JPS5965764A - Oxygen sensing composition - Google Patents
Oxygen sensing compositionInfo
- Publication number
- JPS5965764A JPS5965764A JP17680482A JP17680482A JPS5965764A JP S5965764 A JPS5965764 A JP S5965764A JP 17680482 A JP17680482 A JP 17680482A JP 17680482 A JP17680482 A JP 17680482A JP S5965764 A JPS5965764 A JP S5965764A
- Authority
- JP
- Japan
- Prior art keywords
- composition
- added
- aluminum hydroxide
- oxygen sensing
- methylene blue
- 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
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
- G01N31/22—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators
- G01N31/223—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators for investigating presence of specific gases or aerosols
- G01N31/225—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators for investigating presence of specific gases or aerosols for oxygen, e.g. including dissolved oxygen
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Molecular Biology (AREA)
- Dispersion Chemistry (AREA)
- Biophysics (AREA)
- Emergency Medicine (AREA)
- Physics & Mathematics (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】
本発明は酸素感知組成物に係り、さらに詳しくは酸素感
知性能および保存安定性に優れた常態が固体の酸素感知
組成物に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an oxygen sensing composition, and more particularly to a normally solid oxygen sensing composition that has excellent oxygen sensing performance and storage stability.
近年、食品添加剤の使用規制等により、パックされた食
品の酸化、腐敗を防止するため、ノｆツク内に酸素吸収
剤を同封する方法が提案され、核酸素吸収剤の酸素吸収
能を感知するために錠剤形式の酸素感知組成物が要望さ
れている。酸素感知組成物は、酸化、還元、により可逆
的に色調変化する酸化還元色素を呈色成分とし、該色素
を還元型に保持しておく還元性物質と還元助剤およびそ
の他賦形剤等の添加物とからなり、該色素が酸素の存在
により還元型から酸化型に変化することにより呈色する
反応を利用するものである。従来、色素としてメチレン
ブルー、蔵元性物質としてＤ−グルコース等の趙元性糖
姻、および還元助剤として水酸化す） ＩＪウムを使用
する水溶液状の酸素感知組成物または該水溶液状組成物
をｐ紙等に含浸させた検知紙等が知られているが、該組
成物は水溶液状であるため呈色反応の反答速度が速い反
面、取扱い上挙都合が多く、特に液状物の存在を嫌う物
とは共存させることができない欠点がある。この欠点を
改良するものとして還元助剤として使用する水酸化ナト
リウムに替えて、アルカリ土類金属組成物を用いる実質
的に固体状の酸素感知組成物が、前記錠剤形式となし得
る組成物として提案（特公昭５６−２４９０６号公報）
されているが、該組成物は水酸化す） ＩＪウムを用い
る場合と同様に保存安定性が極めて悪い欠陥を有してい
る。In recent years, due to restrictions on the use of food additives, etc., a method of enclosing an oxygen absorber inside a container has been proposed in order to prevent packed foods from oxidation and spoilage. There is a need for an oxygen sensing composition in tablet form. The oxygen-sensing composition uses a redox dye that reversibly changes color due to oxidation or reduction as a coloring component, and contains a reducing substance that maintains the dye in a reduced form, a reduction aid, and other excipients. It utilizes a reaction in which the dye changes from a reduced form to an oxidized form in the presence of oxygen, resulting in coloration. Conventionally, an aqueous oxygen-sensing composition using methylene blue as a dye, a sugar complex such as D-glucose as a storage substance, and hydroxylated as a reducing agent, or an aqueous oxygen sensing composition using the aqueous solution composition as Detection papers made by impregnating paper, etc. are known, but since the composition is in the form of an aqueous solution, the reaction speed of the coloring reaction is fast, but it is difficult to handle, and it particularly dislikes the presence of liquid substances. It has the disadvantage that it cannot coexist with things. In order to improve this drawback, a substantially solid oxygen sensing composition using an alkaline earth metal composition instead of sodium hydroxide used as a reducing aid has been proposed as a composition that can be in the form of a tablet. (Special Publication No. 56-24906)
However, the composition has the defect of extremely poor storage stability, as in the case of using hydroxylated IJium.
本発明は前記公知の酸素感知組成物の欠陥を改良した、
すなけち酸素感知性能および保存安定性に優れた常態が
固体状の酸素感知組成物を提供することをその目的とす
る。The present invention improves the deficiencies of the known oxygen sensing compositions.
The object of the present invention is to provide an oxygen sensing composition that is normally solid and has excellent oxygen sensing performance and storage stability.
本発明者等は前記目的を達成すべく鋭意研究した結果、
メチレンブルー、還元性物質、還元剤および賦形剤等の
添加物とからなる組成物に水酸化アルミニウムを添加す
ることにより保存安定性が改良し得ること、ならびに、
さらに隠ぺい剤を焼畑することにより呈色時に鮮やかな
色調が得られ結果として優れた酸素感知性能が得られる
ことを見出し本発明を完成した。As a result of intensive research by the present inventors to achieve the above objective,
Storage stability can be improved by adding aluminum hydroxide to a composition consisting of methylene blue, a reducing substance, a reducing agent, and additives such as excipients, and
Furthermore, the present invention was completed by discovering that by slash-and-burning the concealing agent, a vivid color tone could be obtained during coloring, resulting in excellent oxygen sensing performance.
本発明は、メチレンブルー、還元性糖類、塩基性物質お
よび水酸化アルミニウムからなる組成物に、隠ぺい剤を
必要に応じ添加することを特徴とする酸素感知組成物で
ある。The present invention is an oxygen sensing composition characterized in that a masking agent is added to a composition consisting of methylene blue, a reducing sugar, a basic substance, and aluminum hydroxide, if necessary.
本発明において、呈色成分としてメチレンブルーを使用
するが、下記一般式（１）
で表わされる酸化還元色素、たとえば、メチレンフルー
、ニューメチレンブルー、ラウスノ々イオレット、メチ
レングリーン等およびメチレンブルーの錯塩類のいずれ
をも使用することができる。色素の使用量は酸素を感知
し呈色するに十分な鷲であればよく、通常、酸素感知組
成物全体１００重菫部に対して０．００１−１０重量部
、好ましくは０．０３〜０．１５重量部である。還元性
糖類はアルカリの存在−ス、Ｄ−ラクトース、Ｄ−がラ
クトース等のい′ずれをも使用できる。特に還元力、入
手の容易さを考慮するとＤ−グルコース、Ｄ−キシロー
スが好ましく用いられる。還元性糖類の使用量はメチレ
ンブルーを還元型に保持し得る量であればよく通常、酸
素検知組成物全体１００重量部に対し１〜側重は部であ
る。塩基性物質は還元助剤として用いる。水酸化ナトリ
ウム、アルカリ土類金属水酸化物類等を用いることもで
きるが、好ましくは、ｐＨ緩衝能を有する塩基性塩類、
すなはち、弱酸性物質と強塩基性物質との塩類、たとえ
ば、リン酸、炭酸、ケイ酸、ホウ酸または有機酸類のア
ルカリ余端塩類もしくはアルカリ土類金属塩類、具体的
には、リンｍ＝ナトリウム、リン酸二ナトリウム、ピロ
リン酸ナトリウム、メタリン酸ナトリウム、ポリリン酸
ナトリウム、リン酸カルシウム、リン酸水素バリウム等
のリン酸塩類、炭酸ナトリウム、重炭酸ナトリウム、塩
基性炭酸マグネシウム等の炭酸塩類、ケイ酸ナトリウム
、メタケイ酸ナトリウム、セスキケイ酸ナトリウム、ケ
イ酸カルシウム、ケイ酸マグネシウム等のケイ酸塩類、
ホウ酸ナトリウム、ホウ酸カルシウム等のホウ酸塩類、
酢酸ナトリウム、シュウ酸ナトリウム、シュウ酸カルシ
ウム等の有機酸塩類等が好ましく使用される。塩基性物
質の使用量は、還元性糖類の種類使用量等により異るが
、通常還元性糖類１重量部に対し０．０５〜１重駄部を
使用する。In the present invention, methylene blue is used as a coloring component, but any of redox dyes represented by the following general formula (1), such as methylene flu, new methylene blue, lausuno iolet, methylene green, etc., and complex salts of methylene blue may be used. can also be used. The amount of the dye to be used is sufficient to sense oxygen and produce a color, and is usually 0.001-10 parts by weight, preferably 0.03-0. .15 parts by weight. As the reducing sugar, any of alkali-based sugars, D-lactose, D-lactose, etc. can be used. In particular, D-glucose and D-xylose are preferably used in consideration of reducing power and ease of availability. The reducing saccharide may be used in an amount that can maintain methylene blue in a reduced form, and is usually 1 to 1 part by weight per 100 parts by weight of the entire oxygen sensing composition. Basic substances are used as reducing aids. Sodium hydroxide, alkaline earth metal hydroxides, etc. can also be used, but preferably basic salts having pH buffering ability,
In other words, salts of weakly acidic substances and strong basic substances, such as phosphoric acid, carbonic acid, silicic acid, boric acid, or alkaline residue salts or alkaline earth metal salts of organic acids, specifically, phosphorus m = Phosphates such as sodium, disodium phosphate, sodium pyrophosphate, sodium metaphosphate, sodium polyphosphate, calcium phosphate, barium hydrogen phosphate, carbonates such as sodium carbonate, sodium bicarbonate, basic magnesium carbonate, silicic acid Silicates such as sodium, sodium metasilicate, sodium sesquisilicate, calcium silicate, magnesium silicate,
Borates such as sodium borate and calcium borate,
Organic acid salts such as sodium acetate, sodium oxalate, and calcium oxalate are preferably used. The amount of the basic substance used varies depending on the type and amount of reducing saccharide used, but it is usually 0.05 to 1 part by weight per 1 part by weight of reducing saccharide.
本発明において、前記メチレンブルー、還元性糖類およ
び塩基性物質から・なる溶液またはスラリーを水酸化ア
ルミニウムに担持させることにより保存安定性に優れた
常態が固体状の酸素感知組成物が得られる。本発明の組
成物は、公知の水酸化マグネシウムを担体として用いた
酸素感知組成物に比較して、その褪色試験においてほぼ
２倍の安定性を示す。また、水酸化アルミニウムに隠ぺ
い剤たとえば酸化チタン、酸化亜鉛、酸化アンチモン、
ＩＪ ）ボン等の白色顔料を添加混合したものを担体と
することにより、メチレンブルー等の酸化還元色素の濃
い色たとえば濃青色を隠ぺいし明るく鮮やかな見やすい
色たとえば澄空色に変えることができる。この隠ぺい剤
は、所望する色調に対し必要に応じて添加する。In the present invention, an oxygen-sensing composition that is normally solid and has excellent storage stability can be obtained by supporting a solution or slurry consisting of methylene blue, a reducing sugar, and a basic substance on aluminum hydroxide. The compositions of the present invention exhibit approximately twice the stability in the fade test compared to known oxygen sensing compositions using magnesium hydroxide as a carrier. In addition, concealing agents such as titanium oxide, zinc oxide, antimony oxide, etc. can be added to aluminum hydroxide.
By using a carrier mixed with a white pigment such as IJ) Bon, it is possible to hide the dark color of redox dyes such as methylene blue, such as deep blue, and change it to a bright, vivid color that is easy to see, such as clear sky blue. This masking agent is added as necessary to achieve a desired color tone.
本発明において、メチレンブルー、還元性糖類、塩基性
物質および水酸化アルミニウムからなる組成物のスラリ
ーに必要圧応じて隠ぺい剤を添加し、さらに保水性物質
、賦形剤等の添加物たとえばケイ酸ｒル、アルミナダル
、ポリエチレングリコール、デリグロビレングリコール
、該グリコール類のエーテル類、カルがキシメチルセル
ロース、ヒドロキシエチルセルロース、ヒドロキシプロ
ピルセルロース等のセルロース誘導体等を添加混合し、
乾燥して粉末状、顆粒状、タブレット状等に成形して実
質固体状の酸素感知組成物が得られる。In the present invention, a masking agent is added to a slurry of a composition consisting of methylene blue, reducing sugars, basic substances, and aluminum hydroxide according to the required pressure, and additives such as water-retentive substances and excipients are added, such as silicic acid r. Alumina dal, polyethylene glycol, deriglobylene glycol, ethers of the glycols, cellulose derivatives such as Calxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, etc. are added and mixed,
The oxygen sensing composition is dried and formed into a powder, granules, tablets, etc. to obtain a substantially solid oxygen sensing composition.
本発明は水酸化アルミニウムを担体組成物とすることに
より保存安定性が増加し、また隠ぺい剤を使用すること
により呈色反応による発色が鮮やかなものとなり酸素感
知性能が向上する。In the present invention, by using aluminum hydroxide as a carrier composition, the storage stability is increased, and by using a masking agent, the coloring reaction becomes vivid and the oxygen sensing performance is improved.
本発明は、保存安定性および酸素感知性能に優れた酸素
感知組成物を提供するものでありその産業的意義は極め
て大きい。The present invention provides an oxygen sensing composition with excellent storage stability and oxygen sensing performance, and has extremely great industrial significance.
以下、実施例および比較例を挙げて本発明をさらに詳細
に説明する。ただし、本発明の範囲は下記実施例に限定
されるものではない。Hereinafter, the present invention will be explained in more detail with reference to Examples and Comparative Examples. However, the scope of the present invention is not limited to the following examples.
以下の実施例および比較例において部は全て重歇部を意
味する。In the following Examples and Comparative Examples, all parts refer to heavy-duty parts.
実施例１
水酸化アルミニウム４５０部、酸化チタン調部の混合物
に、Ｄ（１）−キシロース８４部、リン酸三ナトリウム
・Ｉ２水塩６部、メチレンブルー０．６部およヒフ１？
ＩＪエチレングリコール１５００ １２部の水溶液状
組成′吻とヒドロキシプロピルセルロース（ＨＰＯ−Ｌ
１日本口達製）３５部のエタノール溶液との混合溶液を
担持させ、乾燥して得られた顆粒を打錠機で打錠し澄空
色のタブレット状組成物を得た。該タブレットを酸素濃
度帆１％以下の窒素雰囲気中に置いた所１８時間で脱色
し白色に変化した。次いで該窒素雰囲気中に酸素を注入
すると該タブレットは澄空色に変化した。呈色、脱色の
繰返しを３日置きに１５回繰返したが変色時間および色
調の変化に何等の変化も観察されなかった。Example 1 A mixture of 450 parts of aluminum hydroxide and titanium oxide, 84 parts of D(1)-xylose, 6 parts of trisodium phosphate I2 hydrate, 0.6 part of methylene blue and 1?
Aqueous composition of 12 parts of IJ ethylene glycol 1500 and hydroxypropyl cellulose (HPO-L)
A mixed solution of 35 parts of ethanol solution (manufactured by Nippon Koutatsu) was supported on the granules, and the resulting granules were dried and compressed using a tablet machine to obtain a clear sky blue tablet-like composition. When the tablet was placed in a nitrogen atmosphere with an oxygen concentration of 1% or less, it was decolored and turned white in 18 hours. Oxygen was then injected into the nitrogen atmosphere and the tablet turned clear blue. Coloration and decolorization were repeated 15 times every 3 days, but no change in color change time or color tone was observed.
実施例２
水酸化アルミニウム３７５部、酸化チタン１０部、Ｄ（
−１−）−キシロース７０部、メチレンブルー０．５部
およびポリエチレングリコール１５００ １５部とから
なる水性スラリーにＨＰＯ−Ｌ ２５部のエタノール溶
液を混合した後乾燥し、得られた顆粒状組成物を打錠し
澄空色のタブレット状組成物を得た。このタブレットを
窒素雰囲気中に置こと調時間で白色に変化した。次いで
大気中に取出すと再び澄空色に変化した。発色、脱色の
操作を３日置きに３回繰り返したが、呈色性に何等の変
化も認められなかった。Example 2 375 parts of aluminum hydroxide, 10 parts of titanium oxide, D(
-1-)-An ethanol solution of 25 parts of HPO-L is mixed into an aqueous slurry consisting of 70 parts of xylose, 0.5 parts of methylene blue, and 15 parts of polyethylene glycol 1500, and then dried, and the resulting granular composition is pounded. A clear sky blue tablet-like composition was obtained. When this tablet was placed in a nitrogen atmosphere, the color changed to white over time. Then, when taken out into the atmosphere, the color changed to clear sky blue again. The color development and decolorization operations were repeated three times at three-day intervals, but no change was observed in the color development.
実施例３〜４
原料の配合を種々変えた以外には実施例１と同様に処理
しタブレット状酸素感知組成物を製造した。Examples 3 to 4 Tablet-shaped oxygen sensing compositions were manufactured in the same manner as in Example 1, except that the composition of the raw materials was variously changed.
該タブレットについて無酸素状態とした場合の脱色時間
を測定し、また色調を観察した。The decolorization time of the tablet in an oxygen-free condition was measured, and the color tone was also observed.
原料組成および測定、観察結果を比較例１と共に第１表
中に示す。The raw material composition, measurement and observation results are shown in Table 1 together with Comparative Example 1.
比較例１
水酸化アルミニウム担体に替えて水酸化マグネシウム担
体とするタブレット状酸素感知組成物を夷遺した。Comparative Example 1 A tablet-shaped oxygen sensing composition was prepared in which a magnesium hydroxide carrier was used instead of an aluminum hydroxide carrier.
該タブレットについて実施例３および４と同一の条件下
で測定観察を行った。原料組成および測定、観察結果を
実施例３および４と共に第１表中に示す。The tablets were measured and observed under the same conditions as in Examples 3 and 4. The raw material composition, measurement and observation results are shown in Table 1 together with Examples 3 and 4.
■
実施例５および比較例２
第２表中に示す原料配合により実施例１と同様にしてタ
ブレット状酸素感知組成物を製造した。(2) Example 5 and Comparative Example 2 Tablet-shaped oxygen sensing compositions were produced in the same manner as in Example 1 using the raw material formulations shown in Table 2.
該タブレットについて４０℃の加熱下、または紫外線照
射下に置き酸素雰囲気中（青色）および窒素雰囲気中（
白色）の色調の変化による保存安定性促進試験を行った
。The tablet was heated at 40°C or irradiated with ultraviolet rays in an oxygen atmosphere (blue) and a nitrogen atmosphere (blue).
A storage stability acceleration test was conducted by changing the color tone (white).
試岐結果を第２表中に示す。The trial results are shown in Table 2.
第 ２ 表Table 2
Claims (1)
水酸化アルミニウムからなる組成物に隠ぺい剤を必要に
応じ添加することを特徴とする酸素感知組成物。 ２、 隠ぺい剤が酸化チタン、酸化亜鉛、酸化アンチモ
ン、リトポン等の白色顔料である特許請求の範囲第１項
記載の組成物。 ３、粉粒状、顆粒状またはタブレット状である特許請求
の範囲第１項記載の組成物。[Scope of Claims] 1. An oxygen sensing composition characterized in that a masking agent is added to a composition consisting of methylene blue, a reducing sugar, a basic substance, and aluminum hydroxide as necessary. 2. The composition according to claim 1, wherein the masking agent is a white pigment such as titanium oxide, zinc oxide, antimony oxide, or lithopone. 3. The composition according to claim 1, which is in the form of powder, granules, or tablets.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17680482A JPS5965764A (en) | 1982-10-07 | 1982-10-07 | Oxygen sensing composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17680482A JPS5965764A (en) | 1982-10-07 | 1982-10-07 | Oxygen sensing composition |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS5965764A true JPS5965764A (en) | 1984-04-14 |
Family
ID=16020126
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP17680482A Pending JPS5965764A (en) | 1982-10-07 | 1982-10-07 | Oxygen sensing composition |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5965764A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003021252A1 (en) * | 2001-09-05 | 2003-03-13 | University Of Strathclyde | Sensor for oxidising agents |
| EP2034306A1 (en) * | 2006-06-29 | 2009-03-11 | Sakura Color Products Corporation | Ink composition for detecting dissolved ozone and method of detecting dissolved ozone |
| US20110097811A1 (en) * | 2009-10-28 | 2011-04-28 | Powdertech Co., Ltd. | Oxygen detector and method for manufacturing oxygen detector |
| US20110136238A1 (en) * | 2008-06-18 | 2011-06-09 | Teknologian Tutkimuskeskus Vtt | Oxygen indicator |
| KR20170081978A (en) * | 2016-01-05 | 2017-07-13 | 동국대학교 산학협력단 | Printing ink composition for UV-activated time temperature integrator and Method for preparing UV-activated time temperature integrator using the same |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5625619A (en) * | 1979-08-07 | 1981-03-12 | Webasto Werk Baier Kg W | Heater |
-
1982
- 1982-10-07 JP JP17680482A patent/JPS5965764A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5625619A (en) * | 1979-08-07 | 1981-03-12 | Webasto Werk Baier Kg W | Heater |
Cited By (8)
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| WO2003021252A1 (en) * | 2001-09-05 | 2003-03-13 | University Of Strathclyde | Sensor for oxidising agents |
| US8114673B2 (en) | 2001-09-05 | 2012-02-14 | University Of Strathclyde | Sensor for oxidising agents |
| EP2034306A1 (en) * | 2006-06-29 | 2009-03-11 | Sakura Color Products Corporation | Ink composition for detecting dissolved ozone and method of detecting dissolved ozone |
| EP2034306A4 (en) * | 2006-06-29 | 2011-10-05 | Sakura Color Prod Corp | Ink composition for detecting dissolved ozone and method of detecting dissolved ozone |
| US20110136238A1 (en) * | 2008-06-18 | 2011-06-09 | Teknologian Tutkimuskeskus Vtt | Oxygen indicator |
| US20110097811A1 (en) * | 2009-10-28 | 2011-04-28 | Powdertech Co., Ltd. | Oxygen detector and method for manufacturing oxygen detector |
| US8415167B2 (en) * | 2009-10-28 | 2013-04-09 | Powdertech Co., Ltd. | Oxygen detector and method for manufacturing oxygen detector |
| KR20170081978A (en) * | 2016-01-05 | 2017-07-13 | 동국대학교 산학협력단 | Printing ink composition for UV-activated time temperature integrator and Method for preparing UV-activated time temperature integrator using the same |
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