JPS6171355A - Analyzing method of phosphoric acid - Google Patents
Analyzing method of phosphoric acidInfo
- Publication number
- JPS6171355A JPS6171355A JP19362884A JP19362884A JPS6171355A JP S6171355 A JPS6171355 A JP S6171355A JP 19362884 A JP19362884 A JP 19362884A JP 19362884 A JP19362884 A JP 19362884A JP S6171355 A JPS6171355 A JP S6171355A
- Authority
- JP
- Japan
- Prior art keywords
- acid
- pipe
- cell
- phosphoric acid
- supplied
- 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.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Description
【発明の詳細な説明】
本発明は、検水中のリン酸を定量的に測定するリン酸の
分析方法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a phosphoric acid analysis method for quantitatively measuring phosphoric acid in sample water.
在米上り、リン酸を分析する方法としてもモリブデンブ
ルー法がある。この方法では、検水中に硫酸を添加して
ｐＨ１程とした後、たとえばモリブデン酸アンモニウム
を添加したｉ＄ｌ！整液に７スコビン酸あるいは２価の
塩化スズ５ｎＣ１２などの還元剤を添加し、約２０分間
加熱してモリブデンブルーの青色の呈色を生じさせる。The molybdenum blue method is also used to analyze phosphoric acid in the United States. In this method, sulfuric acid is added to the sample water to adjust the pH to about 1, and then, for example, ammonium molybdate is added. A reducing agent such as 7scobic acid or divalent tin chloride 5nC12 is added to the solution, and the mixture is heated for about 20 minutes to produce a molybdenum blue color.
この呈色液の吸光度を測定することによってリン酸濃度
の定量が行なわれていた。しかしこのような定量方法で
は、黄色いリンモリブデン酸の生成が遅く、前記の加熱
の条件たとえば加熱温度や加熱時間の僅かな違いによっ
てモリブデンブルーの呈色が不均一になる。さらにアス
コビン酸などの還元剤が能力が低下し、１日程度で試薬
の作り替えを行なわなければならないので、連続分析に
は不適である。The phosphoric acid concentration was determined by measuring the absorbance of this colored liquid. However, in such a quantitative method, the production of yellow phosphomolybdic acid is slow, and the coloration of molybdenum blue becomes uneven due to slight differences in the heating conditions, such as heating temperature and heating time. Furthermore, the ability of reducing agents such as ascobic acid decreases, and the reagent must be replaced every day or so, making it unsuitable for continuous analysis.
本発明の目的は、迅速かつ正確にリン酸量を連続的に定
量することができるリン酸の分析方法を提供することで
ある。An object of the present invention is to provide a method for analyzing phosphoric acid that can rapidly and accurately continuously quantify the amount of phosphoric acid.
図面は、本発明に従って構成される分析装置の一実施例
を示す簡略化した系統図である。リン酸の分析装置は、
定量ポンプＰｉ、Ｐ２．Ｐ３．Ｐ４と反応槽１とカラム
２と吸光光度計３とを備える。The drawing is a simplified system diagram showing one embodiment of an analysis device constructed in accordance with the present invention. The phosphoric acid analyzer is
Metering pump Pi, P2. P3. It is equipped with P4, a reaction tank 1, a column 2, and an absorption photometer 3.
リン酸の定量が行なわれる検水と、モリブデン酸化合物
を溶かした硫酸酸性溶液と、有は溶媒であるエタノール
とが反応槽１内で混合さｈる。検水は、定量ポンプＰ１
によって吸入管５を介して一定流量吸入され、管路６を
介して反応ＷＪ１に供給される。モリブデン酸化合物を
溶かした硫酸酸性溶液は、定量ポンプＰ２によって吸入
管７を介して一定流量吸入され、管路８を介して反応Ｗ
ｉ１に供給される。モリブデン酸化合物を溶かした硫酸
酸性Ｓａは、たとえば濃度１２規定の硫酸にモリブデン
酸化合物を濃度が２モルになるように溶かしたものであ
る。モリブデン酸化合物は、たとえばモリブデン陵アン
モニウムあるいはモリブデン酸カリなどである。エタノ
ールは、定量ポンプ３によって吸入管９を介して一定流
量吸入され、管路１０を介して叉応槽１に供給される。A sample water in which phosphoric acid is to be determined, an acidic sulfuric acid solution in which a molybdic acid compound is dissolved, and ethanol, which is a solvent, are mixed in a reaction tank 1. For water testing, metering pump P1
A constant flow rate is sucked in through the suction pipe 5 and supplied to the reaction WJ1 through the pipe line 6. A sulfuric acid acidic solution containing a molybdate compound dissolved therein is sucked in at a constant rate via a suction pipe 7 by a metering pump P2, and is passed through a pipe 8 to a reaction W.
i1. The sulfuric acid acidic Sa in which a molybdate compound is dissolved is, for example, a molybdate compound dissolved in sulfuric acid with a concentration of 12N to a concentration of 2 molar. The molybdate compound is, for example, ammonium molybdate or potassium molybdate. Ethanol is sucked in at a constant flow rate by the metering pump 3 through the suction pipe 9, and is supplied to the reaction tank 1 through the pipe line 10.
検水と、モリブデン酸化合物を溶かした硫酸酸性溶液と
、エタ／−ルとの混合の割合はたとえば２０ ：２ ：
５である１反応′Ｗ１１には、スターテ１５が設置され
る。スターテ１５は、モータ２Ｇによって回転する。検
水と、モリブデン酸化合物を溶かした硫酸酸性溶液と、
エタノールとの混合溶液１２は、反応ｆｆ１ｌ内におい
てスターテ１５によって攪拌され、その混合溶液１２は
酸性となり、黄色−１リンモリブデン酸を生じる。リン
モリブデン酸の生成は、エタ／−ルによって加速され、
たとえば約１分ぐらいで生成される。さらにリンモリブ
デン酸の生成量は、従来ではリン酸の１０％が黄色シ１
リンモリブデン酸として生成するが、本発明によると約
５０％の生成量である。The mixing ratio of sample water, sulfuric acid acidic solution containing a molybdate compound, and ethanol is, for example, 20:2:
A starter 15 is installed in 1 reaction 'W11 which is 5. The starter 15 is rotated by the motor 2G. A water sample, a sulfuric acid solution containing a molybdate compound,
The mixed solution 12 with ethanol is stirred by the starter 15 in the reaction ff1l, and the mixed solution 12 becomes acidic to produce yellow-1-phosphomolybdic acid. The formation of phosphomolybdic acid is accelerated by ethanol,
For example, it will be generated in about 1 minute. Furthermore, the amount of phosphomolybdic acid produced is conventionally 10% yellowish.
It is produced as phosphomolybdic acid, and according to the present invention, the production amount is about 50%.
生成した黄色いリンモリブデン酸を含む混合浴８１１２
は、定量ポンプＰ４によって１分間に２ｍｌの割合で吸
入管１１を介して吸入され、管路１２を介してカラム２
に送られる。カラム２は、円柱状のガラス製であり、た
とえば内径が４１１−φ、長さが２０ｃ曽であろ、カラ
ム２内には、１−鋤φ程度の球状の金属還元Ｍなと乏は
ニッケルが充填される。カラム２に送られた黄色いリン
モリブデン酸は、カラム２内を流過し、カラム２内に充
填された金属還元剤によって還元され青色を呈する。生
成した物質の維成は不明であるが、モリブデンブルーと
呼ばれる。その生成はリン酸の濃度に比例するので、生
成したモリブデンブルーの呈色液を管路１３を介して吸
光光度計３に導入し、波長８１０ｍ−で吸光度を測定す
ることによって検水中のリン酸の定量分析を行なう。Mixed bath 8112 containing produced yellow phosphomolybdic acid
is inhaled through the suction pipe 11 at a rate of 2 ml per minute by the metering pump P4, and is injected into the column 2 through the pipe line 12.
sent to. Column 2 is made of cylindrical glass, and may have an inner diameter of 411 mm and a length of 20 cm. Inside column 2, there is a spherical metal reduction M of about 1 mm diameter and nickel. Filled. The yellow phosphomolybdic acid sent to column 2 flows through column 2 and is reduced by the metal reducing agent packed in column 2, giving it a blue color. Although the nature of the substance produced is unknown, it is called molybdenum blue. Since its production is proportional to the concentration of phosphoric acid, the produced molybdenum blue colored liquid is introduced into the spectrophotometer 3 through the pipe 13, and the absorbance is measured at a wavelength of 810 m. Perform quantitative analysis of
混合溶液が、カラム２を流過する際、混合５ｗＬ１２に
はエタノールが混入それているので、金属還元剤たとえ
ばニッケルによる還元が可能となる。When the mixed solution flows through the column 2, since ethanol is mixed into the mixed solution 5wL12, reduction with a metal reducing agent such as nickel becomes possible.
すなわち混合浴ｗ１．１２は酸性であるので金属還元剤
を入れると水素が発生するが、エタノールにより水素の
発生が抑えられる。That is, since the mixed bath w1.12 is acidic, hydrogen is generated when a metal reducing agent is added, but ethanol suppresses the generation of hydrogen.
リン酸の定を分析を終了した後、反応′Ｗｉｌ内に残る
混合浴７１１１２は定量ポンプＰ４によって吸入され、
管路１２を介してカラム２に送らずに排液を行なう、そ
の後、分析装置は蒸留水によって洗浄が行なわれる。After finishing the analysis of the phosphoric acid concentration, the mixed bath 71112 remaining in the reaction 'Wil is sucked by the metering pump P4,
After draining without sending to column 2 via line 12, the analyzer is rinsed with distilled water.
このようにして迅速かつ連続的にリン酸の定量分析が行
なえる。In this way, quantitative analysis of phosphoric acid can be performed rapidly and continuously.
上述の実施例はカラム２内を流過することによって還元
するようにしでいたが、カラム２を設けずにリンモリブ
デン酸を含む混合浴？［！１２に粉末状の金属還元剤た
とえばニッケルなどを添加して還元するようにしてもよ
い、さらにエタノールに代えて他の有機溶媒が用いられ
てもよい。In the above embodiment, the reduction was carried out by flowing through the column 2, but it is possible to use a mixed bath containing phosphomolybdic acid without providing the column 2. [! A powdered metal reducing agent such as nickel may be added to 12 for reduction.Furthermore, other organic solvents may be used in place of ethanol.
以上のように本発明によれば、検水に硫酸溶液とモリブ
デン酸塩との混合液を加えて酸性溶液にする際、有機溶
媒を加えるようにしたので、黄色いリンモリブデン酸の
生成が速くなり、生成量が多くなる。そのことによって
迅速かつ正確にリン酸の定量分析が行なえるようになる
。さらに有機溶媒を加えることによって金Ｓ還元剤を使
用することができるので７スコビン酸などの還元剤のよ
うに１日程度で試薬の作り替元を行なわなくてもよく、
連続分析が可能になる。As described above, according to the present invention, an organic solvent is added when adding a mixture of a sulfuric acid solution and a molybdate salt to a sample water to make it an acidic solution, which speeds up the production of yellow phosphomolybdic acid. , the amount of production increases. This allows rapid and accurate quantitative analysis of phosphoric acid. Furthermore, since the gold S reducing agent can be used by adding an organic solvent, there is no need to change the reagent source every day or so, unlike reducing agents such as 7scobic acid.
Continuous analysis becomes possible.
【図面の簡単な説明】
図面は、本発明に従って溝成される分析装置の一実施例
を示す簡略化した系統図である。BRIEF DESCRIPTION OF THE DRAWINGS The drawing is a simplified system diagram showing one embodiment of an analytical device constructed according to the present invention.
Claims (1)
検水に混合して酸性にした後、その混合溶液中に生じた
黄色いリンモリブデン酸を金属還元剤によって還元し、
モリブデンブルーに呈色された混合溶液の吸光度を測定
することによってリン酸の定量を行なうことを特徴とす
るリン酸の分析方法。After making the test water acidic by mixing an acidic solution containing a molybdenum compound and an organic solvent, the yellow phosphomolybdic acid produced in the mixed solution is reduced with a metal reducing agent.
A method for analyzing phosphoric acid, which comprises quantifying phosphoric acid by measuring the absorbance of a mixed solution colored molybdenum blue.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19362884A JPS6171355A (en) | 1984-09-14 | 1984-09-14 | Analyzing method of phosphoric acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19362884A JPS6171355A (en) | 1984-09-14 | 1984-09-14 | Analyzing method of phosphoric acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6171355A true JPS6171355A (en) | 1986-04-12 |
Family
ID=16311100
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19362884A Pending JPS6171355A (en) | 1984-09-14 | 1984-09-14 | Analyzing method of phosphoric acid |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6171355A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0634646A1 (en) * | 1993-07-14 | 1995-01-18 | Shimadzu Corporation | Method of and apparatus for analyzing nitrogen compounds and phosphorus compounds contained in water |
| KR100816657B1 (en) | 2006-11-24 | 2008-03-26 | 테크노세미켐 주식회사 | Method for quantitatively analyzing mixed acid liquid |
| JP2008185363A (en) * | 2007-01-26 | 2008-08-14 | Shimane Univ | Simplified determination method and simplified determination measuring instrument of underwater environmental pollutant |
-
1984
- 1984-09-14 JP JP19362884A patent/JPS6171355A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0634646A1 (en) * | 1993-07-14 | 1995-01-18 | Shimadzu Corporation | Method of and apparatus for analyzing nitrogen compounds and phosphorus compounds contained in water |
| US5567621A (en) * | 1993-07-14 | 1996-10-22 | Shimadzu Corporation | Method of and apparatus for analyzing nitrogen compound and phosphorus compound contained in water |
| KR100816657B1 (en) | 2006-11-24 | 2008-03-26 | 테크노세미켐 주식회사 | Method for quantitatively analyzing mixed acid liquid |
| JP2008185363A (en) * | 2007-01-26 | 2008-08-14 | Shimane Univ | Simplified determination method and simplified determination measuring instrument of underwater environmental pollutant |
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