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1.
Cereol Group Center of Expertise, Budapest, Hungary Solid‐phase microextraction (SPME) was developed to determine volatile substances from liquid, gas or even solid materials. This technique has been successfully applied for soil, waste water, blood and urine samples, but in spite of its advantages there are still few applications for vegetable oils. SPME is applicable to determine the aroma and other volatile compounds of the oil, which are characteristic to its origin and oxidative status. In this study the sensitivity and selectivity of some commercially available SPME adsorption materials (polydimethylsiloxane, divinylbenzene, carboxen) were compared. The diverse types of stationary phases were investigated by applying standard oils containing volatile substances from 9‐90 mg/kg concentrations. SPME fibre was placed into the headspace of an oil sample in a 30‐ml headspace vial thermostated at 80 °C for 45 min. The extracted volatile materials were desorbed from the fiber in the injection port of the gas chromatograph at 250 °C. Identification of the extracted compounds is based on pure standards and mass spectra. The reliability of the SPME sampling method was studied by parallel measurements. The 2‐cm long fibre coated with divinylbenzene (50 μm) and carboxen (30 μm) proved to be the most appropriate to determine the volatile oxo‐materials from vegetable oils. The method was successfully applied to follow up the formation of volatile substances (e.g. hexanal, t‐2‐hexenal, t‐2‐heptenal, t‐2‐octenal, nonanal, t, t‐2, 4‐nonadienal, t‐2‐nonenal, t‐2‐decenal, t, c‐ and t, t‐2, 4‐decadienal, 2‐pentylfuran, 1‐octen‐3‐ol) during deep frying in sunflower oil.  相似文献   

2.
采用固相微萃取法,对液态奶味香精中的挥发性香成分进行了萃取条件的优化研究,得到了较佳的萃取条件。以23种奶味香料化合物组成的模拟奶味香精体系为研究对象,对预热温度(30~80℃),萃取时间(10~180 min),样品量(1~11 mL)和SPME纤维种类(65μm CWAX/DVB,65μm PDMS/DVB,75μm CAR/PDMS和50/30μm DVB/CAR/PDMS)4个因素进行了考察。发现这4个因素对香精中挥发性香成分萃取的选择性和对检出限的灵敏性均有显著性影响。结果表明,PDMS/DVB纤维对奶味香精中挥发性化合物的选择性最好,灵敏度最高,其次是DVB/CAR/PDMS。通过单因素实验,得到优化的固相微萃取条件是:预热温度50℃,萃取时间40 min,样品量5 mL。将得到的优化参数集中用于市售奶味香精样品分析,与对照组的固相微萃取结果相比,挥发性香成分的种类增加了30种,总峰面积增加了20倍,验证了固相微萃取参数优化的实用性。  相似文献   

3.
金博艳 《化学世界》2012,53(2):82-84
探讨了硝酸镍对石墨炉吸收法测定食品中铅的基体改进作用。实验表明:在200mg/L硝酸镍的基体改进剂存在下,仪器信号灵敏度提高3倍;在最佳测试条件下,铅特征质量为4.1pg/0.0044A,检出限为0.001mg/kg;12.5ng/mL铅标准溶液11次测定的RSD为1.2%;10μg/mL的Ca、Cd、Cr、Cu、Fe、K、Zn、Mg、Mn和Sn对12.5ng/mL铅标准溶液的测定无干扰作用。该法克服了国家标准《GB 5009.12-2010食品中铅的测定》第一法石墨炉原子吸收光谱法信号灵敏度低、稳定性差、重复性低等缺点。  相似文献   

4.
The dynamic headspace (DHS) thermal desorption principle using Tenax GR tube, as well as the solid phase micro‐extraction (SPME) tool with carboxen/polydimethylsiloxane 50/30 µm CAR/PDMS SPME fiber, both coupled to GC/MS were implemented for the isolation and identification of both lipid and Strecker derived volatiles in marine phospholipids (PL) emulsions. Comparison of volatile extraction efficiency was made between the methods. For marine PL emulsions with a highly complex composition of volatiles headspace, a fiber saturation problem was encountered when using CAR/PDMS‐SPME for volatiles analysis. However, the CAR/PDMS‐SPME technique was efficient for lipid oxidation analysis in emulsions of less complex headspace. The SPME method extracted volatiles of lower molecular weights more efficient than the DHS method. On the other hand, DHS Tenax GR appeared to be more efficient in extracting volatiles of higher molecular weights and it provided a broader volatile spectrum for marine PL emulsion than the CAR/PDMS‐SPME method.  相似文献   

5.
The potential toxicity oftrans-4-hydroxy-2-nonenal (HNE), a product formedin vivo during lipid peroxidation, which is also present in foods, was investigated in Fisher 344 rats. Five groups of five male rats each were given by gavage 1000, 300, 100, 30 or 10 mg/kg body weight HNE dissolved in 0.5 mL corn oil. The sixth group, the control, received corn oil alone. Two rats died 6 and 8 hr after being treated with 1000 mg/kg HNE. These two rats showed extensive acute tubular necrosis of the kidney, but had very little liver damage. Diffuse liver cell necrosis was observed in a dose dependent manner in all the rats killed 14 days after treatment, whereas renal change was mild. Interestingly, body weight of the lowest dosage group was significantly higher than that of the control group at termination of the experiment. The results of this study show that HNE has almost the same toxicity as other enals, such astrans-2-heptenal, and that kidney and liver are the main organs affected by toxicity of HNE. Although animals may have efficient defense systems, such as glutathione, to detoxify low to moderate dosages of HNE, at high doses of HNE this defense system is overwhelmed, resulting in serious renal and hepatic damage.  相似文献   

6.
The aim of this study is to explore naturally occurring sorbents that have high affinity for heavy metal treatment. In this respect, series of polymer‐clay composite beads that consists of Na‐alginate and montmorillonite clay were prepared using CaCl2 as crosslinker. The prepared composite bead was characterized by scanning electron microscope (SEM). Removal of lead from aqueous solution using this bead was then studied in batch adsorption experiments. The amount of lead removed was found to increase as the percent of Na‐alginate increase in the composite beads. The experimental results also showed that the equilibrium contact time was obtained within ∼ 100 min with (t1/2) of 50% adsorption in less than 10 min. Lead adsorption was found to be strongly pH‐dependent and display a maximum uptake capacity (244.6 mg/g) at pH 6 and minimum uptake (76.6 mg/g) at pH 1. Maximum lead adsorption was found to increase with increasing initial lead concentration in the feed solution and with decreasing temperature of experiment. Based on alginate‐montmorillonite beads packed columns, a highly efficient method for Pb(II) removal from aqueous solution was developed. The effect of flow rate on adsorption of 100 mg/L Pb(II) in the packed‐bed column was investigated by changing the flow rate between 0.5 and 2.5 mL min−1. The recovery of 100 mg/L Pb(II) in the packed‐bed column was found to be 100% at flow rates 0.5 and 1 mL min−1 then lowered to be 93% and 84% at flow rates 1.5 and 2.5 mL min−1, respectively. The effect of Pb(II) flow concentration ranging from 10 to 1000 mg/L on the adsorption of lead ions at constant flow rate 1.0 mL min−1 was also studied using column procedure. Technical feasibility for the uses of the prepared composite beads for the treatment of actual polluted wastewater samples collected from some industrial cities in Egypt was investigated. The evaluation of the system was performed by a complete analysis of heavy metals in the wastewater samples before and after the treatment process. The results showed a promising possibility for producing wastewater of better quality using such prepared beads. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2011  相似文献   

7.
A kind of adsorbent, strong alkaline anion exchange fiber loaded with zirconium strong alkaline anion exchange fiber (Zr@SAAEF) was prepared. Zr(IV) was uniformly distributed on SAAEF through chemical bonds and physical deposition. Zr@SAAEF has a decent effect on the removal of fluorine in water and scanning electron microscopy images and Fourier transform infrared spectroscopy spectrum showed that the Zr(IV) was successfully loaded on the fiber by chemical bonding. The average adsorption capacity of fluorine was 28.14 mg/g with pH ranging from 5.0 to 8.9, when fluorine solution (100 mg/L) was adsorbed by 0.1 g SAAEF, and the extent of removal exceed 96% when the adsorbent dose was 0.3 g. The adsorption isotherms were well fitted with Langmuir equation, and the maximum adsorption capacities calculated by Langmuir equation were close to the experiment results. The adsorption was an endothermic reaction. These results implied that fluorine adsorption onto Zr@SAAEF belonged to chemical adsorption using monolayer coverage on surface of the fiber. The adsorption kinetics of fluorine onto Zr@SAAEF could be described by pseudo‐second‐order rate mode. Zr@SAAEF showed a decent ability for fluorine removal from aqueous solution. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 45855.  相似文献   

8.
An ICP‐OES method using a new poly(acrylphenylamidrazone‐phenylhydrazide) chelating fiber to enrich and separate trace Au(III) and Ru(III) ions from solution samples is established. The results show that 50–500 ng/mL of Au or Ru ions can be enriched quantitatively by 0.1 g of the fiber at pH 4, with recoveries > 96%. The ions can be desorbed quantitatively with 10 mL of 4 M HCl and 3.0% CS(NH2)2 solution from the fiber column, with recoveries > 97%, and 200–1000‐fold excesses of Cu(II), Zn(II), Ca(II), Mg(II), Mn(II), Cr(III), Fe(III), Ba(II), and Al(III) caused little interference in the determination of these ions by ICP–OES. The chelating fiber can be reused eight times, and the recoveries are all > 95%. The relative standard deviations for enrichment and determination of 50 ng/mL of Au and Ru are in the range 1.8–1.9% (1.9% for Au and 1.8% for Ru). The recoveries of trace Au and Ru ions added to real waste water and alloy samples are 96–98%. The concentration of each ion found in the alloy samples was in good agreement with that provided by the plant. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 81: 2656–2660, 2001  相似文献   

9.
《分离科学与技术》2012,47(16):2322-2328
Solid-phase microextraction (SPME) with an ionic liquid (IL) coating was developed for headspace extraction of a group of low molecular weight alcohols (ethanol, n-propanol, butanol, and isopropyl alcohol), acetone, ethyl acetate, and acetonitrile. A first SPME fiber was simply coated with a dedicated IL whose synthesis is described. A second SPME fiber was prepared by gluing silica (Si) particles on which the synthesized IL was chemically bonded. The analytes SPME extraction was optimized for time, temperature, and NaCl salting out content. The headspace extracted analytes were determined by simple temperature desorption into the hot injection port of a gas chromatograph. The coated-IL fiber did not have enough extracting material to be useful. The bonded-IL-Si particle fiber had much more extracting material. Its analytical capabilities were compared to those of two commercially available fibers. The extraction yields of the bonded-IL-Si fiber were inferior to those of the two commercial fibers because they contained a significantly higher amount of extracting material. The linear concentration range could reach up to 120 μg/mL. The recoveries, trueness, and precision (RSD) were in the 97.4–109.5%, 0.1–9.5%, and 0.7–16.5 ranges, respectively. The bonded-IL-Si fiber showed a specific affinity for ethanol giving an ethanol peak height equal or greater than that of the two commercial fibers tested with the same sample.  相似文献   

10.
Functional fiber containing iso‐thiourea group was prepared by reactive chloromethylated poly(vinyl acetate)‐graft‐polystyrene–divinylbenzene (PVA‐g‐PS–DVB) being reacted with thiourea. The functional group content of the fiber was 2.90 mmol/g. The chloromethylated PVA‐g‐PS–DVB reacted with sulfur atoms in the thiourea molecules; this made the fiber containing iso‐thiourea group. The results of static adsorption experiments showed that the adsorption amount of the fiber toward Au(III) reached a maximum amount, 1000 mg/g, at pH 1.5. It reduced the adsorbed Au(III) into Au(0), and the maximum reduction percentage was 90% at pH 2.0. The amount of Au(III) adsorbed by the fiber increased with increasing solution temperature but decreased with the increasing ionic strength of the solution. It was proven by electron spectroscopy for chemical analysis that some of the sulfur atoms in the fiber were oxidized into sulfone groups or sulfate ions. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 81: 1985–1990, 2001  相似文献   

11.
Chloramine T (N-chloro-p-toluenesulfonamide sodium salt) and iodine (2:1, w/w) in carbon tetrachloride and acetic acid (1:1, vol/vol), referred to as reagent (I) was found to be effective for the determination of Iodine value of edible oils. Reagent (I) reacted quantitatively with the double bonds of oils of known weight. The reagent left unreacted after 20–25 min was titrated against standard sodium thiosulfate solution (0.04 M) in presence of potassium iodide (10%, 5 mL). The difference in volume of sodium thiosulfate solution consumed by reagent (I) without and with oil was a basis to calculate the iodine value of oils used. The iodine values of different oils were also determined separately following the standard procedure of Wijs, and calculated iodine value was obtained from the gas chromatographic profile of fatty acids. The iodine value obtained by the new method was in agreement with the results of the standard methods. The results obtained indicate that the method could be a complementary or an alternative to the Wijs method.  相似文献   

12.
To apply sericite effectively in the adsorption process, it was immobilized by entrapment method using sodium alginate. Since the immobilized sericite beads have excellent mechanical strength and swelling characteristics, channeling of flow and the increase of pressure drop were not observed through column operations. In addition, it was also stable under pH 10 and 45 °C of cesium solution. The maximum adsorption capacity and Langmuir adsorption constant was 1.430mg/g and 2.329 L/mg, respectively, at initial pH 5 of cesium solution in batch type and the Langmuir model with higher correlation coefficient of 0.997 fits experimental data better than Freundlich model. The breakthrough point emerged around 15 (1.0 mL/min) and 20 bed volumes (0.5 mL/min), and the cesium ions bound to the immobilized sericite beads were readily released and quantitatively recovered by a few bed volumes of 1.0M of HNO3 solution. Furthermore, bed volumes of cesium ions for firstly reused sericite beads can be still maintained as 18, which shows good regeneration ability.  相似文献   

13.
Chloramine T (N-chloro-p-toluenesulfonamide sodium salt) and iodine (2:1, w/w) in carbon tetrachloride and acetic acid (1:1, vol/vol), referred to as reagent (I) was found to be effective for the determination of Iodine value of edible oils. Reagent (I) reacted quantitatively with the double bonds of oils of known weight. The reagent left unreacted after 20–25 min was titrated against standard sodium thiosulfate solution (0.04 M) in presence of potassium iodide (10%, 5 mL). The difference in volume of sodium thiosulfate solution consumed by reagent (I) without and with oil was a basis to calculate the iodine value of oils used. The iodine values of different oils were also determined separately following the standard procedure of Wijs, and calculated iodine value was obtained from the gas chromatographic profile of fatty acids. The iodine value obtained by the new method was in agreement with the results of the standard methods. The results obtained indicate that the method could be a complementary or an alternative to the Wijs method.  相似文献   

14.
In the work, poly(ethylene terephthalate) (PET) fibers were grafted with 4‐vinyl pyridine (4‐VP) monomer using benzoyl peroxide (Bz2O2) as initiator in aqueous media. The removal of Hg(II) ions from aqueous solution by the reactive fiber was examined by batch equilibration technique. Effects of various parameters such as pH, graft yield, adsorption time, initial ion concentration, and adsorption temperature on the adsorption amount of metal ions onto reactive fibers were investigated. The optimum pH of Hg(II) was found 3. The maximum adsorption capacity was found as 137.18 mg g?1. Moreover such parameters as the adsorption kinetics, the adsorption isotherm, desorption time and the selectivity of the reactive fiber were studied. The adsorption kinetics is in better agreement with pseudo‐first order kinetics, and the adsorption data are good fit with Freundlich isotherms. The grafted fiber is more selective for Hg(II) ions in the mixed solution of Hg(II)‐Ni(II), Hg(II)‐Zn(II), and Hg(II)‐Ni(II)‐Zn(II) at pH 3. Adsorbed Hg(II) ions were easily desorbed by treating with 1M HNO3 at room temperature. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012  相似文献   

15.
BACKGROUND: The removal of heavy metals using adsorption techniques with low cost biosorbents is being extensively investigated. The improved adsorption is essentially due to the pores present in the adsorbent. One way of improving the porosity of the material is by irradiation of the precursor using microwaves. In the present study, the adsorption characteristics of nickel onto microwave‐irradiated rice husks were studied and the process variables were optimized through response surface methodology (RSM). RESULT: The adsorption of nickel onto microwave‐irradiated rice husk (MIRH) was found to be better than that of the raw rice husk (RRH). The kinetics of the adsorption of Ni(II) from aqueous solution onto MIRH was found to follow a pseudo‐second‐order model. Thermodynamic parameters such as standard Gibbs free energy (ΔG°), standard enthalpy (ΔH°), and standard entropy (ΔS°) were also evaluated. The thermodynamics of Ni(II) adsorption onto MIRH indicates that it is spontaneous and endothermic in nature. The response surface methodology (RSM) was employed to optimize the design parameters for the present process. CONCLUSION: Microwave‐irradiated rice husk was found to be a suitable adsorbent for the removal of nickel(II) ions from aqueous solutions. The adsorption capacity of the rice husk was found to be 1.17 mg g?1. The optimized parameters for the current process were found as follows: adsorbent loading 2.8 g (100 mL)?1; Initial adsorbate concentration 6 mg L?1; adsorption time 210 min.; and adsorption temperature 35 °C. Copyright © 2008 Society of Chemical Industry  相似文献   

16.
A simple and rapid procedure for the determination of polycyclic aromatic hydrocarbons (PAHs) in cigarette filter tar using solid-phase microextraction (SPME) was developed. The analysis was carried out using high-performance liquid chromatography equipped with an ultraviolet detector. The effects of the SPME experimental parameters on the extraction recovery were studied simultaneously using a central composite design (CCD) after a 26?2 fractional factorial experimental design. The SPME variables of interest were the extraction temperature, the extraction time, and the stirring speed, as well as the pH and the concentrations of NaCl (%, w/v) and acetonitrile (ACN). The optimal SPME conditions were as follows: an extraction temperature of 65°C, an extraction time of 50 min, a stirring speed of 800 rpm, 0% NaCl (w/v), 10% ACN in the sample, and a source pH of 8.0. The extraction calibration plots were linear over the range of 0.25?20 ng mL?1 (r2 > 0.9912) and the limits of detection (LODs) for the 6 PAHs studied were from 0.17–5.02 ng cigarette?1. The relative standard deviation (RSD) ranged from 7.1–13.5% for intra-day variation and from 8.5–18.4% for inter-day variation. The performance of the proposed method was evaluated for extraction and determination PAHs in real samples (various brands of cigarettes). The total amounts of all of the studied PAHs found in the filter tar of the three brands of cigarettes were 320.2, 17.9, and 66.7 ng cigarette?1, respectively.  相似文献   

17.
《分离科学与技术》2012,47(3):327-348
Abstract

The dimensional and UF performance characteristics of hollow fiber membranes produced by the solution spinning technique using three polymer solutions (C3, C4, and C5) were studied experimentally. The polymer (polyethersulfone, PES)/solvent (1-methyl-2-pyrrolidone, NMP)/additive (polyvinyl pyrrolidone, PVP) concentration (wt%) used were 20/65/15, 20/60/20, and 25/63/12, respectively, for C3, C4, and C5 solutions, and their corresponding viscosities were 9222, 22,809, and 29,286 cP. The extrusion pressures (EP) used in fiber production were 5 to 15, 20 to 40, and 20 to 60 psig, respectively, for C3, C4, and C5 solutions; the internal coagulant water flow rate (WFR) used were 7.5 and 10 mL/min for C3 fibers, and 5 mL/min for C4 and C5 fibers; and the length of air gap (LAG) was held constant at 80 cm in the production of all the fibers. An increase in EP always tended to increase OD, while ID decreased, increased, or remained constant depending on the WFR used. An increase in PVP concentration in the fiber spinning solution contributed to greater fiber swelling effects. Nascent fiber velocity (NFV) tended to increase with an increase in EP, but it decreased considerably with an increase in PVP concentration in the fiber spinning solution and the consequent increase in solution viscosity. Both fiber dimensions and skin layer morphology were found to be governed by the combined effects of desolvation, fiber swelling, and fiber stretching during fiber production.  相似文献   

18.
Processing of vegetative material containing pentoses has been shown to result in the formation of furfural. Furfural exhibits a spectrophotometric absorption peak at 518 nm when complexed with aniline acetate. Headspace solid-phase microextraction (HS-SPME) method has been successfully used to confirm the presence of furfural in crude palm oil (CPO). Solid phase microextraction (SPME) fiber composed of divinylbenzene/Carboxen/polydimethylsiloxane (DVB/PDMS/CAR) was used to absorb the volatiles in the headspace of the oil. The isolated compounds from the fiber was desorbed and separated on a capillary polar column of a gas chromatograph. Response surface methodology (RSM) was used to optimize the SPME fiber condition for maximum absorption of furfural from CPO. The optimized temperature and time for furfural extraction onto the SPME fiber are 70 °C for 40 min. Oils obtained from the mill were found to contain between 2 and 13% furfural.  相似文献   

19.
Three kinds of redox fibers (fibers II, III, and IV) are prepared by amination of the reactive chloromethylated poly(vinyl acetate) grafting polystyrene‐divinylbenzene fiber (fiber I) with diethanolamine, ethanolamine, or triethanolamine. The N‐content of the fibers is 2.26, 2.71, and 1.86 mmol g−1, respectively. Results of static adsorption experiments show that the adsorption amount of fibers II, III, and IV toward Au(III) reaches 550 mg g−1, 620 mg g−1, and 409 mg g−1, respectively, between pH 2.0 and pH 3.0. Some adsorbed Au(III) can be reduced to Au(0). The reduction percentage of Au(III) adsorbed by fiber II increases with rising pH value of the solution and can be as high as 87% at pH 5.0. The amount of Au(III) adsorbed by fiber II increases with solution temperature, but decreases with ionic strength of the solution. The adsorption amount of fibers II and III toward Au(III) is less in ethanol or in acetacetate medium than in water. Kinetic adsorption data indicates that 50 min is needed for fiber II to adsorb half of its saturate adsorption amount of Au(III). It was proved by elemental analysis, infrared spectroscopy, nuclear magnetic resonance, and electron spectroscopy for chemical analysis determinations that the carbon atoms connecting with the hydroxy groups near the nitrogen atoms were easily oxidized into carbonyl ones during redox adsorption reaction of fibers II, III, and IV with Au(III). Some grains of gold adsorbed on fiber II were discovered under scanning electron microscopy. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 73: 47–54, 1999  相似文献   

20.
温佐钧  赖永忠 《广州化工》2011,39(10):112-115
建立了饮用水源水中10种氯苯系化合物的检测方法———顶空固相微萃取-气质联用法(HS-SPME-GC-MS),监测项目包括氯苯、二氯苯、三氯苯、四氯苯和六氯苯。水中目标物用带75μm CarboxenTM-Polydimethylsiloxane(CAR-PDMS)涂层的萃取头顶空萃取,萃取物用GC-MS检测,联合MS的选择离子模式和内标定量法对目标物进行定量分析。实验优化了一些萃取条件,如萃取柱涂层、样品体积、萃取温度和萃取时间等。在优化后的萃取条件下,获得良好的校准曲线线性关系(r:0.9991~0.9999),检出限(3.143SD)介于0.003~0.06μg.L-1,0.100和0.500μg.L-1标准点的RSD均在8.0%以内(六氯苯除外)。除六氯苯外,饮用水源水实际样品中其余9种氯苯系物的加标回收率和RSD分别为93.1%~112%和2.0%~7.0%。此方法用于饮用水源水中氯苯系化合物的监测具有简单和环保的优势。  相似文献   

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