• Journal of Korean Society of Water and Wastewater
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• v.32 no.6
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• pp.559-572
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• 2018

The aim of this study was to evaluate pretreatment methods for 27 pharmaceuticals and personal care products (PPCPs) in various sewage samples using a modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) and online solid-phase extraction with LC-MS/MS. Extraction efficiencies of PPCPs in the solid phase under different experimental conditions were evaluated, showing that the highest recoveries were obtained with the addition of sodium sulfate and ethylenediaminetetraacetic acid disodium salt dehydrate in acidified conditions. The recoveries of target compounds ranged from 91 to 117.2% for liquid samples and from 61.3 to 137.2% for solid samples, with a good precision. The methods under development were applied to sewage samples collected in two sewage treatment plants (STPs) to determine PPCPs in liquid and solid phases. Out of 27 PPCPs, more than 19 compounds were detected in liquid samples (i.e., influent and effluent) of two STPs, with concentration ranges of LOQ-33,152 ng/L in influents and LOQ-4,523 ng/L in effluents, respectively. In addition, some PPCPs such as acetylsalicylic acid, ibuprofen, and ofloxacin were detected at high concentrations in activated sludge as well as in excess sludge. This methodology was successfully applied to sewage samples for the determination of the target compounds in STPs.

• Environmental Engineering Research
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• v.16 no.1
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• pp.41-45
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• 2011

The aim of this investigation was to demonstrate a rapid bioluminescence bioassay for comparison of the toxicity of whole solids and the aqueous extracts of various environmental solid samples. With regard to the toxicities, those for the soil extracts were mostly found to be lower than those of whole soils, which may have been caused by un-extracted pollutants or dilution during the extraction process. Solid samples from dam-reservoir sediments and municipal refuses were also tested. The toxicities of the solid extracts (0-34%; refuses and sediments) were much lower than those of the whole solids (13-91%). The bioluminescence inhibition test indicated that the harmful effects of the contaminated solids samples were greater than those of the solid extracts.

• Journal of Korean Society on Water Environment
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• v.32 no.6
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• pp.600-627
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• 2016

Korea is one of the countries with a large veterinary antibiotics market, although antimicrobial resistance in bacteria is becoming a serious issue in many countries. The Korean government started to take interest in estimating the effects of livestock manure on rivers and agricultural soils and in monitoring of heavy metals, organic pollutants and antibiotics in the ambient water and soil. In this paper, pre-treatment methods to separate the selected antibiotics from solid samples were reviewed. It is essential to select an efficient and appropriate procedure for pre-treatment due to the high proportion of proteins and organics in biosolid samples. Pre-treatment consists of extraction followed by clean-up. Initially, homogenized samples were extracted by sonication, mechanical agitation or pressurized liquid extraction with methanol/acetonitrile/water mixture under acidic/basic conditions depending on the compound. However, aminoglycosides and colistin were extracted with 5% trichloroacetic acid and HCl, respectively. Since the ${\beta}-lactams$ are easily decomposed in acidic and basic conditions, they were extracted in neutral pH. Filtration with a membrane (pore size, $0.2{\mu}m$) or solid phase extraction with HLB and methanol, as eluents, was normally applied for the clean-up. At least, three different pre-treatment procedures should be adopted to screen all the selected antibiotics in solid samples.

• Journal of Soil and Groundwater Environment
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• v.12 no.6
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• pp.46-52
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• 2007

A toxicity method using bioluminescence producing bacteria, Escherichia coli DH5 RB1436, was developed and applied on solid environmental samples. In the assay, 1 g soil sample was mixed with 4 ml RB1436 strain. Sets amended with p-buffer were employed for control in soil test, showing approximately 108% of sets amended with combusted soils. Measurable differences were observed between relatively more polluted groups (HP) and less polluted groups (LP) of soil samples, showing average toxicity 43 and 26%, respectively, in direct soil toxicity test. $EC_{50}$'s for all soil groups appeared in the range of $1.8{\sim}4.6\;g$, but those of sediments from dam reservoir and refuses were below 0.22 g. This developed bioassay should prove useful as a screening test for toxicity in various types of environmental solid samples.

• Journal of Industrial and Engineering Chemistry
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• v.67
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• pp.461-468
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• 2018

A highly sensitive, selective and rapid method for the determination of lead based on the reaction of lead (II) with 5-(4'-chlorophenylazo)-6-hydroxypyrimidine-2,4-dione (CPAHPD) and the solid phase extraction of the Pb(II)-CPAHPD complex with Amberlite XAD-2000 was developed, in the presence of pH 5.6 buffer solution and Triton X-114 medium. CPAHPD reacts with lead to form a violet complex with a molar ratio of 2:1 (CPAHPD to lead). This complex was enriched by the solid phase extraction with Amberlite XAD-2000. An enrichment factor of 500 was obtained by elution of the complex from the resin with a minimal amount of isopentyl alcohol(0.2 mL). In isopentyl alcohol medium,the molar absorptivity of the complex is $1.13{\times}10^6L\;mol^{-1}cm^{-1}$ at 647 nm. Beer's law is obeyed in the range of $5.0-160ng\;mL^{-1}$ in the measured solution. The relative standard deviation for 10 replicate samples of $50ng\;mL^{-1}$ level is 1.26%. The detection and quantification limits reaches 1.5 and $4.7ng\;mL^{-1}$ in the original samples. The presented procedure was successfully applied for determination of lead content in real samples such as vegetables, waters, biological and soil samples with satisfactory results.

• Journal of the Korean Wood Science and Technology
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• v.44 no.6
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• pp.890-896
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• 2016

Paulownia tomentosa is one of fast-growing wood species in Korea. In order to evaluate the solid bioenergy properties of Paulownia tree, this study examined the heating value, moisture content (MC), pH and proximate analysis of stem, branch, root, bark and leaf. The heating values of wood parts were slightly higher than those of bark and leaf, and that of branch was the highest among all the samples. The higher moisture content of bark and leaf referred to their lower heating value. Also, the pH of stem, branch and root was similar and lower than those of bark and leaf. The ash content of bark and leaf was much higher than that of wood parts, which is the one of the reasons for effect on the lower heating value and higher pH. While, the volatile matter content (VMC) of bark and leaf was lower than those of wood parts. The bark showed the highest fixed carbon content (FCC), while the FCC of stem was the lowest among all the samples. The obtained results are encouraging that the Paulownia tree could be totally utilized as alternative fuels for bioenergy production.

• Bulletin of the Korean Chemical Society
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• v.28 no.3
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• pp.373-378
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• 2007

A micro organism Agrobacterium tumifacient as an immobilized cell on a solid support was presented as a new biosorbent in a simple and sensitive spectrophotometry determination of Ni(II) in various samples using 4-hydroxy benzaldehyde-4-bromophenyl hydrazone as a color developing agent (λmax 497 nm) at pH 4.0 ± 0.2. Beer's law was obeyed over the range of 0.01-0.1 μg L-1. The molar absorptivity and Sandell's sensitivity were 1.285 × 105 L mol-1cm-1 and 0.007245 μg cm-2 respectively. Under these conditions, the preconcentration factor obtained was 82, and the detection limit achieved was 0.05 μg L-1. The detailed study of various interfering ions made the method more sensitive and selective. The recovery of Ni(II) from various samples range from 97.75 to 99.35%. The present method was successfully applied for the determination of Ni(II) in spiked, natural water and alloy samples. The proposed method was compared with reported methods in terms of Student's ‘t'-test and Variance ratio ‘f'-test which indicates that there is no significant difference between proposed and literature method at 95% confidence level.

• Environmental Engineering Research
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• v.20 no.2
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• pp.127-132
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• 2015

Perfluorooctane sulfonate (PFOS) and Perfluorooctanoic acid (PFOA) are persistent environmental pollutants, extremely stable, and possibly adversely affect human health. They are widely used in many industries and consumer goods, including sunscreen products. These substances are stable chemicals made of long carbon chains, having both lipid- and water-repellent qualities. The research objectives are (1) to find the most effective method for the preparation of semi-liquid samples by comparing solid phase extraction (SPE) and centrifugation after Pressurized liquid extraction (PLE), and (2) to determine the contamination levels of PFOS and PFOA in waterproof sunscreen samples. All sunscreen samples were analyzed by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). Sunscreen samples were purchased from domestic and international brands sold in Thailand. Special chemical properties were considered for the selection of samples, e.g., those found in waterproof, sweat resistant, water resistant, and non-stick products. Considering the factors of physical properties, e.g., operation time, chemical consumption, and recovery percentage for selecting methods to develop, the centrifugation method using 2 mL of extracted sample with the conditions of 12,000 rpm and $5^{\circ}C$ for 1 hour after PLE was chosen. The highest concentrations of PFOS and PFOA were detected at 0.0671 ng/g and 21.0644 ng/g, respectively. Even though present concentrations are found at ng/g levels, the daily use of sunscreen products is normally several grams. Therefore, a risk assessment of PFOS and PFOA contamination in sunscreen products is an important concern, and more attention needs to be paid to the long-term effects on human health.

• Journal of Korean Society on Water Environment
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• v.21 no.6
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• pp.549-563
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• 2005

The study was carried out to develop and standardize the analytical method of 1,4-dioxane in water. The National Institute of Environmental Research in Korea has monitored for 1,4-dioxane in water since 1998 and it has been detected in environmental water occasionally. But the environmental pollution and analytical method in water is not well known over the world. The trace analytical method at low-${\mu}/L$ level is prerequisite in order to evaluate the residue of 1,4-dioxane in water. Evaluation of the method was demonstrated by comparing and analyzing with liquid-liquid extraction, solid-phase extraction and purge & trap technique. As a result of experiment by standard solutions and raw samples, the precision and accuracy for three methods were obtained within error rate of about 10%. Therefore, three methods were standardized as official monitoring method in Korea. Also, a convenient and simple liquid-liquid extraction method for the analysis of 1,4-dioxane in water was developed by combined with gas chromatography/mass spectrometry and applied to the water samples in Korea

• Bulletin of the Korean Chemical Society
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• v.28 no.12
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• pp.2293-2298
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• 2007

In this study, a dithizone extraction technique involving purge & trap GC-MS was developed for the determination of methylmercury in biological samples, especially blood and fish. After alkaline digestion, methylmercury in biological samples was extracted into dithizone and back-extracted into aqueous sulfide solution. The extracted methylmercury was converted to the volatile ethyl derivative, purged and trapped onto a solid-phase collection medium, and then introduced into the GC-MS system. The determined MDLs of the established method were 0.9 ng·g?1 for biological samples and its accuracy and precision were found to be 93% and 3.8%, respectively. The method was validated by analysis of CRMs such as SRM 966, BCR 463 and IAEA 407 and all analytical results were within certified ranges with average RSDs of less than 6%. The analytical results of field-sampled fish also showed that the method can be successfully used as an alternative for commonly used distillation method followed by GC-CVAFS detection.