JP3343161B2 - Moisture measurement method - Google Patents
Moisture measurement methodInfo
- Publication number
- JP3343161B2 JP3343161B2 JP31875493A JP31875493A JP3343161B2 JP 3343161 B2 JP3343161 B2 JP 3343161B2 JP 31875493 A JP31875493 A JP 31875493A JP 31875493 A JP31875493 A JP 31875493A JP 3343161 B2 JP3343161 B2 JP 3343161B2
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- JP
- Japan
- Prior art keywords
- water
- sample
- absorbance
- surfactant
- 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.)
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Description
【0001】[0001]
【産業上の利用分野】本発明は、水分濃度未知の試料中
に溶解又は分散している水分量を測定する方法に関し、
更に詳細には、電子部品又は精密部品類の洗浄液等にお
ける水分濃度測定に好適な水分測定方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for measuring the amount of water dissolved or dispersed in a sample whose water concentration is unknown.
More specifically, the present invention relates to a moisture measuring method suitable for measuring a moisture concentration in a cleaning solution or the like of electronic parts or precision parts.
【0002】[0002]
【従来の技術及び発明が解決しようとする課題】従来、
溶液中の水分濃度を測定する方法としては、赤外吸収
法、誘電率法、超音波速度法、カールフィッシャー法等
が使用されていたが、これらの測定方法は、測定機器が
高価であったり、測定操作に熟練を要すなどの問題があ
り、安価で簡便な水分測定方法が必要とされていた。2. Description of the Related Art
As a method for measuring the water concentration in a solution, an infrared absorption method, a dielectric constant method, an ultrasonic velocity method, a Karl Fischer method, and the like have been used.However, these measurement methods require expensive measurement equipment. In addition, there is a problem that the measurement operation requires skill, and an inexpensive and simple method for measuring moisture has been required.
【0003】一方、精密部品又は治工具類等の洗浄分野
においては、近年オゾン層破壊防止の面から、廃止が進
められている塩素系溶剤及びフロン系溶剤を用いる洗浄
液の代替品として、テルペン系溶剤、炭化水素系溶剤、
アルコール系溶剤等の溶剤系洗浄液や、界面活性剤等を
含有する水系洗浄液等の代替洗浄液が開発されている。On the other hand, in the field of cleaning precision parts and jigs, terpene-based cleaning liquids have been replaced with chlorine-based and chlorofluorocarbon-based cleaning liquids, which have been abolished in recent years in order to prevent ozone layer destruction. Solvent, hydrocarbon solvent,
Alternative cleaning liquids such as a solvent-based cleaning liquid such as an alcohol-based solvent and an aqueous cleaning liquid containing a surfactant or the like have been developed.
【0004】上記代替洗浄液においては、溶剤や界面活
性剤の持つ引火性を無くして非危険物化する目的で水を
添加しているものもあり、このような代替洗浄液で洗浄
を行なう場合、洗浄液中の水分がある濃度以下になると
洗浄液が危険物化し、逆に水分がある濃度以上になると
洗浄効率が低下するため水分管理が必須である。このよ
うな理由から、洗浄分野においても上述の如き水分測定
方法が用いられているが、前記溶液中の水分濃度を測定
する場合と同様に安価で簡便な水分測定方法が必要とさ
れていた。In some of the above alternative cleaning solutions, water is added for the purpose of eliminating the flammability of the solvent or the surfactant and making the material non-hazardous. When the water content is lower than a certain concentration, the cleaning liquid becomes a hazardous substance. On the contrary, when the water content is higher than a certain concentration, the cleaning efficiency is reduced, so that water management is essential. For this reason, the above-described method for measuring the moisture content is also used in the field of cleaning. However, as in the case of measuring the concentration of moisture in the solution, an inexpensive and simple method for measuring the moisture content has been required.
【0005】安価で簡便に測定する方法として、分析化
学の分野では、濾紙に塩化コバルト水溶液を含ませ乾燥
させた試験紙を用いる方法(特開平2−91551号公
報)があるが、上記試験紙は、空気中の水分を吸収して
しまうため非常に不安定であり、正確な測定が困難であ
るという問題があった。In the field of analytical chemistry, there is a method of inexpensively and simply measuring using a test paper obtained by drying a filter paper containing an aqueous solution of cobalt chloride (JP-A-2-91551). Is very unstable because it absorbs moisture in the air, and there is a problem that accurate measurement is difficult.
【0006】また、無水エチルアルコールに塩化コバル
ト(II)無水和物を溶解して得られる671nmに吸収
極大を持つ溶液に水を加えると、吸光度が変化すること
を利用した水分の定量方法〔日本化学会編“新実験化学
講座15 分析”p121(1991)〕も報告されて
いるが、該方法では、疎水性試料を測定する際に、均一
な液が得られない場合があった。又、発色効率が低いた
め、試料が多く必要となり、着色した試料を測定する場
合に色の識別が困難になるという問題点があった。Also, a method for quantifying water utilizing the fact that when water is added to a solution having an absorption maximum at 671 nm obtained by dissolving cobalt (II) chloride anhydrate in anhydrous ethyl alcohol, the absorbance changes [Japan “Chemical Society of Japan,“ New Experimental Chemistry Lecture 15 Analysis ”p121 (1991)] has been reported, but in this method, when measuring a hydrophobic sample, a uniform liquid could not be obtained in some cases. In addition, since the coloring efficiency is low, a large number of samples are required, and there is a problem that it is difficult to identify colors when measuring a colored sample.
【0007】従って、本発明の目的は、水分濃度未知の
試料中の水分を、簡便且つ安価に、しかも広範囲の水分
濃度において精度良く測定することができる水分測定方
法を提供することにある。Accordingly, it is an object of the present invention to provide a method for measuring moisture in a sample whose moisture concentration is unknown, which can be simply and inexpensively measured with high accuracy over a wide range of moisture concentrations.
【0008】[0008]
【課題を解決するための手段】本発明者らは、塩化コバ
ルトのアルコール溶液が水分により変色することに着目
して種々検討を重ねた結果、ハロゲン化コバルト又はハ
ロゲン化銅を界面活性剤と疎水性溶媒との混合液に溶解
した水分測定試薬を用いて検量線を作成することによ
り、上記目的を達成し得ることを見出し、本発明を完成
するに至った。The present inventors have SUMMARY OF THE INVENTION As a result of extensive studies by paying attention to the alcoholic solution of cobalt chloride is discolored by water, a halogenated cobalt or copper halide and surfactant hydrophobic The inventors have found that the above object can be achieved by preparing a calibration curve using a water measurement reagent dissolved in a mixed solution with a neutral solvent, and have completed the present invention.
【0009】即ち、本発明は、各々水分濃度の異なる複
数の水分濃度既知の検定液に、ハロゲン化コバルト又は
ハロゲン化銅を界面活性剤と疎水性溶媒との混合液に溶
解した水分測定試薬を、各々所定の割合で添加混合し
て、水分濃度に応じて着色度の異なる複数の標本を作成
し、上記水分測定試薬における上記ハロゲン化コバルト
又はハロゲン化銅と上記界面活性剤との割合が、上記界
面活性剤100重量部に対して、上記ハロゲン化コバル
ト又はハロゲン化銅0.1〜2.0重量部であり、得ら
れた各標本の所定温度における所定の吸収波長の吸収度
を測定し、各標本の吸収度と水分濃度との関係を表す検
量線を作成し、一方、水分濃度が未知の試料である、界
面活性剤及び/又は溶剤と水とを含有する洗浄液に、上
記水分測定試薬を、上記所定割合にて添加混合して該試
料を着色し、着色した該試料の上記所定温度における上
記の所定の吸収波長の吸収度を測定し、着色した上記試
料の吸収度と上記検量線とから、上記試料の水分を定量
することを特徴とする水分測定方法を提供するものであ
る。That is, according to the present invention, cobalt halide or copper halide is dissolved in a mixture of a surfactant and a hydrophobic solvent in a plurality of test solutions having different water concentrations and known in water concentration. The water measurement reagents were added and mixed at predetermined ratios to prepare a plurality of samples having different degrees of coloring according to the water concentration, and the cobalt halide in the water measurement reagent was prepared.
Or, the ratio of the copper halide and the surfactant is
With respect to 100 parts by weight of the surfactant,
0.1 to 2.0 parts by weight of copper halide or copper halide, and measures the absorbance at a predetermined absorption wavelength at a predetermined temperature of each obtained sample, and expresses the relationship between the absorbance of each sample and the moisture concentration. A calibration curve was created, while the boundary was
The water measurement reagent is added and mixed at a predetermined ratio to a cleaning solution containing a surfactant and / or a solvent and water to color the sample, and the colored sample is colored at a predetermined temperature at the predetermined temperature. the absorption at the absorption wavelength is measured, and an absorbance and the calibration curve colored the sample, is to provide a moisture measuring how that comprises determining the moisture of the sample.
【0010】以下、本発明の水分測定方法について詳細
に説明する。本発明において標本を作成する際に用いら
れる検定液としては、水分と溶媒及び/又は界面活性剤
とを含有する溶液が挙げられる。上記溶媒としては、特
に限定されるものではないが、例えば、低級アルコール
(エタノール、イソプロピルアルコール等)、ケトン
(アセトン等)、グリコール類(ポリエチレングリコー
ル等)等の親水性溶媒が挙げられる。上記界面活性剤と
しては、特に限定されるものではないが、後述する試料
に用いられている界面活性剤として列挙した界面活性剤
と同様の物質が挙げられる。また、溶媒と界面活性剤と
を含有する場合は、溶媒として前記の親水性溶媒を用い
てもよく、ケロシン、ベンゼン、ヘキサン等の疎水性溶
媒を用いることもできる。[0010] will be described in detail below the onset Akira method of moisture measurement. As the test solution used when preparing a specimen in the present invention, a solution containing water, a solvent and / or a surfactant can be used. Examples of the solvent include, but are not particularly limited to, hydrophilic solvents such as lower alcohols (eg, ethanol and isopropyl alcohol), ketones (eg, acetone), and glycols (eg, polyethylene glycol). The surfactant is not particularly limited, and includes the same substances as the surfactants listed as surfactants used in the samples described below. When a solvent and a surfactant are contained, the above-mentioned hydrophilic solvent may be used as the solvent, and a hydrophobic solvent such as kerosene, benzene, and hexane may be used.
【0011】本発明において用いられる水分測定試薬
は、ハロゲン化コバルト又はハロゲン化銅を界面活性剤
と疎水性溶媒との混合液に溶解した試薬である。[0011] The water content measuring reagent used in the present invention comprises cobalt halide or copper halide as a surfactant.
And a reagent dissolved in a mixed solution of a solvent and a hydrophobic solvent .
【0012】上記水分測定試薬に用いられる上記ハロゲ
ン化コバルト又はハロゲン化銅におけるハロゲンとして
は、特に限定されないが、塩素又は臭素が好ましく、ま
た、上記ハロゲン化コバルトとしては、塩化コバルト、
臭化コバルト等が挙げられ、上記ハロゲン化銅として
は、塩化銅、臭化銅等が挙げられる。また、コバルトの
吸収度は銅の吸収度より大きいので、特にハロゲン化コ
バルトが好ましい。上記水分測定試薬における上記ハロ
ゲン化コバルト又はハロゲン化銅と、界面活性剤と疎水
性溶媒との混合液とを溶解させる割合は、界面活性剤1
00重量部に対して、上記ハロゲン化コバルト又はハロ
ゲン化銅0.1〜2.0重量部である。The halogen in the cobalt halide or copper halide used in the water content measuring reagent is not particularly limited, but is preferably chlorine or bromine. Examples of the cobalt halide include cobalt chloride,
Cobalt bromide and the like are mentioned, and the above-mentioned copper halide is, for example, copper chloride and copper bromide. Further, since the absorbance of cobalt is larger than that of copper, cobalt halide is particularly preferable. The cobalt halide or the copper halide in the water measurement reagent , a surfactant and a hydrophobic agent;
Proportion of dissolving the mixture of sexual solvents, interfacial active agent 1
Against 00 parts by weight, the halogenated cobalt or copper halide 0. 1 to 2.0 parts by weight.
【0013】上記水分測定試薬に用いられる上記界面活
性剤としては、アニオン性、カチオン性、両イオン性、
非イオン性界面活性剤が用いられるが、水分測定の精度
を考慮すると、活性剤製品中の水分が少ない非イオン性
界面活性剤(ノニオン性界面活性剤)が好ましく、具体
例としては、下記の化合物等が挙げられる。The above-mentioned surfactant used in the above-mentioned moisture measuring reagent includes anionic, cationic, zwitterionic,
Nonionic surfactants are used, but in consideration of the accuracy of moisture measurement, nonionic surfactants (nonionic surfactants) having a small amount of water in the surfactant product are preferable, and specific examples include the following. And the like.
【0014】上記非イオン性界面活性剤としては、例え
ばアルキルエーテル型、アルキルアリルエーテル型、ア
ルキルチオエーテル型等のエーテル型;アルキルエステ
ル型、ソルビタンアルキルエステル型等のエステル型;
ポリオキシアルキレンアルキルアミン等のアミンとの縮
合型;ポリオキシアルキレンアルキルアマイド等のアミ
ドとの縮合型;ポリオキシエチレンとポリオキシプロピ
レンとをランダム又はブロック縮合させたプルロニック
又はテトロニック型;ポリエチレンイミン系等の界面活
性剤が挙げられる。陰イオン性界面活性剤としては、ア
ルキルベンゼンスルホン酸塩、アルキル又はベンゼンス
ルホン酸塩、アルキル又はアルケニルエーテル硫酸塩、
アルキル又はアルケニル硫酸塩、オレフィンスルホン酸
塩、アルカンスルホン酸塩、高級脂肪酸塩、α−スルホ
脂肪酸塩又はエステル、アルキル又はアルケニルエーテ
ルのカルボン酸塩等が挙げられる。陽イオン性界面活性
剤及び両性界面活性剤としては、アルキル又は/及びア
ルケニルアミン塩、第4級アンモニウム塩、アルキルベ
タイン、アルキルアミンオキサイド、アルキルアラニ
ン、ポリアミート、ポリアミン塩、イミダゾリン型両性
界面活性剤、スルホベタイン型両性界面活性剤等が挙げ
られる。ここで、常温で液体又は固体のいずれの界面活
性剤も、用いることができる。Examples of the nonionic surfactant include ether types such as alkyl ether type, alkyl allyl ether type and alkyl thioether type; ester types such as alkyl ester type and sorbitan alkyl ester type;
Condensed type with an amine such as polyoxyalkylene alkylamine; Condensed type with an amide such as polyoxyalkylene alkyl amide; Pluronic or tetronic type obtained by random or block condensation of polyoxyethylene and polyoxypropylene; Polyethyleneimine And the like. Examples of the anionic surfactant include alkyl benzene sulfonate, alkyl or benzene sulfonate, alkyl or alkenyl ether sulfate,
Examples thereof include an alkyl or alkenyl sulfate, an olefin sulfonate, an alkane sulfonate, a higher fatty acid salt, an α-sulfofatty acid salt or ester, and a carboxylate of an alkyl or alkenyl ether. Examples of the cationic surfactant and the amphoteric surfactant include an alkyl or / and alkenyl amine salt, a quaternary ammonium salt, an alkyl betaine, an alkyl amine oxide, an alkyl alanine, a polyamine, a polyamine salt, an imidazoline type amphoteric surfactant, And sulfobetaine-type amphoteric surfactants. Here, any surfactant liquid or solid at normal temperature can also be used.
【0015】また、上記水分測定試薬は、上記ハロゲン
化コバルト又は上記ハロゲン化銅を上記界面活性剤と上
記疎水性溶媒との混合液に溶解した液として用いること
により、試料中の水分と水分測定試薬中のハロゲン化コ
バルト又はハロゲン化銅とが効率良く水和反応し発色の
効率が高くなり精度の良い測定を行うことができる。Further, the moisture measurement reagent Rukoto used on SL halogenated cobalt or the copper halide as a liquid which was dissolved in a mixture of the surfactant and the hydrophobic solvent
More, it is possible to perform good measure moisture and halogenated cobalt or copper halide moisture measurement reagent is accurate the higher the efficiency of efficiently hydration colored in a sample.
【0016】上記水分測定試薬に用いられる上記疎水性
溶媒としては、水を水和しにくい溶媒であれば、特に限
定されないが、水和量が小さいほどコバルトと水和する
水の量が増え、測定感度が上昇することから水和量が小
さければ小さい程よい。例えば、ケロシン、ベンゼン、
ヘキサン、キシレン等の炭化水素溶媒が挙げられる。上
記疎水性溶媒と上記界面活性剤との混合比率は、疎水性
溶媒、界面活性剤、試料の種類、水分量により変動する
ものであり、特に限定されるものではないが、界面活性
剤100重量部に対して、疎水性溶媒を10000重量
部以下とするのが好ましく、100〜3000重量部と
するのが更に好ましい。The hydrophobic solvent used in the moisture measuring reagent is not particularly limited as long as it is a solvent that does not easily hydrate water, but the smaller the hydration amount, the larger the amount of water that hydrates with cobalt. Since the measurement sensitivity increases, the smaller the amount of hydration, the better. For example, kerosene, benzene,
Examples include hydrocarbon solvents such as hexane and xylene. The mixing ratio of the upper <br/> Symbol hydrophobic solvent and the surfactant, a hydrophobic solvent, surfactant, type of sample, which varies with moisture content, but are not limited to, against surfactant 100 parts by weight, it is preferable to be less than 1 0000 parts by weight of hydrophobic solvent, further preferably set to 100 to 3000 parts by weight.
【0017】また、上記水分測定試薬には、水分測定時
に上記水分測定試薬の乳化が生じるような該水分測定試
薬と試料との組合わせの場合に、乳化を抑制し、精度の
良い測定をするために、必要に応じて乳化抑制剤を添加
することもできる。上記乳化抑制剤としては、乳化抑制
機能のある物質であれば特に限定されないが、高級脂肪
酸、高級アミン等が挙げられる。In the case of a combination of the water measurement reagent and the sample that causes the emulsification of the water measurement reagent during the water measurement, the water measurement reagent suppresses emulsification and performs accurate measurement. For this purpose, an emulsifier may be added as necessary. The emulsification inhibitor is not particularly limited as long as it has a function of suppressing emulsification, and examples thereof include higher fatty acids and higher amines.
【0018】また、上記水分測定試薬の調製時に、上記
ハロゲン化コバルト又はハロゲン化銅の溶解を容易にす
るために、エタノール等の低級アルコールを添加しても
良い。また、標本の変色域を調製するために予め水を添
加しても良い。Further, at the time of preparing the moisture measuring reagent, a lower alcohol such as ethanol may be added to facilitate dissolution of the cobalt halide or the copper halide. In addition, water may be added in advance to adjust the discoloration range of the specimen.
【0019】本発明において、水分測定に供される試料
は、界面活性剤及び/又は溶剤と水とを含有する洗浄液
である。[0019] In the present invention, a sample to be subjected to moisture measurement, interfacial active agent and / or washing solution containing the solvent and water
It is .
【0020】上記界面活性剤及び/又は溶剤と水とを含
有する洗浄液としては、具体的には、後述する溶剤の一
種又は二種以上の混合物に危険物化するのを防止するた
めに水を添加してなる溶剤系洗浄液;後述する界面活性
剤の一種又は二種以上の混合物と水とからなり、必要に
応じて上記溶剤を添加してなる水系洗浄液等が挙げら
れ、特に電子部品又は精密機械類の洗浄に用いられるフ
ロン代替洗浄液が好ましく挙げられる。The washing liquid containing the surfactant and / or the solvent and water is, specifically, added with water in order to prevent a solvent or a mixture of two or more solvents described below from becoming a hazardous substance. A solvent-based cleaning liquid comprising: a water-based cleaning liquid comprising one or a mixture of two or more surfactants described below and water, if necessary, to which the above-mentioned solvent is added. Preferable examples include a CFC-substitute cleaning solution used for cleaning of a kind.
【0021】上記洗浄液に含有される溶剤としては、特
に限定はないが、動植物から得られるd−リモネン等の
テルペン類を有効成分とするテルペン系溶剤、ケロシ
ン、ベンゼン、キシレン等の炭化水素を有効成分とする
炭化水素系溶剤、イソプロピルアルコール、エチルアル
コール、メチルアルコール等の低級アルコールを有効成
分とするアルコール系溶剤等が挙げられる。The solvent contained in the washing solution is not particularly limited, but terpene solvents containing terpenes such as d-limonene obtained from animals and plants as active ingredients, and hydrocarbons such as kerosene, benzene and xylene are effective. Examples thereof include a hydrocarbon solvent as a component, and an alcohol solvent containing a lower alcohol such as isopropyl alcohol, ethyl alcohol, and methyl alcohol as an active ingredient.
【0022】また、上記洗浄液に含有される界面活性剤
としては、アニオン性、カチオン性、両イオン性、非イ
オン性界面活性剤等が用いられるが電子部品等の部材へ
の影響を考慮すると、非イオン性界面活性剤が好まし
く、例えば、アルキルエーテル型、アルキルアリルエー
テル型、アルキルチオエーテル型等のエーテル型;アル
キルエステル型、ソルビタンアルキルエステル型等のエ
ステル型;ポリオキシアルキレンアルキルアミン等のア
ミンとの縮合型;ポリオキシアルキレンアルキルアマイ
ド等のアミドとの縮合型;ポリオキシエチレンとポリオ
キシプロピレンをランダム又はブロック縮合させたプル
ロニック又はテトロニック型;ポリエチレンイミン系等
の界面活性剤が挙げられ、これらのうち、特に、炭素数
4〜22の炭化水素基を有するものが好ましく挙げられ
る。As the surfactant contained in the cleaning solution, anionic, cationic, amphoteric, nonionic surfactants and the like are used, but considering the influence on members such as electronic parts, Nonionic surfactants are preferred, for example, alkyl ether type, alkyl allyl ether type, ether type such as alkyl thioether type; alkyl ester type, ester type such as sorbitan alkyl ester type; amine such as polyoxyalkylene alkylamine; Condensed type with an amide such as polyoxyalkylene alkyl amide; pluronic or tetronic type obtained by random or block condensation of polyoxyethylene and polyoxypropylene; and surfactants such as polyethyleneimine. Among them, in particular, hydrocarbons having 4 to 22 carbon atoms Those having a are preferably exemplified.
【0023】また、上記洗浄液としては、上記の成分の
ほか、必要に応じてビルダー、キレート剤、防錆剤、消
泡剤等の添加剤を含有するものでもよく、また、上記添
加剤を用途に応じて任意に2種以上組み合わせて使用し
たものでもよい。The washing liquid may contain additives such as a builder, a chelating agent, a rust preventive and an antifoaming agent, if necessary, in addition to the above-mentioned components. May be arbitrarily used in combination of two or more.
【0024】而して、本発明の洗浄液の水分測定方法
(一つの態様)を実施するには、各々水分濃度の異なる
複数の水分濃度既知の上記検定液に、上記水分測定試薬
を、各々所定割合で添加混合して、水分濃度に応じて着
色度の異なる複数の標本を作成し、得られた各標本の所
定温度における所定の吸収波長の吸収度を測定し、各標
本の吸収度と水分濃度との関係を表す検量線を作成し、
一方、水分濃度未知の上記試料に、上記水分測定試薬
を、上記所定割合にて添加混合して該試料を着色し、着
色した該試料の上記所定温度における上記の所定の吸収
波長の吸収度を測定し、着色した上記試料の吸収度と上
記検量線とから、上記試料の水分を定量する。In order to carry out the method (one embodiment) of measuring the water content of the cleaning liquid of the present invention, the above-mentioned water measurement reagents are respectively added to a plurality of the above-mentioned test liquids each having a different water concentration and having a known water concentration. The samples were added and mixed in proportions to prepare a plurality of samples having different degrees of coloring according to the water concentration, and the absorbance of each of the obtained samples at a predetermined absorption wavelength at a predetermined temperature was measured. Create a calibration curve representing the relationship with concentration,
On the other hand, to the sample whose water concentration is unknown, the water measurement reagent is added and mixed at the predetermined ratio to color the sample, and the absorbance of the colored sample at the predetermined temperature at the predetermined absorption wavelength is measured. From the measured and colored absorbance of the sample and the calibration curve, the water content of the sample is quantified.
【0025】上記の複数の検定液における各々の水分濃
度は、測定する試料において必要とされる水分濃度によ
り変動するものであり、特に限定されるものではない
が、例えば各々の水分濃度を0〜20重量%の範囲で測
定する場合は、0.1〜4重量%毎に異ならせるのが好
ましく、その個数も3〜40個とするのが好ましい。The water concentration in each of the plurality of test solutions varies depending on the water concentration required for the sample to be measured, and is not particularly limited. When the measurement is performed in the range of 20% by weight, it is preferable that the difference is made every 0.1 to 4% by weight, and the number thereof is also preferably 3 to 40.
【0026】上記水分測定試薬を上記検定液及び試料に
添加する際における上記所定割合は、検定液に含まれる
水分により適宜設定すればよいが、例えば検定液水分が
10重量%の場合、上記検定液1に対して、上記水分測
定試薬を0.5〜100の範囲とするのが好ましい。上
記所定割合が、0.5未満であると、試料中に含まれる
着色成分により水分測定試薬の吸収度の変化を判断でき
なくなる場合があり、また100を超えると、試薬の吸
収度の変化が小さくなり、誤差が大きくなるため好まし
くない。The above-mentioned predetermined ratio when the above-mentioned water measurement reagent is added to the above-mentioned test solution and the sample may be appropriately set depending on the water contained in the test solution. It is preferable that the above-mentioned water measurement reagent is set in the range of 0.5 to 100 with respect to the liquid 1. If the predetermined ratio is less than 0.5, it may not be possible to determine the change in the absorbance of the moisture measurement reagent due to the coloring components contained in the sample. It is not preferable because it becomes small and the error becomes large.
【0027】上記の着色した検定液及び着色した試料は
測定用容器に充填される(上記の着色した検定液を測定
用容器に充填したものは上記標本として用いられる)。
上記測定用容器としては、透明で吸収度の測定ができる
ものであれば特に限定されないが、ガラス製、石英製、
プラスチック製等のセル等が挙げられる。The colored assay solution and the colored sample are filled in a measuring container (the colored assay solution filled in the measuring container is used as the specimen).
The measurement container is not particularly limited as long as it is transparent and can measure the absorbance, but is made of glass, quartz,
A cell made of plastic or the like may be used.
【0028】本発明における上記の所定の吸収波長は、
用いる試薬により異なるが、例えば、塩化コバルトを使
用した場合には、550〜700nmに吸収が現れる。The predetermined absorption wavelength in the present invention is:
Depending on the reagent used, for example, when cobalt chloride is used, absorption appears at 550 to 700 nm.
【0029】本発明において、上記標本の吸収度を測定
する際における上記所定温度は、0〜70℃の範囲とす
るのが好ましい。上記温度が、0℃未満であると、検定
液が凍る可能性があり、また、70℃を超えると、測定
中に検定液中の水分が蒸発し、正しい水分濃度が測定で
きなくなるので好ましくない。In the present invention, the predetermined temperature when measuring the absorbance of the sample is preferably in the range of 0 to 70 ° C. If the temperature is lower than 0 ° C., the test solution may freeze, and if the temperature is higher than 70 ° C., the water in the test solution evaporates during the measurement, and the correct water concentration cannot be measured. .
【0030】そして、上記の各標本の上記所定温度にお
ける上記の吸収度を測定するには、吸収測定装置を用い
る等して測定することができる。上記吸収測定装置とし
ては、上記の所定の吸収波長の吸収度が定量できるもの
であれば、特に限定されないが、例えば、吸光光度計な
どが挙げられ、該吸光光度計を用いた場合には、上記吸
収度は吸光度として求められる。In order to measure the absorbance of each of the above-mentioned specimens at the predetermined temperature, the absorbance can be measured by using an absorption measuring device or the like. The absorption measurement device is not particularly limited as long as the absorbance at the predetermined absorption wavelength can be quantified, and examples thereof include an absorptiometer, and when the absorptiometer is used, The absorbance is determined as absorbance.
【0031】また、上記検量線を作成するには、吸収度
と水分濃度とを、それぞれグラフの縦軸及び横軸に設定
し、得られたデータを該グラフにプロットし、プロット
した各点を結んで関数グラフにする等して作成すること
ができる。In order to create the above calibration curve, the absorbance and the water concentration are set on the vertical and horizontal axes of the graph, respectively, and the obtained data is plotted on the graph. It can be created by tying it into a function graph.
【0032】上記水分測定試薬を上記試料に添加する際
における上記所定割合は、上述した水分測定試薬を上記
検定液に添加する際における所定割合と同様である。ま
た、着色した試料の吸収度を測定する際における温度及
び吸収波長は、上記標本を作成する際における上記所定
温度及び上記の所定の吸収波長と同様であり、吸収度の
測定も上述の標本の吸収度の測定と同様に行うことがで
きる。The above-mentioned predetermined ratio when adding the above-mentioned water measurement reagent to the above-mentioned sample is the same as the above-mentioned predetermined ratio when adding the above-mentioned water measurement reagent to the above-mentioned test solution. The temperature and the absorption wavelength when measuring the absorbance of the colored sample are the same as the predetermined temperature and the predetermined absorption wavelength when the sample is prepared, and the measurement of the absorbance is also performed on the sample. The measurement can be performed in the same manner as the measurement of the absorbance.
【0033】また、上記水分測定試薬として、温度が異
なると吸収度の領域がずれる水分測定試薬を使用した場
合には、異なる温度、例えば0℃と25℃との様に標本
及び試料を加温または冷却して測定する際の温度を調節
することにより、吸収度の領域を測定の上限下限に調整
することができる。即ち、本発明においては、標本の吸
収度が著しく変化する水分濃度を、標本の温度を変化さ
せることにより、測定する試料に応じて最適な水分濃度
の範囲へシフトさせることができるので、1つの水分測
定試薬でも測定する際の上記所定温度を変えることによ
って、比色が困難な試料の水分濃度を容易に測定するこ
とができる。When a moisture measuring reagent whose absorption range shifts at different temperatures is used as the moisture measuring reagent, the sample and the sample are heated to different temperatures, for example, 0 ° C. and 25 ° C. Alternatively, by adjusting the temperature at the time of measurement after cooling, the region of absorbance can be adjusted to the upper and lower limits of the measurement. That is, in the present invention, by changing the temperature of the sample, the water concentration at which the absorbance of the sample significantly changes can be shifted to the range of the optimum water concentration according to the sample to be measured. By changing the above-mentioned predetermined temperature at the time of measuring even with a moisture measuring reagent, the moisture concentration of a sample whose colorimetry is difficult can be easily measured.
【0034】また、上記試料の吸収度と上記検量線とか
ら上記試料の水分を定量するには、上記試料の吸収度を
上記検量線と対比し、上記検量線上における上記試料の
吸収度となる際の水分濃度を確認する等して定量するこ
とができる。To determine the water content of the sample from the absorbance of the sample and the calibration curve, the absorbance of the sample is compared with the calibration curve, and the absorbance of the sample on the calibration curve is obtained. It can be quantified by confirming the water concentration at the time.
【0035】次に、本発明により実施できる試料の水分
測定方法の他の態様について、詳細に説明する。尚、特
に説明しない点、即ち、具体的な測定方法については、
上述した水分測定方法の一つの態様で記載した事項が全
て適用可能である。Next, another embodiment of the method for measuring the water content of a sample which can be carried out according to the present invention will be described in detail. In addition, about the point which is not specifically described, that is, about a specific measuring method,
All the items described in one embodiment of the above-described moisture measurement method are applicable.
【0036】本発明の他の態様を実施するには、各々水
分濃度の異なる複数の水分濃度既知の検定液に、上記水
分測定試薬を、各々所定割合で添加混合して、水分濃度
に応じて着色度の異なる複数の標本を作成し、得られた
各標本の種々の温度における所定の吸収波長の吸収度を
測定し、各標本の吸収度、温度及び水分濃度の関係を記
憶装置に記憶させてデータベースを作成し、一方、水分
濃度未知の上記試料に、上記水分測定試薬を、上記所定
割合にて添加混合して該試料を着色し、着色した該試料
の任意の温度における上記所定の吸収波長の吸収度を測
定し、着色した上記試料の吸収度と上記の任意の温度と
を上記データベースのデータと比較して、上記試料の水
分を定量するIn order to carry out another embodiment of the present invention, the above-mentioned water measuring reagents are added and mixed at predetermined ratios to a plurality of test solutions having known water concentrations, each having a different water concentration. A plurality of samples having different degrees of coloring are prepared, the obtained samples are measured for absorbance at a predetermined absorption wavelength at various temperatures, and the relationship between the absorbance, temperature, and moisture concentration of each sample is stored in a storage device. In the meantime, a database is created, and on the other hand, the moisture measurement reagent is added and mixed at the above-mentioned predetermined ratio to the above-mentioned sample whose water concentration is unknown, and the sample is colored. The absorbance of the wavelength is measured, and the absorbance of the colored sample and the above-mentioned arbitrary temperature are compared with the data of the database to determine the water content of the sample.
【0037】上記標本の吸収度を測定する際における上
記種々の温度の範囲は、前述の水分測定方法の一つの態
様における所定温度と同様に0〜70℃の範囲とするの
が好ましい。また、試料の測定を行う際の上記の任意の
温度についても同様に0〜70℃の範囲とするのが好ま
しい。そして、試料の測定を行う際の上記の任意の温度
を上記範囲内で特に制限されずに選択できるように、上
記標本の吸収度を測定する際の上記種々温度としては、
多くの温度条件を採用することが好ましく、例えば、1
〜10℃毎に測定しておくことが好ましい。The range of the various temperatures at the time of measuring the absorbance of the sample is preferably in the range of 0 to 70 ° C. in the same manner as the predetermined temperature in one embodiment of the above-mentioned moisture measurement method. Further, it is preferable that the above-mentioned arbitrary temperature at the time of measuring the sample is also in the range of 0 to 70 ° C. Then, as the various temperatures when measuring the absorbance of the sample, so that the arbitrary temperature at the time of measuring the sample can be selected without being particularly limited within the above range,
Preferably, a number of temperature conditions are employed, for example, 1
It is preferable to measure every 10 to 10 ° C.
【0038】また、記憶装置としては、コンピュータの
ハードディスクやフロッピーディスク等を好ましく用い
ることができる。As a storage device, a hard disk or a floppy disk of a computer can be preferably used.
【0039】着色した上記試料の吸収度と上記任意の温
度とを上記データベースのデータと比較して、上記試料
の水分を定量するには、下記1)及び2)等の方法が挙
げられる。 1)検量線法:標本の吸収度と水分量の関係を捕間する
関数を作成し、該関数をもとに試料の吸収度から水分を
換算する方法。 2)テーブル法:標本の吸収度と水分量の関係を表に
し、該表をもとに試料の吸収度から水分を換算する方
法。 また、上記検量線法においては、上記データベースに上
記検量線が得られる関数を入力しておくことにより、試
料の吸収度及び測定諸条件を入力するだけで、即座に水
分の定量ができるシステムを構築することもできる。In order to determine the water content of the sample by comparing the absorbance of the colored sample and the arbitrary temperature with the data of the database, the following methods 1) and 2) can be mentioned. 1) Calibration curve method: A method of creating a function that captures the relationship between the absorbance of a sample and the amount of moisture, and converting moisture from the absorbance of the sample based on the function. 2) Table method: A method in which the relationship between the absorbance of a sample and the amount of moisture is tabulated, and the moisture is converted from the absorbance of the sample based on the table. In the above-mentioned calibration curve method, by inputting a function for obtaining the above-mentioned calibration curve in the above-mentioned database, a system capable of instantaneously quantifying moisture simply by inputting the absorbance of the sample and various measurement conditions. Can also be built.
【0040】[0040]
【作用】本発明は、ハロゲン化コバルトの結晶水による
吸収度の変化を利用したものである。例えば、塩化コバ
ルトを例に取ると、無水塩化コバルトの溶液に水分を添
加すると、水和して、添加した水分の量に応じて吸収度
が変化する。従って、水分濃度の異なる検定液に無水塩
化コバルトの溶液を添加することにより、種々吸収度が
異なる標本を得ることができ、各標本の吸収度と水分濃
度とから作成した検量線と、被測定液である試料に同様
の操作を行うことにより得られる着色された試料の吸収
度とを、対比することにより、試料の水分を定量でき
る。The present invention utilizes the change in the absorbance of cobalt halide due to water of crystallization. For example, taking cobalt chloride as an example, when water is added to a solution of anhydrous cobalt chloride, it hydrates, and the absorbance changes according to the amount of water added. Therefore, by adding a solution of anhydrous cobalt chloride to a test solution having a different water concentration, samples having various absorbances can be obtained, and a calibration curve created from the absorbance and the water concentration of each sample, and a measured curve. The water content of the sample can be quantified by comparing the absorbance of a colored sample obtained by performing the same operation on the liquid sample.
【0041】[0041]
【実施例】以下、実施例により本発明を更に詳細に説明
するが、本発明はこれらに限定されるものではない。EXAMPLES The present invention will be described in more detail with reference to the following Examples, but it should not be construed that the present invention is limited thereto.
【0042】〔参考例1〕 塩化コバルト(II)無水和物をポリオキシエチレン(酸
化エチレン付加モル数=10モル)オクチルフェニルエ
ーテルに溶解し、塩化コバルト(II)無水和物の濃度
が、1g/リットルである水分測定試薬を得た。また、
イソプロピルアルコールに水を添加して、水分濃度が0
〜20重量%まで4重量%刻み(0重量%、4重量%、
8重量%、12重量%、16重量%、20重量%)に調
整された6種の検定液を得た。各検定液2mlと水分測定
試薬2mlとを10ml試験管内で混合し静置して、6種の
標本を得た。得られた標本の20℃における660nm及
び600nmの吸収度(吸光度)を吸光光度計で測定し、
得られた各標本の吸収度(吸光度)と水分濃度との関係
をグラフにプロットして検量線を作成した。得られた検
量線を図1に示す。 Reference Example 1 Cobalt (II) chloride anhydrate was dissolved in polyoxyethylene (ethylene oxide added mole = 10 mol) octyl phenyl ether, and the concentration of cobalt (II) chloride anhydrate was 1 g. Per liter of water was obtained. Also,
Water is added to isopropyl alcohol so that the water concentration becomes zero.
4% by weight (0%, 4%,
(8 wt%, 12 wt%, 16 wt%, 20 wt%) were obtained. 2 ml of each test solution and 2 ml of a water measurement reagent were mixed in a 10 ml test tube and allowed to stand to obtain 6 kinds of specimens. The absorbance (absorbance) at 660 nm and 600 nm at 20 ° C. of the obtained specimen was measured with an absorptiometer,
A calibration curve was prepared by plotting the relationship between the absorbance (absorbance) of each sample and the water concentration on a graph. The obtained calibration curve is shown in FIG.
【0043】次いで、水分未知の試料(イソプロピルア
ルコールと水との組成物)2mlと、水分測定試薬2mlと
を10ml試験管内で混合し静置して、上記試料を着色し
た。そして、着色した試料の20℃における660nmの
吸収度(吸光度)を吸光光度計で測定したところ、吸光
度は0.27であった。得られた測定値と図1に示す検
量線とから上記試料の水分濃度を求めたところ、8.0
%であった。Next, 2 ml of a sample of unknown water content (composition of isopropyl alcohol and water) and 2 ml of a water measurement reagent were mixed in a 10 ml test tube and allowed to stand to color the sample. The absorbance at 660 nm (absorbance) of the colored sample at 20 ° C. was measured with an absorptiometer, and the absorbance was 0.27. The water concentration of the sample was determined from the measured values obtained and the calibration curve shown in FIG.
%Met.
【0044】〔実施例1〕 塩化コバルト(II)無水和物をヘキサン90重量%及び
ポリオキシエチレン(酸化エチレン付加モル数=10モ
ル)オクチルフェニルエーテル10重量%の混合液に溶
解し、塩化コバルト(II)無水和物の濃度が、1g/リ
ットルである水分測定試薬を得た。また、イソプロピル
アルコールに水を添加して、水分濃度が0〜5重量%ま
で1重量%刻み(0重量%、1重量%、2重量%、3重
量%、4重量%、5重量%)に調整された6種の検定液
を得た。各検定液2mlと水分測定試薬2mlとを10ml試
験管内で混合し静置して、6種の標本を得た。得られた
標本の20℃における660nmの吸収度(吸光度)を吸
光光度計で測定し、得られた各標本の吸収度(吸光度)
と水分濃度との関係をグラフにプロットして検量線を作
成した。得られた検量線を図2に示す。Example 1 Cobalt (II) chloride anhydride was dissolved in a mixture of 90% by weight of hexane and 10% by weight of polyoxyethylene (the number of moles of ethylene oxide added: 10 moles) of octylphenyl ether. (II) A moisture measurement reagent having an anhydrate of 1 g / liter was obtained. In addition, water is added to isopropyl alcohol, and the water concentration is reduced to 0 to 5% by weight in increments of 1% by weight (0%, 1%, 2%, 3%, 4%, 5%). Six adjusted test solutions were obtained. 2 ml of each assay solution and 2 ml of a water measurement reagent were mixed in a 10 ml test tube and allowed to stand, thereby obtaining six kinds of specimens. The absorbance (absorbance) at 660 nm of the obtained sample at 20 ° C. was measured with an absorptiometer, and the absorbance (absorbance) of each obtained sample was measured.
A calibration curve was created by plotting the relationship between the water content and the water concentration on a graph. The obtained calibration curve is shown in FIG.
【0045】次いで、水分未知の試料(イソプロピルア
ルコールと水との組成物)2mlと、水分測定試薬2mlと
を10ml試験管内で混合し静置して、上記試料を着色し
た。そして、着色した試料の20℃における660nmの
吸収度(吸光度)を吸光光度計で測定したところ、吸光
度は0.81であった。得られた測定値と図2に示す検
量線とから上記試料の水分濃度を求めたところ、2.0
重量%であった。Next, 2 ml of a sample of unknown water content (composition of isopropyl alcohol and water) and 2 ml of a water measurement reagent were mixed in a 10 ml test tube and allowed to stand, and the sample was colored. The absorbance at 660 nm (absorbance) of the colored sample at 20 ° C. was measured with an absorptiometer, and the absorbance was 0.81. The water concentration of the sample was determined from the measured values obtained and the calibration curve shown in FIG.
% By weight.
【0046】〔実施例2〕 塩化コバルト(II)無水和物をヘキサン90重量%、ポ
リオキシエチレン(酸化エチレン付加モル数=10モ
ル)オクチルフェニルエーテル10重量%の混合液に溶
解し、塩化コバルト(II)無水和物の濃度が、1g/リ
ットルである水分測定試薬を得た。また、ポリオキシエ
チレン(酸化エチレン付加モル数=2モル)ブチルエー
テルに水を添加して、水分濃度が2重量%、4重量%、
6重量%、7重量%に調整された4種の検定液を得た。
各検定液2mlと水分測定試薬2mlとを10ml試験管内で
混合し静置して、4種の標本を得た。得られた標本の2
0℃における660nmの吸収度(吸光度)を吸光光度計
で測定し、得られた各標本の吸収度(吸光度)と水分濃
度との関係をグラフにプロットして検量線を作成した。
得られた検量線を図3に示す。Example 2 Cobalt (II) chloride anhydrous was dissolved in a mixture of 90% by weight of hexane and 10% by weight of octylphenyl ether of polyoxyethylene (the number of moles of ethylene oxide added: 10 mol), and cobalt chloride was dissolved in the mixture. (II) A moisture measurement reagent having an anhydrate of 1 g / liter was obtained. Further, water was added to polyoxyethylene (ethylene oxide added mole number = 2 mole) butyl ether, and the water concentration was 2% by weight, 4% by weight,
Four kinds of test solutions adjusted to 6% by weight and 7% by weight were obtained.
2 ml of each test solution and 2 ml of a water measurement reagent were mixed in a 10 ml test tube and allowed to stand to obtain four types of specimens. 2 of the obtained specimen
The absorbance at 660 nm (absorbance) at 0 ° C. was measured with an absorptiometer, and the relationship between the absorbance (absorbance) of each obtained sample and the water concentration was plotted on a graph to prepare a calibration curve.
The obtained calibration curve is shown in FIG.
【0047】次いで、水分未知の洗浄液〔ポリオキシエ
チレン(酸化エチレン付加モル数=2モル)ブチルエー
テルと水との組成物〕2mlと、水分測定試薬2mlとを1
0ml試験管内で混合し静置して、上記試料を着色した。
そして、着色した試料の20℃における660nmの吸収
度(吸光度)を吸光光度計で測定したところ、吸光度は
0.11であった。得られた測定値と図3に示す検量線
とから上記試料の水分濃度を求めたところ、4.0重量
%であった。Next, 2 ml of a washing solution whose water content is unknown (composition of polyoxyethylene (addition of mole number of ethylene oxide = 2 mol) butyl ether and water) and 2 ml of a water measurement reagent were added to 1 ml
The above sample was colored by mixing and standing in a 0 ml test tube.
The absorbance at 660 nm (absorbance) of the colored sample at 20 ° C. was measured with an absorptiometer, and the absorbance was 0.11. The water content of the sample was determined from the obtained measured values and the calibration curve shown in FIG. 3, and was found to be 4.0% by weight.
【0048】〔参考例2〕 塩化コバルト(II)無水和物をオクチルアルコールに溶
解し、塩化コバルト(II)無水和物の濃度が、5g/リ
ットルである水分測定試薬を得た。また、イソプロピル
アルコールに水を添加して、水分濃度が5重量%、8重
量%、12重量%、15重量%に調整された4種の検定
液を得た。各検定液2mlと水分測定試薬2mlとを10ml
試験管内で混合し静置し4種の標本を得た。得られた標
本の20℃における660nmの吸収度(吸光度)を吸光
光度計で測定し、得られた各標本の吸収度(吸光度)と
水分濃度との関係をグラフにプロットして検量線を作成
した。得られた検量線を図4に示す。 REFERENCE EXAMPLE 2 Cobalt (II) chloride anhydrate was dissolved in octyl alcohol to obtain a water measurement reagent having a cobalt (II) chloride anhydrate concentration of 5 g / l. In addition, water was added to isopropyl alcohol to obtain four kinds of test solutions whose water concentrations were adjusted to 5% by weight, 8% by weight, 12% by weight, and 15% by weight. 10 ml of 2 ml of each test solution and 2 ml of water measurement reagent
The mixture was mixed in a test tube and allowed to stand to obtain four types of specimens. The absorbance (absorbance) at 660 nm of the obtained sample at 20 ° C. was measured with an absorptiometer, and the relationship between the absorbance (absorbance) of each obtained sample and the water concentration was plotted on a graph to prepare a calibration curve. did. The obtained calibration curve is shown in FIG.
【0049】次いで、水分未知の洗浄液(イソプロアル
コールと水との組成物)2mlと、水分測定試薬2mlとを
10ml試験管内で混合し静置して、上記洗浄液を着色し
た。そして、着色した洗浄液の20℃における660nm
の吸収度(吸光度)を吸光光度計で測定したところ、吸
光度は0.7であった。得られた測定値と図4に示す検
量線とから上記洗浄液の水分濃度を求めたところ、8.
0重量%であった。Next, 2 ml of a washing liquid of unknown water (composition of isoproalcohol and water) and 2 ml of a water measuring reagent were mixed in a 10 ml test tube and allowed to stand to color the washing liquid. 660 nm of the colored cleaning solution at 20 ° C.
Was measured with an absorptiometer to find that the absorbance was 0.7. The water concentration of the washing solution was determined from the measured values obtained and the calibration curve shown in FIG.
It was 0% by weight.
【0050】〔参考例3〕 塩化コバルト(II)無水和物をアセトンに溶解し、塩化
コバルト(II)無水和物の濃度が、1g/リットルであ
る水分測定試薬を得た。また、ポリオキシエチレン(酸
化エチレン付加モル数=2モル)ブチルエーテルに水を
添加して、水分濃度が5重量%、8重量%、12重量
%、15重量%に調整された4種の検定液を得た。各検
定液2mlと水分測定試薬2mlとを10ml試験管内で混合
し静置し4種の標本を得た。得られた標本の20℃にお
ける600nmの吸収度(吸光度)を吸光光度計で測定
し、得られた各標本の吸収度(吸光度)と水分濃度との
関係をグラフにプロットして検量線を作成した。得られ
た検量線を図5に示す。 Reference Example 3 Anhydrous cobalt (II) chloride was dissolved in acetone to obtain a water content measuring reagent having a concentration of anhydrous cobalt (II) chloride of 1 g / liter. In addition, water was added to polyoxyethylene (ethylene oxide added mole number = 2 mole) butyl ether to adjust the water concentration to 5% by weight, 8% by weight, 12% by weight, and 15% by weight. I got 2 ml of each test solution and 2 ml of a water measurement reagent were mixed in a 10 ml test tube and allowed to stand to obtain four types of specimens. The absorbance (absorbance) at 600 nm of the obtained sample at 20 ° C. was measured with an absorptiometer, and the relationship between the absorbance (absorbance) of each obtained sample and the water concentration was plotted on a graph to prepare a calibration curve. did. The obtained calibration curve is shown in FIG.
【0051】次いで、水分未知の洗浄液〔ポリオキシエ
チレン(酸化エチレン付加モル数=2モル)ブチルエー
テルと水との組成物〕2mlと、水分測定試薬2mlとを1
0ml試験管内で混合し静置して、上記洗浄液を着色し
た。そして、着色した洗浄液の20℃における600nm
の吸収度(吸光度)を吸光光度計で測定したところ、吸
光度は、0.19であった。得られた測定値と図5に示
す検量線とから上記洗浄液の水分濃度を求めたところ、
12.0重量%であった。Next, 2 ml of a washing solution whose water content is unknown [composition of polyoxyethylene (polyethylene oxide added mole number = 2 moles) butyl ether and water] and 2 ml of a water content measuring reagent were added.
The above washing liquid was colored by mixing and standing in a 0 ml test tube. Then, 600 nm of the colored cleaning solution at 20 ° C.
Was measured with an absorptiometer to find that the absorbance was 0.19. When the water concentration of the cleaning solution was determined from the obtained measured values and the calibration curve shown in FIG. 5,
12.0% by weight.
【0052】[0052]
【発明の効果】本発明の洗浄液の水分測定方法によれ
ば、水分濃度未知の試料中の水分を、簡便且つ安価に、
広範囲の水分濃度において精度良く測定することができ
る。従って、本発明の洗浄液の水分測定方法は、電子部
品や精密部品類の洗浄に用いられる洗浄液で、水分を添
加し非危険物化している洗浄液の水分管理を行う際等に
おいて、特に好適に用いることができる。According to the method for measuring the water content of a cleaning solution of the present invention, the water content of a sample whose water content is unknown can be easily and inexpensively determined.
It can be measured accurately over a wide range of moisture concentrations. Therefore, the method for measuring the water content of the cleaning liquid of the present invention is particularly preferably used in a cleaning liquid used for cleaning electronic parts and precision parts, for example, when performing water management of a cleaning liquid that is added as water and is made non-hazardous. be able to.
【図1】図1は、参考例1で得られた検量線を示すグラ
フである。FIG. 1 is a graph showing a calibration curve obtained in Reference Example 1.
【図2】図2は、実施例1で得られた検量線を示すグラ
フである。FIG. 2 is a graph showing a calibration curve obtained in Example 1 .
【図3】図3は、実施例2で得られた検量線を示すグラ
フである。FIG. 3 is a graph showing a calibration curve obtained in Example 2 .
【図4】図4は、参考例2で得られた検量線を示すグラ
フである。FIG. 4 is a graph showing a calibration curve obtained in Reference Example 2 .
【図5】図5は、参考例3で得られた検量線を示すグラ
フである。FIG. 5 is a graph showing a calibration curve obtained in Reference Example 3 .
───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.7,DB名) G01N 31/00 - 31/22 G01N 21/75 - 21/83 ──────────────────────────────────────────────────続 き Continued on the front page (58) Field surveyed (Int. Cl. 7 , DB name) G01N 31/00-31/22 G01N 21/75-21/83
Claims (1)
知の検定液に、ハロゲン化コバルト又はハロゲン化銅を
界面活性剤と疎水性溶媒との混合液に溶解した水分測定
試薬を、各々所定の割合で添加混合して、水分濃度に応
じて着色度の異なる複数の標本を作成し、上記水分測定
試薬における上記ハロゲン化コバルト又はハロゲン化銅
と上記界面活性剤との割合が、上記界面活性剤100重
量部に対して、上記ハロゲン化コバルト又はハロゲン化
銅0.1〜2.0重量部であり、 得られた各標本の所定温度における所定の吸収波長の吸
収度を測定し、各標本の吸収度と水分濃度との関係を表
す検量線を作成し、 一方、水分濃度が未知の試料である、界面活性剤及び/
又は溶剤と水とを含有する洗浄液に、上記水分測定試薬
を、上記所定割合にて添加混合して該試料を着色し、着
色した該試料の上記所定温度における上記の所定の吸収
波長の吸収度を測定し、 着色した上記試料の吸収度と上記検量線とから、上記試
料の水分を定量することを特徴とする水分測定方法。1. A water measurement reagent obtained by dissolving a cobalt halide or copper halide in a mixture of a surfactant and a hydrophobic solvent is added to a plurality of test solutions each having a different water concentration and a known water concentration. It was added at a ratio, to create a plurality of samples having different coloring degree according to water concentration, the water content measurement
The above-mentioned cobalt halide or copper halide in the reagent
And the ratio of the surfactant is 100 weight of the surfactant.
Parts by weight of the above-mentioned cobalt halide or halogenated
0.1 to 2.0 parts by weight of copper. Measure the absorbance of each sample obtained at a predetermined temperature at a predetermined absorption wavelength, and create a calibration curve representing the relationship between the absorbance of each sample and the moisture concentration. On the other hand, a surfactant and / or a sample whose water concentration is unknown
Alternatively , the water measurement reagent is added to and mixed with the cleaning liquid containing the solvent and water at the predetermined ratio to color the sample, and the absorbance of the colored sample at the predetermined temperature at the predetermined absorption wavelength is measured. And measuring the water content of the sample from the absorbance of the colored sample and the calibration curve.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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JP31875493A JP3343161B2 (en) | 1993-06-25 | 1993-12-17 | Moisture measurement method |
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
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JP15572293 | 1993-06-25 | ||
JP5-155722 | 1993-06-25 | ||
JP31875493A JP3343161B2 (en) | 1993-06-25 | 1993-12-17 | Moisture measurement method |
Publications (2)
Publication Number | Publication Date |
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JPH0772086A JPH0772086A (en) | 1995-03-17 |
JP3343161B2 true JP3343161B2 (en) | 2002-11-11 |
Family
ID=26483652
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JP31875493A Expired - Fee Related JP3343161B2 (en) | 1993-06-25 | 1993-12-17 | Moisture measurement method |
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JP2007085881A (en) * | 2005-09-22 | 2007-04-05 | Miura Co Ltd | Method and instrument for measuring concentration of component |
JP5888649B2 (en) * | 2012-06-29 | 2016-03-22 | 国立研究開発法人物質・材料研究機構 | Water detection reagent and method for quantitatively measuring water concentration in aprotic polar solvent |
RU2751452C1 (en) * | 2020-11-09 | 2021-07-14 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Казанский государственный энергетический университет" | Method for determining moisture content of transformer oil |
CN112525760A (en) * | 2020-11-24 | 2021-03-19 | 厦门市健康医疗大数据中心(厦门市医药研究所) | Method for digitally and quantitatively evaluating moisture absorption strength of substance |
CN113125785B (en) * | 2021-03-29 | 2024-02-27 | 深圳市科曼医疗设备有限公司 | Method for detecting high-concentration sample and invoking time sequence |
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