JPH0723867B2 - Quantitative analysis method for NOx nitrogen - Google Patents
Quantitative analysis method for NOx nitrogenInfo
- Publication number
- JPH0723867B2 JPH0723867B2 JP60210289A JP21028985A JPH0723867B2 JP H0723867 B2 JPH0723867 B2 JP H0723867B2 JP 60210289 A JP60210289 A JP 60210289A JP 21028985 A JP21028985 A JP 21028985A JP H0723867 B2 JPH0723867 B2 JP H0723867B2
- Authority
- JP
- Japan
- Prior art keywords
- nox
- membrane
- quantitative analysis
- nitrogen
- nitrogen concentration
- 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 - Lifetime
Links
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims description 172
- 229910052757 nitrogen Inorganic materials 0.000 title claims description 89
- 238000000034 method Methods 0.000 title claims description 60
- 238000004445 quantitative analysis Methods 0.000 title claims description 36
- 239000012528 membrane Substances 0.000 claims description 55
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 49
- 238000005273 aeration Methods 0.000 claims description 37
- 239000000126 substance Substances 0.000 claims description 21
- 230000002452 interceptive effect Effects 0.000 claims description 13
- 239000010802 sludge Substances 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- 150000003839 salts Chemical class 0.000 claims description 11
- 239000012466 permeate Substances 0.000 claims description 9
- 229910002651 NO3 Inorganic materials 0.000 claims description 3
- 238000001223 reverse osmosis Methods 0.000 claims description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- JVMRPSJZNHXORP-UHFFFAOYSA-N ON=O.ON=O.ON=O.N Chemical compound ON=O.ON=O.ON=O.N JVMRPSJZNHXORP-UHFFFAOYSA-N 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 238000012360 testing method Methods 0.000 description 30
- 238000010521 absorption reaction Methods 0.000 description 14
- 238000004065 wastewater treatment Methods 0.000 description 13
- 238000004458 analytical method Methods 0.000 description 12
- 238000002835 absorbance Methods 0.000 description 10
- 239000002351 wastewater Substances 0.000 description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 238000007796 conventional method Methods 0.000 description 6
- 229910017464 nitrogen compound Inorganic materials 0.000 description 6
- 150000002830 nitrogen compounds Chemical class 0.000 description 6
- 150000002894 organic compounds Chemical class 0.000 description 5
- 239000000356 contaminant Substances 0.000 description 4
- YRIUSKIDOIARQF-UHFFFAOYSA-N dodecyl benzenesulfonate Chemical compound CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 YRIUSKIDOIARQF-UHFFFAOYSA-N 0.000 description 4
- 229940071161 dodecylbenzenesulfonate Drugs 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 241000894006 Bacteria Species 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000852 hydrogen donor Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- -1 salt Chemical class 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000000108 ultra-filtration Methods 0.000 description 2
- FUSNOPLQVRUIIM-UHFFFAOYSA-N 4-amino-2-(4,4-dimethyl-2-oxoimidazolidin-1-yl)-n-[3-(trifluoromethyl)phenyl]pyrimidine-5-carboxamide Chemical compound O=C1NC(C)(C)CN1C(N=C1N)=NC=C1C(=O)NC1=CC=CC(C(F)(F)F)=C1 FUSNOPLQVRUIIM-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- RRKTZKIUPZVBMF-IBTVXLQLSA-N brucine Chemical compound O([C@@H]1[C@H]([C@H]2C3)[C@@H]4N(C(C1)=O)C=1C=C(C(=CC=11)OC)OC)CC=C2CN2[C@@H]3[C@]41CC2 RRKTZKIUPZVBMF-IBTVXLQLSA-N 0.000 description 1
- RRKTZKIUPZVBMF-UHFFFAOYSA-N brucine Natural products C1=2C=C(OC)C(OC)=CC=2N(C(C2)=O)C3C(C4C5)C2OCC=C4CN2C5C31CC2 RRKTZKIUPZVBMF-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000005446 dissolved organic matter Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 1
- 239000010840 domestic wastewater Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012493 hydrazine sulfate Substances 0.000 description 1
- 229910000377 hydrazine sulfate Inorganic materials 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000001546 nitrifying effect Effects 0.000 description 1
- 125000001477 organic nitrogen group Chemical group 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 238000006864 oxidative decomposition reaction Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 150000003018 phosphorus compounds Chemical class 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 238000010187 selection method Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
Landscapes
- Investigating Or Analysing Materials By Optical Means (AREA)
Description
【発明の詳細な説明】 （産業上の利用分野） 本発明は、NOx態窒素濃度の定量分析方法および定量分
析装置に関し、更に詳しくは活性汚泥法による排水処理
における排水あるいは処理水のNOx態窒素濃度の定量分
析に有用である定量分析方法および定量分析装置に関す
る。TECHNICAL FIELD The present invention relates to a quantitative analysis method and a quantitative analysis apparatus for NOx nitrogen concentration, and more specifically, NOx nitrogen of wastewater or treated water in wastewater treatment by activated sludge method. The present invention relates to a quantitative analysis method and a quantitative analysis device useful for quantitative analysis of concentration.
（従来の技術） 従来、生活排水あるいは産業排水の浄化方法としては、
活性汚泥を用いて排水中の種々の有機物等を分解して排
水を浄化する方法が広く行なわれている。これらの活性
汚泥法は一般に広大な設備面積を有するという欠点があ
るため、近年は制限曝気法と称される回分式の活性汚泥
法が提案され、且つ広く使用されつつある。該制限曝気
法は、１個の処理槽内でBOD酸化菌と硝化菌による好気
工程と、該好気工程で生成したNOx態窒素を脱窒菌を利
用して窒素ガスに還元して除去する嫌気工程とを繰返し
て行う方法であるが、使用する活性汚泥を効率良く利用
し、排水中の窒素化合物は勿論その他有機物やリン化合
物等を十分に除去するためには、曝気槽混合液中のNOx
態窒素濃度を十分にコントロールすることが必要であ
る。(Prior Art) Conventionally, as a method for purifying domestic wastewater or industrial wastewater,
A method of purifying wastewater by decomposing various organic substances in wastewater using activated sludge is widely used. Since these activated sludge methods generally have a large facility area, a batch type activated sludge method called a limited aeration method has been proposed and widely used in recent years. In the limited aeration method, an aerobic process using BOD-oxidizing bacteria and nitrifying bacteria in one treatment tank, and NOx nitrogen generated in the aerobic process is reduced to nitrogen gas using denitrifying bacteria and removed. It is a method of repeating the anaerobic process, but in order to efficiently use the activated sludge to be used and sufficiently remove not only nitrogen compounds but also other organic substances and phosphorus compounds in the wastewater, NOx
It is necessary to adequately control the state nitrogen concentration.
このようなNOx態窒素濃度をコントロールするために
は、曝気槽混合液中のNOx態窒素濃度を随時定量分析
し、NOx態窒素濃度が低すぎる場合には曝気を延長し、
またNOx態窒素濃度が高すぎる時は曝気を中断したり、
アルコールや原排水等の水素供与体の注入を行うことに
よりNOx態窒素濃度をコントロールする。In order to control such NOx-state nitrogen concentration, the NOx-state nitrogen concentration in the aeration tank mixture is quantitatively analyzed from time to time, and when the NOx-state nitrogen concentration is too low, aeration is extended,
When NOx nitrogen concentration is too high, aeration may be interrupted,
NOx nitrogen concentration is controlled by injecting hydrogen donor such as alcohol or raw waste water.
このようなNOx態窒素濃度の定量分析方法としては、ブ
ルシン吸光光度法（JISK0102）、硫酸ヒドラジン還元法
（環境庁告示第59号）、エチレンジアミン法（JISK010
2）、紫外吸光度法等の方法が行なわれている。As a quantitative analysis method for such NOx nitrogen concentration, brucine absorptiometry (JISK0102), hydrazine sulfate reduction method (Environmental Agency Notification No. 59), ethylenediamine method (JISK010
2) Methods such as the ultraviolet absorption method are used.
そして、いずれの定量分析方法を利用するとしても、正
確な分析値を期待するには、分析前に検水（例えば曝気
槽混合液）中の浮遊固形物、溶存有機または無機化合物
あるいは活性汚泥等の分析妨害物質を十分に除去するこ
とが必要である。このような妨害物質の除去方法として
は、微細な網目スクリーンやカートリッジ瀘過器等の一
般的な固液分離法が使用されている。And regardless of which quantitative analysis method is used, in order to expect accurate analysis values, suspended solids, dissolved organic or inorganic compounds, activated sludge, etc. in the test water (eg, aeration tank mixture) should be analyzed before analysis. It is necessary to sufficiently remove the substance that interferes with the analysis. As a method for removing such an interfering substance, a general solid-liquid separation method such as a fine mesh screen or a cartridge filter is used.
（発明が解決しようとしている問題点） 以上の如き従来の曝気槽混合液中のNOx態窒素濃度の定
量分析方法における検水の前処理装置、すなわち妨害物
質を除去するための前処理装置が瀘過器、例えば微細な
網目スクリーンやカートリッジ瀘過器の場合には、瀘過
効果が不十分であり、コロイド状あるいは溶解状態の有
機および無機妨害物質を除去できないため、正確なNOx
態窒素濃度の定量が困難である。またこれらの瀘過器は
目詰りし易いので、頻繁な瀘材の交換や瀘材の逆洗が必
要であり、特に排水処理設備を自動制御する際には多く
の不都合を生じる。(Problems to be Solved by the Invention) A pretreatment device for test water in the conventional method for quantitatively analyzing NOx-nitrogen concentration in an aeration tank mixture, that is, a pretreatment device for removing interfering substances, is used. In the case of filters, such as fine mesh screens and cartridge filters, the filtration effect is insufficient and it is not possible to remove organic and inorganic interfering substances in colloidal or dissolved state, so accurate NOx
It is difficult to quantify the nitrogen concentration. Further, since these filters are apt to be clogged, it is necessary to frequently replace the filters and backwash the filters, which causes many inconveniences especially when the wastewater treatment facility is automatically controlled.
また、前処理した検水の従来の分析方法のいずれもが多
くの分析試薬を必要としたり、定温反応や蒸留操作等の
測定条件の設定が繁雑であり、このような分析方法は、
特に排水処理設備を自動制御する場合には多くの不都合
が生じる。In addition, any of the conventional analysis methods for pretreated sample water requires many analysis reagents, and setting of measurement conditions such as constant temperature reaction and distillation operation is complicated.
In particular, there are many inconveniences when automatically controlling wastewater treatment equipment.
また、NOx態窒素濃度の定量分析方法として紫外吸光度
法も知られているが、この紫外吸光度法は、検水を予め
アルカリ性ペルオキソ二硫酸カリウム等による酸化分解
を行い、検水中の窒素化合物をすべてNOx態窒素に変え
る方法であるため、NOx態窒素以外の窒素系化合物もNOx
態窒素として定量され、NOx態窒素濃度のみを正確に把
握することができない。検水を酸化しない場合には、窒
素系有機化合物あるいはベンゼン環や不飽和構造をもつ
有機化合物等が妨害物質として作用し、同様に正確なNO
x態窒素濃度を把握できない。An ultraviolet absorption method is also known as a quantitative analysis method for the NOx nitrogen concentration, but this ultraviolet absorption method performs oxidative decomposition of the test water with alkaline potassium peroxodisulfate in advance to remove all nitrogen compounds in the test water. Since it is a method of changing to NOx-type nitrogen, NOx-containing compounds other than NOx-type nitrogen
It is quantified as state nitrogen, and it is not possible to accurately grasp only the concentration of NOx state nitrogen. If the sample water is not oxidized, nitrogen-based organic compounds or organic compounds with benzene rings or unsaturated structures act as interfering substances, and the same accurate NO
Cannot determine x-nitrogen concentration.
従って、活性汚泥法による排水処理設備、特に回分式の
制限曝気法による排水処理設備の自動制御化に際して
は、その曝気槽混合液中のNOx態窒素濃度の分析妨害物
質を十分に除去し、且つその中のNOx態窒素濃度のみを
迅速且つ正確に定量分析できる分析方法および分析装置
が強く要望されている。Therefore, when automatically controlling the wastewater treatment equipment by the activated sludge method, especially the wastewater treatment equipment by the batch type limited aeration method, sufficiently remove the substances that interfere with the analysis of the NOx nitrogen concentration in the aeration tank mixture, and There is a strong demand for an analytical method and an analytical device that can quickly and accurately quantitatively analyze only the NOx-state nitrogen concentration therein.
（問題点を解決するための手段） 本発明者は上記の如き従来技術の要望に応えるべく鋭意
研究の結果、曝気槽混合液中のNOx態窒素濃度を紫外吸
光度法により定量分析するに際して、特定の膜により検
水を前処理することによって、上述の如き種々の問題を
生じることなく、曝気槽混合液中のNOx態窒素濃度のみ
が迅速且つ正確に定量分析でき、従って排水処理設備の
自動制御化に有用であることを知見して本発明を完成し
た。(Means for Solving Problems) As a result of earnest research to meet the demands of the prior art as described above, the present inventor has specified that the NOx nitrogen concentration in the aeration tank mixture is quantitatively analyzed by an ultraviolet absorption method. By pre-treating the sample water with the membrane of No. 3, it is possible to quantitatively analyze only the NOx nitrogen concentration in the mixed liquid of the aeration tank quickly and accurately without causing the above-mentioned various problems. The present invention has been completed by discovering that it is useful for the application.
すなわち、本発明は、活性汚泥法における曝気槽中の硝
酸性および／または亜硝酸性窒素（以下NOx態窒素とい
う）を含有する曝気槽混合液中のNOx態窒素濃度を紫外
吸光光度法により定量分析する方法において、定量分析
前に検水中の妨害物質を、NOx態窒素を実質的に透過す
る逆浸透膜（以下RO膜という）および／または限外透過
膜（以下UF膜という）により除去した後、得られた透過
水中のNOx態窒素を定量分析することを特徴とするNOx態
窒素の定量分析方法である。That is, the present invention quantifies the NOx nitrogen concentration in an aeration tank mixed solution containing nitrate and / or nitrite nitrogen (hereinafter referred to as NOx nitrogen) in the aeration tank in the activated sludge method by an ultraviolet absorption spectrophotometric method. In the method of analysis, interfering substances in the test water were removed by a reverse osmosis membrane (hereinafter referred to as RO membrane) and / or an ultrapermeable membrane (hereinafter referred to as UF membrane) that substantially permeate NOx nitrogen before quantitative analysis. After that, it is a quantitative analysis method of NOx-state nitrogen characterized by quantitatively analyzing NOx-state nitrogen in the obtained permeated water.
次に本発明を更に詳細に説明すると、本発明を第１に特
徴づける点は、検水、例えば活性汚泥法による排水処理
設備の曝気槽混合液中のNOx態窒素濃度を定量分析する
にあたり、定量分析前に該検水をRO膜またはUF膜あるい
は両者により処理する点である。Next, the present invention will be described in more detail. The first feature of the present invention is that in the test water, for example, in quantitative analysis of NOx nitrogen concentration in an aeration tank mixture of a wastewater treatment facility by an activated sludge method, The point is that the sample water is treated with an RO membrane or a UF membrane or both before quantitative analysis.
本発明者の詳細な研究によれば、検水、特に曝気槽混合
液は、原排水からの種々雑多の浮遊固形物を含有する
外、種々雑多な有機および無機の溶解物質、多くの種類
の微生物（活性汚泥）を含有しており、これらの多くの
夾雑物がNOx態窒素濃度の定量分析の妨害物質になり得
るものであり、従来の瀘過器等を用いる検水の前処理で
は、前述の如き妨害物質の十分な除去が不可能であり、
例えば紫外吸光度法によりNOx態窒素濃度の定量分析を
行うと、NOx態窒素以外の有機態窒素分までがNOx態窒素
濃度として定量分析され、正確なNOx態窒素濃度の定量
分析が不可能であった。According to a detailed study by the present inventor, the test water, especially the aeration tank mixture, contains various suspended solids from the raw wastewater, as well as various organic and inorganic dissolved substances, and many types of dissolved solids. It contains microorganisms (activated sludge), and many of these contaminants can be interfering substances in the quantitative analysis of NOx nitrogen concentration, and in the pretreatment of the test water using a conventional filter, etc., It is impossible to remove the interfering substances as described above,
For example, when quantitative analysis of NOx-type nitrogen concentration is carried out by the ultraviolet absorption method, organic nitrogen components other than NOx-state nitrogen are quantitatively analyzed as NOx-state nitrogen concentration, and accurate quantitative analysis of NOx-state nitrogen concentration is impossible. It was
これに対して、検水、特に曝気槽混合液を適当な孔サイ
ズのRO膜および／またはUF膜で透過処理することによ
り、検水中のNOx態窒素のみを実質的に透過させ、そそ
の他上記の如き種々の妨害物質の大部分が除去され、次
いでこの前処理した検水を紫外吸光度法によりNOx態窒
素濃度の定量分析を行うことにより、従来方法の如く定
量分析前に検水の酸化処理を行う等の繁雑な操作を必要
とすることなく正確なNOx態窒素濃度を直接定量分析す
ることができることを知見したものである。On the other hand, when the test water, especially the aeration tank mixture is permeated with an RO membrane and / or UF membrane having an appropriate pore size, only NOx nitrogen in the test water is substantially permeated, and other Most of the various interfering substances such as the above are removed, and then the pretreated sample water is subjected to a quantitative analysis of the NOx nitrogen concentration by the ultraviolet absorption method. It was discovered that an accurate NOx-state nitrogen concentration can be directly quantitatively analyzed without requiring complicated operations such as performing.
本発明において使用するRO膜とは、海水の淡水化、種々
の溶液中の溶質の濃縮あるいは分離技術として広く知ら
れている逆浸透法に使用される膜であり、主として比較
的小さい分子の溶質の溶液の分離、濃縮あるいは精製等
に使用されているものである。The RO membrane used in the present invention is a membrane used in the reverse osmosis method, which is widely known as a technique for desalinating seawater, concentrating or separating solutes in various solutions, and is a solute of relatively small molecules. It is used for separating, concentrating or purifying the solution.
またUF膜とは、限外瀘過膜として公知であり、上記のRO
膜による溶質よりも大きい分子量の溶質の濃縮、分離あ
るいは精製を行う限外瀘過方法に使用されているもので
ある。The UF membrane is known as an ultrafiltration membrane, and the RO
It is used in an ultrafiltration method for concentrating, separating or purifying a solute having a molecular weight higher than that of a membrane.
このようなRO膜およびUF膜は、Abcor Inc.Ajax lntl.Co
rp.、Amicon Corp.、Aqua−chem.lnc.、Culligan lntl.
Co.、Dorr−oliver.lnc.、Dow chemical Co.、Dupont.C
o.、Envirogenics Co.、General Electric Co.その他多
くのメーカーから、種々の孔径のRO膜またはUF膜として
市販されており、これらのものがいずれも入手でき選択
して本発明に使用することができる。Such RO and UF membranes are available from Abcor Inc. Ajax lntl.
rp., Amicon Corp., Aqua-chem.lnc., Culligan lntl.
Co., Dorr-oliver.lnc., Dow chemical Co., Dupont.C
O., Envirogenics Co., General Electric Co. and many other manufacturers are commercially available as RO membranes or UF membranes with various pore sizes, and any of these can be selected and used in the present invention. it can.
以上の如きRO膜および／またはUF膜は、食塩等の小さい
分子の無機塩等を透過しないものから、無機塩等は透過
するが中程度の分子量の有機化合物あるいは高分子有機
化合物を透過しないもの等種々の孔径のものが入手し且
つ使用できるので、予め検水となる排水の種類からその
内に含まれる各種夾雑物の種類を調べておき、NOx態窒
素は実質的に透過できるが、それらより分子量の大なる
夾雑物、例えば各種界面活性剤、洗剤、石鹸、微生物等
は実質的に透過しないRO膜またはUF膜をを採用するのが
好ましい。The RO membrane and / or UF membrane as described above does not permeate inorganic salts of small molecules such as salt, but permeates inorganic salts but does not permeate organic compounds or high molecular weight organic compounds of moderate molecular weight. Since various types of pore sizes are available and can be used, the type of various contaminants contained in it is checked in advance from the type of wastewater used as the test water, and NOx-state nitrogen can be substantially permeated. It is preferable to employ an RO membrane or a UF membrane that is substantially impermeable to contaminants having a larger molecular weight, such as various surfactants, detergents, soaps and microorganisms.
例えば、好ましいRO膜あるいはUF膜の選定方法として
は、排水中に含有されていると考えられる上記の如き各
種の夾雑物およびNOx態窒素を水に溶解して疑似排水を
作成し、この疑似排水を用いて種々の孔径のRO膜および
／またはUF膜により、NOx態窒素を実質的に透過する
が、NOx態窒素より大きな分子量の夾雑物は実質的に透
過しないRO膜またはUF膜を採用することができる。また
これらのRO膜とUF膜とを組合せて使用することもでき
る。For example, as a preferable RO membrane or UF membrane selection method, various contaminants and NOx-like nitrogen, which are considered to be contained in the waste water, are dissolved in water to create a pseudo waste water. RO membranes and / or UF membranes with various pore sizes are used, and RO membranes or UF membranes that substantially permeate NOx-state nitrogen, but do not substantially permeate impurities having a molecular weight larger than NOx-state nitrogen, are adopted. be able to. Moreover, these RO membranes and UF membranes can be used in combination.
本発明者の研究によれば、１つの好ましいRO膜は、塩除
去率が30〜70％のRO膜であることを知見した。According to the research conducted by the present inventors, one preferable RO membrane was found to have a salt removal rate of 30 to 70%.
すなわち、食塩とドデシルベンゼンスルホン酸ナトリウ
ム（DBS）と含有する疑似排水を調製し、この疑似排水
中の食塩とDBSのRO膜による除去率を測定したところ、
塩除去率が30〜70％のRO膜が、NOx態窒素の大部分を実
質的に透過させ、且つDBSを実質上透過しないことを知
見したものである。勿論、このようなRO膜の物質透過率
（除去率）は、使用するRO膜の運転条件、特に使用する
運転圧力によって大いに影響されるので、適切な運転条
件の設定も重要である。このような運転条件に関する本
発明者の詳細な検討によれば、RO膜の通常の運転圧力は
モジュール入側が20〜50kgf/cm2であるが、運転圧力と
して通常の圧力より低い圧力、例えば３〜5kgf/cm2のモ
ジュール入側圧力を採用するときは、DBS等の中〜高分
子量の除去率は通常の圧力の場合と殆ど変化しないが、
NOx態窒素等の無機塩等の透過率は著しく大となり、従
ってこのような運転条件を採用することによって、NOx
態窒素を殆ど透過させ、且つ種々の夾雑物を十分に除去
できることを見い出した。That is, when pseudo drainage containing sodium chloride and sodium dodecylbenzenesulfonate (DBS) was prepared and the removal rate of the salt and DBS in the pseudo drain by the RO membrane was measured,
It has been found that an RO membrane having a salt removal rate of 30 to 70% substantially permeates most of NOx-state nitrogen and substantially does not permeate DBS. Of course, the substance permeability (removal rate) of such an RO membrane is greatly influenced by the operating conditions of the RO membrane used, particularly the operating pressure used, so that it is also important to set appropriate operating conditions. According to a detailed study by the present inventor regarding such operating conditions, the normal operating pressure of the RO membrane is 20 to 50 kgf / cm 2 on the module inlet side, but the operating pressure is lower than the normal pressure, for example, 3 When a module inlet pressure of ~ 5 kgf / cm 2 is adopted, the removal rate of medium to high molecular weight such as DBS is almost the same as that under normal pressure.
The permeability of inorganic salts such as NOx-like nitrogen becomes remarkably high. Therefore, by adopting such operating conditions, NOx
It has been found that most of the nitrogen is permeable and various impurities can be sufficiently removed.
尚、上記の如き運転条件によっても、NOx態窒素はRO膜
によってある程度、例えば５〜15％程度は除去されるの
で、あらかじめRO膜等のNOx態窒素除去率を求めておい
て、紫外吸光度による実際のNOx態窒素濃度分析値を補
正することが望ましい。Even under the above operating conditions, the NOx-nitrogen is removed to some extent by the RO membrane, for example, about 5 to 15%. It is desirable to correct the actual NOx nitrogen concentration analysis value.
次に本発明を第２に特徴づける点は、上記の如くのRO膜
および／またはUF膜により前処理した検水を紫外吸光度
法によって検水中のNOx態窒素濃度を直接定量分析する
点である。The second feature of the present invention is that the NOx-state nitrogen concentration in the test water is directly quantitatively analyzed by the ultraviolet absorption method for the test water pretreated by the RO membrane and / or the UF membrane as described above. .
紫外吸光度法による水中の窒素化合物を定量分析する方
法自体は公知であり、例えば、従来の方法では、検水中
の窒素化合物を定量分析する場合には、まず検水にアル
カリ性ペルオキソ二硫酸カリウム等の酸化剤を加えて、
検水中の窒素化合物をすべて硝酸イオンに変化させ、波
長210〜230nmの紫外線の吸光度を測定し、NOx態窒素濃
度を算出するものである。The method itself for quantitatively analyzing nitrogen compounds in water by the ultraviolet absorption method is known, and, for example, in the conventional method, when quantitatively analyzing nitrogen compounds in test water, first, in the test water, alkaline potassium peroxodisulfate, etc. Add an oxidant,
The nitrogen compounds in the test water are all changed to nitrate ions, the absorbance of ultraviolet rays having a wavelength of 210 to 230 nm is measured, and the NOx-state nitrogen concentration is calculated.
しかしながら、本発明における紫外吸光度法の利用は、
上記の従来方法と異なり、検水中の全窒素化合物を定量
分析するものではなく、検水中のNOx態窒素濃度のみを
定量分析するものであるので、検水を予め酸化処理する
必要はなく、また前述の通り、検水中の妨害物質は予め
RO膜および／またはUF膜により実質的に除去されている
ため、直ちに紫外線の吸光度からNOx態窒素濃度を求め
ることができる点に特徴がある。However, the use of the ultraviolet absorption method in the present invention is
Unlike the above-mentioned conventional method, it does not quantitatively analyze all nitrogen compounds in the test water, but only quantitatively analyzes the NOx nitrogen concentration in the test water, so there is no need to oxidize the test water in advance, and As mentioned above, the interfering substances in the test water are
Since it is substantially removed by the RO membrane and / or the UF membrane, it is characterized in that the NOx nitrogen concentration can be immediately obtained from the absorbance of ultraviolet rays.
特に好ましい方法は、210〜230nmの波長の吸光度を測定
することであり、最も好ましい波長は220nmであり、こ
の220nm付近では共存する他の無機塩の妨害が少ないた
め良好な測定結果を得ることができる。A particularly preferable method is to measure the absorbance at a wavelength of 210 to 230 nm, the most preferable wavelength is 220 nm, and in the vicinity of this 220 nm, it is possible to obtain good measurement results because there is little interference with other inorganic salts that coexist. it can.
前処理した検水中に溶解した有機物が殆ど存在しない場
合には、上記の特定波長の吸光度の測定によって十分に
信頼できる値を得ることができるが、前処理した検水中
に低分子量の有機物等の妨害物質がある程度存在する場
合には、これらの有機物等は250〜270nmの波長において
吸収を示すため、波長210〜230nmの吸光度と波長250〜2
70nmの吸光度の両方を測定し、下記式に従ってNOx態窒
素濃度の測定値を補正することによって正確なNOx態窒
素濃度を求めることができる。When there is almost no dissolved organic matter in the pretreated test water, a sufficiently reliable value can be obtained by measuring the absorbance at the above-mentioned specific wavelength. When some interfering substances are present, these organic substances and the like absorb at a wavelength of 250 to 270 nm, so the absorbance at a wavelength of 210 to 230 nm and the wavelength of 250 to 2
An accurate NOx-state nitrogen concentration can be obtained by measuring both the absorbance at 70 nm and correcting the measured value of the NOx-state nitrogen concentration according to the following formula.
NOx態窒素濃度（mg/）＝（E1−E2×ａ）×Ｋ ここでElは波長210〜230nmの吸光度であり、E2は波長25
0〜270nmの吸光度であり、ａは試料中の有機物のE1/E2
であり、且つＫはNOx態窒素の波長210〜230nmにおける
係数である。NOx nitrogen concentration (mg /) = (E1−E2 × a) × K where El is the absorbance at a wavelength of 210 to 230 nm and E2 is a wavelength of 25
The absorbance is 0 to 270 nm, and a is E1 / E2 of organic matter in the sample.
And K is a coefficient of NOx nitrogen at a wavelength of 210 to 230 nm.
本発明のNOx態窒素濃度の定量分析方法は、以上の如
く、検水を予めRO膜および／またはUF膜により前処理す
ること、およびこのように定量分析した検水を紫外吸光
度法により、検水の酸化処理を行うことなく直接NOx態
窒素濃度を定量分析することを主たる特徴とするもので
あり、それら以外の各種操作は従来方法におけると同様
でよい。As described above, the method for quantitative analysis of NOx nitrogen concentration according to the present invention comprises pretreating the test water with an RO membrane and / or UF membrane in advance, and detecting the test water quantitatively analyzed in this way by an ultraviolet absorption method. The main feature is that the NOx nitrogen concentration is directly quantitatively analyzed without oxidizing the water, and other various operations may be the same as in the conventional method.
本発明の第２の発明は、検水の前処理部の妨害物質の分
離機器として上述の通りのRO膜および／またはUF膜を有
する装置を使用し、且つNOx態窒素濃度の測定部として
上述の如き紫外吸光度測定装置を使用し、これらを組合
せたことを特徴としているものであり、その他の構成は
いずれの従来のNOx態窒素濃度の分析装置と同様でよい
ものである。The second invention of the present invention uses an apparatus having the RO membrane and / or UF membrane as described above as a device for separating interfering substances in the pretreatment unit of the test water, and as the measuring unit for the NOx nitrogen concentration, It is characterized by using an ultraviolet absorption measuring device such as the one described above and combining them, and other constitutions may be the same as any of the conventional analyzers for NOx nitrogen concentration.
（作用・効果） 以上の如き本発明のNOx態窒素濃度の定量分析方法およ
び装置によれば、検水の前処理が極めて容易であり、且
つ容易に各種妨害物質を除去することができる。また、
前処理した検水の紫外吸光度法によるNOx態窒素濃度の
定量分析においては、従来技術の如き煩雑な分析試薬の
使用や測定条件の設定が不要であり、前処理した検水の
紫外吸光度を測定するのみで容易に且つ迅速に検水中の
NOx態窒素濃度を定量することができるものである。(Operation / Effect) According to the method and apparatus for quantitative analysis of NOx nitrogen concentration of the present invention as described above, pretreatment of test water is extremely easy and various interfering substances can be easily removed. Also,
In the quantitative analysis of NOx nitrogen concentration by the UV absorption method of pretreated test water, it is not necessary to use complicated analytical reagents and setting of measurement conditions as in the prior art, and the UV absorbance of pretreated test water can be measured. Simply and quickly
It is possible to quantify the NOx nitrogen concentration.
従って本発明の定量分析方法および装置は、一般の排水
その他の水質検査に有用であるばかりでなく、特に活性
汚泥を使用する排水処理設備のNOx態窒素濃度の制御機
器として有用である。例えば、本発明のNOx態窒素濃度
の定量分析方法および装置を排水処理設備の曝気槽中の
NOx態窒素濃度の制御機器として利用することにより、
これらの排水処理設備の自動制御が実現できる。このこ
とは、従来のNOx態窒素濃度の定量分析方法では、検水
の前処理およびNOx態窒素濃度の測定にあたり、種々の
繁雑な作業が要求されるため、いずれもかなりの分析時
間を要し、曝気槽中のNOx態窒素濃度の変化を直ちに把
握できなかったのに対し、本発明のNOx態窒素濃度の定
量分析方法および装置によれば曝気槽中のNOx態窒素濃
度の定量分析に殆ど時間を要せず、刻々と曝気槽中のNO
x態窒素濃度の変化を把握できることによる。Therefore, the quantitative analysis method and apparatus of the present invention are not only useful for general water and other water quality inspections, but also particularly useful as NOx nitrogen concentration control equipment for wastewater treatment equipment that uses activated sludge. For example, the method and apparatus for quantitative analysis of NOx nitrogen concentration of the present invention can be applied to an aeration tank of wastewater treatment equipment.
By using it as a NOx nitrogen concentration control device,
Automatic control of these wastewater treatment facilities can be realized. This means that in the conventional quantitative analysis method for NOx nitrogen concentration, various complicated work is required for pretreatment of sample water and measurement of NOx nitrogen concentration. While the change in the NOx-type nitrogen concentration in the aeration tank could not be immediately grasped, the method and apparatus for quantitative analysis of the NOx-state nitrogen concentration of the present invention showed that almost no quantitative analysis of the NOx-state nitrogen concentration in the aeration tank was made. NO in the aeration tank moment by moment
This is because it is possible to understand the change in x-nitrogen concentration.
従って、本発明の方法および装置を排水処理設備の制御
機器として使用することにより、曝気槽中のNOx態窒素
濃度を常に適正な値に制御して、曝気槽の適切な曝気時
間、曝気の中断時間、適当な水素供与体の添加量等が容
易に設定できるため、排水処理における排水浄化効率が
著しく改善され、且つ使用薬剤やランニングコストの大
幅な節減が実現される。Therefore, by using the method and apparatus of the present invention as a control device for wastewater treatment equipment, the NOx nitrogen concentration in the aeration tank is always controlled to an appropriate value, and an appropriate aeration time of the aeration tank and interruption of aeration. Since the time, an appropriate amount of hydrogen donor added, etc. can be easily set, the efficiency of wastewater purification in wastewater treatment is significantly improved, and the chemicals used and the running cost are significantly reduced.
次に実施例を挙げて本発明を更に具体的に説明する。
尚、文中、％とあるのは特に断りのない限り重量基準で
ある。Next, the present invention will be described more specifically with reference to examples.
In the text,% is based on weight unless otherwise specified.
実施例１ 第１図に図解的に示す如く、紫外吸光度法による分光光
度計３と制限曝気式排水処理設備（処理能力2m3/回のパ
イロットプラント）の曝気槽１との間に、塩除去率が50
％のRO膜を有する前処理装置２を設置および連結し、本
発明のNOx態窒素濃度定量分析装置とした。この分析装
置を有する制限曝気式排水処理設備によって、下水を対
象とした連続通水試験を実施した。Example 1 As shown schematically in FIG. 1, salt removal was performed between the spectrophotometer 3 by the ultraviolet absorption method and the aeration tank 1 of the restricted aeration type wastewater treatment equipment (processing capacity 2 m 3 / pilot plant). Rate 50
A pretreatment device 2 having a% RO membrane was installed and connected to obtain a NOx nitrogen concentration quantitative analysis device of the present invention. A continuous water flow test for sewage was carried out by the restricted aeration type wastewater treatment facility having this analyzer.
検水は、第１図ポンプＰ−１にて曝気槽１より採水し、
塩除去率50％のRO膜２へと供給される。この時の運転圧
力はモジュール入側が5kgf/cm2、出側が4.5kgf/cm2であ
る。透過水は次工程へと進み、非透過水は曝気槽１へ戻
される。透過水の一部をポンプＰ−２にて採水し、これ
にポンプＰ−３よりpH調整用の1N−HClおよびポンプＰ
−４より稀釈水を供給し、混合されて分光光度計３へと
導かれる。検水の紫外吸光度は前述の演算方法によりNO
x態窒素濃度に換算され記録計４に記録される。The test water is taken from the aeration tank 1 by the pump P-1 shown in FIG.
It is supplied to the RO membrane 2 having a salt removal rate of 50%. Operating pressure in this module inlet side 5 kgf / cm 2, the exit side is 4.5 kgf / cm 2. The permeated water proceeds to the next step, and the non-permeated water is returned to the aeration tank 1. A part of the permeated water is sampled by the pump P-2, and 1N-HCl for adjusting the pH and the pump P are supplied from the pump P-3.
The diluted water is supplied from -4, mixed, and led to the spectrophotometer 3. The UV absorbance of the test water is NO according to the above calculation method.
Converted to x-nitrogen concentration and recorded in recorder 4.
１サイクル時における本発明方法および装置により定量
分析されたNOx態窒素濃度の値と従来法による手分析値
の相関関係を第２図に示す。第２図に示す通り従来法に
よる値（縦軸、mg/）の方が本発明による値（横軸、m
g/）より５〜15％程度高い値を示しているが、これは
RO膜２によるNOx態窒素の除去分を考慮していないため
であり、RO膜２によるNOx態窒素の除去率を10％として
補正することにより、手分析値とよく一致した値とな
る。FIG. 2 shows the correlation between the NOx-state nitrogen concentration value quantitatively analyzed by the method and apparatus of the present invention during one cycle and the manual analysis value by the conventional method. As shown in FIG. 2, the value by the conventional method (vertical axis, mg /) is the value by the present invention (horizontal axis, m
It is about 5 to 15% higher than g /), but this is
This is because the amount of NOx-state nitrogen removed by the RO membrane 2 is not taken into consideration, and by correcting the NOx-state nitrogen removal rate by the RO membrane 2 to 10%, a value that is in good agreement with the manual analysis value is obtained.
このパイロットプラントは回分式であり、曝気工程３時
間の後メタノール添加および嫌気攪拌工程1.5時間をも
って脱窒素を行うものであるが、本発明によるNOx態窒
素濃度定量分析方法および装置を用い、曝気終了時のNO
x態窒素濃度を定量分析し、これに相当する量のメタノ
ールを添加した。その結果、安定した窒素処理および有
機物の処理が達成された。This pilot plant is a batch type and performs denitrification with methanol addition and anaerobic stirring step 1.5 hours after aeration step 3 hours. Using the NOx nitrogen concentration quantitative analysis method and apparatus according to the present invention, aeration is completed. NO of time
The x-nitrogen concentration was quantitatively analyzed, and a corresponding amount of methanol was added. As a result, stable nitrogen treatment and organic matter treatment were achieved.
第１図は本発明のNOx態窒素濃度定量分析方法および装
置を図解的に示し、第２図は本発明方法によるNOx態窒
素濃度の定量分析値および手分析によるNOx態窒素濃度
の定量分析値を示す。 1;曝気槽 2;検水前処理装置 3;分光光度計 4;記録計 P1〜4;ポンプFIG. 1 schematically shows the NOx-type nitrogen concentration quantitative analysis method and device of the present invention, and FIG. 2 shows the NOx-state nitrogen concentration quantitative analysis value by the method of the present invention and the NOx-state nitrogen concentration quantitative analysis value by manual analysis. Indicates. 1; Aeration tank 2; Water sample pretreatment device 3; Spectrophotometer 4; Recorder P1-4; Pump
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 昭61−18135（ＪＰ，Ａ) 特開 昭55−65139（ＪＰ，Ａ) 実開 昭56−151951（ＪＰ，Ｕ) ─────────────────────────────────────────────────── ─── Continuation of the front page (56) References JP 61-18135 (JP, A) JP 55-65139 (JP, A) JP 56-151951 (JP, U)
Claims (4)
び／または亜硝酸性窒素（以下NOx態窒素という）を含
有する曝気槽混合液中のNOx態窒素濃度を紫外吸光光度
法により定量分析する方法において、定量分析前に曝気
槽混合液中の妨害物質を、NOx態窒素を実質的に透過す
る逆浸透膜（以下RO膜という）および／または限外透過
膜（以下UF膜という）により除去した後、得られた透過
水中のNOx態窒素を定量分析することを特徴とするNOx態
窒素の定量分析方法。1. A quantitative analysis of NOx nitrogen concentration in an aeration tank mixture containing nitrate and / or nitrite nitrogen (hereinafter referred to as NOx nitrogen) in the aeration tank in the activated sludge method by an ultraviolet absorptiometry. In the method described above, the interfering substances in the aeration tank mixed solution are analyzed by a reverse osmosis membrane (hereinafter referred to as RO membrane) and / or an ultrapermeable membrane (hereinafter referred to as UF membrane) that substantially permeate NOx-nitrogen before quantitative analysis. A method for quantitative analysis of NOx-state nitrogen, which comprises quantitatively analyzing NOx-state nitrogen in the obtained permeated water after removal.
許請求の範囲第（１）項に記載の定量分析方法。2. The quantitative analysis method according to claim 1, wherein the RO membrane is an RO membrane having a salt removal rate of 30 to 70%.
許請求の範囲第（１）項に記載の定量分析方法。3. The quantitative analysis method according to claim 1, wherein the operating pressure of the RO membrane is 3 to 5 Kgf / cm 2 .
光光度および波長250〜270nmの紫外吸光光度を測定し、
これらの測定値から曝気槽混合液中のNOx態窒素濃度を
求める特許請求の範囲第（１）項に記載の定量分析方
法。4. The ultraviolet absorptivity of wavelength 210 to 230 nm and the ultraviolet absorptivity of wavelength 250 to 270 nm of the aeration tank mixture are measured,
The quantitative analysis method according to claim (1), wherein the NOx nitrogen concentration in the aeration tank mixture is calculated from these measured values.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60210289A JPH0723867B2 (en) | 1985-09-25 | 1985-09-25 | Quantitative analysis method for NOx nitrogen |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60210289A JPH0723867B2 (en) | 1985-09-25 | 1985-09-25 | Quantitative analysis method for NOx nitrogen |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6270734A JPS6270734A (en) | 1987-04-01 |
| JPH0723867B2 true JPH0723867B2 (en) | 1995-03-15 |
Family
ID=16586930
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP60210289A Expired - Lifetime JPH0723867B2 (en) | 1985-09-25 | 1985-09-25 | Quantitative analysis method for NOx nitrogen |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0723867B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102391262B1 (en) | 2017-11-28 | 2022-04-28 | 오르가노 가부시키가이샤 | Element analysis method and analysis device |
| CN112179858A (en) * | 2020-09-22 | 2021-01-05 | 杭州启绿科技有限公司 | Water quality detection method based on turbidity compensation technology |
| CN112461774A (en) * | 2020-11-20 | 2021-03-09 | 杭州绿洁环境科技股份有限公司 | Turbidity compensation method for total nitrogen analyzer |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5330379A (en) * | 1976-09-01 | 1978-03-22 | Agency Of Ind Science & Technol | Measurement of inorganic form nitrogen |
| JPS6019452B2 (en) * | 1978-11-10 | 1985-05-16 | 株式会社堀場製作所 | Nitrate/nitrite ion concentration measurement method and device |
| JPS56151951U (en) * | 1980-04-14 | 1981-11-13 |
-
1985
- 1985-09-25 JP JP60210289A patent/JPH0723867B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6270734A (en) | 1987-04-01 |
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