JP2008256636A - Methods of quantitatively determining nitrate nitrogens, anions, and nitrogens in three states - Google Patents

Methods of quantitatively determining nitrate nitrogens, anions, and nitrogens in three states Download PDF

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JP2008256636A
JP2008256636A JP2007101398A JP2007101398A JP2008256636A JP 2008256636 A JP2008256636 A JP 2008256636A JP 2007101398 A JP2007101398 A JP 2007101398A JP 2007101398 A JP2007101398 A JP 2007101398A JP 2008256636 A JP2008256636 A JP 2008256636A
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Naoko Hosono
奈穂子 細野
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Meidensha Corp
Meidensha Electric Manufacturing Co Ltd
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Abstract

<P>PROBLEM TO BE SOLVED: To simultaneously comprehend the processing behavior of ammonia nitrogen and decomposition behavior of organic materials in a sample without influence by oxalic acid in the sample. <P>SOLUTION: In this quantitative determination method of nitrate nitrogen, nitrate ion in a sample is quantitatively determined by an anion chromatography using a carbonic acid-based eluent as the eluent. Alternatively, nitrite and nitrate ions in the sample are quantitatively determined by the anion chromatography using the carbonic acid based eluent as the eluent. By the anion determination method of this invention, oxalate, nitrite, and nitrate ions in the sample are quantitatively determined by the anion chromatography using the carbonic acid-based eluent as the eluent. By this quantitative determination method of nitrogen in three states, first oxalate, nitrite, and nitrate ions in the sample are quantitatively determined by the anion chromatography using the carbonic acid-based eluent as the eluent, then ammonium ions in the sample are quantitatively determined by the cation chromatography. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

本発明は下水処理水中の硝酸態窒素、陰イオン及び三態窒素の定量方法に関する。   The present invention relates to a method for quantifying nitrate nitrogen, anions and trinitrogen in sewage treated water.

下水処理の大きな役割の一つとして下水中のアンモニア態窒素の除去がある。下水に混入しているし尿やその他の有機物から由来するアンモニア態窒素は下水処理工程における生物的処理過程で亜硝酸態窒素または硝酸態窒素を経て窒素ガスとして大気中に放出される。このため、下水処理工程の評価にはアンモニア態窒素、亜硝酸態窒素、硝酸態窒素の存在比を知ることが重要である。硝酸態窒素の分析方法としては、非特許文献１に例示されているように、ブルシン法、還元蒸留法、銅・カドミウム還元−ナフタレンエチレンジアミン吸光光度法、イオンクロマト法がある。特に、前記イオンクロマト法によれば亜硝酸態窒素と硝酸態窒素を同時に分析することができる。
日本下水道協会編，「下水試験方法」，１９９７ One of the major roles of sewage treatment is removal of ammonia nitrogen from sewage. Ammonia nitrogen derived from urine and other organic substances mixed in sewage is released into the atmosphere as nitrogen gas through nitrite nitrogen or nitrate nitrogen in the biological treatment process in the sewage treatment process. For this reason, it is important to know the abundance ratio of ammonia nitrogen, nitrite nitrogen, and nitrate nitrogen for the evaluation of the sewage treatment process. Examples of nitrate nitrogen analysis methods include brucine method, reductive distillation method, copper / cadmium reduction-naphthalene ethylenediamine absorptiometry, and ion chromatography method, as exemplified in Non-Patent Document 1. In particular, according to the ion chromatography method, nitrite nitrogen and nitrate nitrogen can be analyzed simultaneously.
Japan Sewerage Association, “Sewage test method”, 1997

ブルシン法、還元蒸留法、及び銅・カドミウム還元−ナフタレンエチレンジアミン吸光光度法はいずれも吸光光度法を行うものであるので発色を得るための前処理工程が非常に煩雑となる。特に、還元蒸留法はイオン電極法にも適用できるがその前処理工程が煩雑であることに変わりはないので分析に時間がかかることに加え分析誤差が生じやすい。   Since the brucine method, the reductive distillation method, and the copper / cadmium reduction-naphthalene ethylenediamine absorptiometry method all perform absorptiometry, the pretreatment process for obtaining a color is very complicated. In particular, the reductive distillation method can be applied to the ion electrode method, but the pretreatment process is still complicated, so that analysis takes time and analysis errors are likely to occur.

一方、イオンクロマト法は硝酸態窒素を亜硝酸態窒素やその他の成分と分析装置のカラムで分離するため煩雑な前処理工程を有しておらず簡便あると共に分析精度が高い。   On the other hand, the ion chromatographic method separates nitrate nitrogen from nitrite nitrogen and other components from the column of the analyzer, and thus does not have a complicated pretreatment step and is simple and has high analysis accuracy.

硝酸態窒素は下水中で硝酸イオンとして存在し、亜硝酸態窒素は亜硝酸イオンとして存在するので、これらのイオンの測定にイオンクロマト法が利用される場合、陰イオン交換クロマトグラフが適用されている。   Nitrate nitrogen exists as nitrate ions in sewage, and nitrite nitrogen exists as nitrite ions. When ion chromatography is used to measure these ions, anion exchange chromatography is applied. Yes.

亜硝酸イオン及び硝酸イオンを定量するには溶離液としてフタル酸の水溶液を使用する陰イオン交換クロマトグラフ法があるが、この方法では、下水処理の有機物の分解によって生成する低分子量有機物の一種であるシュウ酸が硝酸イオンの溶出位置と完全に重複する。このため、硝酸イオンの正確な濃度の定量ができなくなり、下水処理工程のアンモニア態窒素の処理挙動を評価することができない。   There is an anion exchange chromatography method using an aqueous solution of phthalic acid as an eluent to quantify nitrite and nitrate ions, but this method is a kind of low molecular weight organic matter produced by decomposition of organic matter in sewage treatment. Some oxalic acid completely overlaps with the nitrate ion elution position. For this reason, the exact concentration of nitrate ions cannot be quantified, and the treatment behavior of ammonia nitrogen in the sewage treatment process cannot be evaluated.

また、シュウ酸は下水中の有機物の分解挙動の指標の一つであるが、一般の陰イオンクロマトグラフでは硝酸イオンと亜硝酸イオンの同時分析をすることができない。   In addition, oxalic acid is one of the indicators of the decomposition behavior of organic substances in sewage, but it is not possible to analyze nitrate ions and nitrite ions simultaneously with a general anion chromatograph.

そこで、請求項１の硝酸態窒素の定量方法は溶離液に炭酸系溶離液を用いた陰イオンクロマトグラフによって試料中の硝酸イオンの定量を行うことを特徴とする。この発明によればシュウ酸を含んだ試料（例えば下水処理水）中の硝酸イオンを定量できる。   Therefore, the nitrate nitrogen quantification method according to claim 1 is characterized in that nitrate ions in a sample are quantified by anion chromatography using a carbonate-based eluent as an eluent. According to this invention, nitrate ions in a sample containing oxalic acid (for example, sewage treated water) can be quantified.

請求項２の硝酸態窒素の定量方法は溶離液に炭酸系溶離液を用いた陰イオンクロマトグラフによって試料中の亜硝酸イオンと硝酸イオンの定量を行うことを特徴とする。この発明によればシュウ酸を含んだ試料（例えば下水処理水）中の亜硝酸イオンと硝酸イオンとを同時に定量できるので前記試料に含まれるアンモニア態窒素の処理挙動の把握が可能となる。   The method for quantifying nitrate nitrogen according to claim 2 is characterized in that nitrite ions and nitrate ions in a sample are quantified by anion chromatography using a carbonate-based eluent as an eluent. According to the present invention, since nitrite ions and nitrate ions in a sample containing oxalic acid (for example, sewage treated water) can be simultaneously determined, it is possible to grasp the treatment behavior of ammonia nitrogen contained in the sample.

請求項３の陰イオンの定量方法は溶離液に炭酸系溶離液を用いた陰イオンクロマトグラフによってシュウ酸イオンと亜硝酸イオンと硝酸イオンとの定量を行うことを特徴とする。この発明によれば、シュウ酸イオンと亜硝酸イオンと硝酸イオンとを同時に定量できるので下水処理における有機物の分解挙動を把握できる。   The method for quantifying anions according to claim 3 is characterized in that oxalate ions, nitrite ions and nitrate ions are quantified by anion chromatography using a carbonate-based eluent as an eluent. According to this invention, since oxalate ions, nitrite ions, and nitrate ions can be simultaneously determined, it is possible to grasp the decomposition behavior of organic substances in sewage treatment.

請求項４の三態窒素の定量方法は、溶離液に炭酸系溶離液を用いた陰イオンクロマトグラフによって試料中のシュウ酸イオンと亜硝酸イオンと硝酸イオンとの定量を行った後に、前記試料を陽イオンクロマトグラフに供して前記試料中のアンモニウムイオンの定量を行うことを特徴とする。この発明によれば、シュウ酸を含んだ試料（例えば下水処理水）中のアンモニウムイオンと亜硝酸イオンと硝酸イオンとを同時に定量できるので前記試料に含まれるアンモニア態窒素の処理挙動の把握が可能となる。   The method for quantifying trinitrogen according to claim 4 is characterized in that the oxalate ion, nitrite ion and nitrate ion in the sample are quantified by anion chromatography using a carbonate-based eluent as the eluent, and then the sample Is subjected to cation chromatography to quantify ammonium ions in the sample. According to the present invention, ammonium ions, nitrite ions, and nitrate ions in a sample containing oxalic acid (for example, sewage treated water) can be simultaneously determined, so that it is possible to grasp the treatment behavior of ammonia nitrogen contained in the sample. It becomes.

したがって、請求項１の発明によれば下水処理の過程で有機物の分解によって生成するシュウ酸を含んだ処理水中の硝酸イオンをシュウ酸の影響を受けずに定量できる。   Therefore, according to the invention of claim 1, nitrate ions in the treated water containing oxalic acid generated by the decomposition of organic substances in the course of sewage treatment can be quantified without being influenced by oxalic acid.

また、請求項２及び請求項４の発明によれば前記シュウ酸を含んだ処理水中のアンモニア態窒素の硝化の過程で発生する亜硝酸態窒素と硝酸態窒素とを同時に定量できるので下水処理の過程でのアンモニア態窒素の処理挙動を効率的に把握できる。   Further, according to the invention of claim 2 and claim 4, since nitrite nitrogen and nitrate nitrogen generated in the process of nitrification of ammonia nitrogen in the treated water containing oxalic acid can be simultaneously determined, sewage treatment It is possible to efficiently grasp the processing behavior of ammonia nitrogen in the process.

さらに、請求項３の発明によれば前記処理水に含まれるシュウ酸、亜硝酸態窒素及び硝酸態窒素を同時に定量できるので下水処理の過程での有機物の処理挙動を把握できる。   Furthermore, according to the invention of claim 3, since oxalic acid, nitrite nitrogen and nitrate nitrogen contained in the treated water can be simultaneously determined, it is possible to grasp the treatment behavior of organic substances in the process of sewage treatment.

図１は発明の実施形態に係る定量方法の手順を示したフローチャートである。   FIG. 1 is a flowchart showing a procedure of a quantitative method according to an embodiment of the invention.

Ｓ１では試料である下水処理水を攪拌して均一にする。   In S1, the sample sewage treated water is stirred and made uniform.

Ｓ２では前記攪拌した下水処理水を保留粒子径０．２１μｍのフィルターでろ過する。   In S2, the stirred sewage treated water is filtered with a filter having a retained particle diameter of 0.21 μm.

Ｓ３では前記ろ過処理した下水処理水を炭酸系の溶離液で分離する陰イオンクロマトグラフで亜硝酸イオン及び硝酸イオンのピーク面積値を算出する。   In S3, peak area values of nitrite ions and nitrate ions are calculated by an anion chromatograph that separates the filtered sewage treated water with a carbonaceous eluent.

Ｓ４では前記陰イオンクロマトグラフに供した下水処理水を陽イオンクロマトグラフに供給してアンモニウムイオンのピーク面積値を算出する。   In S4, the sewage treated water supplied to the anion chromatograph is supplied to the cation chromatograph, and the peak area value of ammonium ion is calculated.

Ｓ５では予め算出した既知濃度の亜硝酸イオン、硝酸イオン、アンモニウムイオンのピーク面積値から試料濃度を計算する。   In S5, the sample concentration is calculated from the peak area values of nitrite ions, nitrate ions, and ammonium ions of known concentrations calculated in advance.

Ｓ６では亜硝酸イオン、硝酸イオン、アンモニウムイオンの濃度比からアンモニア態窒素の処理挙動を評価する。   In S6, the treatment behavior of ammonia nitrogen is evaluated from the concentration ratio of nitrite ions, nitrate ions, and ammonium ions.

図２は実施例として陰イオンクロマトグラフの溶離液に炭酸酸系溶離液を用いて得られた下水処理水の陰イオンクロマトグラムである。このクロマトグラムは図１のフローチャートに基づき下水処理生成物であるシュウ酸を含む下水処理水が保留粒子径０．２１μｍのフィルターによってろ過された後に炭酸系の溶離液（１．８ｍＭのＮａ2ＣＯ3及び１．７ｍＭのＮａＨＣＯ3の水溶液。流速は１．５ｍｌ／分に設定した。）を用いた陰イオン交換分離するイオンクロマトグラフ（ダイオネクス製ＤＸ−ＡＱ）に供されて下水処理水中の硝酸イオンが検出されて得られたものである。イオンの検出には電気伝導度検出器（ダイオネクス製）を用いた。 FIG. 2 is an anion chromatogram of sewage treated water obtained by using a carbonate-based eluent as an eluent of an anion chromatograph as an example. This chromatogram is based on the flow chart of FIG. 1, and sewage treated water containing oxalic acid, which is a sewage treatment product, is filtered through a filter having a retained particle diameter of 0.21 μm, and then a carbonate-based eluent (1.8 mM Na 2 CO 3 and 1.7 mM aqueous solution of NaHCO 3 (flow rate set at 1.5 ml / min)) and subjected to ion chromatography (Dionex DX-AQ) using anion exchange separation, nitric acid in sewage treated water This is obtained by detecting ions. An electric conductivity detector (Dionex) was used for ion detection.

一方、図３は比較例として従来法に基づき陰イオンクロマトグラフの溶離液にフタル酸系溶離液を用いて得られた下水処理水の陰イオンクロマトグラムである。このクロマトグラムは図１のフローチャートに基づき下水処理生成物であるシュウ酸を含む下水処理水が保留粒子径０．２１μｍのフィルターによってろ過された後に、フタル系の溶離液（２．５ｍＭフタル酸及び２．５ｍＭトリスバッファを含む。流速は１．０ｍＬ／分に設定した。）で陰イオン交換分離するイオンクロマトグラフ（東亜電波工業製ＩＣＡ−３０００）に供されて下水処理水中の硝酸イオンが検出されて得られたものである。イオンの検出には電気伝導度検出器（東亜電波工業製）を用いた。   On the other hand, FIG. 3 is an anion chromatogram of sewage treated water obtained as a comparative example using a phthalic acid-based eluent as an eluent of an anion chromatograph based on a conventional method. This chromatogram is based on the flow chart of FIG. 1, after sewage treatment water containing oxalic acid, which is a sewage treatment product, is filtered through a filter having a retention particle size of 0.21 μm, a phthalic eluent (2.5 mM phthalic acid and It contains 2.5 mM Tris buffer. The flow rate was set at 1.0 mL / min.) And was subjected to ion chromatograph (ICA-3000 manufactured by Toa Denpa Kogyo Co., Ltd.) to detect nitrate ions in sewage treated water. It was obtained. An electric conductivity detector (manufactured by Toa Denpa Kogyo Co., Ltd.) was used for ion detection.

また、表１にはフタル酸系溶離液（比較例）、炭酸系溶離液（実施例）をそれぞれ用いた陰イオンクロマトグラフによって測定された試料（下水処理前の下水及び下水処理後の下水）の亜硝酸イオン及び硝酸イオンの濃度（ｍｇ／Ｌ）を示した。   Table 1 shows samples measured by anion chromatography using phthalic acid-based eluent (comparative example) and carbonic acid-based eluent (example) (sewage before sewage treatment and sewage after sewage treatment). The concentration (mg / L) of nitrite ion and nitrate ion was shown.

図２に示されたように炭酸系溶離液を用いた陰イオンクロマトグラフによるとシュウ酸は硝酸イオンと完全に分離独立して溶出し、硝酸イオンの検出の妨害にならならないことが確認できる。このようにこの陰イオンクロマトグラフの溶離液に炭酸系の処理液が用いられるとシュウ酸が亜硝酸イオンとも完全に分離独立して溶出し、硝酸イオン、亜硝酸イオンともに正確に定量できることが示された。   As shown in FIG. 2, according to the anion chromatograph using a carbonic acid-based eluent, it can be confirmed that oxalic acid elutes completely and independently from nitrate ions and does not interfere with detection of nitrate ions. Thus, when a carbonic acid treatment solution is used as the eluent of this anion chromatograph, oxalic acid is completely separated and separated from nitrite ions, indicating that both nitrate ion and nitrite ion can be accurately determined. It was done.

一方、図３に示されたように比較例に係るフタル酸系溶離液を用いた陰イオンクロマトグラフの場合、シュウ酸は硝酸イオンと分離しないで溶出し、硝酸イオンの検出の妨害となってしまうことが確認できる。このことは表１に示された比較例と実施例の硝酸イオン濃度の比較からも明らかである。   On the other hand, in the case of the anion chromatograph using the phthalic acid-based eluent according to the comparative example as shown in FIG. 3, oxalic acid elutes without being separated from nitrate ions, which hinders detection of nitrate ions. Can be confirmed. This is also clear from the comparison of nitrate ion concentrations in the comparative example and the example shown in Table 1.

次いで、下水処理生成物である炭酸系の溶離液で陰イオン交換分離するイオンクロマトグラフを用いて、下水処理水中のシュウ酸を定量した。図４に定量方法の手順を示したフローチャートを示した。   Next, oxalic acid in the sewage treated water was quantified using an ion chromatograph that performs anion exchange separation with a carbonate-based eluent that is a sewage treatment product. FIG. 4 shows a flowchart showing the procedure of the quantification method.

Ｓ４１では試料である下水処理水を攪拌して均一にする。   In S41, the sample sewage treated water is agitated and made uniform.

Ｓ４２では前記攪拌した下水処理水を保留粒子径０．２１μｍのフィルターでろ過する。   In S42, the agitated sewage treated water is filtered through a filter having a retained particle diameter of 0.21 μm.

Ｓ４３では前記ろ過処理した下水処理水を炭酸系の溶離液で分離する陰イオンクロマトグラフに供してシュウ酸のピーク面積値を算出する。   In S43, the peak area value of oxalic acid is calculated by subjecting the filtered sewage treated water to an anion chromatograph that separates with a carbonate-based eluent.

Ｓ４４では予め算出した既知濃度のシュウ酸のピーク面積値から試料濃度を計算する。   In S44, the sample concentration is calculated from the peak area value of oxalic acid having a known concentration calculated in advance.

Ｓ４５ではシュウ酸濃度から下水中の有機物の分解挙動を評価する。   In S45, the decomposition behavior of organic matter in sewage is evaluated from the oxalic acid concentration.

以上のフローチャートに基づきシュウ酸を含む下水処理水を保留粒子径０．２１μｍのフィルターでろ過した後に炭酸系の溶離液（１．８ｍＭのＮａ2ＣＯ3及び１．７ｍＭのＮａＨＣＯ3の水溶液。流速は１．５ｍｌ／分に設定した。）で陰イオン交換分離するイオンクロマトグラフ（ダイオネクス製ＤＸ−ＡＱ）を用いて下水処理水中のシュウ酸を定量した。シュウ酸の検出には電気伝導度検出器（ダイオネクス製）を用いた。 Based on the above flowchart, sewage-treated water containing oxalic acid is filtered through a filter having a retention particle size of 0.21 μm, and then a carbonate-based eluent (an aqueous solution of 1.8 mM Na 2 CO 3 and 1.7 mM NaHCO 3 . Was set at 1.5 ml / min.), And oxalic acid in sewage treated water was quantified using an ion chromatograph (DX-AQ manufactured by Dionex) that performs anion exchange separation. An electric conductivity detector (manufactured by Dionex) was used for detection of oxalic acid.

表１にフタル酸系溶離液（比較例）、炭酸系溶離液（実施例）をそれぞれ用いた陰イオンクロマトグラフによって測定した試料（下水処理前の下水及び下水処理後の下水）のシュウ酸の濃度（ｍｇ／Ｌ）を示した。そして、前記検出電気伝導度検出器の検出によって得られた図２及び図３に記載の陰イオンクロマトグラムに基づき有機物の分解挙動を評価した。   Table 1 shows the oxalic acid concentrations of samples (sewage before sewage treatment and sewage after sewage treatment) measured by anion chromatography using phthalic acid-based eluent (comparative example) and carbonic acid-based eluent (example). Concentration (mg / L) was indicated. And the decomposition | disassembly behavior of organic substance was evaluated based on the anion chromatogram of FIG.2 and FIG.3 obtained by the detection of the said detection electrical conductivity detector.

図２のクロマトグラムから明らかなように炭酸系の溶離液を用いた陰イオンクロマトグラフによれば硝酸イオン及び亜硝酸イオンと同時にシュウ酸を定量することができ、簡便に下水処理における有機物の分解を把握できることが確認された。一方、図３のクロマトグラムに示されたようにフタル酸系の溶離液を用いた陰イオンクロマトグラフではシュウ酸の定量が不可能であることが確認された。   As can be seen from the chromatogram in Fig. 2, anion chromatography using a carbonate-based eluent can quantitate oxalic acid simultaneously with nitrate and nitrite ions. Was confirmed. On the other hand, as shown in the chromatogram of FIG. 3, it was confirmed that oxalic acid could not be quantified by anion chromatography using a phthalic acid-based eluent.

次いで、図１に示されたフローチャートに基づき下水処理生成物であるシュウ酸を含む下水処理水を保留粒子径０．２１μｍにフィルターでろ過し、陽イオンクロマトグラフ（東亜電波工業製ＩＣＡ−３０００）でアンモニウムイオンを定量した。その結果を表１に示した。   Next, based on the flowchart shown in FIG. 1, sewage treatment water containing oxalic acid, which is a sewage treatment product, is filtered through a filter to a retained particle size of 0.21 μm, and a cation chromatograph (ICA-3000 manufactured by Toa Denpa Kogyo Co., Ltd.). The ammonium ions were quantified with The results are shown in Table 1.

また、前記下水処理水を保留粒子径０．２１μｍのフィルターでろ過し、炭酸系の溶離液（１．８ｍＭのＮａ2ＣＯ3及び１．７ｍＭのＮａＨＣＯ3の水溶液。流速は１．５ｍｌ／分に設定した。）で陰イオン交換分離するイオンクロマトグラフ（ダイオネクス製ＤＸ−ＡＱ）を用いて、前記下水処理水中の亜硝酸イオン及び硝酸イオンを定量した。アンモニウムイオン、亜硝酸イオン及び硝酸イオンの検出には電気伝導度検出器（ダイオネクス製）を用いた。この検出によって得られたクロマトグラムが図２に示されている。 The sewage-treated water is filtered through a filter having a retention particle size of 0.21 μm, and a carbonate-based eluent (1.8 mM Na 2 CO 3 and 1.7 mM NaHCO 3 aqueous solution. The flow rate is 1.5 ml / min. The nitrite ions and nitrate ions in the sewage treated water were quantified using an ion chromatograph (DX-AQ manufactured by Dionex) that performs anion exchange separation. An electric conductivity detector (manufactured by Dionex) was used to detect ammonium ions, nitrite ions and nitrate ions. The chromatogram obtained by this detection is shown in FIG.

一方、比較例として前記下水処理水を保留粒子径０．２１μｍのフィルターでろ過し、フタル酸系の溶離液（２．５ｍＭフタル酸及び２．５ｍＭトリスバッファを含む。流速は１．０ｍＬ／分に設定した。）で陰イオン交換分離するイオンクロマトグラフ（東亜電波工業製ＩＣＡ−３０００）を用いて、前記下水処理水中の亜硝酸イオン及び硝酸イオンを定量した。この検出によって得られたクロマトグラムが図３に示されている。   On the other hand, as a comparative example, the sewage treated water is filtered through a filter having a retention particle size of 0.21 μm, and a phthalic acid-based eluent (including 2.5 mM phthalic acid and 2.5 mM Tris buffer. The flow rate is 1.0 mL / min. The nitrite ions and nitrate ions in the sewage treated water were quantified using an ion chromatograph (ICA-3000, manufactured by Toa Denpa Kogyo Co., Ltd.) that performs anion exchange separation. The chromatogram obtained by this detection is shown in FIG.

表１、図２及び図３に示された下水処理前後の下水中のアンモニウムイオン、亜硝酸イオン、硝酸イオンの濃度の比較から明らかなように炭酸系の溶離液を用いた陰イオンクロマトグラフによる陰イオンの定量方法によればシュウ酸の影響を受けることなくアンモニア態窒素の処理挙動を評価できることが確認された。   As can be seen from the comparison of the ammonium ion, nitrite ion, and nitrate ion concentrations in the sewage before and after the sewage treatment shown in Table 1, FIG. 2 and FIG. 3, an anion chromatograph using a carbonate-based eluent was used. It was confirmed that the treatment behavior of ammonia nitrogen could be evaluated by the anion determination method without being affected by oxalic acid.

Figure 2008256636
Figure 2008256636

以上のように陰イオンクロマトグラフの溶離液に炭酸系溶離液を用いた本発明に係る定量方法によれば下水処理の過程で有機物の分解によって生成するシュウ酸を含んだ処理水中の硝酸イオンをシュウ酸の影響を受けずに定量できる。また、前記シュウ酸を含んだ処理水中のアンモニア態窒素の硝化の過程で発生する亜硝酸態窒素と硝酸態窒素とを同時に定量できるので下水処理の過程でのアンモニア態窒素の処理挙動を効率的に把握できる。さらに、前記処理水に含まれるシュウ酸、亜硝酸態窒素及び硝酸態窒素を同時に定量できるので下水処理の過程での有機物の処理挙動を把握できる。   As described above, according to the quantification method according to the present invention using the carbonic acid-based eluent as the eluent of the anion chromatograph, nitrate ions in the treated water containing oxalic acid generated by the decomposition of organic substances in the process of sewage treatment can be obtained. Can be quantified without being affected by oxalic acid. In addition, nitrite nitrogen and nitrate nitrogen generated in the nitrification process of ammonia nitrogen in the treated water containing oxalic acid can be determined simultaneously, so that the treatment behavior of ammonia nitrogen in the process of sewage treatment is efficient. Can grasp. Furthermore, since oxalic acid, nitrite nitrogen, and nitrate nitrogen contained in the treated water can be simultaneously determined, it is possible to grasp the treatment behavior of organic substances during the sewage treatment process.

発明の実施形態に係る定量（亜硝酸イオン、硝酸イオン、アンモニウムイオンの定量）方法の手順の一例を示したフローチャート。The flowchart which showed an example of the procedure of the fixed_quantity | quantitative_assay (quantitative determination of nitrite ion, nitrate ion, ammonium ion) which concerns on embodiment of invention. 実施例として陰イオンクロマトグラフの溶離液にフタル酸系溶離液を用いた場合の下水処理水の陰イオンクロマトグラム。The anion chromatogram of the sewage treated water at the time of using a phthalic acid system eluent as an eluent of an anion chromatograph as an Example. 比較例として従来法に基づき陰イオンクロマトグラフの溶離液にフタル酸系溶離液を用いた場合の下水処理水の陰イオンクロマトグラム。An anion chromatogram of sewage treated water when a phthalic acid-based eluent is used as an eluent of an anion chromatograph based on a conventional method as a comparative example. 発明の実施形態に係る定量（シュウ酸濃度の定量）方法の手順の一例を示したフローチャート。The flowchart which showed an example of the procedure of the fixed_quantity | quantitative_assay (quantification of an oxalic acid density | concentration) method which concerns on embodiment of invention.

Claims (4)

溶離液に炭酸系溶離液を用いた陰イオンクロマトグラフによって試料中の硝酸イオンの定量を行うことを特徴とする硝酸態窒素の定量方法。   A method for quantifying nitrate nitrogen, comprising quantifying nitrate ions in a sample by anion chromatography using a carbonate-based eluent as an eluent. 溶離液に炭酸系溶離液を用いた陰イオンクロマトグラフによって試料中の亜硝酸イオンと硝酸イオンの定量を行うことを特徴とする硝酸態窒素の定量方法。   A method for quantifying nitrate nitrogen, comprising quantifying nitrite ions and nitrate ions in a sample by anion chromatography using a carbonate-based eluent as an eluent. 溶離液に炭酸系溶離液を用いた陰イオンクロマトグラフによって試料中のシュウ酸イオンと亜硝酸イオンと硝酸イオンとの定量を行うことを特徴とする陰イオンの定量方法。   A method for quantifying anions, comprising quantifying oxalate ions, nitrite ions and nitrate ions in a sample by anion chromatography using a carbonate-based eluent as an eluent. 溶離液に炭酸系溶離液を用いた陰イオンクロマトグラフによって試料中のシュウ酸イオンと亜硝酸イオンと硝酸イオンとの定量を行った後に、前記試料を陽イオンクロマトグラフに供して前記試料中のアンモニウムイオンの定量を行うことを特徴とする三態窒素の定量方法。   After quantifying the oxalate ion, nitrite ion and nitrate ion in the sample by anion chromatography using a carbonate-based eluent as the eluent, the sample was subjected to a cation chromatograph and subjected to cation chromatography. A method for quantifying trivalent nitrogen, comprising quantifying ammonium ions.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106596770A (en) * 2016-12-13 2017-04-26 四川大学 Low-pressure anion-cation chromatographic-spectrophotometric method for simultaneous online automatic analysis of trace ammonium ions and nitrite ions in water sample
CN111398478A (en) * 2020-04-23 2020-07-10 珠江水利委员会珠江水利科学研究院 Gas-mass spectrum chromatography combined detection method for ammonia nitrogen and isotope content thereof in water sample
CN111521693A (en) * 2019-02-01 2020-08-11 鲁南制药集团股份有限公司 Method for detecting isosorbide mononitrate

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106596770A (en) * 2016-12-13 2017-04-26 四川大学 Low-pressure anion-cation chromatographic-spectrophotometric method for simultaneous online automatic analysis of trace ammonium ions and nitrite ions in water sample
CN106596770B (en) * 2016-12-13 2019-03-29 四川大学 Simultaneously in on-line automatic analysis water-like micro ammonium ion and nitrite ion low pressure anions and canons chromatography-photometry
CN111521693A (en) * 2019-02-01 2020-08-11 鲁南制药集团股份有限公司 Method for detecting isosorbide mononitrate
CN111521693B (en) * 2019-02-01 2021-01-29 鲁南制药集团股份有限公司 Method for detecting isosorbide mononitrate
CN111398478A (en) * 2020-04-23 2020-07-10 珠江水利委员会珠江水利科学研究院 Gas-mass spectrum chromatography combined detection method for ammonia nitrogen and isotope content thereof in water sample
CN111398478B (en) * 2020-04-23 2022-09-02 珠江水利委员会珠江水利科学研究院 Gas-mass spectrometry-chromatography combined detection method for ammonia nitrogen and isotope content thereof in water sample

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