JPH04157182A - Method for continuously measuring acidity - Google Patents
Method for continuously measuring acidityInfo
- Publication number
- JPH04157182A JPH04157182A JP27892590A JP27892590A JPH04157182A JP H04157182 A JPH04157182 A JP H04157182A JP 27892590 A JP27892590 A JP 27892590A JP 27892590 A JP27892590 A JP 27892590A JP H04157182 A JPH04157182 A JP H04157182A
- Authority
- JP
- Japan
- Prior art keywords
- hydrogen
- acidity
- hydrogen gas
- gas
- concentration
- 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 abstract description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 239000001257 hydrogen Substances 0.000 claims abstract description 17
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 17
- 239000012159 carrier gas Substances 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims description 25
- 239000002923 metal particle Substances 0.000 claims description 5
- 239000002184 metal Substances 0.000 abstract description 5
- 229910052751 metal Inorganic materials 0.000 abstract description 5
- 239000012488 sample solution Substances 0.000 abstract description 4
- 238000011109 contamination Methods 0.000 abstract description 3
- 238000005275 alloying Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 11
- 239000000523 sample Substances 0.000 description 8
- 239000011701 zinc Substances 0.000 description 8
- 239000002253 acid Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 229910052725 zinc Inorganic materials 0.000 description 4
- 238000005259 measurement Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 238000000691 measurement method Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 238000009125 cardiac resynchronization therapy Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 239000007793 ph indicator Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- ing And Chemical Polishing (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は液中の酸度評価、例えばテレビ、 ＣＲＴ等の
シャドーマスク製造用のエツチング液（以下Ｅ液）の酸
度測定を行う連続的酸度測定方法に関する。[Detailed Description of the Invention] [Field of Industrial Application] The present invention is a continuous acidity measurement method for evaluating the acidity in a liquid, for example, measuring the acidity of an etching solution (hereinafter referred to as E solution) for manufacturing shadow masks for televisions, CRTs, etc. Regarding the method.
従来は、−船釣には試料液をピペット等により採取し、
電位差またはｐＨ指示薬を用いて標準アルカリ液により
滴定し定量してきた。さらには試料液を分取し純水等に
より希釈してｐＨ計または他の水質分析計で測定した。Conventionally, when fishing on a boat, the sample liquid was collected using a pipette, etc.
It has been quantified by titration with a standard alkaline solution using a potential difference or a pH indicator. Furthermore, the sample liquid was taken out, diluted with pure water, etc., and measured with a pH meter or other water quality analyzer.
上記従来技術では次のような問題点があった。 The above conventional technology has the following problems.
（１）手作業にともなう個人的誤差がある。(1) There are individual errors associated with manual work.
（２）測定が非連続かつ、かなりの測定時間を必要とす
る。(2) Measurement is discontinuous and requires a considerable amount of measurement time.
（３）Ｅ液等の酸度変化が手分析では連続的に把握でき
ずかつＥ液の酸度制御がリアルタイムで実施できにくい
。(3) Changes in the acidity of liquid E, etc. cannot be continuously monitored by manual analysis, and it is difficult to control the acidity of liquid E in real time.
（４）一方Ｅ液は強い腐食作用を有しかつＥｌ中には一
般にエツチングによる多量の金属ビオ２１粒子状物質等
を含む。(4) On the other hand, the E solution has a strong corrosive effect, and the El generally contains a large amount of metal bio-21 particulate matter due to etching.
このため、従来技術のｐＨ計または他の水質分析計（以
下ｐＨ計等）による自動・連続分析を試みたとしても検
出器の損傷、汚染等による不具合が生じ、液相でＥ液の
酸度分析を行なうことには多くの不具合がある。For this reason, even if automatic and continuous analysis is attempted using a conventional pH meter or other water quality analyzer (hereinafter referred to as a pH meter, etc.), problems may occur due to damage to the detector, contamination, etc., and acidity analysis of liquid E in the liquid phase may occur. There are many drawbacks to doing so.
本発明は上記課題を解決するため次の手段を講する。 The present invention takes the following measures to solve the above problems.
すなわち、連続的酸度測定方法として、連続的に一定量
の試料液を、金属粒を充填した反応塔シこ送って水素ガ
スを発生させ、上記反応塔にキャリヤガスを送って、上
記水素ガスを水素分析計に導き水素ガス濃度を求め、同
水素ガス濃度より上記試料液の酸度をデータ処理器によ
り計算するようにした。That is, as a continuous acidity measurement method, a fixed amount of sample liquid is continuously sent through a reaction tower filled with metal particles to generate hydrogen gas, and a carrier gas is sent to the reaction tower to generate the hydrogen gas. The sample solution was introduced into a hydrogen analyzer to determine the hydrogen gas concentration, and the acidity of the sample solution was calculated from the hydrogen gas concentration using a data processor.
〔作 用］
上記手段により、連続的に一定量の試料液が、金属粒を
充填した反応塔に送られる。反応塔で試料液と金属粒が
反応し水素ガスが発生する。反応塔にキャリヤガスが送
られ、上記水素ガスがキャリヤガスとともに水素分析計
に導かれ、水素ガス濃度が計測される。計測濃度がデー
タ処理器に入力され試料液の酸度が計算出力される。[Function] By the above means, a certain amount of sample liquid is continuously sent to a reaction tower filled with metal particles. The sample liquid and metal particles react in the reaction tower, generating hydrogen gas. A carrier gas is sent to the reaction tower, and the hydrogen gas is led together with the carrier gas to a hydrogen analyzer, where the hydrogen gas concentration is measured. The measured concentration is input to the data processor, and the acidity of the sample liquid is calculated and output.
このようにして試料液の酸度が連続的に測定されるよう
になる。したがってプラント等に使用すれば酸液の連続
的検出方法として、プラントの制御等に大いに役立つ。In this way, the acidity of the sample liquid can be measured continuously. Therefore, if used in a plant etc., it will be very useful for plant control etc. as a method for continuously detecting acid liquid.
１実施例：
本発明の方法に係る一実施例を第１図と第２図により説
明する。1 Embodiment: An embodiment of the method of the present invention will be described with reference to FIGS. 1 and 2.
第１図にて、Ｅｅ本流配管１０から分岐して、順次弁２
１．フィルタ１．フィーダ７、流量計３１を経て反応塔
２の上部入口につながれる。またキャリヤガス源３から
順次弁２３．流量計３２を経て反応塔２の下部入口につ
ながれる。さらにＺｎ （亜鉛）貯蔵器１１は弁２５を
介して、反応塔２の上部につながれる。In FIG. 1, branching from the Ee main pipe 10, valves 2
1. Filter 1. It is connected to the upper inlet of the reaction tower 2 via a feeder 7 and a flow meter 31. Also, sequentially from the carrier gas source 3 to the valve 23. It is connected to the lower inlet of the reaction tower 2 via a flow meter 32. Furthermore, the Zn (zinc) storage 11 is connected to the upper part of the reaction column 2 via a valve 25.
また反応塔２の上端部から、順次ガス洗浄器４゜ガス分
取器、水素分析計５につながれる。水素分析計５の出力
はデータ処理システムへ送られる。Further, the upper end of the reaction tower 2 is connected to a gas scrubber 4, a gas fractionator, and a hydrogen analyzer 5 in this order. The output of hydrogen analyzer 5 is sent to a data processing system.
以上の構成において、Ｅ液本流配管ｌＯから、Ｅ液がフ
ィーダ７によって、一定の流量で、フィルタ１で除しん
された後、流量計３１を経て反応塔２に送られる。In the above configuration, the E liquid is removed from the E liquid main flow pipe 10 by the feeder 7 at a constant flow rate by the filter 1, and then sent to the reaction tower 2 via the flow meter 31.
一方、反応塔２にはＺｎ貯藏器１１から粒子状亜鉛が弁
２５を経て反応塔２に常に充填されている。したがって
反応塔２において、（１）式の反応により水素ガスが発
生する。On the other hand, the reaction tower 2 is always filled with particulate zinc from the Zn storage vessel 11 via the valve 25. Therefore, in the reaction tower 2, hydrogen gas is generated by the reaction of formula (1).
Ｚｎ−’−，２ＨＣＲ−＋ＺｎＣＲ２＋Ｈｚ
−−−−−−１１）発生した水素ガスは、キャリヤガス
源３から流量計３２を経て、一定流量で送られるキャリ
ヤガスとともにガス洗浄器４に送られ、洗浄される。そ
の後、ガス分取器９で分取され、水素分析計５へ送られ
、水素濃度が測定される。水素濃度信号はデータ処理シ
ステム６へ送られ、Ｅ液の酸濃度が算出され、親プラン
トの制御装置にフィードバックされ利用される。Zn-'-, 2HCR-+ZnCR2+Hz
-------11) The generated hydrogen gas is sent from the carrier gas source 3 through the flow meter 32 to the gas washer 4 together with the carrier gas sent at a constant flow rate, where it is cleaned. Thereafter, the gas is fractionated by the gas separator 9 and sent to the hydrogen analyzer 5, where the hydrogen concentration is measured. The hydrogen concentration signal is sent to the data processing system 6, where the acid concentration of liquid E is calculated, and fed back to the control device of the parent plant for use.
水素濃度はキャリヤガス量、Ｅ液量、が一定量であれば
Ｅ液の酸濃度に比例するからデータ処理システム６で直
ちに酸濃度が算出できる。If the amount of carrier gas and the amount of E liquid are constant, the hydrogen concentration is proportional to the acid concentration of E liquid, so the data processing system 6 can immediately calculate the acid concentration.
以上に準した装置を組立て、実施した結果を以下に示す
。The results of assembling and implementing a device based on the above are shown below.
−Ｈｃｚｉ１度 ２ｇ／ｌ ｔＭ’Ｊ液。-Hczi 1 degree 2 g/l tM'J liquid.
（０，０５４８ｍｏｌ／ ｌ ）
・液供給量 １００ ｄ／ｗｉｎ・反応塔
２０閣φＸ２５０ｍＨ・充填金属 Ｚｎ粒（
粒径３ｆｆｌＩＩｌφ平均）約１００ｇｒ 充填
・キャリヤガス 空気
５００ ｄ／ｍｉｎ
・洗浄器 純水、接液層高約１５０圓・ガス分
取量 １００ａｆ／ｍｉｎ （分析計へ）・分析計
接触酸化式水素計、入口ガス温度２０°Ｃ１
分析結果の時間変化を第２回に示す。(0,0548mol/l) ・Liquid supply amount 100 d/win・Reaction tower
20 cabinets φX250mH・Filled metal Zn grains (
Particle size 3fflIIlφ average) approx. 100gr Filling/Carrier gas Air 500 d/min Cleaner Pure water, wetted layer height approx. 150mm Gas separation amount 100af/min (to analyzer) Analyzer Contact oxidation hydrogen meter , inlet gas temperature 20° C. The time changes in the analysis results are shown in the second part.
第２閏で求めた平均水素濃度は１０４６％であった。The average hydrogen concentration determined in the second leap was 1046%.
反応計算から求めた水素濃度は１０．７％である。The hydrogen concentration determined from reaction calculations was 10.7%.
測定結果は多少の誤差、水芸気圧補正における温度の変
動等を考慮すれば非常によく液中の算濃度を把握できて
いることを裏付けている。The measurement results confirm that the calculated concentration in the liquid can be determined very well if some errors and temperature fluctuations due to water pressure correction are taken into account.
検出器についてはガスクロマトグラフ、空気密度方式な
ども応用したが、いずれも所期の目的を達成できた。し
たがって本実施例はＥ液の酸度を把握しうる有力な手段
となり、かつ発生するガスは洗浄もされてクリーンであ
り分析計の損耗につながることもない。Gas chromatographs and air density methods were also used as detectors, and both were able to achieve the intended purpose. Therefore, this embodiment is an effective means for determining the acidity of liquid E, and the generated gas is clean and does not cause wear and tear on the analyzer.
以上では、試料として、塩酸で説明したが他の酸でもよ
い。また金属も亜鉛粒を使用したが錫等でもよい。In the above explanation, hydrochloric acid was used as the sample, but other acids may be used. Furthermore, although zinc particles were used as the metal, tin or the like may also be used.
以上に説明したように、本発明は次の効果を奏する。 As explained above, the present invention has the following effects.
（］）強い腐食性を有する強酸の液の酸度を測定する方
法として、亜鉛、錫などの金属粒と液を所定量づつ反応
させ発生する水素をキャリヤガスによって水素分析計に
送り、水素ガス濃度のみを測定することによりほぼ連続
的にかつ条件設定後は無人に近い状態で酸度が求められ
る。( ]) As a method of measuring the acidity of a strong acid solution that has strong corrosive properties, the hydrogen gas generated by reacting a predetermined amount of the solution with metal particles such as zinc or tin is sent to a hydrogen analyzer using a carrier gas, and the hydrogen gas concentration is By measuring only the acidity, the acidity can be determined almost continuously and almost unattended after the conditions are set.
（２） ｐＨ電極法等にみられる直接法ではないため
、検出器の汚染、損耗もなく、長時間、安定して液の酸
度を正確に知ることができる。(2) Since it is not a direct method such as the pH electrode method, there is no contamination or wear and tear on the detector, and the acidity of the liquid can be accurately determined over a long period of time.
第１図は本発明の一実施例の構成系統図、第２図は同実
施例の作用説明図である。
１・・・フィルタ、 ２・・・反応塔。
３・・・キャリヤガス源、４・・・ガス洗浄器。
５・・・水素分析計、 ６・・・データ処理システ
ム。
７・・・フィーダ、 ８・・・温度計。
９・・・ガス分取器、１０・・・Ｅ液本流。
１１・・・Ｚｎ貯蔵器。FIG. 1 is a structural diagram of an embodiment of the present invention, and FIG. 2 is an explanatory diagram of the operation of the embodiment. 1... Filter, 2... Reaction tower. 3...Carrier gas source, 4...Gas cleaner. 5...Hydrogen analyzer, 6...Data processing system. 7... Feeder, 8... Thermometer. 9...Gas separator, 10...E liquid main stream. 11...Zn storage.
Claims (1)
に送って水素ガスを発生させ、上記反応塔にキャリヤガ
スを送って、上記水素ガスを水素分析計に導き水素ガス
濃度を求め、同水素ガス濃度より上記試料液の酸度をデ
ータ処理器により計算することを特徴とする連続的酸度
測定方法。A certain amount of sample liquid is continuously sent to a reaction tower filled with metal particles to generate hydrogen gas, a carrier gas is sent to the reaction tower, and the hydrogen gas is led to a hydrogen analyzer to determine the hydrogen gas concentration. , a continuous acidity measuring method characterized in that the acidity of the sample liquid is calculated by a data processor from the hydrogen gas concentration.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27892590A JPH04157182A (en) | 1990-10-19 | 1990-10-19 | Method for continuously measuring acidity |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27892590A JPH04157182A (en) | 1990-10-19 | 1990-10-19 | Method for continuously measuring acidity |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04157182A true JPH04157182A (en) | 1992-05-29 |
Family
ID=17603995
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP27892590A Pending JPH04157182A (en) | 1990-10-19 | 1990-10-19 | Method for continuously measuring acidity |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04157182A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0531149A2 (en) * | 1991-09-05 | 1993-03-10 | C. Uyemura & Co, Ltd | Etching rate determining method and apparatus |
-
1990
- 1990-10-19 JP JP27892590A patent/JPH04157182A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0531149A2 (en) * | 1991-09-05 | 1993-03-10 | C. Uyemura & Co, Ltd | Etching rate determining method and apparatus |
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