JPS58180949A - Analysis of phosphoric acid - Google Patents
Analysis of phosphoric acidInfo
- Publication number
- JPS58180949A JPS58180949A JP6413482A JP6413482A JPS58180949A JP S58180949 A JPS58180949 A JP S58180949A JP 6413482 A JP6413482 A JP 6413482A JP 6413482 A JP6413482 A JP 6413482A JP S58180949 A JPS58180949 A JP S58180949A
- Authority
- JP
- Japan
- Prior art keywords
- solution
- acid
- phosphoric acid
- heteropolyacid
- molybdenum
- 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
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/22—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Molecular Biology (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Biophysics (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (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敏的＃１１１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 determining phosphoric acid in sample water using a method of #111 determination.
成る先行技術では、検水中のリン酸の分析において、検
水中に硫酸を添加してｐ Ｈ１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調１１ｉＫアスコル
ビンＮＩあるいは二価の塩化スズ５ｎＣ７２などの還元
剤を添加し、約２０分間加熱してモリブデングルーの青
色の呈色を生じさせる。この呈色液の吸光省を測定する
ことによって、リン酸ｌｌ！Ｉ廖の定量が行なわれてい
た。しかし、この定敵方法では、還元に長時間を要し、
前記加熱の条件たとえば加熱＠嗜や加熱時間のわずかの
違いＫよって、モリブデン酸Ｖ−の呈色が不均一になる
とともに、得られたモリブデンブルーの吸光係数が小さ
いので吸光省測定時の検出感廖が劣る欠点がある。In the prior art, in the analysis of phosphoric acid in a sample water, sulfuric acid is added to the sample water to bring the pH to about 1, and then a reducing agent such as 11iK ascorbin NI or divalent tin chloride 5nC72 to which ammonium molybdate is added is added. The molybdenum glue is added and heated for about 20 minutes to produce the blue coloration of the molybdenum glue. By measuring the absorbance of this colored liquid, phosphoric acid ll! Quantification of I Liao was being carried out. However, with this fixed enemy method, it takes a long time to return
Due to the above-mentioned heating conditions, e.g. heating@temperature or slight difference in heating time, the coloration of molybdic acid V- becomes non-uniform, and the absorption coefficient of the obtained molybdenum blue is small, resulting in poor detection sensitivity during absorption measurement. There is a disadvantage that Liao is inferior.
また、他の先行技術のリン酸の分析は、前述の先行技術
で述べた調整液を電解上ｋに導入し、その櫨元電流値を
測定するいわゆる電量分析によって行なわれた。この方
法では、還元電流値の検出感零が劣り、そのためリン酸
の定量値の信頼性が劣る。In another prior art analysis of phosphoric acid, the adjustment solution described in the prior art described above was introduced into an electrolytic solution and the current value was measured by so-called coulometric analysis. In this method, the detection sensitivity of the reduction current value is poor, and therefore the reliability of the quantitative value of phosphoric acid is poor.
本発明の目的は、このような先行技術の問題点を解決し
て、操作が簡単であり、迅速かつ正確にリン酸量を定置
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 solve the problems of the prior art and provide a method for analyzing phosphoric acid that is easy to operate and can quickly and accurately determine the amount of phosphoric acid.
第１図は、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
、定置ポンプ２，５．１０と、ミキシンゲジョイント３
．８と、カラム１８と、電解セＡ／１５と、吸光光賓計
１７とを備える。検水ｌは、定量ポンプ２によって一定
流量吸入され、ミキシングジヨイント８に管路４を介し
て送られ、定量ポンプ５によって管路６を介して供給さ
れる１２規定硫酸酸性溶液７と、ミキシングジヨイント
３内で混合され、約ｐＨ１に調整される。ミキシングジ
ヨイント８では、管路９を介して送られるその調整され
た酸性溶液と、定量ポンプ１０によって管路１１を介し
て供給されるたとえばモリブデン酸アンモニウム、モリ
ブデン酸カリなどのモリブデン酸塩溶液１２とが混合さ
れる。この混合液は、カラム１８に導入され、カラム１
８内で８価または４価のリンと６価のモリブデンとを含
む黄色のへテロポリ酸を生じる。FIG. 1 is a simplified system diagram showing one embodiment of an analyzer constructed in accordance with the present invention. The phosphoric acid analyzer consists of stationary pumps 2, 5.10 and mixing joint 3.
．． 8, a column 18, an electrolytic cell A/15, and an absorption photometer 17. The test water l is sucked in at a constant flow rate by a metering pump 2 and sent to a mixing joint 8 via a pipe 4, and mixed with a 12N sulfuric acid acidic solution 7 supplied by a metering pump 5 via a pipe 6. Mix in joint 3 and adjust to approximately pH 1. In the mixing joint 8, the adjusted acid solution is sent via line 9 and a molybdate solution 12, for example ammonium molybdate, potassium molybdate, etc., is supplied via line 11 by a metering pump 10. are mixed. This mixture is introduced into column 18, and column 1
A yellow heteropolyacid containing 8- or 4-valent phosphorus and 6-valent molybdenum is produced.
次にこのヘテロ１ＩＪｌ！！！を含む溶液は、管路１４
を介して電解セル１５内に導入される。このＭｔＭセＡ
／１５は、たとえば白金めっきガラスまたは銀めっきガ
ラスなどから形成され九作用電極と、たとえばステンレ
ス鋼製の対極とを有し、両電極間にたとえば２００ ｍ
Ｖの電圧を印加する。これ罠よって電解セＡ／１５内で
、ヘテロポリ酸は、約５秒間で還元されてモリブデンブ
ルーの鮮やかな青色を呈する。この電解セル１５は、市
販の連続電量測定装置によって実現されてもよい。Next is this hetero 1IJl! ! ! The solution containing
It is introduced into the electrolytic cell 15 via. This MtM SEA
/15 has nine working electrodes made of, for example, platinum-plated glass or silver-plated glass, and a counter electrode made of, for example, stainless steel, with a distance of, for example, 200 m between the two electrodes.
Apply a voltage of V. As a result, the heteropolyacid is reduced in about 5 seconds in the electrolytic cell A/15 and exhibits the bright blue color of molybdenum blue. This electrolytic cell 15 may be realized by a commercially available continuous coulometric measuring device.
前記モリブデンプＶ−の呈色液を管路１６を介して吸光
光嗜計１７〜導入して波長７００ ｎｍ付近の吸′ｙｔ
、崖を測定することによって、検水中のリン酸の分析を
行なう。The coloring liquid of molybstarch V- is introduced into the absorption light meter 17 through the pipe 16 to absorb light at a wavelength of around 700 nm.
, conduct the analysis of phosphoric acid in the sample water by measuring the cliff.
第２図は、この吸光光嗜計１７によって測定された結果
を示すグラフである。図中、＊Ｉ！１８で示すように、
波長的７００ ｎＩｎで、モリブデンブルーの青色の吸
収によってピークが表れる。このピーク高さＨの計１１
によってモリブデンブルーの量が求められ、これによっ
てリン酸量が定量される。前述の先行技術で述べたアス
コルビン酸での還元によって得られたモリブデンプＶ−
の呈色液の測定例は、仮想線１９によって示されている
。FIG. 2 is a graph showing the results measured by this absorbance meter 17. In the figure, *I! As shown in 18,
A peak appears at a wavelength of 700 nIn due to blue absorption of molybdenum blue. A total of 11 peak heights H
The amount of molybdenum blue is determined by the method, and the amount of phosphoric acid is determined thereby. Molybstarch V- obtained by reduction with ascorbic acid as described in the above prior art
An example of measurement of a colored liquid is shown by a phantom line 19.
＠２図から明らかなように１先行技術のような還元方法
では、ポリへテロ酸を充分に還元して、モリブデンブル
ーの呈色を生じせしめることが困難なため、吸光嗜のピ
ークは小さい。このため正確なリン酸の定ｔは困難であ
った。これに対して本発明によれば、モリブデンブルー
の吸光係数が大きくなり、吸光簿のピークは大きくなる
ので正確なリン酸の定量が可能である。@2 As is clear from Figure 1, with the reduction method as in the prior art, it is difficult to sufficiently reduce the polyheteroacid to produce a molybdenum blue coloration, so the absorption peak is small. For this reason, it has been difficult to accurately determine phosphoric acid. On the other hand, according to the present invention, the extinction coefficient of molybdenum blue becomes large and the peak of the absorption chart becomes large, so that accurate quantification of phosphoric acid is possible.
本発明によれば、リンとモリブデンのポリへテロ酸の還
元を電解上Ｖを用いて行なうことによって、操作が簡単
であり、モリブデンブルーの青色の呈色を迅速かつ均一
に行なうことが可能となり、この吸光係数の大きいモリ
ブデンプＶ−の呈色液の吸光肴を測定するので、リン酸
の定量を精廖よ〈行なうことが可能となる。しかも、本
発明に従うポリへテロ酸の還元は短時間で完了するので
、検水中のリン酸は、所定時間ごと、あるいは連続的に
分析することが可能である。According to the present invention, by electrolytically reducing the polyheteroacid of phosphorus and molybdenum using V, the operation is simple and it is possible to quickly and uniformly develop the blue color of molybdenum blue. Since the absorbance of the colored solution of molybstarch V-, which has a large extinction coefficient, is measured, it becomes possible to precisely quantify phosphoric acid. Moreover, since the reduction of polyheteroacids according to the present invention is completed in a short time, it is possible to analyze phosphoric acid in sample water at predetermined intervals or continuously.
第１図は、本発明に従って構成される測定装置の一実施
例を示す簡略化した系統図、第２図は第１図に示す吸光
光９計１７によって得られたグラフである。
ｌ・・・検水、２．６．１０・・・定量ポンプ、８．８
・・・ミキシングジヨイント、７・・・１２規定硫峻酸
性溶液、１２・・・モリブデン酸塩溶液、１Ｂ・・・カ
ラム、１５・・・電解セル、１７・・・吸光光廖計代珊
人 弁理士 西教圭一部FIG. 1 is a simplified system diagram showing one embodiment of a measuring device constructed according to the present invention, and FIG. 2 is a graph obtained by using the nine absorbing lights 17 shown in FIG. l... Water test, 2.6.10... Metering pump, 8.8
... Mixing joint, 7 ... 12N sulfuric acid solution, 12 ... Molybdate solution, 1B ... Column, 15 ... Electrolytic cell, 17 ... Absorption light metering cell Person Patent Attorney Kei Nishi
Claims (1)
ンとモリブデンとのヘデロポリ酸を生成させた溶液を電
解セルに導入して還元し、モリブデンブルーに呈色され
た溶液の吸光嗜を測定することによってリン酸の定置を
行なうことを特徴とするリン酸の分析方法。The sample water is acidified with sulfuric acid, a molybdic acid compound is added, a solution of hederopolyic acid of phosphorus and molybdenum is introduced into an electrolytic cell, and reduced, and the absorbance of the solution colored molybdenum blue is measured. A method for analyzing phosphoric acid, which is characterized in that phosphoric acid is placed in place by:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6413482A JPS58180949A (en) | 1982-04-16 | 1982-04-16 | Analysis of phosphoric acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6413482A JPS58180949A (en) | 1982-04-16 | 1982-04-16 | Analysis of phosphoric acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS58180949A true JPS58180949A (en) | 1983-10-22 |
Family
ID=13249293
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP6413482A Pending JPS58180949A (en) | 1982-04-16 | 1982-04-16 | Analysis of phosphoric acid |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS58180949A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4821941B1 (en) * | 2010-07-30 | 2011-11-24 | 三浦工業株式会社 | Determination of total phosphorus |
| WO2012011422A1 (en) * | 2010-07-21 | 2012-01-26 | 三浦工業株式会社 | Method for quantification of total phosphorous |
| WO2012014257A1 (en) * | 2010-07-30 | 2012-02-02 | 三浦工業株式会社 | Total phosphorous quantity determination method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5364094A (en) * | 1976-11-19 | 1978-06-08 | Hitachi Ltd | Analysis of semi-metal and apparatus therefor |
-
1982
- 1982-04-16 JP JP6413482A patent/JPS58180949A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5364094A (en) * | 1976-11-19 | 1978-06-08 | Hitachi Ltd | Analysis of semi-metal and apparatus therefor |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012011422A1 (en) * | 2010-07-21 | 2012-01-26 | 三浦工業株式会社 | Method for quantification of total phosphorous |
| JP2012042450A (en) * | 2010-07-21 | 2012-03-01 | Miura Co Ltd | Quantitative method of total phosphorus |
| CN102472734A (en) * | 2010-07-21 | 2012-05-23 | 三浦工业株式会社 | Method for quantification of total phosphorous |
| JP4821941B1 (en) * | 2010-07-30 | 2011-11-24 | 三浦工業株式会社 | Determination of total phosphorus |
| WO2012014257A1 (en) * | 2010-07-30 | 2012-02-02 | 三浦工業株式会社 | Total phosphorous quantity determination method |
| WO2012014346A1 (en) * | 2010-07-30 | 2012-02-02 | 三浦工業株式会社 | Total phosphorous quantity determination method |
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