分析化学
Print ISSN : 0525-1931
59 巻 , 12 号
選択された号の論文の13件中1~13を表示しています
総合論文
  • 南 知晴, 肥後 衣里, 中塚 清次, Abigail Parcasio Cid, Thi Dieu Huong Vu, 則末 和宏, 宗林 ...
    原稿種別: 総合論文
    2010 年 59 巻 12 号 p. 1087-1096
    発行日: 2010年
    公開日: 2011/01/24
    ジャーナル フリー
    生物活性微量金属(bioactive trace metals)は,生物にとって必須又は毒性の高い元素を指す.海洋環境において特に重要な生物活性微量元素は,Al,Mn,Fe,Co,Ni,Cu,Zn,Cd,Pbである.これらは,一般に海水中で数十nmol kg−1以下の微量成分である.従来の分析法では,目的元素の汚染混入(コンタミネーション),主要成分による妨害,不完全な回収率(特にAl,Mn)が問題であった.著者らは,固相抽出-誘導結合プラズマ質量分析(ICP-MS)法に基づく9元素の分析法を開発した.本法では,エチレンジアミン三酢酸基とイミノ二酢酸基を有する新しいキレート吸着剤を充填したカラムを閉鎖式濃縮系で使用した.本法により,9元素すべてを海水主要成分から分離し,定量的に同時濃縮することが可能となった.Mn,Co,Ni,Cu,Cdの操作ブランク値はICP-MSの検出限界(1 mol L−1硝酸をICP-MSで測定して得られるバックグラウンドの標準偏差の3倍)以下であったが,Al,Fe,Zn,Pbでは操作ブランクが検出され,それぞれ0.14,0.03,0.07,0.003 nmol kg−1であった.また,8倍濃縮時の検出限界は,Al,Mn,Fe,Co,Ni,Cu,Zn,Cd,Pbに対して,それぞれ0.24,0.01,0.04,0.002,0.01,0.01,0.06,0.01,0.001 nmol kg−1であった.本稿では,この分析法の開発と,外洋海水を用いる国際相互較正に本法を適用した結果について概説する.
報文
  • 伊藤 彰英, 山口 真実, 山田 亜矢子, 新垣 輝生, 可部 徳子, 我那覇 翔子
    原稿種別: 報文
    2010 年 59 巻 12 号 p. 1097-1104
    発行日: 2010年
    公開日: 2011/01/24
    ジャーナル フリー
    本研究では,イオン対形成メンブランフィルター捕集濃縮法を併用したモリブデンブルー法により沖縄島内3か所の沿岸海水中のリン化合物を2007年~2008年にかけて2か月に一度測定を行い,「溶存態リン」,「粒子吸着態リン」,「酸難溶粒子態リン」,「全リン」の存在形態別濃度分布から沖縄沿岸の海域別の水質の特徴を考察した.その結果,人口密集地から離れた郊外域に位置する瀬底島試料と那覇市市街域に位置する泊港試料では異なる特徴が明らかになった.瀬底島試料では全リンは平均14.0 μg L−1であり,溶存態リンの平均割合が16%,酸難溶粒子態リンの平均割合は65% であった.これに対して,泊港試料では全リンは平均62.6 μg L−1であり,溶存態リンの平均割合は64% であった.両者の相違は,サンゴ礁が生息し人為影響が少ない海域と,市街域に位置し人為影響を受けやすい海域の特徴の違いを反映したものと考えられる.また,溶存リン酸イオンと栄養塩型微量金属元素との関連性を検討した結果,瀬底島沿岸海水中の〔Cd〕/〔PO43−〕比は1.46~3.7×10−3となり,測定した他の沖縄沿岸海域及び北太平洋の外洋表層海水の文献値より特異的に高いことが明らかになった.この理由は明らかではないが,Cdが瀬底島沿岸域に何らかの要因で流入している可能性,あるいはサンゴ礁海域の植物プランクトンの溶存リン酸イオンの取り込み速度の違いによる可能性が考えられる.
  • 南 尚嗣, 坂上 寛敏, 白 俊玲, 万徳 佳菜子, 原田 大資, 高橋 信夫, 厚谷 郁夫, 深澤 達矢, 濱田 浩美, 五十嵐 聖貴, ...
    原稿種別: 報文
    2010 年 59 巻 12 号 p. 1105-1111
    発行日: 2010年
    公開日: 2011/01/24
    ジャーナル フリー
    摩周湖は,国連環境計画GEMS/Water(Global Environment Monitoring System/Water)プログラムのベースラインモニタリングステーションとして登録されている日本で唯一の湖である.本研究では,摩周湖水中ニッケル濃度の深度プロファイルを明らかにし,ニッケルの供給源に関する知見を得ることを目的に検討を行った.その結果,成層期の表層湖水中ニッケル濃度は温度躍層より深部の湖水中濃度に比べて高く,湖岸の降雨試料及びカルデラ壁上部の積雪試料中ニッケル濃度は,表層湖水中濃度より更に高いことを明らかにした.これらの傾向はバナジウム濃度にも見られた.雪試料中ニッケル濃度とバナジウム濃度の比は,石油燃焼ばい塵中の両元素濃度比の報告値と一致した.一方,温度躍層深度でニッケル濃度の高濃度異常が観察された.湖水中両元素濃度の深度分布挙動,雨及び雪試料中の両元素濃度と湖水中濃度との比較を通して,湖水中ニッケルの一部は化石燃料燃焼排気が起源と考えられる粒子状物質として,大気経由で摩周湖に供給されている可能性を示した.
  • 江草 清行, 金子 聡, 近藤 欣正, 勝又 英之, 鈴木 透, 太田 清久
    原稿種別: 報文
    2010 年 59 巻 12 号 p. 1113-1117
    発行日: 2010年
    公開日: 2011/01/24
    ジャーナル フリー
    タンパク質を用いたバイオソープション前濃縮法と黒鉛炉原子吸光分析法を組み合わせ,環境水中の銀の定量を行った.タンパク質には,ヌトロース(カゼインナトリウム)を用いた.試料溶液のpH,撹拌時間,ヌトロース量,灰化温度,原子化温度,マトリックス元素などの影響を調べ,前濃縮条件を最適化した.最適な灰化温度と原子化温度は,それぞれ350℃ と1400℃ であった.本法による銀の濃縮倍率は15.5倍であった.検量線のダイナミックレンジは,銀0.1~3 ng/mLであった.検出限界(3S/N)は9 pg/mLであった.銀1.0 ng/mLを7回測定した場合の再現性は,相対標準偏差(R.S.D.)で5.6% であった.他元素の影響を検討したが,干渉はほとんど見られなかった.本法を池水中の銀の定量に適応し,満足いく結果が得られた.
  • 富田 陽子, 三原 義広, 田中 俊逸
    原稿種別: 報文
    2010 年 59 巻 12 号 p. 1119-1123
    発行日: 2010年
    公開日: 2011/01/24
    ジャーナル フリー
    ドデシル硫酸ナトリウム(SDS)によって底質から多環芳香族炭化水素類(PAHs)を抽出し,界面活性剤を塩酸によって相分離した後にHPLC-蛍光検出する方法について検討した.抽出の際のSDSの添加量,相分離の際の塩酸濃度,加熱温度,時間等について検討し,最適条件を試料中のSDS濃度を0.1 M,塩酸濃度を4 M,加熱温度を60℃,濃縮時間を90分間とした.PAHsの濃縮率は,キニザリングリーンSSを濃縮指標とし,相分離の前後でのキニザリングリーンSSの濃度変化から求めることができた.最適化条件におけるSDS界面活性剤相へのPAHsの濃縮率はおよそ10倍,模擬底質からのアントラセン,フルオランテン,ピレンの添加回収率は95% 以上を示した.中国東北部吉林省松花江の底質のPAHs分析に同法を適用したところ,アントラセン,フルオランテン,ピレンの濃度はそれぞれ80 μg/kg,230 μg/kg,220 μg/kgとなった.
ノート
  • 山本 孝, 黒谷 功, 山下 歩美, 河合 潤, 今井 昭二
    原稿種別: ノート
    2010 年 59 巻 12 号 p. 1125-1131
    発行日: 2010年
    公開日: 2011/01/24
    ジャーナル フリー
    The elemental analysis of a 1M hydrochloric acid leaching solution from soil samples in the mountain district of Shikoku was carried out by a portable liquid electrode plasma (LEP) atomic emission spectrometer. The contents of Na, K, Ca, Mg, Mn, and Fe were determined, and compared with those by flame photometry, flame atomic absorption spectrometry, ICP-MS and ICP-AES. The 600 V of the applied voltage was found to be suitable for the present sample solution at the use of a sample holder made of resin. The precision of the emission intensities for iterative measurements was improved by a normalization procedure with an emission line from the atomic hydrogen, and the relative standard deviations were ca. 20%. Results of quantitative analysis of soil-extracts by LEP atomic emission spectrometry were discussed based on geological data around the sampling area.
  • 田口 茂, 藤井 絢子, 起 孝志, 倉光 英樹, 波多 宣子
    原稿種別: ノート
    2010 年 59 巻 12 号 p. 1133-1136
    発行日: 2010年
    公開日: 2011/01/24
    ジャーナル フリー
    The photo-oxidation of Cr(III) to Cr(VI) with OH radicals formed under the irradiation of vacuum ultraviolet (VUV) was applied to the successive determination of Cr(VI) and total chromium by FIA. A sample solution containing Cr(III) was introduced into a quartz tube contacted to a VUV lamp radiating the light of 185 nm and 254 nm. Chromium(III) was oxidized to Cr(VI) quantitatively while passing through the quartz tube. The Cr(VI) was converted into a colored species with diphenylcalbazide in a reaction coil and the colored species was detected with an UV detector. For a sample solution containing Cr(III) and Cr(VI), without VUV irradiation, only Cr(VI) was determined. On the other hand, under VUV irradiation the total concentration of chromium, that is Cr(III) plus Cr(VI), was determined. The speciation of Cr(III) and Cr(VI) was easily performed by on/off switching the VUV lamp. Linear calibration was obtained at 0.05 – 1.0 mg dm−3 for both Cr(III) and Cr(VI). More than four samples were analyzed in one hour. This technique was successfully applied to synthesized plating wastewater.
  • 越川(金尾) 昌美, 渡邊 未来, 越川 海, 小松 一弘, 今井 章雄, 稲葉 一穂, 高松 武次郎
    原稿種別: ノート
    2010 年 59 巻 12 号 p. 1137-1142
    発行日: 2010年
    公開日: 2011/01/24
    ジャーナル フリー
    Speciation of aluminum (Al), including inorganic monomeric Al (Ali, the sum of aquo, hydroxy, and inorganically complexed forms), organic monomeric Al (Alo, the organically complexed form), and colloidal mineral Al (Alc, the fine particulate form that passes through a 0.4-μm pore size membrane filter), was investigated in circumneutral (pH 7–9) eutrophic Lake Kasumigaura, Japan. The mean concentrations calculated from the result of monthly observations during the period from January to December 2003 were compared among ten stations. Ali decreased downstream from the mouth of the influent rivers (0.07–0.10 μM) to the mouth of the effluent river (0.03 μM). Alc, which also decreased downstream (from 0.11 to 0.06 μM), was the major fraction (>50%) of total dissolved Al at all stations. Alo remained around 0.02 μM at all stations. In Lake Kasumigaura, a high concentration of Si (average 0.23 mM) seems to be involved in the removal of Ali and formation of Alc. Also, a high concentration of Ca (ave. 0.43 mM) seems to be acting as a competitive cation for complexation with a high concentration of dissolved organic carbon (ave. 0.26 mM), and inhibit the formation of Alo.
  • 丸尾 雅啓, 永岡 一樹, 小林 一星, 小沢 佳那子, 小畑 元
    原稿種別: ノート
    2010 年 59 巻 12 号 p. 1143-1147
    発行日: 2010年
    公開日: 2011/01/24
    ジャーナル フリー
    The pH conditions for the colorimetric determination of Fe(II) in oxic natural water samples were reexamined for analyses using PDTS (ferrozine) or bathophenanthroline disulfonic acid salt for the fixation of Fe(II) onboard a boat without an electricity supply. Bathophenanthroline disulfonic acid salt enhanced the reduction of Fe(III) to Fe(II), and produced an overestimation of the Fe(II) concentration in the water of a natural lake. PDTS enhanced the reduction of Fe(III) at pH 4.0, but showed almost no reduction of Fe(III) at pH 6.8. Oxidation of Fe(II) was observed at pH 9.0. PDTS at pH 6.8 showed no variation in Fe redox speciation in water within 30 h. As analyzed in the field onboard a boat, the Fe(II) concentration of a Japanese lake was measured by using the latter conditions with a solid-phase Fe(II)-ferrozine complex. Under irradiation with sunlight, the formation of Fe(II) on the lake surface was observed during the daytime. In contrast, the Fe(II) concentration in another lake that received no sunlight did not show a significant change within 6 h of sampling. This finding suggests that a portion of Fe(II) is stabilized by complexation with ligands present in the water. This estimate is supported by the difference between the Fe(II) concentration of identical river water samples measured using this method (26 nmol L−1) and chemiluminescence (0.8 nmol L−1).
  • 唐沢 宏樹, 木村 匡恵, 和久田 千晴, 栗原 路子, 辻野 兼範, 谷 幸則, 橋本 伸哉
    原稿種別: ノート
    2010 年 59 巻 12 号 p. 1149-1154
    発行日: 2010年
    公開日: 2011/01/24
    ジャーナル フリー
    Simultaneous determination method for 12 volatile halogenated organic compounds (VHOCs) in brackish water and seawater has been developed, based on purge and trap-gas chromatography/mass spectrometry. The limits of detection for VHOCs were <0.04 pmol L−1 for bromomethane, iodoethane and tribromomethane, <0.13 pmol L−1 for bromochloromethane, chloroiodomethane, chlorodibromomethane and bromoiodomethane, <0.21 pmol L−1 for chloromethane, dibromomethane, bromodichloromethane, and diiodomethane and 0.67 pmol L−1 for iodomethane. Good linearities of the calibration curves for 12 VHOCs were obtained in the concentration range up to100 pmol L−1. The correlation coefficients were >0.997 for bromochloromethane, chlorodibromomethane, bromodichloromethane, bromoiodomethane and tribromomethane, >0.981 for chloromethane, iodomethane, iodoethane, chloroiodomethane and diiodomethane, 0.967 for dibromomethane and 0.923 for bromomethane. Using this developed method, the concentrations of VHOCs in brackish water, coastal seawater and open ocean seawater were measured. The coefficients of variation were approximately <20% in all samples. Thus, this simultaneous highly sensitive analysis method was valuable for determination of trace levels of VHOCs concentrations in natural water.
  • 管原 庄吾, 圦本 達也, 鮎川 和泰, 木元 克則, 千賀 有希子, 奥村 稔, 清家 泰
    原稿種別: ノート
    2010 年 59 巻 12 号 p. 1155-1161
    発行日: 2010年
    公開日: 2011/01/24
    ジャーナル フリー
    We developed a simple in situ extraction method for dissolved sulfide (H2S, HS, S2−) in sandy mud sediments. All analytical procedures were performed in a sealed system of glass syringes to prevent the volatilization of hydrogen sulfide and the oxidation of sulfide by air. An adequate amount of sandy mud sediment was put in a graduated glass syringe on site immediately after sampling. This procedure was performed using a unique and useful tool ; a plastic syringe had its front portion cut, so as to avoid the attachment of sediment to the inside wall of the syringe. To the sediment sample in the syringe, distilled water, deoxygenated by babbling with nitrogen gas, was injected via a three-way stopcock with another syringe. After mixing well, the sample was filtrated into the other syringe through a filter (0.45 μm). In addition, zinc acetate solution was added to the filtrate in the syringe, and was then spectrophotometrically determined by the methyleneblue method after being brought back to laboratory. The proposed method was successfully applied to bottom sediment samples taken from northeast of Ariake Bay. A high concentration of dissolved sulfide was detected in a warmer season. This method should be useful to evaluate sediment quality and to assess the influence of dissolved sulfide on benthos such as bivalves.
  • 南澤 宏明, 水島 健人, 朝本 紘充, 南澤 麿優覧, 斎藤 和憲, 中釜 達朗
    原稿種別: ノート
    2010 年 59 巻 12 号 p. 1163-1167
    発行日: 2010年
    公開日: 2011/01/24
    ジャーナル フリー
    Chromium exists widely in nature as both trivalent and hexavalent forms. Although, Cr(III) is an essential element for humans at trace levels, Cr(VI) has great toxicity and carcinogenicity at low concentrations. Cr(VI) is typically present in aqueous solutions, such as CrO42− anion. Polyurethane foam (PUF) was impregnated with hydrochroric acid (HCl-PUF) and then used to remove Cr(VI) from environmental water samples. However, Cr(VI) was not adsorbed on PUF, Cr(VI) was adsorbed on HCl-PUF. In this study, the adsorption conditions of Cr(VI) on HCl-PUF were investigated, such as the adsorption time and the solution pH. Further, the deadsorption conditions of Cr(VI) from HCl-PUF were investigated, such as the kind of eluents and their concentrations. Cr(VI) was quantitatively adsorbed on HCl-PUF at a pH range 3.0-8.0 from aqueous solutions and their adsorption isotherms were fitted by the Freundlich equation. The Cr(VI) adsorbed on HCl-PUF as eluted with 3.0 mol dm−3 nitric acid. The property of HCl-PUF was extended to the preconcentration and determination of trace amounts of Cr(VI) in water samples by Inductively Coupled Plasma Emission Spectrometry (ICP-AES).
アナリティカルレポート
  • 冨岡 典子, 小松 一弘, 越川(金尾) 昌美, 今井 章雄, 松重 一夫, 稲葉 一穂
    原稿種別: アナリティカルレポート
    2010 年 59 巻 12 号 p. 1169-1174
    発行日: 2010年
    公開日: 2011/01/24
    ジャーナル フリー
    In order to learn about the environmental conditions of Lake Kasumigaura, National Institute for Environmental Studies has been pursued in a limnological survey of the Lake monthly from 1977. The concentrations of copper and iron in surface water of Lake Kasumigaura were monitored at five sites from 1989. The concentrations of copper were about 0.6-1 μg L−1 for St. 1, 3, 9 and 12, whereas they were 0.8-1.4 μg L−1 for St. 7. This similarity may be due to the formation of a stable soluble complex species, and also small variations of the copper concentrations in inflowed rivers. The seasonal changes in the copper concentrations became unclear in the middle 1990s. The iron concentrations in the Lake were lower than 10 μg L−1, except those at St. 1. It seems that most of the iron is supplied from rivers, and it precipitates at the river-mouth region. The concentrations of iron at St. 1 were 50 μg L−1 before the early 1990s, whereas they became 20 μg L−1 after the late 1990s. Although the reasons for the changes in the late 1990s are very complicated, the change in the surface level of the lake water, by controlling the Hitachi River Watergate, which started in 1996, may be one of the reasons. The surface level of the lake water became 30 cm higher after control of the Watergate ; this may have moved the sedimentation-active river-mouth area to the upper side of the lake.
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