JPH0765965B2 - Chemiluminescent humic acid determination method - Google Patents
Chemiluminescent humic acid determination methodInfo
- Publication number
- JPH0765965B2 JPH0765965B2 JP3243513A JP24351391A JPH0765965B2 JP H0765965 B2 JPH0765965 B2 JP H0765965B2 JP 3243513 A JP3243513 A JP 3243513A JP 24351391 A JP24351391 A JP 24351391A JP H0765965 B2 JPH0765965 B2 JP H0765965B2
- Authority
- JP
- Japan
- Prior art keywords
- humic acid
- intensity
- formaldehyde
- concentration
- determination method
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 239000004021 humic acid Substances 0.000 title claims description 39
- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 title claims description 36
- 238000000034 method Methods 0.000 title claims description 8
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 28
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 16
- 238000004020 luminiscence type Methods 0.000 claims description 8
- 238000011088 calibration curve Methods 0.000 claims description 6
- 238000011002 quantification Methods 0.000 claims description 4
- 238000000295 emission spectrum Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 239000007788 liquid Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000011282 treatment Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 3
- 150000002894 organic compounds Chemical class 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000002572 peristaltic effect Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- RSPISYXLHRIGJD-UHFFFAOYSA-N OOOO Chemical compound OOOO RSPISYXLHRIGJD-UHFFFAOYSA-N 0.000 description 1
- 229930040373 Paraformaldehyde Natural products 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000007859 condensation product Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000008098 formaldehyde solution Substances 0.000 description 1
- QOSATHPSBFQAML-UHFFFAOYSA-N hydrogen peroxide;hydrate Chemical compound O.OO QOSATHPSBFQAML-UHFFFAOYSA-N 0.000 description 1
- 238000001748 luminescence spectrum Methods 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- -1 nitrogen-containing compound Chemical class 0.000 description 1
- 229920002866 paraformaldehyde Polymers 0.000 description 1
- 150000004965 peroxy acids Chemical class 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Description
【０００１】[0001]
【産業上の利用分野】この発明は、水道水等の分析その
他の工業用分析処理等に適用される化学発光を用いたフ
ミン酸定量法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for quantifying humic acid using chemiluminescence which is applied to analysis of tap water and other industrial analytical treatments.
【０００２】[0002]
【従来の技術】一般にフミン酸は土壌または低石炭化度
の石灰質中に存する酸性有機物であって、その化学構造
はよく知られていないものであるが、その主要構造は、
多価フェノール形の芳香族化合物と含窒素化合物との縮
合物であると考えられている。BACKGROUND ART Humic acid is an acidic organic substance generally existing in soil or calcareous matter with low coalification degree, and its chemical structure is not well known, but its main structure is
It is considered to be a condensation product of a polyhydric phenol type aromatic compound and a nitrogen-containing compound.
【０００３】上記フミン酸は上水道の原水にも含まれて
いるが、この原水を塩素で殺菌処理したときに、これが
トリハロメタンに変性する可能性がある。トリハロメタ
ンは、人または動物の機能に重大な危害を与える劇薬で
あり、前記殺菌処理前の原水中の前駆物質たるフミン酸
の濃度を知ることで浄水処理対策を講じる必要がある。The humic acid is also contained in the raw water of the water supply, but when this raw water is sterilized with chlorine, it may be transformed into trihalomethane. Trihalomethane is a powerful drug that seriously impairs human or animal functions, and it is necessary to take measures for water purification treatment by knowing the concentration of humic acid which is a precursor in the raw water before the sterilization treatment.
【０００４】このようなフミン酸の定量法としては、Ｅ
ＤＴＡ錯塩でマスキングし、フミン酸の可視部（４１０
〜４８０ｎｍ）における吸光度を測定する方法が採用さ
れていた。As a method for quantifying such humic acid, E
Masked with DTA complex salt, visible part of humic acid (410
(-480 nm) has been adopted.
【０００５】[0005]
【発明が解決しようとする課題】しかし、上記従来のフ
ミン酸の定量法では、マスキング等の前処理に時間がか
かると共にセル等の操作も煩雑であり、また測定結果を
連続して得ることができないという問題点も有してい
た。However, in the above-mentioned conventional method for quantifying humic acid, pretreatment such as masking takes time, operation of cells and the like is complicated, and measurement results can be obtained continuously. It also had a problem that it could not be done.
【０００６】この発明は、上記従来のフミン酸定量法に
おける問題点を解決し、検体中のフミン酸の測定を高精
度で迅速に行ない得て、上水道浄化処理装置等に付設さ
れる連続分析測定装置等にも適用し得るフミン酸定量法
を提供することを課題としている。The present invention solves the above-mentioned problems in the conventional humic acid determination method, can measure humic acid in a sample with high accuracy and speed, and can perform continuous analytical measurement attached to a water purification treatment device or the like. It is an object to provide a humic acid determination method that can be applied to devices and the like.
【０００７】[0007]
【課題を解決するための手段】上記の課題を解決するた
め、この発明においては、フミン酸含有検体に過酸化水
素およびホルムアルデヒドを添加して化学発光させ、そ
の発光スペクトルのうち所定波長における発光強度を光
電管によって電気信号化して測定し、前記発光強度と別
途測定した前記所定波長における発光強度−フミン酸濃
度検量線とを対比して定量する手段を採用したのであ
る。In order to solve the above problems, in the present invention, hydrogen peroxide and formaldehyde are added to a humic acid-containing sample to cause chemiluminescence, and the luminescence intensity at a predetermined wavelength in the luminescence spectrum thereof. Was measured by converting it into an electric signal by a photoelectric tube, and quantified by comparing the emission intensity and the emission intensity at the predetermined wavelength separately measured with the humic acid concentration calibration curve.
【０００８】[0008]
【作用】この発明に係る化学発光を用いたフミン酸定量
法は、フミン酸を含有する検体中に、過酸化水素および
ホルムアルデヒドを加えて反応させた際、生成した過酸
やヒドロキシペルオキシドによって、特有の化学構造か
らなるフミン酸のみが効率よく化学発光し、その場合の
発光強度は検体中に他の有機化合物が存在した場合のそ
の酸化による発光強度とは比較にならないほど強いとい
う事実を本願の発明者が発見したことに基づいている。
そしてこのように、フミン酸の発光スペクトルが他の有
機化合物の酸化による発光とは明瞭に区別できるので、
他の有機化合物とは区別可能な適当な波長（好ましくは
最大発光波長）におけるフミン酸の発光強度を光電管か
ら電気信号として測定できる。一方、フミン酸濃度既知
の検体に前記過酸化水素およびホルムアルデヒドを同じ
条件で添加し、反応させて前記波長で作成した発光強度
−フミン酸濃度の検量線に前記発光強度を対比すれば、
迅速かつ精密に検体中のフミン酸成分が定量される。The method for quantifying humic acid using chemiluminescence according to the present invention is one in which a sample containing humic acid contains hydrogen peroxide and
Peracid generated when reacting by adding formaldehyde
Or a unique chemical structure depending on hydroxyperoxide
Humic acid consisting of
The luminescence intensity is measured when other organic compounds are present in the sample.
It is said to be so strong that it cannot be compared with the emission intensity due to the oxidation of
This is based on the fact that the inventor of the present application has discovered the fact.
Thus, the emission spectrum of humic acid is
Since it can be clearly distinguished from the luminescence due to the oxidation of organic compounds,
Distinct suitable wavelength and other organic compounds (preferably maximum emission wavelength) Ru can measure the emission intensity of humic acid in the electric signal from the photoelectric tube. On the other hand, if the hydrogen peroxide and formaldehyde were added to a specimen of known humic acid concentration under the same conditions, and the reaction was made by comparing the luminescence intensity to the calibration curve of the luminescence intensity-humic acid concentration prepared at the wavelength,
Quickly and precisely humic acid component in the sample is quantified.
【０００９】[0009]
【実施例】この発明に用いるホルムアルデヒドは、ＨＣ
ＨＯの４０％水溶液である市販のホルマリンを適当な濃
度として用いる他、ホルムアルデヒドの誘導体であるパ
ラホルムアルデヒド、ポリホルムアルデヒド等を選択的
に用いることも可能である。EXAMPLE Formaldehyde used in the present invention is HC
Commercially available formalin, which is a 40% aqueous solution of HO, may be used at an appropriate concentration, or paraformaldehyde, polyformaldehyde or the like, which is a formaldehyde derivative, may be selectively used.
【００１０】また、この発明に用いる過酸化水素を分解
反応し易くするために、適宜、水酸化ナトリウム等のア
ルカリを添加して反応容器内のＰＨを４〜５程度に調整
しておくことが望ましい。In order to facilitate the decomposition reaction of hydrogen peroxide used in the present invention, the pH in the reaction vessel may be adjusted to about 4 to 5 by appropriately adding an alkali such as sodium hydroxide. desirable.
【００１１】また、上記ＰＨ以外の化学発光反応時の条
件として金属触媒を添加すれば、発光強度が増すので、
一層高感度の測定が可能となる。If a metal catalyst is added as a condition for the chemiluminescence reaction other than PH, the luminescence intensity increases.
It is possible to measure with higher sensitivity.
【００１２】この発明における発光強度の測定に使用し
得る波長、すなわち、光電管に入力し得る波長を調べる
ために、以下の実験を行なった。The following experiment was carried out in order to investigate the wavelength that can be used for measuring the emission intensity in the present invention, that is, the wavelength that can be input to the photoelectric tube.
【００１３】すなわち、ホルムアルデヒドおよび過酸化
水素の量と濃度を任意に設定し、ＰＨを調整してこれら
をフミン酸と効率よく反応させ、波長範囲１８５〜８５
０ｎｍに分光感度をもつ光電子増倍管を用いて最大発光
波長６４０ｎｍの光を検出した。That is, the amounts and concentrations of formaldehyde and hydrogen peroxide are arbitrarily set, the pH is adjusted, and these are reacted efficiently with humic acid to obtain a wavelength range of 185 to 85.
Light with a maximum emission wavelength of 640 nm was detected using a photomultiplier tube having a spectral sensitivity of 0 nm.
【００１４】次に、上記実験で調べた最大発光強度の波
長を用いた定量装置の実験例について説明する。Next, an experimental example of the quantification device using the wavelength of the maximum emission intensity investigated in the above experiment will be described.
【００１５】〔実験例〕まず、図１に示す装置を用い
て、発光強度−フミン酸濃度検量線を作製した。すなわ
ち、１０、２０、４０、１００ｐｐｍの濃度でフミン酸
標準濃度液１をペリスタポンプ２を介して毎分２ミリリ
ットルの流量で混合管３に供給し、一方、３％の過酸化
水素水４を毎分２ミリリットルの流量で攪拌容器５に導
入し、この攪拌容器５には、さらに市販のホルムアルデ
ヒドの５％水溶液６を毎分２ミリリットル、また１モル
濃度の水酸化ナトリウム水溶液７を毎分２ミリリットル
の流量でペリスタポンプ２から攪拌容器５に導入し、攪
拌後の混液をさらに混合管３に供給して前記フミン酸標
準濃度液１と混合し、反応容器８に供給した。この反応
容器８内での反応条件は、常温、常圧とした。Experimental Example First, an emission intensity-humic acid concentration calibration curve was prepared using the apparatus shown in FIG. That is, the humic acid standard concentration liquid 1 having a concentration of 10, 20, 40, and 100 ppm was supplied to the mixing pipe 3 at a flow rate of 2 ml / min through the peristaltic pump 2, while the 3% hydrogen peroxide solution 4 was supplied every time. The mixture was introduced into the stirring container 5 at a flow rate of 2 ml / min, and in this stirring container 5, 2 ml / min of a commercially available 5% aqueous solution of formaldehyde 6 and 2 ml / min of a 1 molar sodium hydroxide aqueous solution 7 were further introduced. Was introduced into the stirring container 5 from the peristaltic pump 2 at a flow rate of 1, and the mixed liquid after stirring was further supplied to the mixing tube 3 to be mixed with the humic acid standard concentration liquid 1 and supplied to the reaction container 8. The reaction conditions in the reaction vessel 8 were room temperature and atmospheric pressure.
【００１６】上記反応容器８は、分光フィルタ付き光電
子増倍管９に連結させて、発生した化学発光の最大発光
波長６４０ｎｍにおける強度を電気信号量として検出
し、増幅器１０を介して発光強度（相対値）を記録計１
１に入力した。得られた各フミン酸濃度における発光強
度を両対数グラフにプロットして、直線関係の検量線
（図２参照）を得た。The reaction vessel 8 is connected to a photomultiplier tube 9 with a spectral filter to detect the intensity of the generated chemiluminescence at the maximum emission wavelength of 640 nm as an electric signal quantity, and the emission intensity (relative to the relative intensity via an amplifier 10). Value) Recorder 1
Entered in 1. The emission intensity at each obtained humic acid concentration was plotted on a logarithmic log graph to obtain a linear calibration curve (see FIG. 2).
【００１７】つぎに、濃度未知のフミン酸含有検体Ａの
濃度は、以下のようにして求めた。Next, the concentration of the humic acid-containing specimen A of unknown concentration was determined as follows.
【００１８】すなわち、フミン酸標準濃度液１に代え
て、フミン酸含有検体Ａを混合管３内に導入し、過酸化
水素水４、ホルムアルデヒド水溶液６、水酸化ナトリウ
ム水溶液７を上記と全く同様にして混合管３に供給し、
発光強度を前記記録された検出線に対比して検体Ａのフ
ミン酸濃度を求めた。反応容器８内の廃液は、真空ポン
プ１２によって廃液溜め１３内に収容した。That is, instead of the humic acid standard concentration liquid 1, the humic acid-containing specimen A is introduced into the mixing tube 3, and the hydrogen peroxide solution 4, the formaldehyde solution 6, and the sodium hydroxide solution 7 are treated in exactly the same manner as above. Supply to the mixing tube 3,
The luminescence intensity was compared with the recorded detection line to determine the humic acid concentration of the sample A. The waste liquid in the reaction container 8 was stored in the waste liquid reservoir 13 by the vacuum pump 12.
【００１９】上記実験例のフミン酸濃度検出限界は１０
ｐｐｂであり、１ｐｐｍにおける５回測定の標準偏差は
２．３％であった。The detection limit of humic acid concentration in the above experimental example is 10
ppb, standard deviation of 5 measurements at 1 ppm was 2.3%.
【００２０】なお、反応容器８内の形状変更とコーティ
ングおよび反応セルの設置などを応用すれば、上記した
以上の測定感度と信頼性を得ることも可能である。If the shape of the reaction container 8 is changed, the coating and the reaction cell are installed, the above-described measurement sensitivity and reliability can be obtained.
【００２１】[0021]
【効果】この発明は、以上説明したように、フミン酸と
過酸化水素およびホルムアルデヒドとの極めて鋭敏な反
応によって発生する化学発光の強度を測定することで、
検体中のフミン酸の存在を直接に検出する定量法である
から、高精度で、しかも迅速に連続してフミン酸の定量
を行なうことができる。[Effect] The present invention, as described above, measures the intensity of chemiluminescence generated by the extremely sensitive reaction of humic acid with hydrogen peroxide and formaldehyde,
Since this is a quantitative method that directly detects the presence of humic acid in a sample, it is possible to perform quantification of humic acid with high accuracy and in rapid succession.
【００２２】したがって、上水道の塩素添加量を制御す
る正確なデータを迅速に得るために、この方法を適用す
ることができ、この発明の産業上の利用価値は極めて高
いものであるということができる。Therefore, this method can be applied to quickly obtain accurate data for controlling the amount of chlorine added to waterworks, and it can be said that the industrial utility value of the present invention is extremely high. .
【図面の簡単な説明】[Brief description of drawings]
【図１】模式化して示す実験例の定量装置図FIG. 1 is a schematic diagram of a quantification device of an experimental example.
【図２】発光強度−フミン酸濃度両対数検量線図FIG. 2 Luminous intensity-humic acid concentration bilogarithmic calibration curve diagram
Ａ フミン酸含有検体 ４ 過酸化水素水 ６ ホルムアルデヒド水溶液 A Humic acid-containing sample 4 Hydrogen peroxide water 6 Formaldehyde aqueous solution
Claims (1)
ルムアルデヒドを添加して化学発光させ、その発光スペ
クトルのうち所定波長における発光強度を光電管によっ
て電気信号化して測定し、前記発光強度と別途測定した
前記所定波長における発光強度−フミン酸濃度検量線と
を対比して定量する化学発光を用いたフミン酸定量法。1. Hydrogen peroxide and formaldehyde are added to a humic acid-containing sample to cause chemiluminescence, and the emission intensity at a predetermined wavelength in the emission spectrum is measured by converting it into an electric signal by a photoelectric tube, and the emission intensity is separately measured. A humic acid quantification method using chemiluminescence in which the luminescence intensity at the predetermined wavelength and a humic acid concentration calibration curve are compared and quantified.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3243513A JPH0765965B2 (en) | 1991-09-24 | 1991-09-24 | Chemiluminescent humic acid determination method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3243513A JPH0765965B2 (en) | 1991-09-24 | 1991-09-24 | Chemiluminescent humic acid determination method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0579988A JPH0579988A (en) | 1993-03-30 |
| JPH0765965B2 true JPH0765965B2 (en) | 1995-07-19 |
Family
ID=17105027
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3243513A Expired - Fee Related JPH0765965B2 (en) | 1991-09-24 | 1991-09-24 | Chemiluminescent humic acid determination method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0765965B2 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| MD4221C1 (en) * | 2012-01-10 | 2013-11-30 | Институт Химии Академии Наук Молдовы | Method for quantitative determination of humic substances in natural waters |
| JP5920712B2 (en) * | 2012-04-13 | 2016-05-18 | 国立研究開発法人農業・食品産業技術総合研究機構 | Simple estimation method of phenylpropanoid polymer content |
| MD4305C1 (en) * | 2013-04-02 | 2015-04-30 | Институт Химии Академии Наук Молдовы | Process for determining water-soluble humic substances in natural waters and solid rocks |
| JP7420333B2 (en) * | 2020-08-19 | 2024-01-23 | 株式会社日吉 | Sensitizer for ammonium ion chemiluminescence measurement, ammonium ion analysis method, and ammonium ion analysis device |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03225262A (en) * | 1990-01-30 | 1991-10-04 | Meidensha Corp | Method and instrument for measuring consumption of oxidizing agent |
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1991
- 1991-09-24 JP JP3243513A patent/JPH0765965B2/en not_active Expired - Fee Related
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| Publication number | Publication date |
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| JPH0579988A (en) | 1993-03-30 |
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