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Akihide ITOH, Taisuke NAGASAWA, Yanbei ZHU, Kyue-Hyung LEE, Eiji FUJIM ...
2004 Volume 20 Issue 1 Pages
29-36
Published: 2004
Released on J-STAGE: July 02, 2004
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In order to elucidate the distributions of the elements among the particulate and dissolved fractions in pond water, major-to-ultratrace elements in different sizes of particles as well as in the filtrate passed through the 0.05 μm filter were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS). The different sizes of particle samples (
ca. 100 - 300 μg each) were collected on the membrane filters with pore sizes of 10, 3.0, 1.2, 0.4, 0.2 and 0.05 μm, respectively, by sequential fractionation. As a result, about 40 elements in different sizes of particles could be determined by ICP-AES and ICP-MS, after acid digestion using HNO
3/HF/HClO
4. Then, the fractional distribution factors of major-to-ultratrace elements among the particulate and dissolved fractions were estimated from the analytical results. The total contents of Al, Fe, Ti, REEs (rare earth elements), Bi, Pb and Ag in the particulate fractions (larger than 0.05 μm) were more than 80 - 90%, while those of Ca, Sr, Cs, W, Ba, Mn and Co in the dissolved fraction, which corresponded to the filtrate passed through the 0.05 μm membrane filter, were more than 80%. It was further found that the fractional distributions of Cu and Zn in the dissolved fraction were
ca. 50%. In addition, the enrichment factors (EFs) of the elements in the particulate fractions with particle sizes of 3.0 - 10 μm and 0.05 - 0.2 μm were estimated to elucidate their geochemical characteristics in natural water.
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Jinghua ZHANG, Toshiko NAGAHAMA, Hiroki OHWAKI, Yasuhiro ISHIBASHI, Yu ...
2004 Volume 20 Issue 1 Pages
37-43
Published: 2004
Released on J-STAGE: July 02, 2004
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To understand the cause of discoloration of the sea laver “
nori,” which is found in the Ariake Sea, the concentrations of pigments and elements in the normal and discolored laver samples were determined. In the discolored samples, a decrease in all of the pigments, chlorophyll
a and carotenoids, and proteinous pigments, phycobiliproteins, was clearly observed. This was accompanied by a decrease in the content of Fe, Zn, Mn, Cu, and P. Good correlations between these elements and chlorophyll
a, as well as between these elements and phycobiliproteins, were confirmed, indicating that, in addition to the deficiency of nitrogen and phosphorus, the deficiency of trace elements (Fe, Zn, Mn, and Cu), which are specifically required for photosynthesis, could be a reason for the discoloration of
nori. The cause of elemental deficiency is also discussed.
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Babu Rajendran RAMASWAMY, Hiroaki TAO, Masashi HOJO
2004 Volume 20 Issue 1 Pages
45-53
Published: 2004
Released on J-STAGE: July 02, 2004
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Uwakai of Japan is famous for pearl and yellowtail fish culture. Recently, pearl culture farming in that region has suffered from a low production of pearls. An illegal use of organotin antifouling paints on fishing nets was reported. In the line of pollution studies, thus, the present investigation was carried out to examine the contamination status and fate of organotin compounds. Totally, 23 water, 10 sediment and 8 pearl oyster tissue samples were analyzed for tributyltin (TBT), triphenyltin (TPT), and their breakdown products (di- and mono compounds) by gas chromatography combined with inductively coupled plasma mass spectrometry (GC/ICP-MS). The results show that the TBT concentrations in water, sediment and biota were in the range from 0.11 to 10.6 ng Sn l
-1, 0.35 to 2500 ng Sn g
-1, and 50.4 to 181 ng Sn g
-1, respectively. The values for sediment and biota are expressed on the dry-weight basis. Triphenyltin in water, sediment and biota were in the range from 0.009 to 0.108 ng l
-1, non-detect to 12.7 ng g
-1, and non-detect to 6.83 ng g
-1, respectively. Although the TBT concentration in seawater is below the tentative assessment level of 10 ng l
-1 set by the Japanese Environment Agency in 1992, it may cause endocrine disruption/other effects in aquatic organisms. Octyltin compounds (mono-, di- and trioctyltin) were also quantified in seawater and sediment. The detection of dibutyldimethyltin (DBDMT) and tributylmonomethyltin (TBMMT) in sediment (methylated butyltins comprised 2.8 - 31% of total butyltins), and TBMMT in seawater suggested that biomethylation of anthropogenic tributyltins is a significant transformation pathway in the coastal environment.
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Ryoichi KIZU, Naoki OTSUKI, Yoshiko KISHIDA, Akira TORIBA, Atsushi MIZ ...
2004 Volume 20 Issue 1 Pages
55-59
Published: 2004
Released on J-STAGE: July 02, 2004
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We developed a new mammalian cell-based luciferase reporter gene assay for androgenic and antiandrogenic activities of chemicals and environmental samples. Environmental samples usually have a complex matrix that may contain the constituents acting as androgen receptor (AR) agonists, AR antagonists or aryl hydrocarbon receptor (AhR) agonists. AhR agonists are known to elicit the antiandrogenic effect through cross-talk between AR and AhR signal transduction pathways. In this study, PC3/AR human prostate carcinoma cells were transiently transfected with a prostate-specific antigen (PSA) promoter-driven luciferase expression plasmid. The cells were treated with a test compound or an environmental sample for 24 h at 37°C and then measured for luciferase activity. The luciferase activity was induced by dihydrotestosterone (DHT) in a concentration-dependent manner in a concentration range from 10 fM to 1 nM. R1881, a synthetic androgen receptor agonist, induced luciferase activity and its inductive effects was additive to that of DHT. The luciferase activity was not induced by cortisol, a glucocorticoid, progesterone, a progestin, and 17
β-estradiol, an estrogen in a concentration range of up to 1 μM. DHT-induced luciferase activity was reduced by bicalutamide and cyproterone acetate, AR antagonists, and also by benzo[
a]pyrene, an aryl hydrocarbon receptor agonist, through AhR-mediated pathways. All of these findings indicate that the present assay system correctly responds to AR agonists, AR antagonists and AhR agonist and, therefore, it is a powerful tool for the sensitive and selective screening of chemicals and environmental samples for their androgenic and antiandrogenic activities. We developed the first assay system, in which the expression of luciferase was driven by the promoter of a prostate-specific antigen gene, a typical human androgen-regulated gene.
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Teruya MAKI, Hiroshi HASEGAWA, Hiroshi WATARAI, Kazumasa UEDA
2004 Volume 20 Issue 1 Pages
61-68
Published: 2004
Released on J-STAGE: July 02, 2004
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A new monitoring system for bacterial communities involving dimethylarsinic acid (DMAA) decomposition was provided by combining the MPN (Most Probable Number) method and RFLP (restriction-fragment-length polymorphism analysis). The abundance of DMAA decomposing bacteria was estimated by the MPN method using a bacterial culture medium, which included DMAA as the sole carbon source, indicating bacterial cell densities of 1700 cells/ml in Lake Kahokugata and 330 cells/ml in Lake Kibagata. After isolating the dominant bacteria using agar plates, the isolates were classified into some genotype groups by RFLP analysis using 16S rDNA sequences. Classification of the RFLP analysis indicated that 14 isolates of Lake Kahokugata were classified into 6 types, which included 2 dominant types related to genus
Pseudomonas, while 8 isolates of Lake Kibagata displayed 6 types including one or two isolates. Moreover, the RFLP types were unique for each lake, suggesting that DMAA decomposing bacteria were specific for the aquatic environment related to the arsenic cycle. The activities of DMAA decomposition mostly matched with the RFLP type category of the isolates. Accordingly, combining the MPN method with the RFLP analysis will play an important role in elucidating the distributions and dynamics of the DMAA-decomposing bacterial community.
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Nobuaki OGAWA, Keiji YOSHIMURA, Ryoei KIKUCHI, Tetsuya ADZUHATA, Toru ...
2004 Volume 20 Issue 1 Pages
69-72
Published: 2004
Released on J-STAGE: July 02, 2004
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Water samples from radiation and upslope types of fog were collected at Takanosu Basin and Hachimantai mountain range of Akita Prefecture in northern Japan, respectively. The effect of the long-range transport of pollutants from the Asian Continent to the basin and the mountain range on the chemical characteristics of two types of fog was studied using chemical analysis data for the water samples as well as the back-trajectories of the air mass. In particular, non-sea-salt (nss)-SO
42- of radiation fog provided a much higher concentration than that of upslope fog, which suggests that nss-SO
42- might be transported mainly from the Asian Continent. The transport and uptake mechanism of pollutants in the radiation fog water were explained based on their accumulation in the basin due to anticyclonic subsidence and by the long-lasting fog behavior.
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Yoshiaki NAKANISHI, Michiaki SUMITA, Kaoru YUMITA, Takashi YAMADA, Tak ...
2004 Volume 20 Issue 1 Pages
73-78
Published: 2004
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Alga as
Achnanthes minutissima among diatoms is a widely adaptable taxon on the state of an aquatic environment. In this study, it was found that diatom had a specific tolerance to heavy metals (Cu, Zn, Pb, and Cd
etc.) in river water samples, because the diatom assemblage consisted of almost only
Achnanthes minutissima in Kakehashi river and Godani river, which were polluted with waste water from Ogoya copper mine. The relationship between the concentrations of heavy metals (Cu, Zn, Pb and Cd) in river water and the attached substances (algae and silt
etc.) and the relative abundances of diatom taxa were investigated in detail. The results indicated that the higher is the concentration of heavy metals in the river environment, the higher is only the relative abundances of
Achnanthes minutissima. Thus, the taxon can be used as a bioindicator of heavy metal pollution. The relative rates of toxic chemical forms of copper in algae were 61 - 92% in the attached substances and 49 - 70% in the sediment on the river bed, respectively. Therefore, it was found that diatom as
Achnanthes minutissima had a tolerance to heavy metals in river water, being able to live in such an environment. Since the water treated with calcium hydroxide from the deposition reservoir of Ogoya mine enters in Godani river, the river is polluted by heavy metals (Cu, Zn, Pb and Cd
etc.). From the viewpoint of both biological and chemical analyses, Godani river is still polluted with heavy metals, because their concentrations in the river samples were very high. On the other hand, in Kakehashi river, the concentrations of heavy metals were very low and the distributions of some diatoms appeared in an unpolluted Nishimata river were observed. Therefore, Kakehashi river seems to be considerably recovered from heavy-metal pollution after closing the Ogoya mine.
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Katsuro ANAZAWA, Yasuhiko KAIDA, Yoshinori SHINOMURA, Takashi TOMIYASU ...
2004 Volume 20 Issue 1 Pages
79-84
Published: 2004
Released on J-STAGE: July 02, 2004
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River water and sediment samples were collected at the same site in a vicinity of an abandoned mine, and the concentrations of major elements and heavy metals were determined. The chemical correlations were observed by principal component analysis (PCA), and the samples were classified by cluster analysis (CA) based on the PCA scores. The PCA results presented a macroscopic viewpoint of covariance structure,
i.e., the chemical elements could be classified into three groups: 1) major elements and heavy metals in the river water, 2) Cd, Fe and Mn in the sediments, and 3) Cu and Zn in the sediments. The CA results implied a similarity of chemical compositions in most parts of the study area, except the ranges close to the abandoned copper mine. At the mixing location of mining water with natural river water, major elements and cadmium showed simple physical mixing (conservative mixing). Other heavy metals (Cu, Fe, Mn and Zn) showed the massive precipitation at the mixing event. The PCA structure was mainly interpreted in terms of the mixing process between mining water and diluted natural river water.
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Jing LIANG, Qiuquan WANG, Benli HUANG
2004 Volume 20 Issue 1 Pages
85-88
Published: 2004
Released on J-STAGE: July 02, 2004
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Non-dispersive atomic fluorescence spectrometry (NDAFS) coupled with vapor generation (VG) sample introduction was applied to the determination of the concentrations of hazardous heavy metals, such as arsenic, cadmium, lead and mercury, in seawater, soils and total airborne particulate matter (PM) collected around the Xiamen area in China. Almost 100% sample introduction efficiency was achieved by using thiourea and ascorbic acid for the pre-reduction of As
V to As
III, K
3Fe(CN)
6 and tartaric acid for pre-oxidation of Pb
II to Pb
IV, and masking the interferences arising from the coexisting transition metals to As, Cd, Hg and Pb during their vapor generation process. Moreover, a novel sample pretreatment device was developed to avoid the loss of mercury, lead, cadmium and arsenic during sample pretreatment. With such methods, the detection limit (DL) of arsenic, cadmium, lead and mercury was down to 0.08, 0.03, 0.05, 0.01 ng mL
-1 (3σ), respectively. The relative standard deviations (RSD,
n = 11) for arsenic, cadmium, lead and mercury at 10 ng mL
-1 were 0.9%, 1.6%, 1.3% and 2.0%, respectively. The concentrations of hazardous heavy metals in the environmental samples collected in Xiamen, China are in the range from 0.02 ± 0.001 ng mL
-1 in seawater to 15.3 ± 0.2 μg g
-1 in soils. Besides flame/GF-AAS and ICP-AES/MS, VG-NDAFS should be another choice for the determination of hazardous heavy metals in environmental samples.
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Hiroshi HASEGAWA, Teruya MAKI, Kohnosuke ASANO, Kentaro UEDA, Kazumasa ...
2004 Volume 20 Issue 1 Pages
89-93
Published: 2004
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The sample preparation and analytical methodology are described for detecting biologically produced iron(III)-binding ligands in laboratory cultures of coastal marine phytoplankton. The iron(III)-binding ligands from the culture media were purified by passage through a column packing with a hydrophobic absorbent. The concentrations and stability constants of the ligands were determined by adsorptive cathodic stripping voltammetry with competitive ligand equilibration. The analytical results of the cultivated cultures suggest that eukaryotic phytoplankton would produce iron(III)-binding ligands in analogy with other microorganisms.
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Mingbiao LUO, Shuping BI, Chenyi WANG, Junzhong HUANG
2004 Volume 20 Issue 1 Pages
95-100
Published: 2004
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In the present work, a new method was established by applying solid-phase extraction (SPE) to preconcentrate and separate polymeric aluminum (Al) and using ICP-AES to determine the polymeric Al, the total monomeric Al, and the total Al in soil extracts, respectively. A modified resin was prepared with impregnated 8-hydroxyquinoline-5-sulfoxinate (HQS) on the anion-exchange resin. It has good recognition ability for Al fractions, compared to the commonly used cation ion-exchange resin, which has a better ability to adsorb cations and a weak ability to recognize detailed Al species. The optimum conditions for Al fractionation sorption, elution and separation and the interference of foreign ions were studied with the prepared resin by continuous column and batch procedures. Monomeric Al was bound to Pyrocathecol Violet (PCV) at pH 6.2, whereas the polymeric Al species did not react with PCV for at least 15 min. Because a stable complex of Al-PCV was not absorbed on the HQS modified resin, the polymeric Al could be preconcentrated on-line by the HQS-modified resin. The adsorbed polymeric Al was eluted with 3 mL of 3 mol L
-1 of HCl, and then detected by ICP-AES. The method has been applied to directly determine polymeric Al in soil extracts with high selectivity as well as a high preconcentration factor. It gives a limit of detection of 0.6 ng mL
-1 with a relative standard deviation of less than 5.7% (
n = 5, 0.24 μg mL
-1 Al).
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Shinji TSUNOI, Hirotaka SHIOJI, Minoru TANAKA
2004 Volume 20 Issue 1 Pages
101-105
Published: 2004
Released on J-STAGE: July 02, 2004
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Derivatization of tributyltin for tandem mass spectrometry is described. Tributyltin (TBT) and triphenyltin (TPT) were derivatized with sodium tetrakis(4-fluorophenyl)borate. After optimization of their MS/MS conditions, derivatization conditions were examined. Under the optimum conditions using
in-situ derivatization, the calibration curves for the TBT and TPT were linear in the ranges of 0.4 - 200 and 1.2 - 200 pg of Sn, respectively. The detection limits for TBT and TPT were 0.07 and 0.43 pg of Sn, respectively. In the case of TBT, the detection limit with 4-fluorophenylation was improved about five times compared with that with pentylation (0.35 pg). This improvement is ascribed to the bonddissociation energy of Sn-aryl being stronger than that of Sn-alkyl. Namely, the selective fragmentation of 4-fluorophenyl TBT resulted in high sensitivity. The relative recoveries of TBT and TPT from seawater were 99 and 109%, respectively. The method was successfully applied to the seawater samples.
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Etsu YAMADA, Yusuke HOSOKAWA, You FURUYA, Kazumasa MATSUSHITA, Yasuro ...
2004 Volume 20 Issue 1 Pages
107-112
Published: 2004
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A simple analysis of volatile organic compounds (VOCs), such as benzene, toluene,
m,p-xylene, and
o-xylene, at low levels in the atmosphere was conducted using passive samplers. The methods were applied to analyzing the behavior and origin of VOCs in Kyoto City. The passive samplers were exposed for 7 - 14 days at sampling sites in Kyoto City and for 30 days in the mountains (Mt. Hiei and Mt. Daimonji). Shibata gas-tube samplers packed with activated carbon were used for the determination of VOCs. The absorbed VOCs were extracted into carbon disulfide (CS
2) and measured by FID-GC. The determination limits and relative standard deviations for VOCs were 0.3 μg/m
3 and 3%, respectively. The samplers were set up at 5 sites in March, 2001 and at 13 stations on Mt. Hiei in November, 2002. The average concentrations of ambient benzene, which were higher than the environmental criterion (3.0 μg/m
3), except for those on Mt. Daimonji from March, 2001, to February, 2002, decreased to below 3.0 μg/m
3 from March, 2002, to February, 2003. The decrease in ambient benzene may have been due to a decrease in the benzene content in gasoline by the end of 1999, and also by implementation of the Pollutant Release and Transfer Register (PRTR) Act in 2001.
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Piyanete SRITHARATHIKHUN, Mitsuko OSHIMA, Yanlin WEI, Jürgen SIMO ...
2004 Volume 20 Issue 1 Pages
113-118
Published: 2004
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A simple and rapid procedure for SO
2 determination in air was developed by using a flow injection analysis (FIA) system coupled with a 3-hole chromatomembrane cell (CMC). The CMC was applied for the on-line collection/concentration of SO
2 from air into a solution of 2 g l
-1 triethanolamine (TEA) solution as an absorbing solution: SO
2 was converted to SO
32- in the alkaline absorbing solution. The solution containing absorbed SO
2 was introduced into the carrier stream of the FIA system. The amount of SO
32- in the absorbing solution was measured by spectrophotometry with a mixed reagent of pararosaniline and formaldehyde, and was converted to the concentration of SO
2 in the air sample. A calibration graph prepared by using standard sodium sulfite aqueous solutions was adopted for the determination of SO
3-2 in the absorbing solution. The SO
2 concentration in indoor air examined was found to be 22.7 ± 0.2 ppbv using 20 ml of air sample with the air flow rate of 5 ml min
-1, where the relative standard deviation was 1.7%. The detection limit for aqueous solutions and air samples were 6.9 × 10
-8 M and 0.48 ppbv, respectively. The measuring time for one sample was about 10 min when a 20 ml air sample was used. The interferences from common anionic species, formaldehyde and acetaldehyde, were also examined.
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Ning TANG, Rina TAGA, Tetsuyuki HATTORI, Kenji TAMURA, Akira TOROBA, R ...
2004 Volume 20 Issue 1 Pages
119-123
Published: 2004
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A method using high-performance liquid chromatography with chemiluminescence detection was developed for analyzing mutagenic nitrobenzanthrone (NBA) isomers in airborne particulates. The method was a modification of our previously described method for analyzing nitropolycyclic aromatic hydrocarbons (NPAHs). The pretreatment and reducing conditions for 1-, 2-, 3- and 10-NBAs were the same as those for NPAHs. In order to separate these NBA isomers, we used a polymeric-type ODS column (Cosmosil 5C-18MS); a mixture of 40% acetonitrile and 60% 10 mM imidazole-HClO
4 buffer was employed as the mobile phase at a flow rate of 1 mL/min. The isomers of 1-, 2-, 3- and 10-NBA were determined in chemiluminescence with linear calibration graphs from 0.1 to 4 pmol, from 200 to 4000 pmol, from 1 to 50 pmol and from 10 to 400 pmol, respectively. The detection limits (
S/N = 3) of 1-, 2-, 3- and 10-NBA isomers were 0.02 pmol, 35 pmol, 0.3 pmol and 3 pmol, respectively. The method was used to analyze airborne particulates at a heavy traffic site in Kanazawa. 2- and 3-NBAs were detected in the extracts of the particulates, while 1-NBA and 10-NBA were not detected. The atmospheric concentrations of 2- and 3-NBAs were 1.83 pmol/m
3 and 24.7 fmol/m
3, respectively.
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Takashi ASADA, Kikuo OIKAWA, Kuniaki KAWATA, Tsutomu IYOBE, Akifumi YA ...
2004 Volume 20 Issue 1 Pages
125-128
Published: 2004
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The ion chromatographic determination of ammonia in air using a sampling tube of porous carbon carbonized at 500°C was examined. When the mean recovery and the reproducibility for a series of five determinations were examined for 1 and 10 ppm ammonia gases, the mean recovery (
n = 5) and the relative standard deviation were 97.0% and 3.5% for 1 ppm and 86.9% and 2.8% for 10 ppm, respectively. Furthermore, the recovery from 10 ppm ammonia gas increased with an increase in the extraction time, and a recovery of 99.7% was obtained for 180 min of extraction time. The mean collection efficiency for 1 and 10 ppm ammonia gas was 102.5% and 96.5%, respectively. The relation between the sampling volume and the peak area was linear, and the linearity was 0.999 of the correlation coefficient. The ammonia gas concentration in an actual goat shed could be determined by this sampling device for a sampling volume of 5 L at a flow rate of 1 L/min; 0.79 ppm of the determination value practically agreed as compare with 0.78 ppm from collection by a boric acid solution.
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Naoya KISHIKAWA, Seigo MORITA, Mitsuhiro WADA, Yoshihito OHBA, Kenichi ...
2004 Volume 20 Issue 1 Pages
129-132
Published: 2004
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This paper describes a highly sensitive and selective method for the determination of hydroxylated polycyclic aromatic hydrocarbons (PAHs-OH) in airborne particulates. PAHs-OH were extracted from airborne particulates with ethanol by ultrasonication. The extractant was further cleaned up by solid phase extraction (SPE) with an aminopropylsilica cartridge, and subsequently analyzed by reversed-phase high-performance liquid chromatography with fluorescence detection. 2-Hydroxy-1-acetonaphthone was used as an internal standard. By the proposed method, 2-hydroxyfluorene and 1-hydroxypyrene were identified in airborne particulates and their concentrations were determined for the first time.
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Yoshiyuki WATABE, Takuya KONDO, Hiroe IMAI, Masatoshi MORITA, Nobuo TA ...
2004 Volume 20 Issue 1 Pages
133-137
Published: 2004
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A new high-performance liquid chromatography (HPLC) method has been developed to detect ultra-low concentrations of bisphenol-A (BPA) (below 1 ng/L (ppt)) using column switching electrochemical detection (ECD). The results were superior to those obtained from manual pretreatment procedure with membrane stationary phase. BPA is inherently ubiquitous in the environment, including tools and solvents used for its analysis; to obtain meaningful results, therefore, the concentration of the overall BPA contamination must be below the detection limit for BPA using the analytical system. Therefore, purified water for preparing the standard BPA solution must be filtered with a hydrophobic membrane to suppress BPA background levels of contamination. In addition, we investigated methods for effectively preserving environmental water containing BPA. The addition of a small amount of ethylenediaminetetraacetic acid (EDTA) provided good recovery even after overnight storage. By employing these precautionary measures and procedures to reduce BPA contamination from the analytical procedure, we could accurately determine 1 - 10 ppt of BPA in environmental water samples using a column switching HPLC system.
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Yasushi SEIKE, Ryoko FUKUMORI, Yukiko SENGA, Hiroki OKA, Kaoru FUJINAG ...
2004 Volume 20 Issue 1 Pages
139-142
Published: 2004
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A new and simple method for the determination of hydroxylamine in environmental water, such as fresh rivers and lakes using hypochlorite, followed by its gas choromatographic detection, has been developed. A glass vial filled with sample water was sealed by a butyl-rubber stopper and aluminum cap without head-space, and then sodium hypochlorite solution was injected into the vial through a syringe to convert hydroxylamine to nitrous oxide. The head-space in the glass vial was prepared with 99.9% grade N
2 using a gas-tight syringe. After the glass vial was shaken for a few minutes, nitrous oxide in the gas-phase was measured by a gas chromatograph with an electron-capture detector. The dissolved nitrous oxide in the liquid-phase was calculated according to the solubility formula. The proposed method was applied to the analysis of fresh-water samples taken from Iu river and Hii river, flowing into brackish Lakes Nakaumi and Shinji, respectively.
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Atsuko NISHIGAKI, Chiaki KUROIWA, Masami SHIBUKAWA
2004 Volume 20 Issue 1 Pages
143-147
Published: 2004
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A liquid chromatography-mass spectrometry (LC/MS) method was developed for the separation and determination of linear alkylbenzenesulfonates (C
10 - C
14 LAS) in environmental water samples using a hydrophilic polymer column (Shodex Mspak GF-310 4D). This method involves a solid-phase extraction of the LAS samples with a Sep-Pak PS-2 cartridge. The LAS components were separated on the column with a mobile phase of 29% (w/v) acetonitrile-water containing 0.8 mM di-
n-butylammonium acetate and 0.2 M acetic acid, and were detected by mass spectrometry with electrospray ionization. Detection limits of the developed method based on selected ion monitoring (SIM) technique for the C
10 - C
14 LAS standards were 13 - 47 ng L
-1. The concentrations of the C
10 - C
14 LAS in the environmental water samples ranged between 5 - 317 μg L
-1 for a river water sample and 0.4 - 6.4 μg L
-1 for a seawater sample. Linear relationships between the logarithms of retention factors and the alkyl chain lengths for each phenyl positional isomer of LAS could successfully be used for the identification of the isomer peaks.
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Noriko HATA, Erini YUWATINI, Kaori ANDO, Mika YAMADA, Issei KASAHARA, ...
2004 Volume 20 Issue 1 Pages
149-152
Published: 2004
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A high-enrichment method was proposed for the HPLC determination of trace di(2-ethylhexyl)phthalate (DEHP) in environmental water. A micro-organic ion-associate phase (IAP) was formed in situ from an aqueous sample by adding 4-trifluoromethylanilinium ion and dodecylbenzenesulfonate ions. Centrifugation of the solution led to the isolation of a liquid organic phase containing DEHP at the bottom of the centrifuge tube. The volume of the phase formed was less than 30 μL. DEHP was extracted into the IAP quantitatively during phase formation. After discarding the aqueous phase, the ion associate was dissolved with 50 μL of 2-methoxyethanol, and DEHP in the concentrate was determined by HPLC with an ultra-violet (UV) diode-array detector. DEHP in the concentrations range from 0.8 to 78 μg L
-1 was determined with good precision. The recovery tests for DEHP added to some river water were satisfactory. The detection limit of DEHP, defined as 3-times the standard deviation of the blank signals, was 0.07 μg L
-1 (
n = 3). The present method is very simple, and was applied to the determination of DEHP in the river water samples collected around Toyama City, Japan.
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Kazuhiko TAKEDA, Hiroshi TAKEDOI, Shuhei YAMAJI, Keiichi OHTA, Hiroshi ...
2004 Volume 20 Issue 1 Pages
153-158
Published: 2004
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The photochemical formation rates of hydroxyl radicals (OH radicals) in river water and seawater were determined by a simple, rapid and sensitive benzene probe method, in which phenol formed by the reaction between benzene and photochemically-generated OH radicals was analyzed by on-line preconcentration HPLC. The OH radical formation rates from well-known OH radical sources, such as nitrate, nitrite and hydrogen peroxide, were in good agreement with those reported previously. River water samples containing high concentrations of nitrate and nitrite were found to show high OH radical formation rates. Ten to 80% of the OH radical formation in river water and seawater was due to the photolysis of nitrate and nitrite, but OH radical formation from hydrogen peroxide was negligible. The OH radical formation from unknown sources other than nitrate, nitrite and hydrogen peroxide was strongly correlated to the amount of fluorescent matter.
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Shinichi AOKI, Yasuro FUSE, Etsu YAMADA
2004 Volume 20 Issue 1 Pages
159-164
Published: 2004
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Humic substances and other dissolved organic matter (DOM) in Lake Biwa and the surrounding rivers were investigated to elucidate their origins and behavior. An annual increase in chemical oxygen demand (COD) has been observed in the northern basin of Lake Biwa since 1985. The concentrations of dissolved organic carbon (DOC) in the northern and southern basins of Lake Biwa were 1.7 - 2.4 mgC/l and 1.9 - 2.6 mgC/l, respectively. The DOC concentrations tended to be high in summer and low in winter, and the seasonal changes in the concentrations of humic substances were small. The humic substances content of DOM was considered to be comparatively small because the ratio of the concentration of humic substances to DOC was in the range of 0.14 - 0.32. From the results of the fractionation of DOM in lake waters, it was estimated that hydrophobic acids, such as humic substances and hydrophilic acids, were about 25% and 45%, respectively. The main origin of hydrophobic acids in Lake Biwa may be humic substances from soils around the rivers that flow into Lake Biwa, while hydrophilic acids may be due to the inner production by phytoplankton. Therefore, the increase of COD in the northern basin of Lake Biwa may be attributed to the contributions of not only humic substances but also hydrophilic acids.
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Md. Mustafizur RAHMAN, Kaoru FUJINAGA, Yasushi SEIKE, Minoru OKUMURA
2004 Volume 20 Issue 1 Pages
165-170
Published: 2004
Released on J-STAGE: July 02, 2004
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A simple
in situ visual and tristimulus colorimetric method for the determination of trace arsenic in environmental water after collecting arsenic on a test paper impregnated with mercury(II) bromide and rosaniline chloride by its reduction aeration has been developed. The color development on the test paper is based on the formations of AsH(HgBr)
2 (yellow) and/or As(HgBr)
3 (brownish yellow) by a reaction between mercury(II) bromide and arsine (AsH
3), which is produced through the reduction of As(III) (arsenite ion) and/or As(V) (arsenate ion) in a sample solution. To a sample solution, potassium iodide, tin(II) chloride, zinc sand and 4 ml of 6 M hydrochloric acid solution were added successively. The liberated arsine was collected on the test paper. The yellow or brownish-yellow color intensity on the test paper was measured by a tristimulus colorimeter and also by a visual method. The established method is applicable to the determination of arsenic in environmental water sample such as river, brackish, and seawater types.
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Shinsuke OHNO, Miho TANAKA, Norio TESHIMA, Tadao SAKAI
2004 Volume 20 Issue 1 Pages
171-175
Published: 2004
Released on J-STAGE: July 02, 2004
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A flow injection-catalytic spectrophotometric method using a serial flow cell was proposed for the successive determination of trace amounts of copper and iron. This method is based on the oxidation coupling of
p-anisidine with
N,N-dimethylaniline in the presence of hydrogen peroxide to form a dye, which has an absorption maximum at 740 nm. In this indicator reaction, ligands such as 1,10-phenanthroline (phen) and diphosphate were achieved to improve the sensitivity and selectivity. Under the optimal experimental conditions, the determinable ranges were 0.05 - 5 ppb for copper and 0.5 - 100 ppb for iron, respectively. The RSDs (
n = 10) were 0.78% for 0.5 ppb copper(II) and 0.5% for 200 ppb iron(III). The sample throughput was 30 h
-1. The present flow-injection method was applied to the determination of copper and iron in standard river water, tap water, and other natural water samples, and also to the analysis of labile and inert complexes in synthesized samples containing humic acid with copper(II) or iron(III).
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Yasuro FUSE, Takeshi YAMADA, Etsu YAMADA
2004 Volume 20 Issue 1 Pages
177-181
Published: 2004
Released on J-STAGE: July 02, 2004
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5′-Chloro-5-dodecyl-2,4,2′-trihydroxyazobenzene (CDTA) impregnated XAD-4 resin (CDTA resin) was prepared, and applied to the preconcentration of trace aluminum from environmental water samples with satisfactory results. Aluminum was measured by flow-injection analysis (FIA) with fluorescence detection by using lumogallion after the preconcentration of aluminum with CDTA resin. Fe
3+ and other coexisting substances had no interference on the determination of aluminum by the present method. Chemical speciation of trace aluminum in environmental water was carried out by using the CDTA resin after the separation of aluminum species with ionic exchangers without changing the pH. About 50% of water-soluble aluminum in Lake Biwa was found to be aluminum organic species (anion species).
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Kyue-Hyung LEE, Yoshiki MURAOKA, Mitsuko OSHIMA, Shoji MOTOMIZU
2004 Volume 20 Issue 1 Pages
183-187
Published: 2004
Released on J-STAGE: July 02, 2004
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A solid phase collection/concentration method using anion exchanger filters and a small syringe packed with chelating resin fibers is adopted as a preconcentration tool for trace elements and a separation tool for matrices in aqueous samples prior to the measurement by inductively coupled plasma-mass spectrometry (ICP-MS). The effects of fiber volume, sample volume, eluent volume, and sample flow rate on metal recoveries were investigated in detail to obtain optimum pretreatment conditions. Several heavy metals (HMs) such as, V, Mn, Co, Ni, Cu, Zn, Ga, Cd, Pb, Th and U, as well as 14 rare earth elements (REEs) in sample solutions at pH 6 were quantitatively collected on the solid phase. These adsorbed elements were completely recovered by eluting with 2 ml of 1.0 M nitric acid. At pH 6, more than 99% of alkali and alkaline earth metals in sample solutions were eliminated. The proposed method was evaluated by analyzing two standard reference materials (SRM): peach leaves (NIST 1547) and pond sediment (NIES No. 2). The solid samples were decomposed by microwave-heating and pressurizing acid digestion technique, and then treated by the proposed syringe-type pretreatment method, followed by the ICP-MS measurement. The analytical results for HMs in the SRMs obtained by the present method agreed well with the certified values.
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Eiji FUJIMORI, Seiko IWATA, Kazuaki MINAMOTO, Kyue-Hyung LEE, Akihide ...
2004 Volume 20 Issue 1 Pages
189-194
Published: 2004
Released on J-STAGE: July 02, 2004
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The partitionings of major-to-ultratrace elements between industrial waste incineration fly ash (IWIFA) and industrial waste incineration bottom ash (IWIBA) in industrial waste incinerators were investigated by measuring their concentration distributions, where the incineration ash samples were collected from three different types of industrial waste incinerators. The concentrations of the elements in the incineration ash samples were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS). As a result,
ca. 40 elements in the concentration range from mg g
-1 to sub-μg g
-1 could be determined in both IWIFA and IWIBA samples. The concentration ratios of
CF/
CB (
CF, concentration in fly ash;
CB, concentration in bottom ash) for analyte elements were used to evaluate the partitionings of the elements between fly and bottom ashes. Then, the correlations between the
CF/
CB values of the elements and the dissociation energies of their monoxides were examined to evaluate the kinetic behaviors of the elements during the incineration processes. It was found that lithophile and siderophile elements, which have a large affinity with oxygen, were almost equally distributed between fly and bottom ashes, regardless of the dissociation energies of their monoxides. On the other hand, chalcophile elements with rather large volatility provided different behaviors; the elements with the smaller dissociation energies of monoxides were more partitioned in fly ashes than those with the larger ones.
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Nyein Nyein AUNG, Tsutomu URYU, Jun YOSHINAGA
2004 Volume 20 Issue 1 Pages
195-198
Published: 2004
Released on J-STAGE: July 02, 2004
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Lead isotope ratios,
viz.
207Pb/
206Pb and
208Pb/
206Pb, of the commercially available certified reference materials (CRMs) issued in Japan are presented with an objective to provide a data set, which will be useful for the quality assurance of analytical procedures, instrumental performance and method validation of the laboratories involved in environmental lead isotope ratio analysis. The analytical method used in the present study was inductively coupled plasma quadrupole mass spectrometry (ICPQMS) preceded by acid digestion and with/without chemical separation of lead from the matrix. The precision of the measurements in terms of the relative standard deviation (RSD) of triplicated analyses was 0.19% and 0.14%, for
207Pb/
206Pb and
208Pb/
206Pb, respectively. The trueness of lead isotope ratio measurements of the present study was tested with a few CRMs, which have been analyzed by other analytical methods and reported in various literature. The lead isotopic ratios of 18 environmental matrix CRMs (including 6 CRMs analyzed for our method validation) are presented and the distribution of their ratios is briefly discussed.
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Lan YANG, Akira KOTANI, Hideki HAKAMATA, Fumiyo KUSU
2004 Volume 20 Issue 1 Pages
199-203
Published: 2004
Released on J-STAGE: July 02, 2004
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A simple and highly sensitive method has been developed for determining
ortho-phenylphenol (OPP) in lemon rind by high-performance liquid chromatography with electrochemical detection using a microbore column (μHPLC-ECD). Based on the voltammetric behavior of OPP, μHPLC-ECD was established using a CAPCELL PAK C-18 UG 120 microbore ODS column, 17 mM acetic acid-sodium acetate buffer (pH 4.0)/acetonitrile (60/40, v/v) as a mobile phase and an applied potential at +0.9 V
vs. Ag/AgCl. The current peak height was found to be linearly related to the amount of OPP injected from 3.4 pg to 1.7 ng (
r > 0.999). The detection limit (
S/N = 3) was 3.4 pg (20 fmol), which was 100 times greater in terms of sensitivity when compared to conventional HPLC with UV detection. Standard OPP at 0.425 ng was detected with a relative standard deviation (RSD) of 1.9% (
n = 10). The OPP contents in several lemon samples were determined by the present method. The recoveries of OPP from lemon rind exceeded 98% with an RSD (
n = 5) of less than 3.01%.
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Jiye JIN, Yasutada SUZUKI, Naoyoshi ISHIKAWA, Toyohide TAKEUCHI
2004 Volume 20 Issue 1 Pages
205-207
Published: 2004
Released on J-STAGE: July 02, 2004
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The present study was aimed at developing a portable miniaturized FIA system with a two-electrode based amperometric detector for on-site monitoring of residual chlorine in environmental samples. The electrode potential control and current data collection were conducted with a home-designed potentiostat with a size of 150 × 100 × 40 mm and the weight of 350 g. It was confirmed that the amperometric response increased in proportion to the chlorine concentration up to 5 μg/ml, and the detection limit for chlorine was 0.05 μg/ml. Besides a drastic reduction in the size of the analytical system, such miniaturization achieved the advantages of increased speed, minimal mobile-phase consumption, and high sensitivity. The proposed method was successfully applied to the determination of residual chlorine in samples of pool water and tap water. The results were well agreed with those obtained by the
N,N-diethyl-
p-phenylenediamine (DPD) photometric method.
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Shin-ichiro FUJII, Takahito TOKUYAMA, Mitsuru ABO, Akira OKUBO
2004 Volume 20 Issue 1 Pages
209-212
Published: 2004
Released on J-STAGE: July 02, 2004
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On-chip fluorescence determination of sulfite and nitrite with
N-(9-acridinyl)maleimide (NAM) and 2,3-diaminonaphthalene (DAN) has been developed using a novel fluorescence detection unit for microchip analysis. Usually, these fluorescence reagents are derivatized and detected separately in microchip analysis because different fluorescence wavelengths are emitted. The proposed fluorescence detection unit has optical fibers with no optical filter, and plural wavelengths of fluorescence were detected sensitively, even in the microchip. In this study, the simultaneous determination of sulfite and nitrite in environmental samples was performed with a polymer microchip analysis system. The calibration curves of sulfite and nitrite showed linear relations (
R2 = 0.998 (sulfite) and
R2 = 0.990 (nitrite)), and the relative standard deviations (RSD) for 4 runs were 2.1% (20 μM sulfite) and 1.3% (20 μM nitrite), respectively. The proposed method was applied to the recovery test of sulfite and nitrite in environmental samples.
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