JPH08129011A - Inorganic carbon measuring device - Google Patents

Inorganic carbon measuring device

Info

Publication number
JPH08129011A
JPH08129011A JP26576294A JP26576294A JPH08129011A JP H08129011 A JPH08129011 A JP H08129011A JP 26576294 A JP26576294 A JP 26576294A JP 26576294 A JP26576294 A JP 26576294A JP H08129011 A JPH08129011 A JP H08129011A
Authority
JP
Japan
Prior art keywords
carbon
sample
reaction
soln
inorg
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
Application number
JP26576294A
Other languages
Japanese (ja)
Inventor
Kenji Iharada
健志 居原田
Original Assignee
Shimadzu Corp
株式会社島津製作所
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Shimadzu Corp, 株式会社島津製作所 filed Critical Shimadzu Corp
Priority to JP26576294A priority Critical patent/JPH08129011A/en
Publication of JPH08129011A publication Critical patent/JPH08129011A/en
Pending legal-status Critical Current

Links

Abstract

PURPOSE: To provide an inorg. carbon measuring device capable of measuring the concn. of inorg. carbon with high accuracy. CONSTITUTION: The aq. soln. sample injected from a sample injection needle 7a is bubbled by the carrier gas supplied along with an IC reaction soln. 6d made acidic to be adjusted to about pH 2-3 through a carrier gas supply pipe 6h and a finely perforated plate 6g. Carbon dioxide extracted from the inorg. carbon component in the aq. soln. sample by bubbling is detected in a CO2 detection part and the concn. of inorg. carbon is measured. As the IC reaction soln. 6d, a pH buffer soln. such as a mixed soln. of potassium hydrogen phthalate and hydrochloric acid is used and, therefore, the measurement of the concn. of inorg. carbon is repeated. Even when the IC reaction soln. 6d is diluted with the aq. soln. sample, it is held to acidity of about pH 2-3 over a long period of time and the concn. of inorg. carbon can be always measured with high accuracy.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【産業上の利用分野】本発明は、排水、海水、河川水等
の水質の測定、管理や、水を用いる各種プラントの水質
管理等に用いられる無機炭素測定装置に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an inorganic carbon measuring device used for measuring and controlling the water quality of wastewater, seawater, river water, etc., and controlling the water quality of various plants using water.

【0002】[0002]

【従来技術】近年、公害調査等のため、上下水道水、各
種プラント用水、河川等の水中に含まれる無機炭素(I
C)の計測が重要な要因の一つとなっており、かかる無
機炭素の計測には無機炭素測定装置が用いられている。
また、有機炭素濃度の計測は、全炭素量から無機炭素量
を差し引くことで求められるのであるが、かかる有機炭
素濃度の計測における無機炭素量の計測にも無機炭素測
定装置が用いられている。
2. Description of the Related Art In recent years, inorganic carbon (I) contained in water such as water and sewage water, water for various plants, water in rivers, etc.
The measurement of C) is one of the important factors, and an inorganic carbon measuring device is used for measuring such inorganic carbon.
Further, the organic carbon concentration is measured by subtracting the inorganic carbon amount from the total carbon amount, and an inorganic carbon measuring device is also used for measuring the inorganic carbon amount in the measurement of the organic carbon concentration.

【0003】かかる無機炭素測定装置は、リン酸や塩酸
等の酸によってPH2〜3程度の酸性にしたIC反応液
が入れられたIC反応器に水溶液試料を注入し、キャリ
アガスによってこれをバブリングすることで試料中の無
機炭素を二酸化炭素として抽出し、抽出した二酸化炭素
量をCO2 検出部で検出することで無機炭素濃度を計測
するよう構成されている。
In such an inorganic carbon measuring apparatus, an aqueous solution sample is injected into an IC reactor containing an IC reaction solution having a pH of about 2 to 3 with an acid such as phosphoric acid or hydrochloric acid, and this is bubbled with a carrier gas. By doing so, the inorganic carbon in the sample is extracted as carbon dioxide, and the amount of extracted carbon dioxide is detected by the CO2 detection unit to measure the inorganic carbon concentration.

【0004】[0004]

【発明が解決しようとする課題】しかしながら、かかる
従来の無機炭素測定装置では、IC反応器中のIC反応
液は、計測を重ねるにつれて注入した水溶液試料によっ
て希釈され、また、注入する水溶液試料がアルカリ性の
場合はIC反応液が希釈されることに加えて中和も受け
るため、IC反応液がPH2〜3程度の酸性を保つよう
に適当な間隔でIC反応器に酸を加えるという再生処理
が頻繁に必要であった。
However, in such a conventional inorganic carbon measuring apparatus, the IC reaction solution in the IC reactor is diluted with the injected aqueous solution sample as the measurement is repeated, and the injected aqueous solution sample is alkaline. In the case of, since the IC reaction solution is not only diluted but also neutralized, a regeneration treatment of frequently adding an acid to the IC reactor at an appropriate interval so that the IC reaction solution maintains an acidity of about pH 2-3. Was needed for.

【0005】また、適当な間隔でIC反応器に酸を加え
た場合であっても、次に酸を加えるまでにIC反応液の
PHが変動するため、二酸化炭素の抽出効率低下による
測定精度への悪影響は避けられなかった。
Further, even when acid is added to the IC reactor at appropriate intervals, the pH of the IC reaction solution varies until the next acid is added. The ill effect of was inevitable.

【0006】そこで、本発明はかかる問題点を解消する
ため、精度の高い無機炭素濃度の計測ができる無機炭素
測定装置の提供を目的とする。
Therefore, in order to solve such a problem, it is an object of the present invention to provide an inorganic carbon measuring device capable of highly accurately measuring the inorganic carbon concentration.

【0007】[0007]

【課題を解決するための手段】上記目的を達成するため
に、本発明は、水溶液試料を酸性のIC反応液と共にバ
ブリングするIC反応部と、バブリングにより抽出した
二酸化炭素を検出するCO2 検出部とを備え、検出した
二酸化炭素の量から無機炭素濃度を計測する無機炭素測
定装置であって、前記IC反応液としてPH緩衝液を用
いたことを特徴とする。
In order to achieve the above object, the present invention provides an IC reaction section for bubbling an aqueous solution sample together with an acidic IC reaction solution, and a CO2 detection section for detecting carbon dioxide extracted by bubbling. And an inorganic carbon measuring device for measuring the inorganic carbon concentration from the detected amount of carbon dioxide, wherein a PH buffer solution is used as the IC reaction solution.

【0008】[0008]

【作用】本発明の作用を図2に基づいて説明すると、試
料注入ニードル7aから注入された水溶液試料は、PH
2〜3程度の酸性にしたIC反応液6dと混合され、こ
の混合液はキャリアガス供給管6h及び細孔板6gを介
して供給されたキャリアガスによってバブリングされ
る。そして、バブリングにより水溶液試料中の無機炭素
成分から抽出された二酸化炭素は、CO2 検出部20
(図1)で検出され、無機炭素濃度が計測される。ここ
で、IC反応液6dには、フタル酸水素カリウムと塩酸
の混合液等のPH緩衝液が用いられているため、無機炭
素濃度の計測を繰り返し、IC反応液6dが水溶液試料
によって希釈される等した場合であっても、IC反応液
6dの酸性は長期にわたってPH2〜3程度に保持され
る。
The operation of the present invention will be described with reference to FIG. 2. The pH of the aqueous solution sample injected from the sample injection needle 7a is
It is mixed with about 2 to 3 acidified IC reaction liquid 6d, and this mixed liquid is bubbled by the carrier gas supplied through the carrier gas supply pipe 6h and the pore plate 6g. The carbon dioxide extracted from the inorganic carbon component in the aqueous solution sample by bubbling is the CO2 detection unit 20.
(Fig. 1), the inorganic carbon concentration is measured. Here, since the PH buffer solution such as a mixed solution of potassium hydrogen phthalate and hydrochloric acid is used as the IC reaction liquid 6d, the measurement of the inorganic carbon concentration is repeated and the IC reaction liquid 6d is diluted with the aqueous solution sample. Even if the above conditions are satisfied, the acidity of the IC reaction liquid 6d is maintained at about PH2 to 3 for a long period of time.

【0009】[0009]

【実施例】以下、本発明の一実施例を図1及び図2に基
づいて説明する。
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS One embodiment of the present invention will be described below with reference to FIGS.

【0010】図1は本発明にかかる無機炭素測定装置と
全炭素測定装置を組み合わせて用いた場合の全体概略図
である。同図において、分析部1内には水溶液試料中の
TC(全炭素)を二酸化炭素として抽出する酸化反応部
2と、水溶液試料中のIC(無機炭素)を二酸化炭素と
して抽出するIC反応部6が設けられており、これらに
非分散型赤外線ガス分析計がCO2 検出部20として接
続されている。
FIG. 1 is an overall schematic view of the case where the inorganic carbon measuring apparatus according to the present invention and the total carbon measuring apparatus are used in combination. In the figure, in the analysis unit 1, an oxidation reaction unit 2 for extracting TC (total carbon) in the aqueous solution sample as carbon dioxide, and an IC reaction unit 6 for extracting IC (inorganic carbon) in the aqueous solution sample as carbon dioxide. Is provided, and a non-dispersive infrared gas analyzer is connected to them as the CO2 detector 20.

【0011】また、水溶液試料の一定量を採取して酸化
反応部2又はIC反応部6へ導くために、試料自動注入
器15が設けられており、試料自動注入器15は4ポー
トバルブ16とマイクロシリンジ17とを備えている。
4ポートバルブ16には水溶液試料容器18が接続され
ており、水溶液試料容器18内の水溶液試料がマイクロ
シリンジ17で一定量採取され、酸化反応部2又はIC
反応部6へ導かれる。ここで、本発明にかかる無機炭素
測定装置は、主に、試料自動注入器15、IC反応部
6、及びCO2 検出部20によって構成される。
Further, an automatic sample injector 15 is provided for collecting a fixed amount of the aqueous solution sample and guiding it to the oxidation reaction section 2 or the IC reaction section 6. The automatic sample injector 15 is a 4-port valve 16. And a microsyringe 17.
An aqueous solution sample container 18 is connected to the 4-port valve 16, and a certain amount of the aqueous solution sample in the aqueous solution sample container 18 is sampled by a microsyringe 17, and the oxidation reaction unit 2 or IC is sampled.
It is guided to the reaction section 6. Here, the inorganic carbon measuring apparatus according to the present invention is mainly configured by the automatic sample injector 15, the IC reaction unit 6, and the CO2 detection unit 20.

【0012】酸化反応部2には酸化触媒が充填された燃
焼管4と加熱炉5が設けられ、水溶液試料は試料注入部
3を介して燃焼管4に注入される。酸化反応部2の出口
はIC反応部6を経てNDIR(非分散型赤外分光光度
計)のCO2 検出部20へ接続されている。IC反応部
6には、IC反応液6d(図2)が充填されたIC反応
器が備えられており、IC試料注入部7を経て試料自動
注入器15から液体試料が注入される。IC反応部6と
CO2 検出部20の間の流路には除湿除塵部11が設け
られている。
The oxidation reaction section 2 is provided with a combustion tube 4 filled with an oxidation catalyst and a heating furnace 5, and the aqueous solution sample is injected into the combustion tube 4 through the sample injection section 3. The outlet of the oxidation reaction section 2 is connected to the CO2 detection section 20 of NDIR (non-dispersive infrared spectrophotometer) via the IC reaction section 6. The IC reaction part 6 is provided with an IC reactor filled with an IC reaction liquid 6d (FIG. 2), and a liquid sample is injected from the automatic sample injector 15 via the IC sample injection part 7. A dehumidifying / dust removing section 11 is provided in the flow path between the IC reaction section 6 and the CO2 detection section 20.

【0013】CO2 検出部20では、光源21からの光
が同量ずつ入射するように試料セル22と比較セル23
が互いに平行に配置されており、試料セル22には酸化
反応部2で全炭素(TC)が二酸化炭素に変換されてキ
ャリアガスと共に導入されるか、又はIC反応部6で無
機炭素(IC)が二酸化炭素に変換されてキャリアガス
により導入される。比較セル23には赤外線を吸収しな
い窒素や空気などの不活性ガスが充填されている。チョ
ッパ24は光源21から試料セル22と比較セル23に
入射される光を同時に断続するものであり、各セル22
と23を透過して検出部27に入射する光の量を調節す
るために各セル22、23と検出部27の間にはそれぞ
れ光量調整器25、26が配置されている。検出部27
はコンデンサマイクロホン方式の検出器であり、チョッ
パ24の回転により検出部27の出力信号は交流信号と
して得られ、その振幅が出力値となる。そして、全炭素
(TC)の測定と無機炭素(IC)の測定を時間をずら
せて行えば、全炭素(TC)、無機炭素(IC)、及び
有機炭素(TOC)濃度それぞれの計測が可能となる。
In the CO 2 detection section 20, the sample cell 22 and the comparison cell 23 are arranged so that the light from the light source 21 enters the same amount.
Are arranged in parallel to each other, and in the sample cell 22, total carbon (TC) is converted into carbon dioxide in the oxidation reaction section 2 and introduced together with the carrier gas, or inorganic carbon (IC) is mixed in the IC reaction section 6. Is converted into carbon dioxide and introduced by the carrier gas. The comparison cell 23 is filled with an inert gas such as nitrogen or air that does not absorb infrared rays. The chopper 24 interrupts the light incident on the sample cell 22 and the comparison cell 23 from the light source 21 at the same time.
Light amount adjusters 25 and 26 are respectively arranged between the cells 22 and 23 and the detection unit 27 in order to adjust the amount of light that passes through the detectors 23 and 23 and is incident on the detection unit 27. Detector 27
Is a condenser microphone type detector, and the output signal of the detection unit 27 is obtained as an AC signal by the rotation of the chopper 24, and its amplitude becomes an output value. If the total carbon (TC) measurement and the inorganic carbon (IC) measurement are performed at different times, the total carbon (TC), inorganic carbon (IC), and organic carbon (TOC) concentrations can be measured. Become.

【0014】図2は、本発明にかかる無機炭素測定装置
のIC反応部6と、試料注入ニードル7a及びガス排出
口7bからなるIC試料注入部7の詳細図である。ここ
で、試料注入ニードル7aからIC反応器6a内に供給
された水溶液試料は、PH2〜3程度の酸性に保持され
たIC反応液6dに注入される。
FIG. 2 is a detailed view of the IC reaction section 6 of the inorganic carbon measuring apparatus according to the present invention and the IC sample injection section 7 including the sample injection needle 7a and the gas discharge port 7b. Here, the aqueous solution sample supplied from the sample injection needle 7a into the IC reactor 6a is injected into the IC reaction liquid 6d which is kept acidic at about PH2 to pH3.

【0015】IC反応器6aには、IC反応液6dを補
充するための反応液供給管6b、抽出したガスをCO2
検出器20へ送り出すためのガス排出管7b、余分なI
C反応液6dを排出するドレン管6f、及びキャリアガ
スを供給するためのキャリアガス供給管6hが接続され
ている。反応液供給管6b及びドレン管6fには、それ
ぞれ電磁弁6c及び6eが配設されており、IC反応液
6dの供給時及び排出時以外は閉じた状態とされる。ま
た、キャリアガスは炭素成分を含むガス濃度が1ppm 以
下の高純度空気で、不図示のマスフローコントローラで
流量制御されてIC反応器6aへ導入され、細かい孔を
多数穿設した細孔板6gを通過するときに泡状となり、
IC反応液6dに対してバブリング作用を施す。このバ
ブリングにより水溶液試料中の無機炭素成分は、二酸化
炭素として抽出され、ガス排出管7bを介して図1のC
O2 検出部20で検出されて、無機炭素濃度が計測され
る。
The IC reactor 6a is provided with a reaction solution supply pipe 6b for replenishing the IC reaction solution 6d, and the extracted gas is CO2.
Gas exhaust pipe 7b for sending to detector 20, extra I
A drain pipe 6f for discharging the C reaction liquid 6d and a carrier gas supply pipe 6h for supplying a carrier gas are connected. Electromagnetic valves 6c and 6e are provided in the reaction liquid supply pipe 6b and the drain pipe 6f, respectively, and are kept closed except when the IC reaction liquid 6d is supplied and discharged. Further, the carrier gas is high-purity air containing a carbon component and having a gas concentration of 1 ppm or less, and is introduced into the IC reactor 6a with its flow rate controlled by a mass flow controller (not shown), and a fine hole plate 6g having a large number of fine holes is formed. When it passes, it becomes foamy,
A bubbling action is applied to the IC reaction liquid 6d. By this bubbling, the inorganic carbon component in the aqueous solution sample is extracted as carbon dioxide, and is extracted through the gas discharge pipe 7b as shown in C in FIG.
The concentration of inorganic carbon is measured by the O2 detector 20.

【0016】ここで、IC反応液6dには、フタル酸水
素カリウムと塩酸の混合液等のPH緩衝液が用いられて
いる。このため、無機炭素濃度の計測を繰り返し、IC
反応液6dが水溶液試料によって希釈されたり、水溶液
試料がアルカリ性で中和作用を有する場合であっても、
IC反応液6dの酸性は長期にわたってPH2〜3程度
に保持される。このため、本発明によれば、計測を繰り
返した場合であっても、IC反応液6dをPH緩衝液の
緩衝能の範囲内においてPHの上昇を抑えることができ
るため、長期にわたってPH2〜3程度の酸性に保持で
き、精度の高い無機炭素濃度計測が可能となる。
Here, a PH buffer solution such as a mixed solution of potassium hydrogen phthalate and hydrochloric acid is used as the IC reaction solution 6d. Therefore, the measurement of the inorganic carbon concentration is repeated, and the IC
Even if the reaction solution 6d is diluted with an aqueous solution sample or the aqueous solution sample is alkaline and has a neutralizing action,
The acidity of the IC reaction liquid 6d is kept at about PH2 to 3 for a long period of time. Therefore, according to the present invention, even when the measurement is repeated, it is possible to suppress the increase in PH within the range of the buffer capacity of the pH buffer solution of the IC reaction solution 6d, so that the PH of about 2 to 3 is maintained over a long period of time. It is possible to maintain the acidity of, and to measure the inorganic carbon concentration with high accuracy.

【0017】なお、PH緩衝液とは、溶液に酸または塩
基を加えたときに起こる水素イオン濃度の変化を小さく
する機能を備えた液をいい、ここでは、フタル酸水素カ
リウムと塩酸の混合液を用いたが、酢酸と酢酸塩、塩酸
とクエン酸ナトリウムなど、一般に弱酸または弱塩基と
その塩等との適当な混合によって、PHの種々な値にお
ける緩衝作用を作ることができ、PHを2〜3程度に保
持できるPH緩衝液であれば何でもよい。
The PH buffer solution is a solution having a function of reducing the change in hydrogen ion concentration that occurs when an acid or a base is added to the solution. Here, a mixed solution of potassium hydrogen phthalate and hydrochloric acid is used. However, buffering action at various values of PH can be made by appropriately mixing weak acids or weak bases such as acetic acid and acetate, hydrochloric acid and sodium citrate, etc. with appropriate pH values. Any PH buffer may be used as long as it can be maintained at about 3 to 3.

【0018】[0018]

【発明の効果】本発明によれば、IC反応液にPH緩衝
液を用いたため、計測を重ねるにつれてIC反応液が注
入した水溶液試料によって希釈される場合や、また、注
入する水溶液試料がアルカリ性で中和作用を受ける場合
であっても、IC反応液を長期にわたって一定の酸性に
保持でき、精度の高い無機炭素濃度計測が可能となる。
According to the present invention, since the PH buffer is used as the IC reaction solution, the IC reaction solution may be diluted with the injected aqueous solution sample as the measurement is repeated, or the injected aqueous solution sample may be alkaline. Even if it receives a neutralizing action, the IC reaction liquid can be kept at a constant acidity for a long period of time, and the inorganic carbon concentration can be measured with high accuracy.

【図面の簡単な説明】[Brief description of drawings]

【図1】本発明にかかる無機炭素測定装置を全有機炭素
測定装置との組み合わせで示した全体概略図である。
FIG. 1 is an overall schematic diagram showing an inorganic carbon measuring apparatus according to the present invention in combination with an all-organic carbon measuring apparatus.

【図2】本発明にかかる無機炭素測定装置のIC反応部
を示す詳細図のである。
FIG. 2 is a detailed view showing an IC reaction part of the inorganic carbon measuring device according to the present invention.

【符号の説明】[Explanation of symbols]

6・・・・・・IC反応部 6a・・・・・IC反応管 6d・・・・・IC反応液 6 ... IC reaction part 6a IC reaction tube 6d IC reaction liquid

Claims (1)

【特許請求の範囲】[Claims] 【請求項1】 水溶液試料を酸性のIC反応液と共にバ
ブリングするIC反応部と、バブリングにより抽出した
二酸化炭素を検出するCO2 検出部とを備え、検出した
二酸化炭素の量から水溶液試料中の無機炭素濃度を計測
する無機炭素測定装置において、 前記IC反応液としてPH緩衝液を用いたことを特徴と
する無機炭素測定装置。
1. An inorganic carbon in an aqueous solution sample, comprising an IC reaction section for bubbling an aqueous solution sample together with an acidic IC reaction solution, and a CO2 detection section for detecting carbon dioxide extracted by bubbling. An inorganic carbon measuring device for measuring a concentration, wherein a PH buffer solution is used as the IC reaction liquid.
JP26576294A 1994-10-28 1994-10-28 Inorganic carbon measuring device Pending JPH08129011A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP26576294A JPH08129011A (en) 1994-10-28 1994-10-28 Inorganic carbon measuring device

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP26576294A JPH08129011A (en) 1994-10-28 1994-10-28 Inorganic carbon measuring device

Publications (1)

Publication Number Publication Date
JPH08129011A true JPH08129011A (en) 1996-05-21

Family

ID=17421673

Family Applications (1)

Application Number Title Priority Date Filing Date
JP26576294A Pending JPH08129011A (en) 1994-10-28 1994-10-28 Inorganic carbon measuring device

Country Status (1)

Country Link
JP (1) JPH08129011A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002075300A1 (en) * 2001-03-16 2002-09-26 Msa Auer Gmbh Method and measuring device for analysing the carbon dioxide content in water
JP5284515B1 (en) * 2012-05-25 2013-09-11 株式会社共立理化学研究所 Measuring device and measuring method for total organic carbon concentration
KR20210017795A (en) * 2019-08-09 2021-02-17 강원대학교산학협력단 A METHOD FOR MEASURING ALKALINITY THROUGH MEASUREMENT OF pH, TEMPERATURE AND INORGANIC CARBON COMPONENTS AND A INSTRUMENT FOR MEASURING ALKALINITY BASED ON THE SAME

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002075300A1 (en) * 2001-03-16 2002-09-26 Msa Auer Gmbh Method and measuring device for analysing the carbon dioxide content in water
JP5284515B1 (en) * 2012-05-25 2013-09-11 株式会社共立理化学研究所 Measuring device and measuring method for total organic carbon concentration
KR20210017795A (en) * 2019-08-09 2021-02-17 강원대학교산학협력단 A METHOD FOR MEASURING ALKALINITY THROUGH MEASUREMENT OF pH, TEMPERATURE AND INORGANIC CARBON COMPONENTS AND A INSTRUMENT FOR MEASURING ALKALINITY BASED ON THE SAME

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