JP2013064603A - 重金属分析装置及び重金属の分析方法 - Google Patents
重金属分析装置及び重金属の分析方法 Download PDFInfo
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Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
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Abstract
【解決手段】一定量の抽出液17aを循環させることにより重金属を含む測定試料16aを充填したカラム16に上記抽出液を通過させて測定試料を洗浄するとともに抽出液に重金属を抽出する重金属抽出部11と、重金属抽出部で重金属を抽出した抽出液から測定対象の重金属を選択的に吸着する重金属吸着部12と、溶離液18により重金属吸着部で吸着した重金属を溶離する溶離部13とを備え、重金属抽出部と重金属吸着部とが第1流路19により相互に接続され、溶離部と重金属吸着部とが第2流路21により相互に接続され、重金属吸着部が第3流路22により溶離液に含まれる溶離した重金属を測定する測定部14に接続されることを特徴とする。
【選択図】図1
Description
しかし、上記特許文献2に示される土壌分析システムは、分析項目に示される通り、土壌中の重金属を対象に分析するものではない。
2段階:炭酸塩と結合している形態
3段階:Fe−Mn酸化物と結合している形態
4段階:コロイド状の有機物あるいは硫黄と結合している形態
5段階:ケイ酸塩岩石などの結晶内に存在し最も溶出しにくい形態(鉱物)
このとき用いられる抽出液は、
1段階:MgCl2(pH7)、
2段階:CH3COOH/CH3COONa(pH5)、
3段階:NH2OH−HCl/CH3COOH(pH3)、
4段階:HNO3−H2O2(pH1〜2)、
5段階:HF−HClO4(pH<1)
となっているが、本発明の分析方法では、機器への影響を考慮して1段階から4段階までの化学形態分析を連続的に行うことができる。これは、重金属に汚染された土壌から、どのpHレベルの水によって溶出するか判定するものであり、特に酸性雨の多い、火山地帯周辺地域での農地、埋め立て処分場、工場跡地などの土壌分析診断に迅速な対応が可能である。なお、上記化学形態分析の5段階目においては、熱を加えなければ土壌を溶かすことできず、加熱によって危険なフッ素や塩素ガスが発生するため、本発明の適用外とした。また、4段階目は1段階目〜3段階目に比べて抽出効率が悪いため、抽出効率を上げるためには、5段階目と同様に熱を加えることが考えられるが、4段階においては、1段階目〜3段階目に比べて流速を半分程度に減少させ、循環(抽出)時間も倍程度に延ばすことで、室温でも重金属を抽出することができる。
先ず、採取した土壌を測定試料とし、粒度は0.01〜1mmに調整した。また図1に示す重金属分析装置10を用いた。次いで、図2に示すように、測定試料16aを充填したカラム16を重金属抽出部11に接続し、このカラム16に導入流路26を介して抽出液(1M塩酸)17aを一定量導入した。そして、図3に示すように、導入した抽出液17aを導入流路26を含む循環流路27を介してカラム16に1時間循環させて、抽出液17aに測定試料に含まれる重金属(Cu、Zn、Pb)を抽出した。次に、カラム16を循環する抽出液17aの循環を停止した後、図4に示すように、抽出液17aを脱イオン化水24aとともに送出流路28を介して重金属吸着部12に送り、図5に示すように、重金属吸着部12の作用電極37と抽出液17aとの間に−0.8Vの電位を印加することにより、測定対象の重金属を選択的に重金属吸着部12に吸着させ、重金属と、鉄やアルミニウム、ナトリウム、カリウム、カルシウム、ケイ素、高分子有機物等のマトリックスとを分離した。次に、溶離液(1M硝酸)18aにより重金属吸着部12に吸着した重金属を溶離させ、溶離液18aに含まれる溶離した重金属を原子吸光装置により測定した。その結果を次の表1にそれぞれ示す。
実施例1と同様の採取した土壌を測定試料とし、公定法(土壌汚染対策法)に基づく溶出試験法を用いて測定試料中に含まれる重金属を測定した。その結果を次の表1にそれぞれ示す。
11 重金属抽出部
12 重金属吸着部
13 溶離部
14 測定部
16 カラム
16a 測定試料
17 第1容器
17a 抽出液
18 第3容器
18a 溶離液
19 第1流路
21 第2流路
22 第3流路
23 第3切換弁
24 第2容器
24a 脱イオン化水
26 導入流路
27 循環流路
28 送出流路
29 第1切換弁
31 第2切換弁
32 第1ポンプ
33 補助流路
34 対極電極
36 参照電極
37 作用電極
38 ポテンショスタット
39 第2ポンプ
Claims (7)
- 一定量の抽出液を循環させることにより重金属を含む測定試料を充填したカラムに前記抽出液を通過させて前記測定試料を洗浄するとともに前記抽出液に重金属を抽出する重金属抽出部と、前記重金属抽出部で重金属を抽出した抽出液から測定対象の重金属を選択的に吸着する重金属吸着部と、溶離液により前記重金属吸着部で吸着した重金属を溶離する溶離部とを備え、
前記重金属抽出部と前記重金属吸着部とが第1流路により相互に接続され、前記溶離部と前記重金属吸着部とが第2流路により相互に接続され、前記重金属吸着部が第3流路により前記溶離液に含まれる溶離した重金属を測定する測定部に接続されることを特徴とする重金属分析装置。 - 前記重金属抽出部が、前記抽出液を貯える第1容器と、脱イオン化水を貯える第2容器と、重金属を含む測定試料を充填可能な前記カラムと、前記カラムに前記抽出液又は前記脱イオン化水を導入するための導入流路と、前記カラムを通過した前記抽出液が循環するための前記導入流路を含む循環流路と、前記第1流路に接続され前記循環した抽出液を前記脱イオン化水とともに送出するための送出流路と、前記第1容器から前記抽出液を前記カラムに導入するように又は前記第2容器から前記脱イオン化水を前記カラムに導入するように切換える第1切換弁と、第1切換位置と第2切換位置を有する第2切換弁と、前記カラムと前記第2切換弁の間の流路に設けられた第1ポンプとを備え、
前記第2切換弁が前記第1切換位置に切換えられたときに、前記第1ポンプが前記導入流路を介して前記抽出液又は前記脱イオン化水を前記カラムに導入しかつ前記抽出液を前記脱イオン化水とともに前記送出流路に送出し、前記第2切換弁が前記第2切換位置に切換られたときに、前記第1ポンプが前記循環流路を介して前記抽出液を循環させるように構成された請求項1記載の重金属分析装置。 - 前記重金属吸着部が、対極電極、参照電極及び高温焼結炭素繊維カラムからなる作用電極を備えた電着セルであり、前記作用電極と前記第1流路で送られてきた前記抽出液との間に測定対象の重金属に応じた電着電位を印加することにより、前記重金属抽出部で抽出された抽出液に含まれる前記測定対象の重金属のみを選択的に前記作用電極に吸着するように構成された請求項1記載の重金属分析装置。
- 前記溶離部が、溶離液を貯える第3容器と、前記溶離液を前記第2流路、前記重金属吸着部及び前記第3流路を経て前記測定部に移送する第2ポンプとを有する請求項1記載の重金属分析装置。
- 前記測定試料が、0.01mm〜0.1mmの粒度を有する、土壌、畜産廃棄物、農産廃棄物、海産廃棄物、焼却灰、食品又は植物を少なくとも1種含む請求項1記載の重金属分析装置。
- 重金属を含む測定試料を充填したカラムに導入流路を介して一定量の抽出液を導入する工程と、
前記導入した抽出液を前記導入流路を含む循環流路を介して前記カラムに一定時間循環させて前記抽出液に重金属を抽出する工程と、
前記カラムを循環する抽出液の循環を停止した後、前記抽出液を脱イオン化水とともに送出流路を介して重金属吸着部に送る工程と、
前記送られてきた抽出液から測定対象の重金属を選択的に前記重金属吸着部に吸着する工程と、
溶離液により前記重金属吸着部に吸着した重金属を溶離する工程と、
前記溶離液に含まれる溶離した重金属を測定する工程と
を含む重金属の分析方法。 - 前記測定試料が、0.01mm〜0.1mmの粒度を有する、土壌、畜産廃棄物、農産廃棄物、海産廃棄物、焼却灰、食品又は植物を少なくとも1種含む請求項6記載の重金属の分析方法。
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