Assisted Distillation Cleanup of Pesticide Residues in Animal Fats: New Beadless Distillation Tube

1987 ◽  
Vol 70 (5) ◽  
pp. 862-865
Author(s):  
Andrew B Heath ◽  
Robert R Black

Abstract A new assisted distillation tube has been developed which contains no glass beads or glass wool. The sample is injected into the top of the tube, and a septum is not required. Large ground-glass joints (10/ 19) are used at the gas inlet and at the Florisil trap connection for maximum strength. Existing assisted distillation apparatus was easily modified to accept the new tubes. Recoveries of 9 organochlorine pesticides from butter and cattle fat ranged from 87 to 104% at a tube temperature of 230°C and a nitrogen flow rate of 250 mL/min. No significant change occurred in recoveries of 8 of the 9 pesticides after 85 uses of the headless tube. Only the recovery of HCB from butter decreased, from 95 to 80%, after 51 runs. The new tube was compared with the Unitrex glass bead-packed concentric tube at flow rates of 230, 400, and 600 mL nitrogen/min. Recoveries from the Unitrex tube were similar to those of the headless tube for all pesticides except DDT which was significantly lower, indicating incomplete distillation at 250 mL/min and possible partial breakdown at 400 and 600 mL/min. A procedure is introduced for pressurized solvent washing of distillation tubes. This procedure is more efficient than vacuum washing

1979 ◽  
Vol 62 (4) ◽  
pp. 757-763
Author(s):  
Andrew B Heath ◽  
Robert R Black

Abstract The sweep co-distillation technique of Storherr et al. was investigated and simplified. Six organochlorine pesticides in animal fats were cleaned up under various distillation conditions as follows: No solvent was used, or solvent injection rates were 1 mL/min or 2 mL/3 min. Distillation tubes of 6.7 and 9.0 mm id diameter were compared. Distillation temperatures were varied from 150 to 300°C The complex condenser of Storherr et al. was compared with a simpler pipet condenser. A U-tube condenser which allows direct introduction onto a Florisil column for secondary cleanup was evaluated. The following modifications to the sweep co-distillation technique resulted: no solvent introduction, distillation temperature 230°C, nitrogen flow rate 600 mL/min, 6.7 mm id distillation tubes with simplified packing, and incorporation of the U-tube condenser. The new technique gave recoveries comparable to those of Storherr et al., but it is faster than most bisolvent partition methods and no large volumes of solvent are required.


2019 ◽  
Vol 27 (01) ◽  
pp. 1950091 ◽  
Author(s):  
JIAOJIAO DU ◽  
HAIBIN ZHOU ◽  
CAIXIA SUN ◽  
HAIJIANG KOU ◽  
ZHONGWEI MA ◽  
...  

A new approach was adopted to improve the corrosion behavior of the chromium nitride (CrNx) hard coating through magnetron sputtering deposition at different nitrogen flow rates. The influence of the nitrogen flow rates on the chemical composition, microstructure, mechanical property and corrosion behavior in artificial seawater of the CrNx coatings was investigated. The results show that with the increase of the nitrogen flow rates, the growth structure of the coatings varied from dense granular growth to coarse columnar growth. Increasing the nitrogen flow rates was helpful to decrease the Cr/N ratio and induce the phase transforming from mixed hexagonal Cr2N and face-centered cubic CrN to single CrN. However, the coatings under different nitrogen flow rates significantly improved the corrosion resistance and hardness of the steel substrate. Furthermore, at high nitrogen flow rate, the coating had high corrosion velocity and low protective capability against the substrate corrosion due to the fast corrosion channels acted by the columnar grain boundaries. While at the middle nitrogen flow rate, the coating with CrN phase, densely granular growth structure and moderate grain size resulted in excellent corrosion resistance and highest hardness.


Materials ◽  
2020 ◽  
Vol 13 (5) ◽  
pp. 1213
Author(s):  
Dae-Young Kim ◽  
Pil-Ryung Cha ◽  
Ho-Seok Nam ◽  
Hyun-Joo Choi ◽  
Kon-Bae Lee

The nitridation-induced self-formed aluminum matrix composite (NISFAC) process is based on the nitridation reaction, which can be significantly influenced by the characteristics of the starting materials (e.g., the chemical composition of the aluminum powder and the type, size, and volume fraction of the ceramic reinforcement) and the processing variables (e.g., process temperature and time, and flow rate of nitrogen gas). Since these variables do not independently affect the nitridation behavior, a systematic study is necessary to examine the combined effect of these variables upon nitridation. In this second part of our two-part report, we examine the effect of nitrogen flow rates and processing temperatures upon the degree of nitridation which, in turn, determines the amount of exothermic reaction and the amount of molten Al in the nitridation-induced self-formed aluminum matrix composite (NISFAC) process. When either the nitrogen flow rate or the set temperature was too low, high-quality composites were not obtained because the level of nitridation was insufficient to fill the powder voids with molten Al. Hence, since the filling of the voids in the powder bed by molten Al is essential to the NISFAC process, the conditions should be optimized by manipulating the nitrogen flow rate and processing temperature.


2019 ◽  
Vol 4 (3) ◽  
pp. 21-31
Author(s):  
Marlenne Gómez-Ramírez ◽  
Lizbeth Soto-Ruvalcaba ◽  
Martín Nieto-Pérez ◽  
Norma G. Rojas-Avelizapa

Microbiological food safety is a major issue and the genus Aspergillus is of great interest given the frequency of its toxin contamination in grains. This paper describes the use of cold plasma generated with argon and a mixture of argonnitrogen as a method of sanitizing lentil beans. Lentil beans were sanitized and exposed to Aspergillus flavus conidia then four different experimental sets were prepared, using only argon and a mixture of argon-nitrogen to generate plasma at nitrogen flow rates of 1.2, 0.81 and 0.32 L/min. Each lentil bean was exposed for 5, 10 and 15 min to plasma. Assays were performed in triplicate. Beans not exposed to plasma were used as controls. All plasma treatments caused a lethal effect on A. flavus conidia within exposure periods of 5 to 15 min. The application of argon plasma showed a log10 reduction of 0.81 (84%) after 15 min. The mixture of argon: nitrogen at 0.81 and 0.32 L/min had a higher lethal effect than argon alone. Although lentil beans sterilization was not completely achieved, an important log10 reduction of 1.43 (96.44 %) and 5.53 (99.99 %) of A. flavus conidia was obtained after 15 min of exposure to the plasma generated by argon-nitrogen mixture using nitrogen at flow rates of 0.81 and 0.32 L/min, respectively. Nitrogen flow rate of 0.32 L/min showed a reduction above 3.0 logarithmic units, so this treatment showed a fungicidal activity. The lowest reduction, 0.3 logarithmic units (50.3 %) was observed at a nitrogen flow rate of 1.2 L/min. Additionally, as a consequence of plasma exposure, conidia of A. flavus showed a delay in germination process and also conidia formation was affected. It was concluded that cold plasma could be used as an alternative to sanitize grains and avoid contamination by microorganisms, which cause grain deterioration and affect its nutritional properties.


2013 ◽  
Vol 440 ◽  
pp. 9-12
Author(s):  
Chien Cheng Liu ◽  
Kuang I Liu ◽  
Yung Chih Chou ◽  
Yung Mao Cheng ◽  
Chih Lung Lin

ZrN films were prepared by magnetron sputtering on die steel substrates. The objective of this study was to investigate the effect of nitrogen flow rate on the microstructure ,morphology, nanohardness properties determined by X-ray diffraction, field-emission scanning electron microscope, nanoindentation, and pin-on-disk, respectively. The XRD shows that ZrN has (111) and (200) preferred orientation under lower nitrogen flow rates. The surface of coatings revealed smaller grains and uniform dense under lower nitrogen flow rates. With increasing the nitrogen flow rates, this result showed ZrN films lead to poor mechanical properties and hardness values. However, films consisted of up high ernitrogen flow rate had much lower friction coefficient.


Coatings ◽  
2019 ◽  
Vol 9 (2) ◽  
pp. 108 ◽  
Author(s):  
Yanlong Fu ◽  
Tengfei He ◽  
Wu Yang ◽  
Jiao Xu ◽  
Bo Mu ◽  
...  

MoSN/MoS2 multilayer films were deposited by a sputtering MoS2 target in alternate Ar and Ar/N2 mixed atmospheres with different nitrogen flow rates. The influence of nitrogen flow rates on the microstructure, mechanical and tribological properties of the prepared films were investigated. The multilayer film exhibited the preferred orientation of (002) plane for MoS2 sublayers and amorphous structure for MoSN sublayers. Introducing N2 into the source gas resulted in a much more compact structure for multilayer films due to the suppression of columnar growth of MoS2 film. With the increase of the nitrogen flow rate, the hardness of the multilayer film firstly increased from 2.3 to 10.5 GPa as the nitrogen flow rate increased from 4 to 10 sccm and then turned downwards to 6.5 GPa at 20 sccm. MoSN/MoS2 film deposited with an optimized microstructure exhibited low friction coefficients below 0.03 and a wear life higher than 1.8×105 revolutions in vacuum. Meanwhile, the optimized film showed an ultralow friction coefficient of 0.004~0.01 and wear rate of 4.7 × 10−7 mm3/N·m in an ultrahigh vacuum. Both the enhanced hardness by N-doping and sustainable formed MoS2 tribofilm contributed to the improved tribological property of MoSN/MoS2 multilayer film.


2001 ◽  
Vol 672 ◽  
Author(s):  
A.B. Agarwal ◽  
B.A. Rainey ◽  
S.M. Yalisove ◽  
J.C. Bilello

ABSTRACTNanoindentation experiments have been performed to assess the mechanical behavior of chromium nitride (CrxNy) thin films sputtered in different deposition geometries and with varying Ar and N2 pressures. The hardness and elastic modulus of chromium nitrides are of great interest with regard to their applications. In the present work, two different deposition geometries, i.e. multi-substrate and confocal, were used to sputter (DC magnetron) a CrxNy layer on Si (100) wafers at varying nitrogen flow rates. The results of the nanoindentation experiments indicate that, over a similar argon and nitrogen regime, the CrxNy films grown in a multi- substrate geometry exhibit higher hardness and elastic modulus on the average than those grown in the confocal geometry. Furthermore, it was found that in the multi-substrate geometry the hardness and elastic modulus of the films were significantly higher than those in the confocally deposited films for a specific regime of the nitrogen flow rate (10-14 sccm). Finally, observations of the mechanical properties trends could be correlated with a higher degree of anisotropic stress for films grown in the multi-substrate in comparison to the confocal geometry.


1980 ◽  
Vol 63 (3) ◽  
pp. 529-531
Author(s):  
Andrew B Heath ◽  
Robert R Black

Abstract The assisted distillation technique, which was developed for the cleanup of pesticide residues from animal fats, has been improved. Nitric acid cleaning of distillation tubes resulted in a significant improvement in the recoveries of hexachlorobenzene (HCB) and lindane (from 76 to 92% and 84 to 89%, respectively). A larger U-tube condenser was developed that condensed 100% of all pesticides studied. With this new condenser, a study of distillation tube flow rates showed that pesticide recoveries at 600 ml nitrogen/min were generally better than those obtained at any other flow rate although recoveries were satisfactory at 400 and 800 mt/min. Recoveries of pesticides at distillation temperatures of 210–240°C were obtained with tubes cleaned with nitric acid, and using the larger U-tube condenser. The distillation temperature of choice was again 230°C because there was little variation from 220 to 240°C.


2004 ◽  
Vol 19 (8) ◽  
pp. 2322-2329 ◽  
Author(s):  
Bao-Shun Yau ◽  
Jow-Lay Huang ◽  
Ding-Fwu Lii

Nanocrystal-(Ti,Al)xN1-x/amorphous-SiyN1-y nanolaminate films were deposited periodically under different nitrogen flow rates. The composition, microstructure and mechanical properties of nanolaminate films were investigated by x-ray photoelectron spectroscope, x-ray diffractometer, scanning and transmission electron microscopy, atomic force microscope, and nanoindentation apparatus. Results indicated that the formation of the compound on the target surface was substantially influenced by the deposition rate, composition and crystallite size of the nanolaminate films. Nanolaminate structure with periodic compositional modulation and sharp interfaces were deposited at different nitrogen flow rate. Smaller nanocrystallite size, round-shaped grain features, smoother surface morphology, higher hardness, and reduced elastic modulus were obtained for nanolaminate films with increasing the nitrogen flow rate.


2018 ◽  
Vol 14 (1) ◽  
pp. 31-60 ◽  
Author(s):  
M. Y. Guida ◽  
F. E. Laghchioua ◽  
A. Hannioui

This article deals with fast pyrolysis of brown algae, such as Bifurcaria Bifurcata at the range of temperature 300–800 °C in a stainless steel tubular reactor. After a literature review on algae and its importance in renewable sector, a case study was done on pyrolysis of brown algae especially, Bifurcaria Bifurcata. The aim was to experimentally investigate how the temperature, the particle size, the nitrogen flow rate (N2) and the heating rate affect bio-oil, bio-char and gaseous products. These parameters were varied in the ranges of 5–50 °C/min, below 0.2–1 mm and 20–200 mL. min–1, respectively. The maximum bio-oil yield of 41.3wt% was obtained at a pyrolysis temperature of 600 °C, particle size between 0.2–0.5 mm, nitrogen flow rate (N2) of 100 mL. min–1 and heating rate of 5 °C/min. Liquid product obtained under the most suitable and optimal condition was characterized by elemental analysis, 1H-NMR, FT-IR and GC-MS. The analysis of bio-oil showed that bio-oil from Bifurcaria Bifurcata could be a potential source of renewable fuel production and value added chemicals.


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