reference material, the separation of four different types of water was obtained. In real PM10 samples the amount of water and its thermal profile differed as a function of the chemical composition of the dust. Mass percentages of 3–4% of water were obtained in most samples, but values up to about 15% were reached in areas where the chemical composition of PM is dominated by secondary inorganic ions and organic matter. High percentages of water were also observed in areas where PM is characterized by the presence of desert dust. A possible identification of the quality of water released from the samples was tried by applying the method to some hygroscopic compounds that are likely contained in PM (pure SiO2, Al2O3, ammonium salts, carbohydrates and dicarboxylic acids) and by comparing the results with those obtained from field samples.


2009 ◽  
Vol 91 (1) ◽  
pp. 133-139 ◽  
Author(s):  
Marina Dos Santos ◽  
Darío Gómez ◽  
Laura Dawidowski ◽  
Eduardo Gautier ◽  
Patricia Smichowski

1990 ◽  
Vol 73 (1) ◽  
pp. 51-53
Author(s):  
James B Noffsinger ◽  
Martha Emery ◽  
Daniel J Hoch ◽  
Jarmila Dokladalova

Abstract A liquid chromatographic (LC) method has been developed to determine the content of polydextrose, a water-soluble 1 calorie/g bulking agent, in food matrixes such as cookies, cakes, fruit spreads, and chocolate toppings. This analysis, which requires use of a blank matrix, provides a feasible means to control the manufacture of foods containing this additive and provides a component for the accurate determination of the caloric value of a particular food product. The method involves aqueous extraction of the polydextrose from the food matrix followed by separation on a carbohydrate analysis column. The LC system uses a mobile phase of 0.005M CaS04*2H2o and a refractive index detector for quantitation. Polydextrose recoveries from the food matrixes varied from 91.5 to 100.9% with assay precision, expressed as coefficient of variation, ranging from 0.7 to 4.3%. Each error estimate was derived from 5 parallel determinations. The present methodology is precise and selective in contrast to the modified classical phenol-sulfuric acid colorimetric method for assaying carbohydrates, which had been used for polydextrose determination in food matrixes in the past. Because the coefficient of variation frequently exceeded 10%, replicate analyses were necessary to achieve quantitation.


Materials ◽  
2021 ◽  
Vol 14 (12) ◽  
pp. 3407
Author(s):  
Wei Song ◽  
Yanrong He ◽  
Yuzhang Wu ◽  
Wei Qu

Crop residue burning is one of the major sources of particulate matter (PM) in the air. The burning behaviors and PM emissions of the three typical crop residues (rice straw, wheat straw, corn straw) in China were characterized by a cone calorimeter (CONE) coupled with a laser dust meter. The water-soluble compounds, carbonaceous content, and morphology of PM were measured by ion chromatography, elemental analyzer, transmission electron microscopy (TEM) and energy-dispersive X-ray spectrometer (EDS). The results showed that thermal stability of corn straw was the worst among the three crop straws. The heat release rate (HRR) curves of the three crop straws were the typical curves of thermally thick charring (residue forming) samples. Wheat straw had the highest smoke yield, which was 2.9 times that of rice straw. The PM emission factor of wheat straw was 180.91 µg/g, which was about three times that of rice straw. The contents of K+, Na+, and Cl− in PM were significantly higher than those of the other six water-soluble inorganic ions. The ratio of organic carbon and elemental carbon (OC/EC) ranged from 14.82 to 30.82, which was similar to the results of open burning. There were mainly three kinds of aggregates in the PM of crop straws: network, chain-like, and soot. Individual particles were mixtures of KCl and organic matters. Core-shell structures were found in PM of rice straw and corn straw. The results in this study were provided based on CONE, an ISO-standard apparatus, which could avoid data conflicts caused by the difference of combustion devices. The relationship between the burning behavior and PM emission characteristics of crop straws was established, which is helpful to understand emissions of crop straws and to find a novel way to solve the problems from the burning of crop residues.


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