JPS5915856A - Apparatus for measuring carbon of specimen containing halogen - Google Patents
Apparatus for measuring carbon of specimen containing halogenInfo
- Publication number
- JPS5915856A JPS5915856A JP11290682A JP11290682A JPS5915856A JP S5915856 A JPS5915856 A JP S5915856A JP 11290682 A JP11290682 A JP 11290682A JP 11290682 A JP11290682 A JP 11290682A JP S5915856 A JPS5915856 A JP S5915856A
- Authority
- JP
- Japan
- Prior art keywords
- carbon
- reaction tube
- halogen
- analysis
- converting
- 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.)
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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
- G01N31/005—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods investigating the presence of an element by oxidation
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Molecular Biology (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (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】
この発明は水中の炭素分の測定装置に係り、さらに詳し
くは、キャリヤガス供給部と、加熱炉を一体に有する無
機性炭素の二酸化炭素への変換用反応管と、ガス分析部
とが順次流路により接続されるとともに、分析部の分析
結果を表示する記録計を一体に備えてなり、上記反応管
内に銀イオンを含む非酸化性酸を充填してなるノ・ロダ
ン含有試料用炭素測定装置およびキャリヤガス供給部と
、加熱炉を一体に有する全炭素の二酸化炭素への変換用
燃焼管と、加熱炉を一体に有する無機性炭素の二酸化炭
素への変換用反応管と、ガス分析部とが順次流路により
接続されるとともに１分析部の分析結果を表示する記録
計全一体に備えてなり、上記燃焼管内に酸化触媒を、上
記反応管内に銀イオンを含む非酸化性酸をそれぞれ充填
してなるノ・ロダン含有試料用炭素測定装置に関するも
のでおる。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an apparatus for measuring carbon content in water, and more specifically, a reaction tube for converting inorganic carbon into carbon dioxide, which integrally includes a carrier gas supply section and a heating furnace; The reaction tube is connected to the gas analysis section by a flow path and is integrally equipped with a recorder for displaying the analysis results of the analysis section, and the reaction tube is filled with a non-oxidizing acid containing silver ions. A carbon measuring device for rodan-containing samples, a carrier gas supply section, a combustion tube for converting all carbon to carbon dioxide, which has a heating furnace integrated therein, and a reaction for converting inorganic carbon to carbon dioxide, which has a heating furnace integrated therein. The tube and the gas analysis section are sequentially connected by a flow path, and the recorder for displaying the analysis results of one analysis section is provided as a whole, and the combustion tube contains an oxidation catalyst and the reaction tube contains silver ions. This invention relates to a carbon measuring device for a sample containing Rodan, each of which is filled with a non-oxidizing acid.
河川水、湖沼水、海水あるいは上水、下水、工揚排水な
どの各種の水に含まれる無機性炭素（Ｉ（３）は、主と
して炭酸、炭酸イオン、炭酸水素イオンなどの炭酸体炭
素として存在している。これらのＩＣを測定する方法と
しては、試料を非酸化性酸□出する方法などがある。Inorganic carbon (I(3)), which is contained in various types of water such as river water, lake water, seawater, tap water, sewage, and pumped wastewater, exists primarily as carbonate carbon such as carbonic acid, carbonate ions, and bicarbonate ions. Methods for measuring these ICs include a method in which a sample is exposed to non-oxidizing acid.
以上のＩＣ測定装置において、ハロゲン化合物を多量に
含む試料を測定した場合、発生するハロゲン生成物によ
る測定の妨害および非分敵影赤外線式ガス分析計の測定
セル内面の劣化などの構成部品に対する腐蝕が重大な問
題であった。ハロゲン化合物の中でも４ＩＫ塩素化合物
は、例えば海水、下水、工場排水などのように多量に含
まれる場合が多く問題であった。When measuring a sample containing a large amount of halogen compounds with the above IC measuring device, the generated halogen products may interfere with the measurement and cause corrosion to the component parts, such as deterioration of the inner surface of the measurement cell of the non-separated shadow infrared gas analyzer. was a serious problem. Among halogen compounds, 4IK chlorine compounds have been problematic in many cases, for example, when they are contained in large amounts in seawater, sewage, industrial wastewater, and the like.
従来例をあげて説明すると、非酸化性酸としてりん酸を
使用し、これを石英ガラスチップに含浸させたものを充
填した反応管中にキャリヤガス（窒素あるいは精製空気
）を流通させ、反応管を約１５０℃に加熱した状態で、
ＩＣを含む試料を反応管に注入すると第１図のような二
酸化炭素によるシャープなピークかえられる。しかし、
塩化ナトリウム３％を含む試料の場合は第２図のような
形状のピークになり、正確な測定が困難になる。To explain a conventional example, phosphoric acid is used as a non-oxidizing acid, and a carrier gas (nitrogen or purified air) is passed through a reaction tube filled with a quartz glass chip impregnated with phosphoric acid. While heating to about 150℃,
When a sample containing IC is injected into a reaction tube, a sharp peak due to carbon dioxide appears as shown in Figure 1. but,
In the case of a sample containing 3% sodium chloride, a peak appears in the shape shown in Figure 2, making accurate measurement difficult.
ハロゲン化合物を含む試料からえられるピークは、ハロ
ゲン化合物の含有量などにより、ピーク形状は左右され
るが、一般にゴーストピーク、テーリング、ベースライ
ンの不安定などを生じる。この原因は、塩化ナトリウム
を例にあげると、次式の反応により発生する塩化水素（
あるいは塩酸ミスト）によるものと考えられる。The shape of the peak obtained from a sample containing a halogen compound is affected by the content of the halogen compound, etc., but generally ghost peaks, tailing, unstable baselines, etc. occur. The reason for this is, taking sodium chloride as an example, hydrogen chloride (
or hydrochloric acid mist).
Ｅ８ＰＯ４＋ Ｎａ０ｌ＝ ＩＪａＨ２ＰＯ，十Ｈｅｌ
従来この対策としては、無機性炭素の二酸化炭素への変
換工程の後に、キャリヤガス中のハロゲン生成物の除去
工程を設けていた。第８図は無機性炭素測定装置を使用
して構成した有機性炭素測定装置の従来例を示すもので
あり、並列状態に配された無機性炭素の二酸化炭素への
変換用反応管（ａ）と全炭素の二酸化炭素への変換用燃
焼管（ｂ）との次工程にハロゲン除去用スクラバー（Ｑ
）が配されていて、この部分でハロゲン生成物はハロゲ
ン化銀（例えば塩化銀）として固定される。（従来例の
ピーク形状−第４図）この従来方式には次の欠点があっ
た。E8PO4+ Na0l= IJaH2PO, 10 Hel
Conventionally, this has been achieved by providing a step for removing halogen products in the carrier gas after the step of converting inorganic carbon to carbon dioxide. Figure 8 shows a conventional example of an organic carbon measuring device constructed using an inorganic carbon measuring device, in which reaction tubes (a) for converting inorganic carbon to carbon dioxide are arranged in parallel. A scrubber for halogen removal (Q
) in which the halogen product is fixed as silver halide (eg, silver chloride). (Peak shape of conventional example - Fig. 4) This conventional method had the following drawbacks.
■スクラバーなどの部品が増え、コストアップになる。■The number of parts such as scrubbers increases, which increases costs.
■常温で反応させるため、除去効率が低い。■Removal efficiency is low because the reaction is carried out at room temperature.
■除去剤の交換のための保守工数が必要である。■Maintenance time is required to replace the remover.
この発明は以上の欠点を解消するものであり、以下にそ
の実施例の説明を行う。This invention solves the above-mentioned drawbacks, and embodiments thereof will be described below.
第５図は無機性炭素用の炭素測定装置の全体構成を示す
もので、装置はキャリヤガス供給部（１）と無機性炭素
を二酸化炭素に変換する反応管（２）と除湿用クーラー
（８）とガス分析部（４）とが順次流路（５）より接続
されて構成されている。反応管（２）はその前端部が試
料の注入部（２）となっており、キャリヤガス供給部（
１）からの流路（５）は試料の注入部（２１の若干後方
部分に接続される。（６）は反応管（２）を加熱すべく
反応管（２）の外周部に設けられる加熱炉であり、（７
）は分析部（４）の分析結果を記録する記録計である。Figure 5 shows the overall configuration of a carbon measuring device for inorganic carbon, which consists of a carrier gas supply section (1), a reaction tube (2) for converting inorganic carbon into carbon dioxide, and a dehumidifying cooler (8). ) and a gas analysis section (4) are successively connected through a flow path (5). The front end of the reaction tube (2) is the sample injection part (2), and the carrier gas supply part (2) is the sample injection part (2).
The flow path (5) from 1) is connected to the slightly rear part of the sample injection part (21). It is a furnace (7
) is a recorder that records the analysis results of the analysis section (4).
そして反応管（２）内に無機性炭素を二酸化炭素に変換
させる非酸化性酸とハロゲン生成物をハロゲン化銀とし
て固定する銀イオンが内蔵されており、その内蔵状態は
下記の通りである。すなわち、反応管（２）内に約ｌＯ
メツシュの石英ガラスチップよりなる保持材（８）に銀
イオンを含むリン酸溶液（非酸化性酸）を含浸したもの
を充填するもので、銀イオンの旋度は１〜１０％の範囲
が適当である。The reaction tube (2) contains a non-oxidizing acid for converting inorganic carbon into carbon dioxide and silver ions for fixing a halogen product as silver halide, and their internal state is as follows. That is, about 1O in the reaction tube (2)
The holding material (8) made of mesh quartz glass chips is filled with a phosphoric acid solution (non-oxidizing acid) containing silver ions, and the rotation of the silver ions is preferably in the range of 1 to 10%. It is.
なお、反応管（２）内へは保持材（８）を使用せず、直
接酸性リン酸ギン塩結晶を充填するようにしてもよいＯ
今、反応管（２）を加熱炉（６）によりｉｏｏ℃〜２０
０℃、好ましくは１６０℃に熱した状態において、キャ
リヤガスを送るとともに試料注入部（２１からハロゲン
化合物を含む試料を注入すると、ハロゲン生成物は保持
材（８）に含浸された銀イオンと反応して、ハロゲン化
銀として反応管（２）内に固定される。Note that the reaction tube (2) may be directly filled with acidic phosphoric acid ginsate crystals without using the holding material (8). ioo℃～20
When heated to 0°C, preferably 160°C, a carrier gas is sent and a sample containing a halogen compound is injected from the sample injection part (21), and the halogen product reacts with the silver ions impregnated in the holding material (8). Then, it is fixed as silver halide in the reaction tube (2).
第６図は有機性炭素用の炭素測定装置の全体構成を示し
、このものは第６図に示す無機性炭素用の炭素測定装置
のキャリヤガス供給部（１）と反応管（２）との間に、
加熱炉（ｄ）ヲ一体に有し内部に酸化銅、白金等の酸化
触媒が保持された石英ウール等の保持材（９）が充填さ
れた、全炭素全二酸化炭素に変換する燃焼管（…が配さ
れているもので、反応管（２）内には第５図に示す炭素
測定装置と同様の保持材（８）が充填されている。Figure 6 shows the overall configuration of a carbon measuring device for organic carbon, which consists of a carrier gas supply section (1) and a reaction tube (2) of the carbon measuring device for inorganic carbon shown in Figure 6. Between,
The heating furnace (d) is integrated with a combustion tube (... The reaction tube (2) is filled with a holding material (8) similar to that of the carbon measuring device shown in FIG.
この装置における有機性炭素の含有量の分析測定は、燃
焼管叫と反応管（２）のそれぞれの注入部から開時に同
一の試料を注入してそれぞれの縦累の含有量を測定し、
その差を求めることによっておこなうものである。この
場合燃焼管αＱから注入された試料に含まれるノ・ロゲ
ン化合物は、燃焼管曲内で反応してハロゲンを含むガス
状物質を生成し、これがキャリヤガスとともに反応管（
２）内に至りこの部分でハロゲンイし銀として同定され
、また、反応管（２）から注入される試料内の７・ロゲ
ン化合物も反応管（２）内に固定される。To analyze and measure the content of organic carbon in this device, the same sample is injected from the injection ports of the combustion tube and the reaction tube (2) when they are opened, and the content in each column is measured.
This is done by finding the difference. In this case, the halogen compounds contained in the sample injected from the combustion tube αQ react within the combustion tube curve to produce a gaseous substance containing halogen, which together with the carrier gas flows into the reaction tube (
2), where it is identified as silver halide, and the 7-halogen compound in the sample injected from the reaction tube (2) is also fixed in the reaction tube (2).
この発明の実施例におけるクロマトグラムにおけるピー
クは、第７図に示す通り完全に７１０ゲン生成物の影響
は除かれる０
この発明は上述のように構成されており、従来のハロゲ
ンスクラバーを反応管で兼用しているため部品数が増え
ず、構成がシンプルとなると共に部品増加によるコスト
アップもなく、また、反応管内で加熱状態において反応
させるため、迅速かつ完全にハロゲン化銀全生成し、ハ
ロゲン生成物の除去効率が高いもので、さらに、ノ・ロ
ゲン生成物除去用の銀イオンを無機性炭素の反応剤とと
もに交換できるので、ハロゲンスクラバーとしての保守
工数を必要としないもので、これら利点は無機性炭素、
有機性炭素の両炭素測定装置においてきわめて有効なも
のである。As shown in FIG. 7, the influence of the 710-gen product is completely removed from the peaks in the chromatogram in the embodiment of this invention. Because they are used for both purposes, the number of parts does not increase, the configuration is simple, and there is no cost increase due to increased parts.Also, since the reaction is carried out in a heated state in the reaction tube, all silver halide is produced quickly and completely, and halogen is produced. Furthermore, since the silver ion for removing halogen products can be exchanged with the inorganic carbon reactant, it does not require maintenance as a halogen scrubber. carbon,
This is an extremely effective device for measuring organic carbon.
第１図はハロゲン化合物を含まない試料のピークを示す
クロマトグラム図、第２図は８％Ｎａ０ｊ’を含む試料
のピークを示すクロマトグラム図、第８図は従来の無機
性炭素測定装置を使用した有機性炭素測定装置の構成説
明図、第４図は従来のノ・ロゲンスクラバーを使用した
際の８％Ｎａ０ｊ’を含む試料のピークを示すクロマト
グラム図、第５図は第１発明の実施例の構成説明図、第
６図は第２発明の実施例の構成説明図、第７図はこの発
明による８％Ｎａ０ｊ’を含む試料のピークを示すクロ
マトグラム図である。
（１）・・・キャリヤガス供給部、（２）・・・無機性
炭素を二酸化炭素に変換する反応管、 （４）・・・ガ
ス分析部、 （５）・・・流路、 （６）、（６１・・
・加熱炉、 （７）・・・記録計、 （８）、（９）・
・・保持材、Ｑｌ・・・燃焼管。
−９−３１−ｚ
厳
蕨
堰
手続補正書
特許庁長官 若杉 和犬 殿
１、事件の表示
昭和５７年特許願第１１２９０６号
２、発明の名称
ハロゲン含有試料用炭素測定装置
３、補正をする者
重着との関係 特許出願人
住 所 京都市中京区河原町通二条■ルーツ船人町３
７８番地名 称 （１９９）株式会社 島沖製作所
代表者横地 節男
４、代理人〒５３０
住 所 大阪市北区西天満５丁目１−３クォーター・
ワンビル５、補正命令の日イｑ （自発）
補正の内容
１、明細書第６頁第１θ行目の「酸性リン酸ギン塩結晶
を充填するようにしてもよ」を［酸性リン酸銀塩結晶を
充填するようにしてもよ」と補正する。
３１９−Figure 1 is a chromatogram showing the peaks of a sample that does not contain halogen compounds, Figure 2 is a chromatogram showing the peaks of a sample containing 8% Na0j', and Figure 8 is a chromatogram using a conventional inorganic carbon measuring device. Fig. 4 is a chromatogram showing the peak of a sample containing 8% Na0j' when using a conventional nitrogen scrubber, and Fig. 5 is a diagram showing the configuration of the organic carbon measuring device according to the first invention. FIG. 6 is an explanatory diagram of the configuration of an example of the second invention, and FIG. 7 is a chromatogram diagram showing peaks of a sample containing 8% Na0j' according to the present invention. (1)...Carrier gas supply section, (2)...Reaction tube for converting inorganic carbon into carbon dioxide, (4)...Gas analysis section, (5)...Flow path, (6 ), (61...
・Heating furnace, (7)...Recorder, (8), (9)・
...Holding material, Ql...Combustion tube. -9-31-z Gonwarabi Weir Procedural Amendments Commissioner of the Japan Patent Office Mr. Kazuinu Wakasugi 1, Indication of the case 1982 Patent Application No. 112906 2, Name of the invention Carbon measuring device for halogen-containing samples 3, Person making the amendment Relationship with heavy clothing Patent applicant address 3, Kawaramachi-dori Nijo, Nakagyo-ku, Kyoto ■ Roots Funatocho
Address 78 Name (199) Shimaoki Seisakusho Co., Ltd. Representative Setsuo Yokochi 4, Agent 530 Address 1-3 Quarter, 5-chome Nishitenma, Kita-ku, Osaka
One Bill 5, date of amendment order (voluntary) Contents of amendment 1, page 6 of the specification, line 1θ, “may be filled with acidic silver phosphate crystals” [acidic silver phosphate crystals] You can try filling it with crystals.'' I corrected him. 319-
Claims (1)
機性炭素の二酸化炭素への変換用反応管と、ガス分析部
とが順次流路により接続されるとともに、分析部の分析
結果を表示する記録計を一体に備えてなり、上記反応管
内に銀イオンを含む非酸化性酸を充填してなるノ・ロダ
ン含有試料用炭素測定装置。 ２、キャリヤガス供給部と、加熱炉を一体に有する全炭
素の二酸化炭素への変換用燃焼管と、加熱炉を一体に有
する無機性炭素の二酸化炭素への変換用反応管と、ガス
分析部とが順次流路により接続されるとともに１分析部
の分析結果を表示する記録計を一体に備えてなり、上記
燃焼管内に酸化触媒を、上記反応管内に銀イオンを含む
非酸化性酸をそれぞれ充填してなるハロゲン含有試料用
炭素測定装置。[Scope of Claims] (1) A carrier gas supply section, a reaction tube for converting inorganic carbon into carbon dioxide integrally having a heating furnace, and a gas analysis section are sequentially connected by a flow path, and the analysis section 1. A carbon measuring device for a sample containing rhodan, which is integrally equipped with a recorder for displaying the analysis results of the above reaction tube and is filled with a non-oxidizing acid containing silver ions. 2. A carrier gas supply section, a combustion tube for converting all carbon to carbon dioxide that has a heating furnace integrated therein, a reaction tube for converting inorganic carbon to carbon dioxide that has an integrated heating furnace, and a gas analysis section are sequentially connected by flow paths and are integrally equipped with a recorder for displaying the analysis results of one analysis section, an oxidation catalyst is placed in the combustion tube, and a non-oxidizing acid containing silver ions is placed in the reaction tube. Carbon measuring device for halogen-containing samples.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11290682A JPS5915856A (en) | 1982-06-29 | 1982-06-29 | Apparatus for measuring carbon of specimen containing halogen |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11290682A JPS5915856A (en) | 1982-06-29 | 1982-06-29 | Apparatus for measuring carbon of specimen containing halogen |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5915856A true JPS5915856A (en) | 1984-01-26 |
| JPH0444695B2 JPH0444695B2 (en) | 1992-07-22 |
Family
ID=14598449
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11290682A Granted JPS5915856A (en) | 1982-06-29 | 1982-06-29 | Apparatus for measuring carbon of specimen containing halogen |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5915856A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01132965U (en) * | 1988-02-26 | 1989-09-11 | ||
| US5473945A (en) * | 1990-02-14 | 1995-12-12 | The Charles Stark Draper Laboratory, Inc. | Micromechanical angular accelerometer with auxiliary linear accelerometer |
| JP2008070134A (en) * | 2006-09-12 | 2008-03-27 | Japan Agengy For Marine-Earth Science & Technology | Pretreatment device for analyzing element |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6702325B2 (en) * | 2015-08-05 | 2020-06-03 | 東亞合成株式会社 | Carbon analysis method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56112647A (en) * | 1980-02-12 | 1981-09-05 | Mitsui Petrochem Ind Ltd | Measuring method for amount of carbon and measuring device therefor |
-
1982
- 1982-06-29 JP JP11290682A patent/JPS5915856A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56112647A (en) * | 1980-02-12 | 1981-09-05 | Mitsui Petrochem Ind Ltd | Measuring method for amount of carbon and measuring device therefor |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01132965U (en) * | 1988-02-26 | 1989-09-11 | ||
| US5473945A (en) * | 1990-02-14 | 1995-12-12 | The Charles Stark Draper Laboratory, Inc. | Micromechanical angular accelerometer with auxiliary linear accelerometer |
| JP2008070134A (en) * | 2006-09-12 | 2008-03-27 | Japan Agengy For Marine-Earth Science & Technology | Pretreatment device for analyzing element |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0444695B2 (en) | 1992-07-22 |
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