JP2815217B2 - Humic acid reagent and water analysis method - Google Patents
Humic acid reagent and water analysis methodInfo
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- JP2815217B2 JP2815217B2 JP8576390A JP8576390A JP2815217B2 JP 2815217 B2 JP2815217 B2 JP 2815217B2 JP 8576390 A JP8576390 A JP 8576390A JP 8576390 A JP8576390 A JP 8576390A JP 2815217 B2 JP2815217 B2 JP 2815217B2
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- humic acid
- water
- acid reagent
- reagent
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Description
【発明の詳細な説明】 （イ）産業上の利用分野 この発明はフミン酸試薬及び水分析法に関する。さら
に詳しくは、河川、浄水等に含有されるフミン成分分析
用のフミン酸試薬及び水分析法に関する。The present invention relates to a humic acid reagent and a water analysis method. More specifically, the present invention relates to a humic acid reagent for analyzing humic components contained in rivers, purified water, and the like, and a water analysis method.
（ロ）従来の技術及び発明が解決しようとする課題 河川水等を浄水として使用するに当たって種々の処理
が行われている。(B) Problems to be Solved by Conventional Techniques and Inventions Various processes are performed in using river water or the like as purified water.
最近では浄水の高度処理について盛んに研究されてき
ている。浄水の高度処理とは、通常の浄水方法では十分
に対応できない処理を目的として導入される活性炭処
理、オゾン処理、生物処理等をいい、このうちオゾン処
理、活性炭処理などは実用化段階に入ろうとしている。Recently, the advanced treatment of purified water has been actively studied. Advanced treatment of purified water refers to activated carbon treatment, ozone treatment, biological treatment, etc., which are introduced for the purpose of not being able to adequately cope with ordinary water purification methods. I have.
上記いずれの高度処理においても除去対象となる物質
は、発癌性の疑惑のあるトリハロメタン形成の主たる前
駆物質であるフミン酸成分である。従って浄水処理及び
その高度処理においては、処理対象の水系（河川水、水
道原水、浄水等）におけるフミン酸成分の含有状況を把
握することが必要である。The substance to be removed in any of the above-mentioned advanced treatments is a humic acid component which is a main precursor of trihalomethane formation which is suspected to be carcinogenic. Therefore, in the water purification treatment and its advanced treatment, it is necessary to grasp the content of the humic acid component in the water system to be treated (river water, tap water, purified water, etc.).
ところでフミン酸は化学構造が不明で、性状・組成が
相違する種々の分子量のものからなる水不溶性高分子物
質としてとらえられており、フミン酸成分と一口にいっ
てもその分子量分布には幅があり特定できない。By the way, the chemical structure of humic acid is unknown, and it is regarded as a water-insoluble polymer composed of various molecular weights with different properties and compositions. Not specified.
この点から、市販されているフミン酸試薬は必ずしも
河川水に含有されるフミン酸成分と一致したものとは言
えない。このため、市販のフミン酸試薬を0.1N−水酸化
ナトリウム溶液で加熱溶解し、塩酸等で中和後倍量に希
釈し、固形物を遠心分離後0.2μフィルタで除去し、濾
液を水道水で100倍に希釈して調製されたものが、処理
対象の水系のフミン酸成分の参照試薬（試験液）として
使用されている。From this point, commercially available humic acid reagents do not always correspond to humic acid components contained in river water. For this purpose, a commercially available humic acid reagent is dissolved by heating with a 0.1 N sodium hydroxide solution, neutralized with hydrochloric acid or the like, diluted to twice the volume, solid substances are removed by centrifugation, and the filtrate is removed with a 0.2 μ filter. The solution prepared by diluting it 100-fold is used as a reference reagent (test solution) for the aqueous humic acid component to be treated.
しかしながら、上記試験液を高速液体クロマトグラフ
ィ（HPLC）に付して得られたクロマトグラムと河川水や
水道原水を同じくHPLCに付して得られたクロマトグラム
とでは、検出されるフミン酸成分に相違が見られ、この
点から上記従来の試験液はその河川水や水道原水の参照
とはならないことが示されている。However, the chromatogram obtained by subjecting the above test solution to high performance liquid chromatography (HPLC) and the chromatogram obtained by subjecting river water and tap water to HPLC also differ in the detected humic acid components. From this point, it is shown that the above-mentioned conventional test liquid cannot be used as a reference for the river water or tap water.
このように、河川水に含まれるフミン酸成分を評価し
うる有効な参照試験（試験液）が無いため、高度処理プ
ロセスにしても除去剤にしても、フミン酸成分の除去効
果を実験室的に把握することが困難であった。As described above, there is no effective reference test (test solution) that can evaluate the humic acid component contained in river water. It was difficult to grasp.
この発明はかかる状況に鑑み為されたものであり、河
川水、水道原水及び浄水等水処理対象の水系の参照とな
りうるフミン酸試薬及び簡便な水分析法を提供しようと
するものである。The present invention has been made in view of such a situation, and an object of the present invention is to provide a humic acid reagent which can be a reference for a water system to be treated, such as river water, raw tap water, and purified water, and a simple water analysis method.
（ハ）課題を解決するための手段及び作用 かくしてこの発明によれば、ポリエチレングリコール
を標準物質としたゲルパーミエーションクロマトグラフ
ィによる分子量分布におけるピーク分子量が、約2000で
あるフミン酸成分を含有するフミン酸試薬、及び、上記
フミン酸試薬を標準液として、水中のフミン酸を定量す
ることからなる水分析法が提供される。(C) Means and Action for Solving the Problems According to the present invention, a humic acid containing a humic acid component having a peak molecular weight of about 2000 in a molecular weight distribution by gel permeation chromatography using polyethylene glycol as a standard substance A water analysis method comprising quantifying humic acid in water using a reagent and the humic acid reagent as a standard solution is provided.
この発明のフミン酸試薬は、ポリエチレングリコール
を標準物質としてゲルパーミエーションクロマトグラフ
ィによる分子量分布において、ピーク分子量が約2000で
あるフミン酸成分を含有して構成される。該フミン酸成
分としては、同クロマトグラフィにおいてピーク分子量
が約2000でかつ分子量分布が1900〜4800のものがさらに
好ましい。この発明のフミン酸試薬は例えば市販のフミ
ン酸試薬を用いて調製することができる。この市販のフ
ミン酸試薬としては例えばKPM 3762（和光純薬工業株式
会社製）、HO 161（東京化成（株）製）の名称で入手可
能である。The humic acid reagent of the present invention comprises a humic acid component having a peak molecular weight of about 2,000 in a molecular weight distribution by gel permeation chromatography using polyethylene glycol as a standard substance. More preferably, the humic acid component has a peak molecular weight of about 2,000 and a molecular weight distribution of 1900 to 4800 in the same chromatography. The humic acid reagent of the present invention can be prepared, for example, using a commercially available humic acid reagent. This commercially available humic acid reagent is available, for example, under the names of KPM 3762 (manufactured by Wako Pure Chemical Industries, Ltd.) and HO 161 (manufactured by Tokyo Chemical Industry Co., Ltd.).
上記市販のフミン酸試薬を用いる場合、まずこのフミ
ン酸試薬をアルカリ性下で加熱して溶解し、次いで高分
子量のフミン酸成分を除去することにより調製できる。When the commercially available humic acid reagent is used, the humic acid reagent can be prepared by first heating and dissolving the humic acid reagent under alkaline conditions, and then removing the high molecular weight humic acid component.
この発明において、上記高分子量のフミン酸成分の除
去には、硫酸アルミニウムが用いられる。すなわちフミ
ン酸試薬のアルカリ溶解液またはこの希釈液に硫酸アル
ミニウムを加えて中和し、このとき生成する凝集沈殿を
濾別することにより、高分子量のフミン酸成分が除去さ
れる。In the present invention, aluminum sulfate is used to remove the high molecular weight humic acid component. That is, aluminum sulfate is added to the alkali solution or diluted solution of the humic acid reagent to neutralize the solution, and the resulting aggregated precipitate is filtered off to remove the high molecular weight humic acid component.
上記高分子量のフミン酸成分が除去された濾液は、さ
らに定量濾紙（No.5c）及び0.2μフィルタで濾過される
ことが好ましい。The filtrate from which the high molecular weight humic acid component has been removed is preferably further filtered through a quantitative filter paper (No. 5c) and a 0.2 μ filter.
上記の手法により得られるこの発明のフミン酸成分
は、前述のゲルパーミエーションクロマトグラフィにお
いて約2000をピークトップとするシャープな分布を示す
ものとなる。The humic acid component of the present invention obtained by the above method has a sharp distribution having a peak top of about 2000 in the aforementioned gel permeation chromatography.
上記のごとくして得られるこの発明のフミン酸試薬
は、該試薬中に含有されるフミン酸成分が、分子量分布
及び全有機炭素量の点で、河川水や水道原水等の水系に
おけるフミン酸成分とほぼ類似するフミン酸成分を含有
するものとして得られることとなる。The humic acid reagent of the present invention obtained as described above is characterized in that the humic acid component contained in the reagent has a molecular weight distribution and total organic carbon content in terms of humic acid component in an aqueous system such as river water or tap water. And a humic acid component substantially similar to the above.
この発明において、上記調製されるフミン酸試薬は、
このまま或はこれを濃縮・希釈することにより、浄水処
理対象の水系の参照とすることができる。In the present invention, the humic acid reagent prepared above is
As it is or by concentrating and diluting it, it can be used as a reference for the water system to be purified.
この発明において、上記のごとく得られるこの発明の
フミン酸試薬の例えば高速液体クロマトグラムにおける
特定吸収に基づいて、浄水処理対象の水系の液体クロマ
トグラムを比較検討することにより、該水系中に含有さ
れるフミン酸成分についての定性・定量分析を行うこと
ができる。In the present invention, the humic acid reagent of the present invention obtained as described above is contained in the water system by comparing and examining the liquid chromatograms of the water system to be treated for water purification based on the specific absorption in, for example, a high performance liquid chromatogram. Qualitative and quantitative analysis of the humic acid component.
従ってこの発明は浄水処理の評価や浄水処理に用いる
活性炭の選択や評価に好適な方法を提供できることとな
る。Therefore, the present invention can provide a method suitable for evaluating water purification treatment and selecting and evaluating activated carbon used for water purification treatment.
以下実施例によりこの発明を詳細に説明するが、これ
によりこの発明は限定されるものではない。Hereinafter, the present invention will be described in detail with reference to examples, but the present invention is not limited thereto.
（ニ）実施例 実施例 ・フミン酸試薬の調製 和光純薬（株）製の試薬フミン酸（ロットNo.KPM 376
2）55gに、0.1N−NaOH 3を加え、沸騰水浴中（100
℃）で４時間加熱溶解させた。(D) Example Example-Preparation of humic acid reagent A reagent humic acid manufactured by Wako Pure Chemical Industries, Ltd. (Lot No. KPM 376)
2) To 55 g, add 0.1N-NaOH 3 and place in a boiling water bath (100
C.) for 4 hours.
次いで蒸留水を加えて10倍に希釈した後、硫酸アルミ
ニウム〔Al2（SO4）３〕溶液及び1N−NaOHを加えて１時
間撹拌した。ここで硫酸アルミニウムは、全液量に対し
てアルミニウム金属換算で130ppm.の濃度になるまで加
え、一方1N−NaOHは液のpHが7.0に維持されるよう適宜
加えた。Next, distilled water was added to dilute the solution by 10 times, and then an aluminum sulfate [Al 2 (SO 4 ) 3 ] solution and 1N-NaOH were added, followed by stirring for 1 hour. Here, aluminum sulfate was added until the concentration became 130 ppm. In terms of aluminum metal with respect to the total amount of the solution, while 1N-NaOH was appropriately added so that the pH of the solution was maintained at 7.0.
撹拌終了後、約10時間静置後、上澄液を分別し、さら
に、0.1μｍ−メンブランフィルタを用いて減圧濾過し
た。得られた濾液をフミン酸試薬とした。After completion of the stirring, the mixture was allowed to stand for about 10 hours, and then the supernatant was separated, followed by filtration under reduced pressure using a 0.1 μm-membrane filter. The obtained filtrate was used as a humic acid reagent.
・ゲルクロマトグラフによるフミン酸成分の分子量（P.
E.G.ベース）の特定 まず、上記調製されたフミン酸試薬を下記条件で高速
液体クロマトグラフィ（HPLC）に付して、このもののク
ロマトグラム（第１図）を得た。-Molecular weight of humic acid component by gel chromatography (P.
First, the prepared humic acid reagent was subjected to high performance liquid chromatography (HPLC) under the following conditions to obtain a chromatogram (FIG. 1) of the humic acid reagent.
次いで、分子量の異なるポリエチレングリコール（P.
E.G.）を用いて同様の条件下HPLCで測定し、検量線（保
持時間vs分子量）を作成した（第２図）。そしてこの検
量線に基づいて上記調製したフミン酸試薬中のフミン酸
成分の分子量を特定した。Next, polyethylene glycols having different molecular weights (P.
Using EG), the measurement was performed by HPLC under the same conditions, and a calibration curve (retention time vs. molecular weight) was prepared (FIG. 2). Then, based on this calibration curve, the molecular weight of the humic acid component in the humic acid reagent prepared above was specified.
分析装置 :shimadzu LC−3A カラム :Asahipak GS−320;7.6mmφ×500mmL 溶離液 :0.1M−Phosphate Buffer（pH12）（KH2PO4
−K3PO4） 流量:1.0ml/min 試料注入量:100μ 測定波長 :260nm 検出器 :shimadzu SPD−2A なお、上記検量線作成には下記試水Ａ〜Ｅを用いた。Analyzer: shimadzu LC-3A Column: Asahipak GS-320; 7.6mmφ × 500mmL Eluent: 0.1M-Phosphate Buffer (pH12) (KH 2 PO 4
−K 3 PO 4 ) Flow rate: 1.0 ml / min Sample injection amount: 100 μ Measurement wavelength: 260 nm Detector: shimadzu SPD-2A The following samples A to E were used for preparing the above calibration curves.
試水Ａ…関東地区で採取した河川水に、アルミニウム金
属（Al）換算5ppm.の硫酸アルミニウムを加えて上記と
同様の凝沈処理した濾液を4.5倍に濃縮したもの（室温
下）。このクロマトグラムを第３図に示す。Sample A: River water collected in the Kanto area was added with 5 ppm of aluminum sulfate in terms of aluminum metal (Al), and the same coagulation-treated filtrate was concentrated 4.5 times (at room temperature). The chromatogram is shown in FIG.
試水Ｂ…北海道で採取した泥炭地水に、Al換算8ppm.の
硫酸アルミニウムを加えて同様に凝沈処理した濾液。こ
のクロマトグラムを第４図に示す。Sample B: A filtrate obtained by adding 8 ppm of aluminum sulfate in terms of Al to peat ground water collected in Hokkaido and coagulating in the same manner. The chromatogram is shown in FIG.
試水Ｃ…大阪府の某浄水場から採取した水道原水を40℃
の温度で４倍の濃度に減圧濃縮した濾液。このクロマト
グラムを第５図に示す。Sample C: Raw water from a certain water purification plant in Osaka Prefecture at 40 ° C
The filtrate was concentrated under reduced pressure to a concentration four times as high as that of the filtrate. The chromatogram is shown in FIG.
試水Ｄ……工場排水を18日間空曝気し、Al換算130ppm.
の硫酸アルミニウムを加えて凝沈処理した濾液。このク
ロマトグラムを第６図に示す。Test water D: Air aeration of factory wastewater for 18 days, converted to 130 ppm Al.
A filtrate obtained by coagulation treatment by adding aluminum sulfate. The chromatogram is shown in FIG.
試水Ｅ…別の工場排水を18日間空曝気し、Al換算30ppm.
を加えて凝沈処理した濾液。このクロマトグラムを第７
図に示す。Test water E: Another factory wastewater was aerated for 18 days and converted to Al at 30 ppm.
The filtrate obtained by adding and coagulating is added. This chromatogram is
Shown in the figure.
また、比較のために、下記従来法により調製したフミ
ン酸試薬について上記と同様の条件下でHPLCに付し、第
８図に示すグロマトグラムを得た。For comparison, the humic acid reagent prepared by the following conventional method was subjected to HPLC under the same conditions as described above to obtain a chromatogram shown in FIG.
（従来法による調製）……試薬フミン酸（ロットNo.KPM
3762;和光純薬（株）製）を0.1N−NaOHで加熱溶解（0.
8g/50ml）。HClで中和後倍量に希釈。固形物を遠心分離
及び0.2μフィルタで除去。濾液を水道水で100倍に希釈
して調製。(Preparation by conventional method) …… Reagent Humic acid (Lot No.KPM
3762; manufactured by Wako Pure Chemical Industries, Ltd.) with 0.1N-NaOH under heating (0.
8g / 50ml). Dilute to twice the volume after neutralization with HCl. Solids are removed by centrifugation and 0.2μ filter. Prepared by diluting the filtrate 100 times with tap water.
また、上記この発明のフミン酸試薬と上記試水Ｃとの
全有機炭素量（TOC）についてTOC計（TOC−10A型 島津
製作所製）を用いて測定したところ、TOC値はそれぞれ
順に8.2ppm.と2.9ppm.であった。Further, the total organic carbon content (TOC) of the humic acid reagent of the present invention and the sample C was measured using a TOC meter (TOC-10A, manufactured by Shimadzu Corporation). And 2.9 ppm.
・結果 第１図で得られる保持時間と第２図の検量線とに基づ
いて、この発明のフミン酸試薬（第２図中にΔで表示）
は、約2000にピークトップを有するシャープな分子量分
布を有するものとなっていることが分かる。-Results Based on the retention time obtained in FIG. 1 and the calibration curve in FIG. 2, the humic acid reagent of the present invention (indicated by Δ in FIG. 2)
Has a sharp molecular weight distribution with a peak top at about 2000.
一方、従来のフミン酸試薬は、第８図及び第２図の結
果から、約4000の辺りを中心にブロードに広がる分子量
分布（具体的には約2000〜約12000）を有するものとな
っていることが分かる。On the other hand, the conventional humic acid reagent has a molecular weight distribution (specifically, about 2000 to about 12000) which broadly spreads around about 4000 from the results of FIGS. 8 and 2. You can see that.
第１図の保持時間と第５図の保持時間とをそれぞれ第
２図の検量線に照らして考察すると、この発明のフミン
酸試薬及び試水Ｃそれぞれに含有されるフミン酸成分の
分子の大きさ及び含有される全有機炭素量において極め
て類似していることが分かる。Considering the retention time in FIG. 1 and the retention time in FIG. 5 with reference to the calibration curve in FIG. 2, respectively, the size of the molecule of the humic acid component contained in each of the humic acid reagent of the present invention and the sample C is shown. It can be seen that they are very similar in terms of the amount and the total amount of organic carbon contained.
以上の結果から、この発明のフミン酸試薬は河川水等
の参照試薬とすることができる。From the above results, the humic acid reagent of the present invention can be used as a reference reagent for river water or the like.
実施例２ 東京化成（株）製の試薬フミン酸HO 161（ニトロフミ
ン酸からなる）を使用して、実施例１と同様にしてフミ
ン酸試薬を調製し、このものを実施例１と同様の分析条
件でHPLCに付し、第９図に示すクロマトグラムを得た。Example 2 A humic acid reagent was prepared in the same manner as in Example 1 using a reagent humic acid HO 161 (consisting of nitrohumic acid) manufactured by Tokyo Chemical Industry Co., Ltd., and was analyzed in the same manner as in Example 1. HPLC was carried out under the conditions to obtain a chromatogram shown in FIG.
これに対し比較例として、同社の試薬フミン酸を上記
従来法に準じて調製し、これについても同様にクロマト
グラム（第10図）を測定した。On the other hand, as a comparative example, the reagent Humic acid of the company was prepared according to the above-mentioned conventional method, and the chromatogram (FIG. 10) was measured in the same manner.
第９図と第10図との比較から、ニトロフミン酸からな
る試薬フミン酸から調製されるフミン酸試薬について
も、上記実施例１と同様に河川水等の参照とすることが
できる。From the comparison between FIG. 9 and FIG. 10, the humic acid reagent prepared from humic acid, which is a reagent composed of nitrohumic acid, can be used as a reference for river water and the like in the same manner as in Example 1.
（ホ）発明の効果 この発明によれば、河川水や水道原水等浄水処理対象
の水系の参照となりうるフミン酸試薬を提供することが
できる。またこのフミン酸試薬により簡便に浄水処理を
評価する方法を提供することができる。(E) Effects of the Invention According to the present invention, it is possible to provide a humic acid reagent that can be used as a reference for a water system to be subjected to water purification treatment such as river water or tap water. Further, it is possible to provide a method for easily evaluating the water purification treatment using the humic acid reagent.
第１図はこの発明のフミン酸試薬の一例のクロマトグラ
ム図、第２図はフミン酸の分子量を特定するための検量
線図、第３〜７図はそれぞれこの発明のフミン酸試薬及
び試水Ａ〜Ｅのクロマトグラム図、第８図は従来のフミ
ン酸試薬のクロマトグラム図、第９図はこの発明のフミ
ン酸試薬の他の例のクロマトグラム図、第10図は従来の
他のフミン酸試薬のクロマトグラム図である。FIG. 1 is a chromatogram of an example of the humic acid reagent of the present invention, FIG. 2 is a calibration curve for specifying the molecular weight of humic acid, and FIGS. FIG. 8 is a chromatogram of a conventional humic acid reagent, FIG. 9 is a chromatogram of another example of the humic acid reagent of the present invention, and FIG. 10 is another conventional humic acid reagent. It is a chromatogram figure of an acid reagent.
───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.6，ＤＢ名) G01N 31/00 G01N 33/18──────────────────────────────────────────────────続 き Continued on front page (58) Field surveyed (Int.Cl. 6 , DB name) G01N 31/00 G01N 33/18
Claims (2)
ゲルパーミエーションクロマトグラフィによる分子量分
布におけるピーク分子量が、約2000であるフミン酸成分
を含有するフミン酸試薬。1. A humic acid reagent containing a humic acid component having a peak molecular weight of about 2,000 in a molecular weight distribution by gel permeation chromatography using polyethylene glycol as a standard substance.
て、水中のフミン酸を定性又は定量することからなる水
分析法。2. A water analysis method comprising qualitatively or quantitatively determining humic acid in water using the humic acid reagent according to claim 1 as a standard solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8576390A JP2815217B2 (en) | 1990-03-30 | 1990-03-30 | Humic acid reagent and water analysis method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8576390A JP2815217B2 (en) | 1990-03-30 | 1990-03-30 | Humic acid reagent and water analysis method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03282366A JPH03282366A (en) | 1991-12-12 |
| JP2815217B2 true JP2815217B2 (en) | 1998-10-27 |
Family
ID=13867909
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP8576390A Expired - Lifetime JP2815217B2 (en) | 1990-03-30 | 1990-03-30 | Humic acid reagent and water analysis method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2815217B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5463243B2 (en) * | 2010-08-30 | 2014-04-09 | 株式会社日立製作所 | Aluminum automatic measuring device |
-
1990
- 1990-03-30 JP JP8576390A patent/JP2815217B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH03282366A (en) | 1991-12-12 |
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