• Food Engineering Progress
• /
• v.14 no.4
• /
• pp.354-358
• /
• 2010

The methods for determining the diffusion parameters for the diffusion of d-limonene, a major volatile compound of orange juice, through a multi-layered food packaging material and predicting its absorption into the packaging material have been investigated. The packaging material used was the 1.5-mm thick multi-layered packaging material composed of high impact polystyrene (HIPS), polyvinylidene chloride (PVDC), and low density polyethylene (LDPE). Orange juice was placed in a cell where volatiles were absorbed in the sample package and kept at $23{\pm}2^{\circ}C$ for 72 hr. The d-limonene absorbed in a 1.5-mm thick multi-layered food packaging material was analyzed by a solid phase micro-extraction (SPME). The absorption parameters for the absorption of d-limonene in the packaging material were determined and absorption of d-limonene into the packaging material was predicted using absorption storage data. The SPME desorption at $60^{\circ}C$ for 1 hr resulted in the most sensitive and reproducible results. The diffusion coefficients of d-limonene in the packaging material and the partition coefficient at $23{\pm}2^{\circ}C$ were approximately $1-2{\times}10^{12}m^2$/s and 0.03, respectively. The absorption profile no earlier than 30 hr was fit well by a model derived from the Fick's law.

• International Journal of Advanced Culture Technology
• /
• v.10 no.1
• /
• pp.284-293
• /
• 2022

After extracting the calcium component from the KR slag and the converter slag using ammonium chloride solution, the extract was reacted with carbon dioxide to synthesize precipitated calcium carbonate (PCC). In order to understand the effect of ultrasonic waves on calcium extraction from slags and calcium carbonate synthesis, the efficiency of calcium carbonate synthesis according to the with or without of ultrasonic waves was analyzed. The synthetic efficiency of PCC was investigated according to various experimental conditions, and the synthesized calcium carbonate was analyzed using XRD and SEM. In both slags, the amount of PCC decreased as the reaction temperature increased. The pH at the end of the experiment capable of synthesizing the maximum PCC in the carbonation reaction was 7 (irradiated with ultrasound) and 8 (irradiated without ultrasound), respectively. Because the pH of the extraction filtrate is different when irradiated with or without ultrasound, the pH was adjusted to 9 by injecting an additive (10 M NaOH) before the carbonation experiment, and then the experiment was performed. When calcium was extracted from KR slag, the crystal phase appeared as calcite regardless of the pH at the end of the experiment. However, when calcium was extracted from the converter slag and the pH was set to 7 at the end of the experiment, the crystal phase of PCC appeared as a mixture of calcite and vaterite.

• Journal of Korean Society of Water and Wastewater
• /
• v.18 no.5
• /
• pp.638-648
• /
• 2004

In many drinking water treatment plants, chlorination process is one of the main techniques used for the disinfection of water. This disinfecting treatment leads to the formation of haloacetic acid (HAAs). In this study, headspace solid-phase microextraction (HS-SPME) was studied as a possible alternative to liquid-liquid extraction for the analysis of HAAs in drinking water. The method involves direct derivatization of the acids to their methyl esters without methyl tert-butyl ether (MTBE) extraction, followed by HS-SPME with a $2cm-50/30{\mu}m$ divinylbenzene/carboxen/polydimethylsiloxane fiber. The effects of experimental parameters such as selection of SPME fiber, the volume of sulphuric acid and methanol, derivatization temperature and time, the addition of salts, extraction temperature and time, and desorption time on the analysis were investigated. Analytical parameters such as linearity, repeatability and limit of detection were also evaluated. The $2cm-50/30{\mu}m$-divinylbenzene/carboxen/polydimethylsiloxane fiber, sulphuric acid of 1ml, methanol of 3ml, derivatization temperature of $50^{\circ}C$ derivatization time of 2hrs, sodium chloride salt of 10g, extraction time of 30 minutes, extraction temperature of $20^{\circ}C$ and desorption time of 1 minute at $260^{\circ}C$ were selected as the optimal experimental conditions for the analysis of HAAs. The linearities ($r^2$), relative standard deviations (%RSD) and limits of detection (LOD) for HAAs were 0.9978~0.9991, 1.1~9.8% and $0.05{\sim}0.2{\mu}g/l$, respectively.

• Analytical Science and Technology
• /
• v.13 no.5
• /
• pp.636-645
• /
• 2000

A method is described for the determination of organotins in water samples by GC/MS. Optimized derivatization methods for ethylation and hydrogenation of organotins were surveyed according to various reaction conditions such as time, pH and concentration of reagents. The organotins were extracted with n-hexane in presence of 0.1% tropolone and hydrogenated with sodium borohydride. Extraction recoveries of organotins with hydrogenation were in the range of 61-112%. After ethylation, organotins in water samples were extracted by liquid-liquid extraction (LLE) and solid-phase extraction (SPE). Using LLE, extraction recoveries were in the range of 74-113%. The recoveries ranged from 61-97% in the case of SPE with styrene-divinylbenzene copolymers. Method detection limits of hydrogenated and ethylated organotins ranged from 0.05 to 0.5 ng/ml and from 0.02 to 0.05 ng/ml, respectively.

• Bulletin of the Korean Chemical Society
• /
• v.30 no.1
• /
• pp.35-42
• /
• 2009

Headspace micro solid phase extraction using mulberry paper bag (HS-MPB-$\mu$-SPE) has been developed and validated for the analysis of volatile flavor compounds from five spice by gas chromatography-mass spectrometry (GC/MS). HS-MPB-$\mu$-SPE was performed with adsorbent particles enclosed inside a mulberry paper bag. Four different kinds of adsorbents such as Tenax TA, Porapack Q, dimethylpolysiloxane and polyethylene glycol were tested. The extraction solvents compared were petroleum ether, methylene chloride, and chloroform. Better results were obtained when Tenax TA and petroleum ether were used. The limit of detection (LOD) and the limit of quantitation (LOQ) were in the range of 1.3 ng/mL and 4.3 ng/mL, respectively, for o-cymene as a model compound of monoterpene. Proposed method showed good reproducibility (3.3%, RSD) and good recoveries (94.0%). The HS-MPB- μ-SPE is very simple to use, inexpensive, rapid, requires small sample amounts and solvent consumption. Because the solvent for extraction is reduced to only a very small volume (0.6 mL), there is minimal waste or exposure to toxic organic solvent and no further concentration step. This method allows successful characterization of the headspace in contact with the five spice sample. Strong trans-anethole from star anise or fennel is a characteristic flavor of five spice powders. HS-MPB-$\mu$-SPE combined with GC/MS can be a promising technique for the broad spectrum measurement of volatile aroma compounds from solid spices.

• Resources Recycling
• /
• v.22 no.6
• /
• pp.19-25
• /
• 2013

Solvent extraction experiments have been conducted to separate Zr(IV) and Hf(IV) from chloride solutions by using LIX63 and Cyanex301. Zr and Hf were extracted by cation exchange reaction in the pH range from 1 to 4 by the extratants. Since the extraction percentage of the two metals was similar to each other, it was difficult to separate the two metals by using LIX63 or Cyanex301. Use of a mixture of LIX63/TBP or Cyanex301/TBP resulted in antagonism in our experimental ranges. Our data showed that there is some possibility of separating the two metals by the mixture of Cyanex301 and TBP because the extraction percentage of Hf decreased more rapidly than that of Zr as HCl concentration was decreased. The mixture of LIX63 and Cyanex301 had little effect on the separation of the two metals.

• Analytical Science and Technology
• /
• v.29 no.5
• /
• pp.219-224
• /
• 2016

불산 중 극미량 음이온의 고상추출과 이온크로마토그래프를 이용한 고감도 분석법이 개발되었다. 불산 중 불소이온이 고상에 의해 제거하였고 이어서 음이온 (F⁻, CH₃COO⁻, Cl⁻, Br⁻, NO₃⁻, PO₄³⁻, SO₄²⁻)들이 이온크로마토그래프를 이용하여 연속적으로 분리하였다. 고상 추출법에 영향을 주는 각 인자들 (흡착제의 선택, 시료의 부피 및 pH, 용출 용액과 용출용액의 부피)을 결정하였으며 그 결과 흡착제로서 Oasis WAX 컬럼이 가장 우수하였고 1.0 mL의 시료부피, 용출용액으로 50 mM 초산암모늄염 5 mL가 분리능에서 가장 우수하였다. 개발한 방법에 의한 음이온 (Cl⁻, Br⁻, NO₃⁻, PO₄³⁻, SO₄²⁻)들의 방법검출한계는 25 % 불산용액 (w/w) 중에 0.04~0.30 µg/L의 범위를 보였고 정밀도는 20.0와 40.0 µg/L의 농도에서 5 % 이내를 보였다. 한 제조회사에 의한 25 % 불산 중 음이온의 4.2에서 47.5 µg/L의 범위로 모두 검출되었다. 이 방법은 시험절차가 간단하고, 재현성 및 감도가 좋아서 반도체회사에서 불산 중 음이온 불순물을 정도 관리하는데 매우 유용한 방법이 될 것으로 판단된다.

• Journal of the Korean Chemical Society
• /
• v.30 no.5
• /
• pp.423-432
• /
• 1986

Atomic absorption spectrophotometric (AAS) determination of hexavalent chromium [Cr(VI)] in a waste water was studied. Cr(VI) was extracted with p-xylene from the wastewater, in the way of ion pair formation with anion exchanger aliquat-336(tri-caprylmethyl ammonium chloride). 100ml waste water, after organic materials were extracted out with toluene, was acidified with conc. HCl adjusting the medium to pH 0.5 and 20ml of p-xylene containing 0.01M aliguat-336 was used to extract Cr(VI) from the acidified solution. The absorbance of chromium was measured with air-acetylene flame at 357.9nm. Standard addition method was used in the determining concentration of Cr(VI) extracted. No interference has been found in the extraction of Cr(VI) by the Al(III), Fe(III) and Cr(III) ion presented. However, Fe(II) decreased the absorbance of Cr(VI), due to the fact Fe(II) reduces Cr(VI) to Cr(III). The contained organic material was removed prior to extracting process, since it may reduced the absorbance of Cr(VI). The recovery of added Cr(VI) was over 96%, which seems to be promising and the relative standard deviation was 3.95%

• Journal of the Korean Chemical Society
• /
• v.52 no.2
• /
• pp.133-139
• /
• 2008

A new sensitive and selective spectrophotometric method for determination of trace amounts of cadmium using a polyvinyl chloride membrane containing bis-(2-ethylhexyl)phthalate as a solid phase extraction medium was investigated. Bis-(2-ethylhexyl)phthalate has used as a plasticizer. Cd(II) in an aqueous solution was trapped on the membrane in the form of colorful Cd (II)-I- - MG complexes (which MG is malachite green) and the cadmium complex was concentrated in the membrane. The absorbance of the green membrane was measured at 629 nm using a spectrophotometer, and then, the concentration of the cadmium was calculated using a calibration curve, which expressed the relationship between the Cd(II) concentration and the membrane absorbance after coloring for 25 min. The calibration curve was linear in the range of 10-760 μgL-1 cadmium in the test solution. The detection limit based on the 3Sbl criterion was 1.8199 μgL-1 and the relative standard deviations (RSD) were less than 4 % (n=5). The proposed method has been successfully applied to the determination of trace amounts of cadmium in the Tadjan River water sample (Sari-Iran), and the mean value of 28.7 μgL-1 was obtained.

• Biomolecules & Therapeutics
• /
• v.15 no.1
• /
• pp.65-72
• /
• 2007

Flax seed(Linseed, Linum usitatissimum L.) and its oil, a richest source of alpha-linolenic acid(ALA)(${\omega}-3$), contain saturated fatty acids, neurotoxic cyanogen glycosides and immuno-suppressive cyclic-nonapeptides. Present paper describes the development of two chemical processes, Process-A and -B, to remove saturated fatty acids and to destroy cyclic nonapeptides and cyanogen glycosides from flax seed oil. Process-A consists of three major steps, i.e., extraction of fatty acid mixture by alkaline saponification, removal of saturated fatty acid by urea-complexation, and triglyceride reconstruction of unsaturated fatty acid via fatty acyl-chloride activation using oxalyl chloride. Process-B consists of preparation of fatty acid ethyl ester by transesterification, elimination of saturated fatty acid ester by urea-complexation, and reconstruction of triglyceride by interesterification with glycerol-triacetate (triacetin). The destruction of lipophilic cyclic nonapeptide during saponification or transesterification processes could be demonstrated indirectly by the disappearance of antibacterial activity of bacitracin, an analogous cyclic-decapeptide. The cyanogen glycosides were found only in the dregs after hexane extraction, but not in the flax seed oil. The reconstructed triglyceride of flax seed oil, obtained by these two different pathways after elimination of saturated fatty acid and toxic components, showed agreeable properties as edible oil in terms of taste, acid value, iodine and peroxide value, glycerine content, and antioxidant activity.