JPH04105042A - Measuring method for underwater dissolved coal dioxide - Google Patents
Measuring method for underwater dissolved coal dioxideInfo
- Publication number
- JPH04105042A JPH04105042A JP2222518A JP22251890A JPH04105042A JP H04105042 A JPH04105042 A JP H04105042A JP 2222518 A JP2222518 A JP 2222518A JP 22251890 A JP22251890 A JP 22251890A JP H04105042 A JPH04105042 A JP H04105042A
- Authority
- JP
- Japan
- Prior art keywords
- gas
- photometer
- gas flow
- gasifier
- measurement
- 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
- 238000000034 method Methods 0.000 title claims description 11
- 239000003245 coal Substances 0.000 title 1
- 238000005259 measurement Methods 0.000 claims abstract description 18
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 53
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000010521 absorption reaction Methods 0.000 claims description 11
- 239000001569 carbon dioxide Substances 0.000 claims description 11
- 230000008016 vaporization Effects 0.000 claims description 5
- 238000004458 analytical method Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 abstract description 26
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract description 10
- 239000012159 carrier gas Substances 0.000 abstract description 4
- 239000011491 glass wool Substances 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 3
- 239000002274 desiccant Substances 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 abstract 2
- 239000000523 sample Substances 0.000 description 8
- 239000007788 liquid Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- MPCRDALPQLDDFX-UHFFFAOYSA-L Magnesium perchlorate Chemical compound [Mg+2].[O-]Cl(=O)(=O)=O.[O-]Cl(=O)(=O)=O MPCRDALPQLDDFX-UHFFFAOYSA-L 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000691 measurement method Methods 0.000 description 2
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- 238000009834 vaporization Methods 0.000 description 2
- 239000006200 vaporizer Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 description 1
- 229910001863 barium hydroxide Inorganic materials 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 229910001631 strontium chloride Inorganic materials 0.000 description 1
- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical compound [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 description 1
Landscapes
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、水（液）中の溶存二酸化炭素を迅速にかつ高
精度に測定する方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for rapidly and highly accurately measuring dissolved carbon dioxide in water (liquid).
従来、水中の溶存二酸化炭素の測定方法としては、水酸
化バリウムや塩化ストロンチウムでｃ。Conventionally, dissolved carbon dioxide in water has been measured using barium hydroxide or strontium chloride.
、を安定化（不溶性塩として沈澱）させた後、その量を
フェノールフタレインを指示薬とし、水酸化ナトリウム
で滴定することによって求める中和滴定法が知られてい
る。is stabilized (precipitated as an insoluble salt), and then its amount is determined by titration with sodium hydroxide using phenolphthalein as an indicator.
しかし、上記従来の方法においては、測定試料により前
処理方法が異なり、多くのガラス器具類を使用しなけれ
ばならないと共に試薬調製にも時間がかかる。However, in the above-mentioned conventional method, the pretreatment method differs depending on the sample to be measured, many glass instruments must be used, and it takes time to prepare the reagent.
また、測定工程として約１〜２時間かかるため、測定操
作中に空気中のＣＯ２を吸収してしまう等により、測定
精度の低下を来すといった問題点がある。Furthermore, since the measurement process takes about 1 to 2 hours, there is a problem that measurement accuracy decreases due to absorption of CO2 in the air during the measurement operation.
本発明の目的は、水中の溶存二酸化炭素を迅速に、かつ
高精度に測定する方法を提供することにある。An object of the present invention is to provide a method for rapidly and highly accurately measuring dissolved carbon dioxide in water.
上記課題を解決するために、本発明はなされたものであ
る。The present invention has been made in order to solve the above problems.
すなわち本発明は、水中の溶存二酸化炭素を測定するに
際して、該水中溶存二酸化炭素（以下水中ＣＯ２という
）の気化手段と非分散型赤外線吸光光度計とを組み合わ
せた分析装置により、測定することを特徴とする水中の
溶存二酸化炭素の測定力法である。That is, the present invention is characterized in that when measuring dissolved carbon dioxide in water, the measurement is carried out using an analysis device that combines a means for vaporizing the carbon dioxide dissolved in water (hereinafter referred to as CO2 in water) and a non-dispersive infrared absorption photometer. This is a power method for measuring dissolved carbon dioxide in water.
本発明において使用される測定サンプルはＣＯ２を含む
すべての溶液について適用することができる。The measurement sample used in the present invention can be applied to all solutions containing CO2.
本発明における水中Ｃ○２の気化手段としては、次のよ
うな手段が用いられる。すなわち、サンプル液中に溶存
する各種炭酸物質は強酸を加えて酸性（ＰＨ＝２以下）
にすると炭酸物質からＣＯ２が遊離して気化する。これ
を利用するのが好ましい。In the present invention, the following means are used to vaporize C○2 in water. In other words, various carbonic substances dissolved in the sample solution are made acidic (PH = 2 or less) by adding a strong acid.
When this happens, CO2 is liberated from the carbonic acid substance and vaporizes. It is preferable to use this.
例えば、硫酸を入れた容器内にマイクロシリンジを介し
て硫酸を注入する等の手段が用いられる。For example, a method such as injecting sulfuric acid into a container containing sulfuric acid via a microsyringe is used.
例えば使用される硫酸は溶液のＰＨを下げて、ＣＯ２を
気化させるためのＰＨ調製用として作用するのである。For example, the sulfuric acid used lowers the pH of the solution and acts as a pH adjuster for vaporizing CO2.
このような気化手段によって気化、遊離されたＣＯ２は
、キャリアーガスで運ばれ、通常ガラスウール、除湿器
、乾燥剤等を通して充分水分が除かれて非分散型赤外線
吸光光度計（１６） （検知器）に送られ、測定される
。キャリアーガスとしては、検知器にて感知されない窒
素、アルゴン等の不活性ガスが用いられる。The CO2 vaporized and liberated by such vaporization means is carried by a carrier gas, and the water is removed sufficiently through glass wool, a dehumidifier, a desiccant, etc., and then the CO2 is transferred to a non-dispersive infrared absorption photometer (16) (detector). ) and measured. As the carrier gas, an inert gas such as nitrogen or argon, which is not detected by the detector, is used.
非分散型赤外線吸光光度計及び電子除湿器の安定時間と
しては、通常３０分〜１時間が必要である。The stabilization time of a non-dispersive infrared absorption photometer and an electronic dehumidifier is usually 30 minutes to 1 hour.
測定時間は、サンプル注入後測定結果が得られるまで、
通常５分以内という短時間である。The measurement time is from sample injection until measurement results are obtained.
It is a short time, usually within 5 minutes.
以下、本発明に係る測定方法の実施の態様を、図面に示
す装置例を参照して具体的に説明する。DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, embodiments of the measuring method according to the present invention will be specifically described with reference to an example of the apparatus shown in the drawings.
第１図は本発明に係る測定方法を実施するための装置例
の概略図である。FIG. 1 is a schematic diagram of an example of an apparatus for carrying out the measuring method according to the present invention.
まず、測定前準備として、非分散型赤外線吸光光度計１
６（島津製作所製赤外線式ガス分析計ＵＲＡ−１０７型
）及び電子除湿器１４の電源を入れて約１時間、装置の
安定化を図る。First, as a preparation before measurement, a non-dispersive infrared absorption photometer 1
6 (infrared gas analyzer model URA-107 manufactured by Shimadzu Corporation) and electronic dehumidifier 14 were turned on and the devices were stabilized for about 1 hour.
装置安定後、ＣＯ２標準ガスの圧力バルブ４を開き切替
コック５を切替え、流量計７で０．１５Ａ／ｍｉｎ、に
ガス流量調整バルブ６で調整する。標準ガスは切替コッ
ク８を経て逆止弁９を通り気液分離器１２、ガラスウー
ル１３、電子除湿器１４、過塩素酸マグネシウム１５を
経て非分散型赤外線吸光光度計１６へと達し、ここで標
準ガス濃度にスパンを合わせ、非分散型赤外線吸光光度
計１６のチエツクを行う。ＣＯ２標準ガスは非分散型赤
外線吸光光度計１６のスパンを合わせ、計器のチエツク
に使用されるのである。After the apparatus is stabilized, the CO2 standard gas pressure valve 4 is opened, the switching cock 5 is switched on, and the flow rate is adjusted to 0.15 A/min using the flow meter 7 using the gas flow rate adjustment valve 6. The standard gas passes through the switching cock 8, the check valve 9, the gas-liquid separator 12, the glass wool 13, the electronic dehumidifier 14, the magnesium perchlorate 15, and reaches the non-dispersive infrared absorption photometer 16, where it is Adjust the span to the standard gas concentration and check the non-dispersive infrared absorption photometer 16. The CO2 standard gas is used to span the non-dispersive infrared spectrophotometer 16 and check the instrument.
切替コック５をＮ２ガス圧力調整バルブ３側、切替コッ
ク８を逆止弁９側に切替える。Switch the switching cock 5 to the N2 gas pressure adjustment valve 3 side and switch the switching cock 8 to the check valve 9 side.
Ｎ、ガス圧力調整バルブ３を開いて、Ｎ２ガス流量がガ
ス流量計７で規定流量（キャリアーガスの流量は通常０
．１５１７ ｍｉｎ、である）になるようにガス流量調
整バルブ６で調節する。Open the N gas pressure adjustment valve 3, and check the N2 gas flow rate at the specified flow rate using the gas flow meter 7 (the carrier gas flow rate is normally 0).
．． 1517 min) using the gas flow rate adjustment valve 6.
ＣＯ７気化器１０に硫酸（規定の希釈率、１＋５０）を
規定量（８〜ｌ０ｍ１）入れる。A specified amount (8 to 10 ml) of sulfuric acid (specified dilution rate, 1+50) is put into the CO7 vaporizer 10.
切替コック８を気化器ｌＯ側に切替える。Ｎ２ガス流量
が低下するので再度ガス流量調整バルブ６でガス流量を
規定流量（０，１５１／ｍｉｎ、 ）に調節する。Switch the switching cock 8 to the carburetor lO side. Since the N2 gas flow rate decreases, the gas flow rate is adjusted again to the specified flow rate (0.151/min) using the gas flow rate adjustment valve 6.
記録計１７のベースラインが安定したら、測定準備完了
となる。When the baseline of the recorder 17 becomes stable, preparation for measurement is completed.
測定は、気化器１０の注入口からフィルター付マイクロ
シリンジ１１で測定試料の規定量（含ＣＯ２世に応じて
通常、５μｍ〜５ｍ１）を注入する。For the measurement, a specified amount of the sample to be measured (usually 5 μm to 5 ml depending on the CO2 content) is injected from the inlet of the vaporizer 10 using the microsyringe 11 with a filter.
注入後、約５分以内に記録計１７にＣＯ２のピークが出
る。After injection, a CO2 peak appears on the recorder 17 within about 5 minutes.
記録紙上の波高を測定して、検量線からＣＯ２濃度を求
める。The wave height on the recording paper is measured and the CO2 concentration is determined from the calibration curve.
以上説明した、第１図に示す本発明に係る測定方法を実
施するための分析装置を用いて異なる箇所から採取した
分析サンプルＡ、Ｂ、Ｃの液中溶存二酸化炭素の測定を
行った。The dissolved carbon dioxide in the liquid of analysis samples A, B, and C collected from different locations was measured using the analyzer for carrying out the measurement method according to the present invention as shown in FIG. 1 as described above.
サンプル−件当たりの測定の所要時間は５分以内である
ことが記録紙から確認された。It was confirmed from the recording paper that the time required for measurement per sample was within 5 minutes.
また、サンプルの測定結果を従来法（中和滴定法）と比
較して第１表に示す。Ａ、 Ｂ、 Ｃはサンプル採取箇
所、ｎは採取時点が異なることを示す。Table 1 also shows the measurement results of the samples in comparison with the conventional method (neutralization titration method). A, B, and C indicate sample collection locations, and n indicates different sampling times.
第
表
該表かられかるように、従来法では測定結果としての数
値が低く出ており、これは分析操作中におけるＣＯ２の
吸収により生じた誤差であると推定される。すなわち、
本発明の測定方法によれば高精度な測定結果が得られる
ことがわかる。As can be seen from Table 1, the measurement results obtained using the conventional method are low, and this is presumed to be an error caused by the absorption of CO2 during the analytical operation. That is,
It can be seen that highly accurate measurement results can be obtained according to the measurement method of the present invention.
本発明の、水中の溶存二酸化炭素をＣＯ２気化手段と非
分散型赤外線吸光光度計とを組み合わせた分析装置を用
いた測定方法によれば、サンプル１外光たりの測定所要
時間がサンプル注入後５分以内という短時間で測定可能
となり、かつ測定値も高精度なため、その効果は極めて
大きいものである。According to the method of measuring dissolved carbon dioxide in water using an analyzer combining a CO2 vaporization means and a non-dispersive infrared absorption photometer according to the present invention, the time required for measurement per external light of one sample is 55 minutes after injection of the sample. The effect is extremely large because it can be measured in a short time, within minutes, and the measured values are highly accurate.
第１図は本発明に係る測定方法を実施するための装置例
の概略図である。
１・・・・Ｎ、ガスボンベ、
２・・・・Ｃ０２標準ガスボンベ、
３・・・・Ｎ２ガス圧力調整バルブ、
４・・・・ＣＯ２標準ガス圧力調整バルブ、５・・・・
切替コック、
６・・・・ガス流量調整／＜ルブ、
７・・・・ガス流量計、 ８・・・・切替コ・ツク、
９・・・・逆止弁、 ＩＯ・・・・気化器、１１・
・・・フィルター付マイクロシリンジ、１２・・・・気
液分離器、 １３・・・・ガラスウール、１４・・・・
電子除湿器、
１５・・・・過塩素酸マグネシウム、
１６・・・・非分散型赤外線吸光光度計、１７・・・・
記録計FIG. 1 is a schematic diagram of an example of an apparatus for carrying out the measuring method according to the present invention. 1...N gas cylinder, 2...C02 standard gas cylinder, 3...N2 gas pressure adjustment valve, 4...CO2 standard gas pressure adjustment valve, 5...
Switching cock, 6...Gas flow rate adjustment/<lub, 7...Gas flow meter, 8...Switching cock,
9... Check valve, IO... Carburizer, 11...
... Microsyringe with filter, 12 ... Gas-liquid separator, 13 ... Glass wool, 14 ...
Electronic dehumidifier, 15... Magnesium perchlorate, 16... Non-dispersive infrared absorption photometer, 17...
recorder
Claims (1)
溶存二酸化炭素の気化手段と非分散型赤外線吸光光度計
とを組み合わせた分析装置により、測定することを特徴
とする水中の溶存二酸化炭素の測定方法。1. Measurement of dissolved carbon dioxide in water, characterized in that when measuring dissolved carbon dioxide in water, the measurement is carried out using an analysis device that combines means for vaporizing the dissolved carbon dioxide in water and a non-dispersive infrared absorption photometer. Method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2222518A JPH04105042A (en) | 1990-08-27 | 1990-08-27 | Measuring method for underwater dissolved coal dioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2222518A JPH04105042A (en) | 1990-08-27 | 1990-08-27 | Measuring method for underwater dissolved coal dioxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04105042A true JPH04105042A (en) | 1992-04-07 |
Family
ID=16783685
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2222518A Pending JPH04105042A (en) | 1990-08-27 | 1990-08-27 | Measuring method for underwater dissolved coal dioxide |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04105042A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20010090641A (en) * | 2000-04-10 | 2001-10-19 | 손정익 | Infrared CO2 analyzing system using sample injection method |
| CN105203502A (en) * | 2015-08-14 | 2015-12-30 | 北京大学 | In-situ online collection analysis meter and method for aerosol carbonaceous components |
-
1990
- 1990-08-27 JP JP2222518A patent/JPH04105042A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20010090641A (en) * | 2000-04-10 | 2001-10-19 | 손정익 | Infrared CO2 analyzing system using sample injection method |
| CN105203502A (en) * | 2015-08-14 | 2015-12-30 | 北京大学 | In-situ online collection analysis meter and method for aerosol carbonaceous components |
| CN105203502B (en) * | 2015-08-14 | 2017-11-07 | 北京大学 | A kind of aerosol carbonaceous components online acquisition analyzer in situ and its method |
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