JP6662524B1 - Detecting material and method for manufacturing the same, and detection tool and method for manufacturing the same - Google Patents
Detecting material and method for manufacturing the same, and detection tool and method for manufacturing the same Download PDFInfo
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- JP6662524B1 JP6662524B1 JP2019015101A JP2019015101A JP6662524B1 JP 6662524 B1 JP6662524 B1 JP 6662524B1 JP 2019015101 A JP2019015101 A JP 2019015101A JP 2019015101 A JP2019015101 A JP 2019015101A JP 6662524 B1 JP6662524 B1 JP 6662524B1
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- white carbon
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- 238000002156 mixing Methods 0.000 claims description 26
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- KSPIHGBHKVISFI-UHFFFAOYSA-N Diphenylcarbazide Chemical compound C=1C=CC=CC=1NNC(=O)NNC1=CC=CC=C1 KSPIHGBHKVISFI-UHFFFAOYSA-N 0.000 claims description 10
- RJNYNDHYSJRRDW-UHFFFAOYSA-N 4-(pyridin-2-yldiazenyl)benzene-1,3-diol Chemical compound OC1=CC(O)=CC=C1N=NC1=CC=CC=N1 RJNYNDHYSJRRDW-UHFFFAOYSA-N 0.000 claims description 5
- LTZURWPSQIZWNH-UHFFFAOYSA-L disodium 4-hydroxy-5-[(2-hydroxyphenyl)methylideneamino]naphthalene-2,7-disulfonate Chemical compound [Na+].OC1=CC(=CC2=CC(=CC(=C12)N=CC=1C(O)=CC=CC=1)S(=O)(=O)[O-])S(=O)(=O)[O-].[Na+] LTZURWPSQIZWNH-UHFFFAOYSA-L 0.000 claims description 4
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- CZMAIROVPAYCMU-UHFFFAOYSA-N lanthanum(3+) Chemical compound [La+3] CZMAIROVPAYCMU-UHFFFAOYSA-N 0.000 description 1
- ZBJWWKFMHOAPNS-UHFFFAOYSA-N loretin Chemical class C1=CN=C2C(O)=C(I)C=C(S(O)(=O)=O)C2=C1 ZBJWWKFMHOAPNS-UHFFFAOYSA-N 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 229960003540 oxyquinoline Drugs 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 239000006179 pH buffering agent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229960004838 phosphoric acid Drugs 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- KAQHZJVQFBJKCK-UHFFFAOYSA-L potassium pyrosulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OS([O-])(=O)=O KAQHZJVQFBJKCK-UHFFFAOYSA-L 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- VBHKTXLEJZIDJF-UHFFFAOYSA-N quinalizarin Chemical compound C1=CC(O)=C2C(=O)C3=C(O)C(O)=CC=C3C(=O)C2=C1O VBHKTXLEJZIDJF-UHFFFAOYSA-N 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 229940087562 sodium acetate trihydrate Drugs 0.000 description 1
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 1
- 229940048086 sodium pyrophosphate Drugs 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229940032330 sulfuric acid Drugs 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 235000019818 tetrasodium diphosphate Nutrition 0.000 description 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
- AEHGQXKBQBMQEK-UHFFFAOYSA-K trisodium 4,5-dihydroxy-3-[(4-sulfonatophenyl)diazenyl]naphthalene-2,7-disulfonate Chemical compound [Na+].[Na+].[Na+].Oc1cc(cc2cc(c(N=Nc3ccc(cc3)S([O-])(=O)=O)c(O)c12)S([O-])(=O)=O)S([O-])(=O)=O AEHGQXKBQBMQEK-UHFFFAOYSA-K 0.000 description 1
- 229940043798 zincon Drugs 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
【課題】流動性が高く容器等に充填しやすく、かつ、検査対象の液体等を吸収しやすく、試験時の発色の均一性に優れた検出材やそれを用いた検出用具等を提供する。【解決手段】ホワイトカーボンに発色剤を担持させた試薬担持ホワイトカーボンと、吸水性樹脂とを含有する検出材２。また、ホワイトカーボンに発色剤を担持させた試薬担持ホワイトカーボンと、吸水性樹脂とを容器（透明容器３および不織布４とを溶着部５で密閉したもの）に収容させた検出用具１。【選択図】 図１PROBLEM TO BE SOLVED: To provide a detection material having high fluidity, easy to be filled in a container or the like, easy to absorb a liquid to be inspected or the like, and excellent in color uniformity during a test, a detection tool using the same, and the like. SOLUTION: The detection material 2 contains a reagent-carrying white carbon in which a coloring agent is carried on white carbon, and a water absorbent resin. Further, the detection tool 1 in which a reagent-carrying white carbon in which a coloring agent is carried on white carbon and a water-absorbent resin are housed in a container (a transparent container 3 and a nonwoven fabric 4 are hermetically sealed by a welding portion 5). [Selection diagram] Fig. 1
Description
本発明は検出材およびその製造方法、ならびに、検出用具およびその製造方法に関する。 The present invention relates to a detection material and a method for manufacturing the same, and a detection tool and a method for manufacturing the same.
産業廃棄物の処理場や工場跡地などの土壌や水系は、重金属等（クロム、ヒ素、鉛、フッ素等）の環境汚染物質による汚染が懸念される土壌となっている場合がある。 In some cases, soil and water systems, such as industrial waste treatment sites and factory sites, are soils where there is concern about pollution by environmental pollutants such as heavy metals (chromium, arsenic, lead, fluorine, etc.).
汚染土壌や水系の浄化を行うためには、各環境汚染物質の有無および汚染源の特定が必要であるが、そのためには、汚染が予測される広範囲な面積を対象とした土壌の採取とその分析が必要となる。ＪＩＳ Ｋ０１０２（非特許文献１）は、広く工場排水試験方法に関する規格であり、土壌汚染の程度を評価するに当たってもこれに準じた試験方法が行われている。このＪＩＳ規格の評価方法では、フッ素（３４．項）については、ランタン−アリザリンコンプレキソン吸光光度法、イオン電極法、イオンクロマトグラフ法、流れ分析法が開示されているが、これらは吸光光度計等を準備し、測定前の煩雑な処理を必要とするものであった。 In order to purify contaminated soil and water systems, it is necessary to identify the presence or absence of each environmental pollutant and the source of the pollutant. For this purpose, sampling and analysis of soil over a wide area where contamination is expected Is required. JIS K0102 (Non-Patent Document 1) is a standard concerning a factory drainage test method, and a test method according to the standard is performed even when evaluating the degree of soil contamination. In the evaluation method of this JIS standard, lanthanum-alizarin complexone spectrophotometry, ion electrode method, ion chromatograph method, and flow analysis method are disclosed for fluorine (34.), but these are spectrophotometers. And the like, and required complicated processing before measurement.
同様に、ＪＩＳ Ｋ０１０２においては、ホウ素（Ｂ）（４７．項）の評価方法としては、メチレンブルー吸光光度法等、鉛（５４．項）の評価方法としては、フレーム原子吸光法等が開示されており、いずれも、厳密な定量を目的とするものが多く、特別な測定装置、測定前の処理を行う必要があり、高度な評価技術を必要とするものであった。大型の装置を用いることなく簡便に環境調査を行うために、例えば特許文献１には、シリカ粒子と色素分子を複合化した水中六価クロム検知材が開示されている。しかしながら、特許文献１に開示された技術が適用できる対象、使用できる環境は限られたものであり、様々な環境で多様な環境汚染物質等の分析を行うには十分なものではなかった。 Similarly, JIS K0102 discloses a method for evaluating boron (B) (Section 47.) such as a methylene blue absorption spectrophotometer and a method for evaluating lead (Section 54.) includes a flame atomic absorption method and the like. In many cases, the objectives are strict quantification, so that a special measuring device and a pre-measurement process must be performed, and a sophisticated evaluation technique is required. In order to easily conduct an environmental investigation without using a large-sized device, for example, Patent Document 1 discloses a hexavalent chromium detection material in water in which silica particles and dye molecules are combined. However, the target to which the technology disclosed in Patent Document 1 can be applied and the environment in which it can be used are limited, and it is not sufficient to analyze various environmental pollutants in various environments.
また、特許文献２は、フッ素イオン含有試料をイオンクロマトグラフで分離した後、ランタン・アリザリンコンプレキソン反応試薬と反応させ、その反応物を分光光度検出器で検出することを特徴とするフッ素イオン分析方法に関するものである。ここでも、フッ素イオンの分析のために、イオンクロマトグラフを行い、分光光度検出器を用いる為、複雑な処理と、特別な装置を必要とするものである。 Patent Document 2 discloses a fluorine ion analysis method in which a fluorine ion-containing sample is separated by ion chromatography, then reacted with a lanthanum-alizarin complexone reaction reagent, and the reaction product is detected with a spectrophotometer. It is about the method. In this case as well, an ion chromatograph is performed for the analysis of fluorine ions and a spectrophotometer is used, so that complicated processing and special equipment are required.
このような従来公知の評価方法の課題を解決するために、例えば、特許文献３〜５のような検出材や検出用具が開示されている。これらを用いることで、簡易な手法で速やかに金属イオンや環境汚染物質の有無を評価することができる。 In order to solve the problems of such conventionally known evaluation methods, for example, detection materials and detection tools as disclosed in Patent Documents 3 to 5 are disclosed. By using these, the presence or absence of metal ions and environmental pollutants can be quickly evaluated by a simple method.
特許文献１や２に開示されているような従来の検査技術は複雑な処理や特別な装置が必要であったり、サンプリングしてから測定結果を確認するまでに時間がかかる場合があった。これらの問題を解決するものとして、特許文献３〜５などが開示されている。 Conventional inspection techniques such as those disclosed in Patent Literatures 1 and 2 require complicated processing and special equipment, and it sometimes takes time from sampling to confirming a measurement result. Patent Documents 3 to 5 and the like are disclosed as solutions to these problems.
特許文献３〜５の吸水性樹脂やホワイトカーボンを用いる検出材等により、懸濁物質（泥水）等を対象としても、それらに含まれる汚染物質の濃度を、簡易に測定することができる。そして、これらを量産化するにあたっては、担体に発色剤を担持させた検出材を、効率よく容器に充填することが求められる。 By using a detection material using a water-absorbent resin or white carbon disclosed in Patent Literatures 3 to 5, even for suspended substances (muddy water) and the like, the concentration of contaminants contained therein can be easily measured. In order to mass-produce these, it is required to efficiently fill a container with a detection material having a coloring agent carried on a carrier.
しかしながら、吸水性樹脂の種類によっては発色剤を含む液を吸収させた後、乾燥させるためにシート状に薄く延ばす必要があり、その状態で乾燥すると、シート状に一体化してしまっているため、さらにそれを粉砕すると１〜３ｍｍのフレーク状になる。このフレーク状の検出材は非常に軽い。さらに、フレーク同士が絡まりあい、充填機などで容器に充填しようとしても、充填機から排出される質量が安定しない場合や、流動性が低く排出されない場合がある。このため、容器への充填作業が難しい場合があった。さらに、ホワイトカーボンのみを担体とすると、ホワイトカーボンの吸水量は比較的少ないことから、試験対象の液の吸収に時間がかかり、試験結果を確認できるまでに長時間を要する場合があった。また、ホワイトカーボン表面の発色試薬の色が検液の方へ抜ける場合がある。また、色の抜け方にも製品間や、検液の液量によるバラつきが生じる場合がある。よって、色で濃度なども判断したいときに、判断が難しくなる場合があった。 However, depending on the type of the water-absorbing resin, after absorbing the liquid containing the color former, it is necessary to thinly spread it in a sheet shape for drying, and when dried in that state, it is integrated into a sheet shape, Further, when it is pulverized, it becomes a flake of 1-3 mm. This flaky detection material is very light. Further, when the flakes are entangled with each other and an attempt is made to fill the container with a filling machine or the like, the mass discharged from the filling machine may not be stable, or the fluidity may not be low enough to be discharged. For this reason, the filling operation of the container was sometimes difficult. Furthermore, when only white carbon is used as the carrier, the water absorption of white carbon is relatively small, so that it takes a long time to absorb the liquid to be tested, and it may take a long time to confirm the test result. In addition, the color of the coloring reagent on the surface of the white carbon may fall off toward the test solution. In addition, there may be variations in the color removal between products or due to the amount of the test solution. Therefore, when it is desired to determine the density or the like by the color, the determination may be difficult.
係る状況下、本発明は、流動性が高く容器等に充填しやすく、かつ、検査対象の液体等を吸収しやすく、試験時の発色の均一性に優れた検出材やそれを用いた検出用具等を提供することを目的とする。 Under such circumstances, the present invention has a high fluidity, is easy to fill a container or the like, and is easy to absorb a liquid to be inspected, etc., and a detection material excellent in uniformity of color development at the time of a test and a detection tool using the same. And so on.
本発明者は、上記課題を解決すべく鋭意研究を重ねた結果、下記の発明が上記目的に合致することを見出し、本発明に至った。すなわち、本発明は、以下の発明に係るものである。 The present inventors have conducted intensive studies to solve the above-mentioned problems, and as a result, have found that the following inventions meet the above objects, and have accomplished the present invention. That is, the present invention relates to the following inventions.
＜１＞ ホワイトカーボンに発色剤を担持させた試薬担持ホワイトカーボンと、吸水性樹脂とを含有する検出材。
＜２＞ 前記試薬担持ホワイトカーボンと、前記吸水性樹脂との混合質量比（試薬担持ホワイトカーボン：吸水性樹脂）が、２００：１〜１：３０である前記＜１＞記載の検出材。
＜３＞ 安息角が、４０度以下である前記＜１＞または＜２＞に記載の検出材。
＜４＞ 前記発色剤が、ランタン−アリザリンコンプレキソン、８−ヒドロキシ−１−（サリチリデンアミノ）−３，６−ナフタレンジスルホン酸・２ナトリウム塩、４−（２−ピリジルアゾ）レゾルシノール、ジフェニルカルバジドからなる群から選択されるいずれかの発色剤である前記＜１＞〜＜３＞のいずれかに記載の検出材。
<1> A detection material containing a reagent-supporting white carbon in which a color former is supported on white carbon, and a water-absorbing resin.
<2> The detection material according to <1>, wherein a mixing mass ratio of the reagent-carrying white carbon and the water-absorbing resin (reagent-carrying white carbon: water-absorbing resin) is 200: 1 to 1:30.
<3> The detection material according to <1> or <2>, wherein the repose angle is 40 degrees or less.
<4> The color former is lanthanum-alizarin complexone, 8-hydroxy-1- (salicylideneamino) -3,6-naphthalenedisulfonic acid disodium salt, 4- (2-pyridylazo) resorcinol, diphenylcarba The detection material according to any one of the above items <1> to <3>, which is any one of the coloring agents selected from the group consisting of zide.
＜５＞ ホワイトカーボンを、発色剤を含む発色剤溶液に接触させ、前記発色剤溶液を吸収した吸液ホワイトカーボンを得る接触工程と、
前記吸液ホワイトカーボンを乾燥させて試薬担持ホワイトカーボンを得る乾燥工程と、
前記試薬担持ホワイトカーボンと、吸水性樹脂とを混合して検出材を得る混合工程と、を有する検出材の製造方法。
＜６＞ ホワイトカーボンに発色剤を担持させた試薬担持ホワイトカーボンと、吸水性樹脂とを容器に収容させた検出用具。
＜７＞ 前記＜１＞〜＜４＞のいずれかに記載の検出材を、容器に収容する収容工程を有する検出用具の製造方法。
<5> contacting white carbon with a color former solution containing a color former to obtain a liquid-absorbing white carbon absorbing the color former solution;
A drying step of drying the liquid-absorbing white carbon to obtain a reagent-carrying white carbon,
A method for producing a detection material, comprising: a mixing step of mixing the reagent-supporting white carbon with a water-absorbing resin to obtain a detection material.
<6> A detection tool in which a reagent-supporting white carbon in which a color former is supported on white carbon and a water-absorbing resin are contained in a container.
<7> A method for manufacturing a detection tool, comprising a step of storing the detection material according to any one of <1> to <4> in a container.
本発明の検出材は、容器に充填しやすく、これを用いることで効率よく検出用具を製造することができる。また、本発明の検出材および検出用具は、短時間で検査対象の液等を吸収し、短時間で検査結果を目視で確認することができる。また、本発明の検出材および検出用具は、発色時の均一性に優れ、発色の有無を観察しやすい。 The detection material of the present invention can be easily filled in a container, and by using this, a detection tool can be manufactured efficiently. Further, the detection material and the detection tool of the present invention can absorb the liquid to be inspected in a short time, and can visually check the inspection result in a short time. Further, the detection material and the detection tool of the present invention have excellent uniformity at the time of coloring, and it is easy to observe the presence or absence of coloring.
以下に本発明の実施の形態を詳細に説明するが、以下に記載する構成要件の説明は、本発明の実施態様の一例（代表例）であり、本発明はその要旨を変更しない限り、以下の内容に限定されない。なお、本明細書において「〜」という表現を用いる場合、その前後の数値を含む表現として用いる。 Hereinafter, embodiments of the present invention will be described in detail. However, the description of constituent elements described below is an example (representative example) of an embodiment of the present invention, and the present invention is described below unless the gist is changed. It is not limited to the content of. In this specification, the expression “to” is used as an expression including numerical values before and after the expression.
［本発明の検出材］
本発明の検出材は、ホワイトカーボンに発色剤を担持させた試薬担持ホワイトカーボンと、吸水性樹脂とを含有する。このような検出材は、流動性が高い状態のため、容器に収容させやすく、これを用いることで効率よく検出材を容器内に収容させた検出用具を製造することができる。また、発色時の均一性に優れ、発色の有無を観察しやすい。
[Detection material of the present invention]
The detection material of the present invention contains a reagent-supporting white carbon in which a color former is supported on white carbon, and a water-absorbing resin. Since such a detection material has a high fluidity, it can be easily stored in a container. By using such a detection material, a detection tool in which the detection material is efficiently stored in the container can be manufactured. In addition, the color uniformity is excellent, and it is easy to observe the presence or absence of color development.
［本発明の検出材の製造方法］
本発明の検出材の製造方法は、ホワイトカーボンを、発色剤を含む発色剤溶液に接触させ、前記発色剤溶液を吸収した吸液ホワイトカーボンを得る接触工程と、前記吸液ホワイトカーボンを乾燥させて試薬担持ホワイトカーボンを得る乾燥工程と、前記試薬担持ホワイトカーボンと、吸水性樹脂とを混合して検出材を得る混合工程と、を有する。このような製造方法により本発明の検出材を効率よく製造することができる。また、このような製造方法は検出材として優れた製造効率で混合できる。
[Production method of detection material of the present invention]
The production method of the detection material of the present invention, white carbon is contacted with a color former solution containing a color former, a contact step of obtaining an absorbent white carbon absorbing the color former solution, and drying the liquid absorbent white carbon And a mixing step of mixing the reagent-supporting white carbon and the water-absorbing resin to obtain a detection material. With such a manufacturing method, the detection material of the present invention can be efficiently manufactured. In addition, such a production method can be mixed with excellent production efficiency as a detection material.
［本発明の検出用具］
本発明の検出用具は、ホワイトカーボンに発色剤を担持させた試薬担持ホワイトカーボンと、吸水性樹脂とを容器に収容させたものである。このような検出用具とすることで、特に吸水性樹脂が検査対象の液を速やかに吸収する。そして、吸水性樹脂が容器内で接触しているホワイトカーボン等に、吸水性樹脂に吸収された液が表面張力等も利用しながら展開する。これにより短時間で検出材の着色の有無を確認することができる。また、検出用具内部の発色剤が発色時の均一性に優れ、発色の有無を観察しやすい。
なお、本発明の検出材の製造方法により本発明の検出材を製造することができる。また、本発明の検出材を用いて本発明の検出用具とすることができる。本願においてそれぞれに対応する構成は相互に利用することができる。
[Detection tool of the present invention]
The detection tool of the present invention is a container in which a reagent-supporting white carbon in which a color former is supported on white carbon and a water-absorbing resin are contained in a container. With such a detection tool, particularly, the water-absorbent resin quickly absorbs the liquid to be inspected. Then, the liquid absorbed by the water-absorbent resin spreads on the white carbon or the like with which the water-absorbent resin is in contact in the container while utilizing the surface tension and the like. Thus, the presence or absence of coloring of the detection material can be confirmed in a short time. Further, the coloring agent inside the detection tool has excellent uniformity at the time of coloring, and it is easy to observe the presence or absence of coloring.
The detection material of the present invention can be manufactured by the method for manufacturing a detection material of the present invention. Further, the detection tool of the present invention can be obtained by using the detection material of the present invention. In the present application, the corresponding configurations can be used mutually.
本発明の検出材を用いれば、試験対象の液等の検出対象の成分の有無等を検査することができる。これは、本発明の検出材に用いられる基材となるホワイトカーボンに担持された発色剤による。検出材は、ホワイトカーボンに担持された発色剤が所定の条件で対象となる汚染物質等の検出対象と反応することで発色し、その発色の有無によって目的とする汚染物質等の有無やその程度を把握することができる。 By using the detection material of the present invention, the presence or absence of a component to be detected such as a liquid to be tested can be inspected. This is due to the color former carried on white carbon, which is the substrate used in the detection material of the present invention. The detection material is colored by the reaction of the coloring agent carried on the white carbon with the detection target of the target contaminant or the like under predetermined conditions. Can be grasped.
発色試験に用いられている発色剤自体は、単独では結晶状の粉末や溶液等のものが多く、単独での取り扱い性が低い。または、実際の試験のための発色剤の必要量は微量であるのに対して、目視等で観察するために必要な量を、試験のたびに用いるには高価すぎたり、発色が強すぎて結果を観察しにくい場合がある。本発明においては、検出対象となる物質とは反応せず、その表面や内部に発色剤を分散担持させることができる基材のホワイトカーボンに、目視観察等に適した量の発色剤を担持させて用いる。 Many color developing agents used alone in the color forming test are in the form of a crystalline powder or a solution, and have low handleability by themselves. Or, while the required amount of the coloring agent for the actual test is very small, the amount required for visual observation or the like is too expensive to use for each test, or the color is too strong. The results may be difficult to observe. In the present invention, it does not react with the substance to be detected, and on the white carbon of the base material capable of dispersing and supporting the colorant on its surface or inside, the colorant is supported in an amount suitable for visual observation or the like. Used.
［ホワイトカーボン］
本発明の検出材等はホワイトカーボンを用いる。ホワイトカーボンは、微粉シリカともよばれ、微粉の無水ケイ酸、含水ケイ酸、ケイ酸カルシウム、ケイ酸アルミニウムの４種を指す。これらの主な製法としては、四塩化ケイ素の熱分解による乾式法や、ケイ酸ナトリウムの酸、二酸化炭素、アンモニウム塩などの複分解による沈殿生成物を得る湿式法、アルコールのような有機液体とシリカゲルをオートクレーブ中で加熱するいわゆるエアロゲル法などにより製造される。
[White carbon]
The detection material of the present invention uses white carbon. White carbon is also called finely divided silica and refers to four types of finely divided silicic anhydride, hydrous silicic acid, calcium silicate, and aluminum silicate. The main production methods include a dry method by pyrolysis of silicon tetrachloride, a wet method of obtaining a precipitation product by double decomposition of acid, carbon dioxide, and ammonium salt of sodium silicate, and an organic liquid such as alcohol and silica gel. Is heated in an autoclave by a so-called airgel method or the like.
［発色剤］
本発明の検出材等は、発色剤を基材であるホワイトカーボンに担持させたものを用いる。この発色剤とは、汚染物質等の検出対象となる物質と接触することで、着色や変色する物質のことである。以下、発色剤を具体的に例示する。
例えば、発色剤として、ランタン-アリザリンコンプレキソンを用いることができ、これは、フッ素（元素記号：Ｆ）の検出に適している。また、アゾメチンＨ（８−ヒドロキシ−１―（サリチリデンアミノ）−３，６−ナフタレンジスルホン酸・２ナトリウム塩）を用いることができ、これはホウ素（元素記号：Ｂ）の検出に適している。また、ＰＡＲ（４−（２−ピリジルアゾ）レゾルシノール）を用いることができ、これは鉛（元素記号：Ｐｂ）の検出に適している。
さらに、カルセインブルー、４,５−ヒドロキシ−３−（４−スルホ−１−ナフチルアゾ）−２,７−ナフタレンジスルホン酸（二ナトリウム）（ＳＰＡＤＮＳ）、または８−ヒドロキシ−７−ヨード−５−キノリンスルホン酸を用いることができ、これらはフッ素の検出に適している。また、キナリザリン、クルクミン、またはメチレンブルーを用いることができ、これらはホウ素の検出に適している。
また、カルボキシアルセナゾ、カルミン酸、キシレノールオレンジ（ＸＯ）、８−キノリノール（オキシン）、ｏ−（サリチリデンアミノ）チオフェノール（ＳＡＴＰ）、ジチゾン（ジフェニルチオカルバゾン）、ジフェニルカルバジド、ジフェニルカルバゾン、ジンコン（二ナトリウム塩）、スルホアルサゼン（ナトリウム塩）、チオオキシン、チオテノイルトリフルオロアセトン（ＳＴＴＡ）、５，１０，１５，２０，−テトラキス（ｐ−スルホフェニル）ポルフィン（ＴＰＰＳ４）、ピロガロールレッド（ＰＲ）、またはブロモピロガロールレッド（ＢＰＲ）を用いることができ、これらは鉛の検出に適している。
また、スチルバゾ（二アンモニウム塩）を用いることができ、これはフッ素およびホウ素の検出に適している。また、ピロカテコールバイオレット（ＰＶ）を用いることができ、これはフッ素、ホウ素および鉛の検出に適している。また、４−ピリジンカルボン酸を用いることができ、これはシアンの検出に適している。また、ナフチルエチレンジアミンを用いることができ、これは亜硝酸の検出に適している。また、ジフェニルカルバジド、またはヨウ化第二銅を用いことができ、これらは水銀の検出に適している。また、ジフェニルカルバジドは、六価クロム等の検出にも適している。また、七モリブデン酸六アンモニウムを用いることができ、これはヒ素の検出に適している。
[Coloring agent]
As the detection material of the present invention, a material in which a color former is supported on white carbon as a base material is used. The coloring agent is a substance that is colored or discolored by being brought into contact with a substance to be detected such as a contaminant. Hereinafter, the color former is specifically exemplified.
For example, lanthanum-alizarin complexone can be used as a color former, which is suitable for detecting fluorine (element symbol: F). Also, azomethine H (8-hydroxy-1- (salicylideneamino) -3,6-naphthalenedisulfonic acid disodium salt) can be used, which is suitable for detecting boron (element symbol: B). I have. Further, PAR (4- (2-pyridylazo) resorcinol) can be used, which is suitable for detecting lead (element symbol: Pb).
Further, calcein blue, 4,5-hydroxy-3- (4-sulfo-1-naphthylazo) -2,7-naphthalenedisulfonic acid (disodium) (SPADNS), or 8-hydroxy-7-iodo-5-quinoline Sulfonic acids can be used, which are suitable for detecting fluorine. Also, quinalizarin, curcumin, or methylene blue can be used, which are suitable for detecting boron.
In addition, carboxyarsenazo, carminic acid, xylenol orange (XO), 8-quinolinol (oxin), o- (salicylideneamino) thiophenol (SATP), dithizone (diphenylthiocarbazone), diphenylcarbazide, diphenylcarba Zon, zincon (disodium salt), sulfoarsazene (sodium salt), thiooxin, thiothenoyltrifluoroacetone (STTA), 5,10,15,20, -tetrakis (p-sulfophenyl) porphine (TPPS4), pyrogallol red ( PR) or bromopyrogallol red (BPR), which are suitable for detecting lead.
Also, stilbazo (a diammonium salt) can be used, which is suitable for detecting fluorine and boron. Alternatively, pyrocatechol violet (PV) can be used, which is suitable for detecting fluorine, boron and lead. Also, 4-pyridinecarboxylic acid can be used, which is suitable for detecting cyan. Also, naphthylethylenediamine can be used, which is suitable for detecting nitrous acid. Also, diphenylcarbazide or cupric iodide can be used, which are suitable for detecting mercury. Diphenylcarbazide is also suitable for detecting hexavalent chromium and the like. Also, hexaammonium heptamolybdate can be used, which is suitable for detecting arsenic.
例えばフッ素化合物に反応するランタン−アリザリンコンプレキソンの場合は以下のような反応性と特徴を有する。フッ素化合物のフッ化物イオン存在下に、ランタン（ＩＩＩ）とアリザリンコンプレキソン（１，２−ジヒドロキシアントラキノン−３−イルメチルアミン−Ｎ，Ｎ−二酢酸二水和物）との錯体（ランタン−アリザリンコンプレキソン）を加え、これがフッ化物イオンと反応して生じる青い色の複合錯体を形成するため、この青色の着色を確認することで、フッ素化合物の有無を確認することができる。
ランタン−アリザリンコンプレキソンを用いた反応については、前述の非特許文献１を参照して、そこで開示されているような各種試薬を調製し加えることで、ｐＨを調整する化合物や、反応阻害物による呈色抑制を防止する化合物等の反応助剤を、適宜、担持させたり、検出材に混合することができる。
For example, a lanthanum-alizarin complexone that reacts with a fluorine compound has the following reactivity and characteristics. Complex of lanthanum (III) with alizarin complexone (1,2-dihydroxyanthraquinone-3-ylmethylamine-N, N-diacetate dihydrate) (lanthanum-alizarin) in the presence of fluoride ion of a fluorine compound Complexone) is added, and this reacts with a fluoride ion to form a complex complex of blue color. By confirming this blue coloration, the presence or absence of a fluorine compound can be confirmed.
Regarding the reaction using lanthanum-alizarin complexone, with reference to the above-mentioned Non-patent Document 1, various reagents as disclosed therein are prepared and added to thereby adjust a pH-adjusting compound or a reaction inhibitor. A reaction aid such as a compound that prevents coloration can be appropriately loaded or mixed with the detection material.
本発明の検出材は、発色剤以外の物質を発色剤溶液などに混合して担持させてもよい。例えば、ｐＨ調整剤や、ｐＨ緩衝剤、マスキング剤などを混合して用いることができる。例えば、フッ素を検出するための検出材に担持されるものとしては、アンモニア、酢酸アンモニウム、酢酸ナトリウム三水和物、酢酸、アセトン、酢酸ナトリウム、硝酸カリウムが挙げられる。なお、このランタン−アリザリンコンプレキソン化合物を用いて各種反応助剤等を混合したフッ素検定試薬としてアルフッソン（登録商標、同仁化学研究所社製）を用いることができる。また、ＰＡＲ（４−（２−ピリジルアゾ）レゾルシノール）を用いる場合、シアン化物等を用いることができる。また、アゾメチンＨ（８−ヒドロキシ−１―（サリチリデンアミノ）−３，６−ナフタレンジスルホン酸）を用いる場合、アスコルビン酸、酢酸アンモニウム、硫酸、リン酸、クエン酸一水和物、ＥＤＴＡ・２Ｎａなどを用いることができる。ジフェニルカルバジドの場合、硫酸、塩酸、酢酸、クエン酸、シュウ酸、硝酸カリウム、ピロリン酸ナトリウム、スルファミン酸、二硫化カリウム、ピロ硫酸カリウムなどを用いることができる。なお、ここで、フッ素、ホウ素、鉛、６価クロムの検出に適した試薬について詳述したが、これらはそれぞれの試薬に適したｐＨの範囲で強酸性〜中性域〜弱アルカリ性（ｐＨ１〜９．５）等で反応するため、それぞれに適したｐＨとするための各種ｐＨ緩衝剤を併せて担持させておいてもよい。 The detection material of the present invention may be carried by mixing a substance other than the color former in a color former solution or the like. For example, a pH adjuster, a pH buffer, a masking agent and the like can be mixed and used. For example, ammonia, ammonium acetate, sodium acetate trihydrate, acetic acid, acetone, sodium acetate, and potassium nitrate are exemplified as those carried on a detection material for detecting fluorine. In addition, Alfusson (registered trademark, manufactured by Dojindo Laboratories) can be used as a fluorine assay reagent obtained by mixing various reaction aids and the like using the lanthanum-alizarin complexone compound. When PAR (4- (2-pyridylazo) resorcinol) is used, cyanide or the like can be used. When azomethine H (8-hydroxy-1- (salicylideneamino) -3,6-naphthalenedisulfonic acid) is used, ascorbic acid, ammonium acetate, sulfuric acid, phosphoric acid, citric acid monohydrate, EDTA. 2Na or the like can be used. In the case of diphenylcarbazide, sulfuric acid, hydrochloric acid, acetic acid, citric acid, oxalic acid, potassium nitrate, sodium pyrophosphate, sulfamic acid, potassium disulfide, potassium pyrosulfate and the like can be used. Here, the reagents suitable for detecting fluorine, boron, lead, and hexavalent chromium have been described in detail, but they are strongly acidic to neutral range to weakly alkaline (pH 1 to 5) in the range of pH suitable for each reagent. In order to carry out the reaction in 9.5) and the like, various pH buffers for adjusting the pH to an appropriate pH may be supported together.
［試薬担持ホワイトカーボン］
試薬担持ホワイトカーボンは、ホワイトカーボンに発色剤を担持させたものである。試薬担持ホワイトカーボンは、試薬を担持していることから、試験対象物質の液等と接したとき、検出対象物質が含まれるとき、反応して発色する。また、発色剤を担持した状態でも流動性に優れており容器内への充填にも適している。なお、試薬担持ホワイトカーボンは、特許第６２８８６６９号公報を適宜参照して作製してもよい。
[Reagent carrying white carbon]
The reagent-supporting white carbon is obtained by supporting a color former on white carbon. Since the reagent-carrying white carbon carries a reagent, it reacts and develops color when it comes into contact with a test substance liquid or the like and when it contains a detection substance. Also, it has excellent fluidity even in the state where the color former is supported, and is suitable for filling in a container. The reagent-carrying white carbon may be produced by appropriately referring to Japanese Patent No. 6288669.
本発明にはホワイトカーボン等を用いる。本発明の検出材や検出用具において、液を吸収するものを吸液材とよぶ。吸液材の吸液量は、吸液材が吸収することができる発色剤溶液量（吸液材が吸収することができる発色剤溶液量／吸液材質量）の計算式から求められる。以下、この計算式により求める吸液量を単に「吸液量」と記載し、発色剤溶液を吸収する特性を「吸液性」と記載する場合がある。本発明に用いられるは、発色剤溶液を、その吸液材の表面や内部に分散担持させることができる。
また、吸液材を用いて検出材を作製することで、発色剤を担持するのみでなく、さらに環境汚染物質等の有無を評価しようとする試験対象の液を吸収し、吸液材自身の表面や内部で発色反応が起こるため、使用時に適宜、この反応を所望の場所で行うことができるものである。
In the present invention, white carbon or the like is used. In the detection material and the detection tool of the present invention, a material that absorbs a liquid is called a liquid absorption material. The liquid absorption amount of the liquid absorbing material is obtained from a calculation formula of the amount of the color forming solution that can be absorbed by the liquid absorbing material (the amount of the color forming solution that can be absorbed by the liquid absorbing material / the mass of the liquid absorbing material). Hereinafter, the amount of liquid absorption obtained by this formula may be simply referred to as “liquid absorption amount”, and the characteristic of absorbing the color former solution may be described as “liquid absorption”. The color former solution used in the present invention can be dispersed and supported on the surface or inside of the liquid absorbing material.
In addition, by preparing the detection material using the liquid absorbing material, not only the color developing agent is carried, but also the liquid to be tested for evaluating the presence or absence of environmental pollutants and the like is absorbed, and the liquid absorbing material itself is absorbed. Since a color development reaction occurs on the surface or inside, this reaction can be appropriately performed at a desired place at the time of use.
この吸収する発色剤溶液量は、具体的には以下の方法で求めることができる。まず乾燥した吸液材の質量を測定した吸液前の吸液材を１００質量部とすると、この吸液材よりも十分量多い発色剤溶液に吸液材を３時間浸漬し、その吸液材が吸液できる最大量の吸液量を吸液させ、その後、浸漬している液から最大量吸液した吸液材を濾別することで取り出し、吸液後の吸液材質量であるＸ質量部を求める。この吸液後の吸液材質量Ｘ質量部から、吸液前の吸液材１００質量部を差し引き、吸液前の吸液材質量１００質量部で割った比を、質量％表記で表す。すなわち、吸液量（質量％）＝［（吸液後の吸液材質量Ｘ質量部−吸液前の吸液材質量１００質量部）／吸液前の吸液材質量１００質量部］×１００の式より求めることができる。
また、この試験を３回行った平均値を求めてその吸液材の吸液量とすることが好ましい。なお、本発明の吸液材は、このような発色剤溶液量を吸収することができる吸液材を用いればよく、実際に、検出材として保管するときなどに担持している量を示すものではない。
The amount of the color former solution to be absorbed can be specifically determined by the following method. First, assuming that the weight of the dried liquid absorbing material is 100 parts by mass, the liquid absorbing material is immersed in a sufficiently large amount of the coloring agent solution for 3 hours. Absorb the maximum amount of liquid that can be absorbed by the material, and then take out the maximum amount of absorbed liquid from the immersed liquid by filtering it out. Determine X parts by mass. The ratio obtained by subtracting 100 parts by mass of the liquid absorbing material before liquid absorption from the mass X of the liquid absorbing material after liquid absorption and dividing by 100 parts by mass of the liquid absorbing material before liquid absorption is expressed in terms of% by mass. That is, the liquid absorption amount (% by mass) = [(mass of liquid-absorbing material after liquid absorption X parts by mass-weight of liquid-absorbing material before liquid absorption 100 parts by mass) / 100 mass parts of liquid-absorbing material before liquid absorption] × It can be obtained from the equation of 100.
In addition, it is preferable that the average value obtained by performing this test three times is determined as the liquid absorption amount of the liquid absorbing material. The liquid-absorbing material of the present invention may be any liquid-absorbing material that can absorb such a color-forming agent solution, and indicates the amount carried when actually stored as a detection material. is not.
本発明の検出材においてホワイトカーボンは吸液材として用いることができ、その吸液量が、５０質量％以上であることが好ましい。好ましくは６０質量％以上や、７０質量％以上である。吸液量がより大きい方が、発色剤を担持させやすく、検出材としたとき試験対象中の液を吸収しやすく安定した測定結果を得やすい。ホワイトカーボンの吸液量の上限は特に定めなくてもよいが、６００質量％以下や、５００質量％以下、４００質量％以下のように上限を設けてもよい。 In the detection material of the present invention, white carbon can be used as a liquid absorbing material, and the liquid absorption amount is preferably 50% by mass or more. It is preferably at least 60% by mass or at least 70% by mass. The larger the amount of liquid absorption, the more easily the color former is carried, and the easier it is to absorb the liquid in the test object as a detection material, and the more stable the measurement results can be obtained. The upper limit of the amount of liquid absorption of white carbon is not particularly limited, but may be set to an upper limit of 600% by mass or less, 500% by mass or less, or 400% by mass or less.
また、本発明における吸液量は単に純水の吸収量ではなく、吸液材は使用する発色剤溶液の量として、前記した範囲の量を吸収する。単に水を吸収することができる吸液材であっても、実際に使用する発色剤溶液は、水と発色剤の他に、ｐＨ緩衝剤や、反応阻害物質抑制剤等、様々な反応、呈色補助剤を加えることが多く、これらはイオンや界面活性剤等、吸液材として使用される物質が吸収する液量に対して大きな影響を与えることが多いものであるから、水の吸収量とは異なる挙動を示す場合があるためである。 Further, the amount of liquid absorption in the present invention is not simply the amount of pure water absorbed, but the amount of the liquid absorbing material absorbed in the above-described range as the amount of the color former solution to be used. Even if it is a liquid absorbing material that can simply absorb water, the color former solution actually used is not limited to water and the color former, but also has various reactions and presentations such as a pH buffering agent and a reaction inhibitor. Color aids are often added, and these often have a large effect on the amount of liquid absorbed by substances used as liquid absorbing materials, such as ions and surfactants. This is because the behavior may be different from the above.
本発明の検出材は、試薬担持ホワイトカーボンを含む。ホワイトカーボンへの発色剤の担持は、具体的な方法として後述するような手段で行うことができる。ここで、吸液材に担持させる発色剤量は、その検出材が検出対象とする環境汚染物質等の濃度によって発色することを確認することができる量であればよい。このときの発色剤の担持量は、この検出材を製造する際の仕込み量としての濃度比から求められる値として管理することもできる。この値は、担持された発色剤溶液中の発色剤質量／吸液前の吸液材質量として、一般的に単位は（μｇ／ｇ）や（ｍｇ／ｇ）、（ｇ／ｇ）で表示される。 The detection material of the present invention contains reagent-carrying white carbon. The loading of the color former on the white carbon can be carried out by a means described later as a specific method. Here, the amount of the coloring agent to be carried on the liquid absorbing material may be an amount that can confirm that the detecting material is colored depending on the concentration of the environmental pollutant to be detected. At this time, the amount of the coloring agent carried can also be managed as a value obtained from a concentration ratio as a charged amount when manufacturing the detection material. This value is represented by (μg / g), (mg / g), or (g / g) in terms of the mass of the coloring agent in the supported coloring agent solution / the mass of the liquid absorbing material before liquid absorption. Is done.
試薬担持ホワイトカーボンの発色剤担持量は、ホワイトカーボンの質量比（発色剤担持量／ホワイトカーボン）で、５μｇ／ｇ〜２．０ｇ／ｇのような範囲で、発色剤の種類や、ホワイトカーボンに吸液させておく量、検出材全体に占める量等を考慮して適宜設定される。発色剤担持量の下限は、１０μｇ／ｇ以上や、０．０５ｍｇ／ｇ以上、０．１ｍｇ／ｇ以上がより好ましい。また、その上限は５０ｍｇ／ｇ以下がより好ましい。上限は、１．０ｇ／ｇ以下や、８００ｍｇ／以下、５００ｍｇ／ｇ以下としてもよい。 The amount of the color former carried by the reagent-supporting white carbon is in the range of 5 μg / g to 2.0 g / g in the mass ratio of white carbon (color former carried amount / white carbon). The amount is set appropriately in consideration of the amount of liquid to be absorbed, the amount of the entire detection material, and the like. The lower limit of the amount of the color former carried is more preferably 10 μg / g or more, 0.05 mg / g or more, and 0.1 mg / g or more. The upper limit is more preferably 50 mg / g or less. The upper limit may be 1.0 g / g or less, 800 mg / g or less, or 500 mg / g or less.
この担持量が少ない場合、発色が弱く目視等での確認が困難となる場合がある。一方、過度に高濃度の発色剤を担持させることは、吸液材を用いる利点を失うものとなるばかりではなく、評価を適切に行えなくなったり、発色が強すぎその発色の程度を確認しにくくなったり、他の反応による呈色の弊害が生じる場合がある。また、検出材の吸液量の限度に近い発色剤溶液を担持させると、土壌や水から吸液することができなくなり、十分に反応させることができない場合もある。 When the amount is small, the color may be weak and it may be difficult to confirm it visually. On the other hand, carrying an excessively high concentration of the color former not only loses the advantage of using the liquid absorbing material, but also makes it impossible to perform evaluation properly or the color is too strong to confirm the degree of the color development. Or the adverse effect of coloration due to other reactions may occur. Further, if a colorant solution having a liquid absorption amount close to the limit of the amount of liquid absorbed by the detection material is carried, the liquid cannot be absorbed from soil or water, and the reaction may not be sufficiently performed.
この好ましい担持量の具体例を例示すると、以下のものがあげられる。
ランタン−アリザリンコンプレキソンは、０．３ｍｇ／ｇ〜１．０ｇ／ｇ程度とすることができ、好ましくは３ｍｇ／ｇ〜０．８ｇ／ｇ程度、さらに好ましくは１５ｍｇ／ｇ〜０．４ｇ／ｇとすることができる。
アゾメチンＨ（８−ヒドロキシ−１―（サリチリデンアミノ）−３，６−ナフタレンジスルホン酸・２ナトリウム塩））は、０．０１ｇ／ｇ〜２．０ｇ／ｇ程度、好ましくは０．１ｇ／ｇ〜１．０ｇ／ｇ程度、さらに好ましくは０．１ｇ／ｇ〜０．５ｇ／ｇとすることができる。
ＰＡＲ（４−（２−ピリジルアゾ）レゾルシノール）は、１μｇ／ｇ〜３０ｍｇ／ｇ程度、好ましくは５０μｇ／ｇ〜３ｍｇ／ｇ程度、さらに好ましくは０．２ｍｇ／ｇ〜２ｍｇ／ｇ程度とすることができる。
ジフェニルカルバジドは、０．０５ｍｇ／ｇ〜１．０ｇ／ｇ程度、好ましくは０．５ｍｇ／ｇ〜０．２ｇ／ｇ程度、さらに好ましくは５ｍｇ／ｇ〜５０ｍｇ／ｇ程度とすることができる。
各発色剤や、測定対象中の汚染物質の濃度に応じて、これらは適宜変更されるが、本発明の検出材は、吸液材に吸液させる発色剤溶液量や濃度を変更することでこれらを簡易に調製することができる点でも優れている。
Illustrative examples of the preferred loading amount include the following.
Lanthanum-alizarin complexone can be about 0.3 mg / g to 1.0 g / g, preferably about 3 mg / g to 0.8 g / g, more preferably 15 mg / g to 0.4 g / g. It can be.
Azomethine H (8-hydroxy-1- (salicylideneamino) -3,6-naphthalenedisulfonic acid disodium salt)) is about 0.01 g / g to 2.0 g / g, preferably 0.1 g / g. g to about 1.0 g / g, more preferably 0.1 g / g to 0.5 g / g.
PAR (4- (2-pyridylazo) resorcinol) may be about 1 μg / g to about 30 mg / g, preferably about 50 μg / g to about 3 mg / g, and more preferably about 0.2 mg / g to about 2 mg / g. it can.
The amount of diphenylcarbazide can be about 0.05 mg / g to 1.0 g / g, preferably about 0.5 mg / g to 0.2 g / g, and more preferably about 5 mg / g to 50 mg / g.
These are appropriately changed according to the concentration of each coloring agent and the contaminant in the measurement object.However, the detection material of the present invention is obtained by changing the amount and concentration of the coloring agent solution to be absorbed by the liquid absorbing material. They are also excellent in that they can be easily prepared.
［吸水性樹脂］
本発明の吸液材の一例である吸水性樹脂とは、吸水性を有する高分子である。このような吸水性樹脂しては、セルロース-アクリロニトリルグラフト共重合体やカルボキシメチルセルロース架橋体等のセルロース系のものや、ポリビニルアルコール架橋体やポリビニルアルコール吸水ゲル凍結・解凍エラストマーのようなポリビニルアルコール系のもの、アクリル酸とナトリウム・ビニルアルコール共重合体やポリアクリル酸ナトリウム架橋体等のアクリル酸系のもの、Ｎ−置換アクリルアミド架橋体等のアクリルアミド系のもの、ポリアルキレンオキサイド系のものが挙げられる。より具体的には、変性ポリアルキレンオキサイド／ノニオン型熱可塑性吸水樹脂、アクリル酸重合体部分ナトリウム塩架橋物等が好ましく用いられる。
なお、これらの吸水性樹脂の分子量等は適宜、本発明の目的を達成することができる範囲で任意に設定することができる。これらの吸水性樹脂は、吸水力が高いものが多く、本発明の発色剤溶液の多くが水系の溶液のため、これらの発色剤溶液を充分量担持した上で、さらに、環境汚染物質の有無を評価するに当たっては、当該評価の対象となる土壌や水中の水分を吸収し、簡易にかつ速やかに使用することができる検出材として機能する。
[Water absorbent resin]
The water-absorbent resin, which is an example of the liquid-absorbing material of the present invention, is a polymer having water absorbency. Examples of such water-absorbent resin include cellulose-based resins such as cellulose-acrylonitrile graft copolymer and carboxymethylcellulose crosslinked product, and polyvinyl alcohol-based such as polyvinyl alcohol crosslinked product and polyvinyl alcohol water-absorbing gel frozen / thawed elastomer. And acrylic acid-based ones such as a crosslinked product of acrylic acid and sodium / vinyl alcohol and sodium polyacrylate, acrylamide-based ones such as N-substituted acrylamide cross-linked ones, and polyalkylene oxide-based ones. More specifically, a modified polyalkylene oxide / nonionic thermoplastic water-absorbing resin, an acrylic acid polymer partial sodium salt crosslinked product, or the like is preferably used.
The molecular weight and the like of these water-absorbing resins can be appropriately set as long as the object of the present invention can be achieved. Many of these water-absorbing resins have a high water-absorbing power, and since most of the color-forming agent solutions of the present invention are aqueous solutions, a sufficient amount of these color-forming agents are supported, and furthermore, the presence or absence of environmental pollutants In evaluating, it functions as a detection material that absorbs moisture in soil or water to be evaluated and can be used easily and quickly.
本発明の検出材に用いられる吸水性樹脂は、吸水することができる吸水量が、２００質量％以上であることが好ましい。この吸水量は、前述した吸液材の吸液量において、発色剤溶液に代えて水に対する値として算出することができる。吸水性樹脂は、予め発色剤溶液を吸水させることなく試薬担持ホワイトカーボンと混合して用いることができる。吸水性樹脂は、本発明の検出材や検出用具として用いるとき、検出対象の水等の液を積極的に吸収し、その液を検出材全体に展開する。 The water-absorbent resin used in the detection material of the present invention preferably has an amount of water absorption capable of absorbing water of 200% by mass or more. This water absorption amount can be calculated as a value for water instead of the color former solution in the liquid absorption amount of the liquid absorbing material described above. The water-absorbing resin can be used by being mixed with the reagent-supporting white carbon without absorbing the color former solution in advance. When the water-absorbent resin is used as the detection material or the detection tool of the present invention, it positively absorbs a liquid such as water to be detected and spreads the liquid throughout the detection material.
吸水性樹脂の吸水量は、好ましくは３００質量％以上や、４００質量％以上である。吸水量がより大きい方が、検出材としたとき試験対象中の液を吸収しやすく安定した測定結果を得やすい。また、その上限は、例えば１００，０００質量％以下や、好ましくは８０，０００質量％以下、より好ましくは６５，０００質量％以下である。吸水量の上限は、吸水材の種類によるためほぼ制限はないが、一方でこれらの値以上である必要性は低く、また、吸水量が大きすぎる場合、試験対象から吸収する液量と検出材とのバランスが崩れ、正しい試験結果を得られない場合がある。 The water absorption of the water-absorbing resin is preferably 300% by mass or more, or 400% by mass or more. The larger the water absorption, the easier it is to absorb the liquid in the test object when used as the detection material, and the more stable the measurement results are obtained. The upper limit is, for example, 100,000% by mass or less, preferably 80,000% by mass or less, more preferably 65,000% by mass or less. There is almost no upper limit to the amount of water absorption because it depends on the type of water-absorbing material.On the other hand, it is not necessary to exceed these values.If the amount of water absorption is too large, the amount of liquid absorbed from the test object and the amount of detection material Balance may be lost and correct test results may not be obtained.
本発明の検出材等に用いる吸水性樹脂は、吸水していない状態で、試薬担持ホワイトカーボンと混合したり、検出材用具の容器内に収容させることが好ましい。吸水していない状態の吸水性樹脂とは、未使用の吸水性樹脂や、低湿環境等で保管したり、検出材等として混合等する前に、乾燥したものである。吸水していない状態は、吸水性樹脂が、凝集して塊状となったり一体化していないことをもって吸水していないとしてよく、粒状や粉状や、これらに準じて取り扱える状態をいう。 It is preferable that the water-absorbent resin used for the detection material of the present invention is mixed with the reagent-carrying white carbon in a state where it does not absorb water, or is contained in the container of the detection material tool. The non-water-absorbing water-absorbing resin is an unused water-absorbing resin, a resin that is dried before being stored in a low-humidity environment or the like, or mixed as a detection material or the like. The state in which water is not absorbed may mean that the water-absorbent resin does not absorb water by agglomerating into a mass or not being integrated, and refers to a state in which the water-absorbent resin can be handled in a granular or powdery state.
本発明の検出材において吸水性樹脂の含水率は、３０％以下であることが好ましい。吸水性樹脂の含水率は、水分計で吸水性樹脂（０．５ｇ〜１ｇ）を１００度で１０分間加熱処理することで吸水していた水が乾燥することから、その乾燥の前後の重量比から求めることができる。含水率は２８％以下がより好ましく、２５％以下がさらに好ましく、１０％以下が特に好ましい。含水率が高い状態で検出用具とするために容器に充填しようとすると、流動性が低く充填しにくい場合がある。また、検出材や検出用具として使用するとき、試験対象液の吸水が遅くなる場合がある。 In the detection material of the present invention, the water content of the water absorbent resin is preferably 30% or less. The water content of the water-absorbent resin is determined by heating the water-absorbent resin (0.5 g to 1 g) with a moisture meter at 100 ° C. for 10 minutes to dry the absorbed water. Can be obtained from The water content is more preferably 28% or less, further preferably 25% or less, and particularly preferably 10% or less. If it is attempted to fill a container with a high water content in order to use it as a detection tool, the fluidity may be low and filling may be difficult. Further, when used as a detection material or a detection tool, water absorption of the test target liquid may be delayed.
［検出材］
検出材は、試験対象物質に接触したとき、その中に検出材の検出対象のものが存在するか否かや、その濃度等を判断することができる着色反応等の変化が生じるものである。検出材は、検出材のまま試験対象の場に散布等したり、試験対象の液に混合分散させたり、容器等に収容した検出用具等の状態として用いることができる。
[Detection material]
When the detection material comes into contact with the test target substance, a change in coloring reaction or the like can be made to determine whether or not the detection target substance exists in the test material and its concentration can be determined. The detection material can be used as a detection material, such as sprayed on a test target site, mixed and dispersed in a test target liquid, or in a state of a detection tool or the like housed in a container or the like.
本発明の検出材は、ホワイトカーボンに発色剤を担持させた試薬担持ホワイトカーボンと、吸水性樹脂とを含有する。本発明の検出材は、試薬担持ホワイトカーボンと、吸水性樹脂との混合質量比（試薬担持ホワイトカーボン：吸水性樹脂）が、２００：１〜１：３０であることが好ましい。このような数値範囲で混合することで、より安定して短時間で発色の有無を確認しやすくなる。吸水性樹脂は比較的少なくてもよい。吸水性樹脂は吸液量が高く、検出材に少量含むことでも使用時の吸液量が向上し発色の有無を短時間で確認しやすくなる。一方、吸水性樹脂が多すぎると、相対的に試薬担持ホワイトカーボンが少なくなるため、発色を確認しにくくなる場合がある。この混合質量比は、試薬担持ホワイトカーボンの方が多い比率として、１５０：１〜や、１２０：１〜、１００：１〜のような範囲を設けてもよい。一方、吸水性樹脂の方が多い比率として、〜１：２５や、〜１：２０、〜１：１５、〜１：１０のような範囲を設けてもよい。 The detection material of the present invention contains a reagent-supporting white carbon in which a color former is supported on white carbon, and a water-absorbing resin. In the detection material of the present invention, the mixing mass ratio of the reagent-carrying white carbon and the water-absorbing resin (reagent-carrying white carbon: water-absorbing resin) is preferably from 200: 1 to 1:30. By mixing in such a numerical range, it becomes easier to more stably confirm the presence or absence of color development in a short time. The water absorbing resin may be relatively small. The water-absorbing resin has a high liquid-absorbing amount. Even if a small amount is contained in the detection material, the liquid-absorbing amount at the time of use is improved, and it becomes easy to confirm the presence or absence of color development in a short time. On the other hand, when the amount of the water-absorbing resin is too large, the amount of the reagent-supporting white carbon is relatively reduced, so that it may be difficult to confirm color development. The mixing mass ratio may be set in a range such as 150: 1, 120: 1, or 100: 1, as the ratio of the reagent-carrying white carbon is larger. On the other hand, a range such as １ ： 1: 25, １ ： 1: 20, １ ： 1: 15, 〜1: 10 may be provided as the ratio of the water-absorbent resin.
検出材の安息角は、４０度以下であることが好ましい。安息角を４０度以下とすることで、より安定して充填などの取り扱いに優れた検出材となる。安息角の測定は、注入法により測定する。注入法は、検出材を容器に容れて自然落下させたとき、落下して平面に堆積した検出材がなす角度を測定するものである。検出材は、試料９．０ｇを用いて、注入法を行う容器として傾斜６３度、排出口幅φ２３ｍｍの漏斗を用いて、漏斗出口から平面までの距離を６０ｍｍとして測定する。３回測定した平均値を用いることが好ましい。安息角は、検出材の場合、試薬担持ホワイトカーボンと吸水性樹脂等とを混合した状態で測定する。安息角を測定する前に、検出材は、充填時を想定した状態で測定することが好ましく、混合後そのまま測定したり、適宜乾燥した状態で測定することができる。例えば、５０度に設定した真空乾燥機で５時間乾燥した状態で測定した値をその安息角の代表値としてもよい。安息角は、３８度以下がより好ましく、３６度以下がさらに好ましく、３０度以下が特に好ましい。 The angle of repose of the detection material is preferably 40 degrees or less. By setting the angle of repose to 40 degrees or less, the detection material becomes more stable and is excellent in handling such as filling. The angle of repose is measured by the injection method. In the injection method, when the detection material is allowed to fall naturally in a container, the angle formed by the detection material that has fallen and deposited on a flat surface is measured. The detection material is measured using 9.0 g of a sample, using a funnel having an inclination of 63 degrees and a discharge port width of 23 mm as a container for performing an injection method, and setting a distance from a funnel outlet to a plane to be 60 mm. It is preferable to use an average value measured three times. In the case of a detection material, the angle of repose is measured in a state where a reagent-carrying white carbon and a water-absorbing resin are mixed. Before measuring the angle of repose, it is preferable to measure the detection material in a state in which it is assumed to be filled, and it can be measured as it is after mixing, or it can be measured in an appropriately dried state. For example, a value measured after drying for 5 hours with a vacuum dryer set to 50 degrees may be used as a representative value of the angle of repose. The angle of repose is preferably 38 degrees or less, more preferably 36 degrees or less, and particularly preferably 30 degrees or less.
［検出材の製造］
本発明の検出材の製造方法について、以下に詳述する。
[Manufacture of detection material]
The method for producing the detection material of the present invention will be described in detail below.
［接触工程］
本発明の検出材の製造方法は、ホワイトカーボンを、発色剤を含む発色剤溶液に接触させ、発色剤溶液を吸収した吸液ホワイトカーボンを得る接触工程を有する。この接触により、液中の発色剤がより含侵されるようにホワイトカーボンの孔内に広く浸透して担持される。この接触は、ホワイトカーボンと発色剤溶液とが接触すればよく、容器内等で、ホワイトカーボンに発色剤溶液を加えてもよいし、発色剤溶液にホワイトカーボンを加えてもよい。発色剤溶液を吸液した状態のホワイトカーボンを、吸液ホワイトカーボンと呼ぶ。
[Contact process]
The method for producing a detection material of the present invention has a contacting step of bringing white carbon into contact with a color former solution containing a color former to obtain a liquid-absorbing white carbon absorbing the color former solution. Due to this contact, the colorant in the liquid is permeated widely and supported in the pores of the white carbon so as to be more impregnated. This contact may be made by contacting the white carbon with the color former solution. The color former solution may be added to the white carbon in a container or the like, or white carbon may be added to the color former solution. White carbon in a state in which the color former solution is absorbed is referred to as liquid-absorbed white carbon.
接触させるときの、ホワイトカーボンと、発色剤溶液との質量比（ホワイトカーボン：発色剤溶液）は、特に制限はなく、ホワイトカーボンが吸液量や、発色剤溶液の発色剤等の濃度、乾燥時間などを鑑み、ホワイトカーボンに発色剤が十分に担持されるように適宜設定される。例えば、ホワイトカーボンの吸液量を考慮し、質量比（ホワイトカーボン：発色剤溶液）が、５：１〜１：１０程度の範囲とすることができ、３：１〜１：５や、２：１〜１：３としてもよい。接触させた発色剤溶液をすべて吸液してもよいし、吸液量が飽和する量で接触させてもよい。また、接触時には、適宜、振とうして、ホワイトカーボン全体と効率よく接触させたり、加圧・減圧してホワイトカーボンの孔内に液が効率よく含侵させてもよい。 The mass ratio between the white carbon and the color former solution (white carbon: color former solution) at the time of contact is not particularly limited, and the white carbon absorbs the liquid, the concentration of the color former in the color former solution, and the drying. In consideration of the time and the like, it is appropriately set so that the color former is sufficiently supported on the white carbon. For example, in consideration of the liquid absorption amount of white carbon, the mass ratio (white carbon: color former solution) can be in the range of about 5: 1 to 1:10, and 3: 1 to 1: 5, 2 : 1 to 1: 3. The color former solution that has been brought into contact may be entirely absorbed, or may be brought into contact with an amount at which the amount of absorbed liquid is saturated. Further, at the time of contact, the liquid may be appropriately shaken to make efficient contact with the whole white carbon, or the liquid may be efficiently impregnated into the pores of the white carbon by applying pressure and pressure.
ホワイトカーボンは、予め乾燥させた状態で用いることが好ましい。発色剤溶液の発色剤濃度は、発色剤の種類や担持させる量を考慮して適宜設定される。また、発色剤溶液の溶媒は、発色剤が分散・溶解する溶媒を適宜用いることができる。ホワイトカーボンは、各種溶媒に耐性が高いため、この溶媒として採用できる溶媒種も多い点でも優れている。 The white carbon is preferably used in a state of being dried in advance. The color-forming agent concentration of the color-forming agent solution is appropriately set in consideration of the type of the color-forming agent and the amount to be carried. Further, as the solvent of the color former solution, a solvent in which the color former is dispersed / dissolved can be appropriately used. Since white carbon has high resistance to various solvents, it is also excellent in that many types of solvents can be employed as this solvent.
［乾燥工程］
本発明の検出材の製造方法は、吸液ホワイトカーボンを乾燥させて試薬担持ホワイトカーボンを得る乾燥工程を有する。吸液ホワイトカーボンを乾燥させたものを、試薬担持ホワイトカーボンと呼ぶ。吸液ホワイトカーボンは、溶媒を吸液した状態のため、吸水性樹脂と混合したり、検出材として使用したり、容器内に収容させるときの流動性を向上させるために、湿潤状態のままでなく、乾燥させて用いることが好ましい。
[Drying process]
The method for producing a detection material of the present invention includes a drying step of drying a liquid-absorbing white carbon to obtain a reagent-carrying white carbon. The dried liquid-absorbing white carbon is referred to as reagent-carrying white carbon. The liquid-absorbing white carbon is in a wet state in order to improve the fluidity when mixed with a water-absorbing resin, used as a detecting material, or contained in a container because the solvent has absorbed the liquid. Preferably, it is dried before use.
乾燥は、ホワイトカーボンが吸液している発色剤溶液の溶媒を除去できる任意の手法で行うことができる。例えば、加熱乾燥や、風乾、減圧乾燥、噴霧乾燥、凍結乾燥等、またこれらを組み合わせた乾燥を行うことができる。乾燥時の温度は、乾燥手法に応じて適宜選択することができる。加熱を伴う乾燥の場合、常温程度〜１５０℃程度でおこなうことができ、５０℃〜８０℃程度で行うことがより好ましい。また凍結乾燥等を行う場合、０℃以下で乾燥してもよい。 Drying can be performed by any method capable of removing the solvent of the color former solution in which the white carbon is absorbing. For example, drying by heating, air drying, drying under reduced pressure, spray drying, freeze drying and the like, or a combination thereof can be performed. The temperature during drying can be appropriately selected according to the drying technique. In the case of drying with heating, the drying can be performed at about room temperature to about 150 ° C, and more preferably at about 50 ° C to 80 ° C. When freeze-drying or the like is performed, drying may be performed at 0 ° C. or less.
また、乾燥時間は、溶媒量等を考慮し、溶媒がある程度揮発し、取り扱い性等に問題がない範囲で適宜設定される。例えば、３０分以上や、１時間以上、３時間以上、６時間以上等とすることができる。乾燥温度等の条件にもよるが、１週間以内や、３日以内、２日以内程度で乾燥終了してもよい。 The drying time is appropriately set in consideration of the amount of the solvent and the like, as long as the solvent is volatilized to some extent and there is no problem in handleability and the like. For example, it can be 30 minutes or more, 1 hour or more, 3 hours or more, 6 hours or more, and the like. Depending on the conditions such as the drying temperature, the drying may be completed within one week, three days, or two days.
この乾燥は、溶媒が完全に除去される程度の乾燥としてもよいが、ある程度揮発すれば、取り扱い性等の問題は解消する。このため、接触工程で接触させ吸液した発色剤溶液の溶媒が十分に除去された段階で乾燥を終了する。この乾燥の程度は、乾燥された吸液ホワイトカーボンの含水率が２０％以下となった状態を目安とすることができる。含水率は１０％以下や、５％以下まで乾燥してもよい。なお、ホワイトカーボンの方が吸水性樹脂よりも短い時間の乾燥で、取り扱いしやすい状態となる点でも吸液ホワイトカーボンを乾燥することは優れている。 This drying may be drying to the extent that the solvent is completely removed, but if volatilized to some extent, problems such as handleability will be resolved. Therefore, the drying is completed when the solvent of the color former solution that has been contacted and absorbed in the contact step is sufficiently removed. The degree of this drying can be a standard when the moisture content of the dried liquid-absorbing white carbon is 20% or less. The moisture content may be dried to 10% or less or 5% or less. Drying liquid-absorbent white carbon is superior in that white carbon is easier to handle in a shorter time than water-absorbent resin.
［混合工程］
本発明の検出材の製造方法は、試薬担持ホワイトカーボンと、吸水性樹脂とを混合して検出材を得る混合工程を有する。
なお、ホワイトカーボンに発色剤を担持することで、ホワイトカーボンは乾燥するだけで優れた流動性を有するものとなるため、乾燥後に粉や粒とするための粉砕工程が必要ない。また、吸水性樹脂に液を加えると、液を展開させるための撹拌が行いにくかった。さらに、その後に粉砕等するために吸液した吸水性樹脂を薄く延ばす工程を設ける方が好ましい。しかし、ホワイトカーボンは撹拌も吸水性樹脂に比べて行いやすく、各ホワイトカーボンの粒が分散しやすいため、延ばしたり粉砕したりする工程を行わず優れた製造効率で製造できる。
[Mixing process]
The method for producing a detection material of the present invention includes a mixing step of mixing a reagent-supporting white carbon and a water-absorbing resin to obtain a detection material.
In addition, by supporting the color former on the white carbon, the white carbon has excellent fluidity only by drying, so that a pulverizing step for forming powder or granules after drying is unnecessary. Further, when the liquid was added to the water-absorbent resin, stirring for developing the liquid was difficult to perform. Further, it is preferable to provide a step of thinly spreading the water-absorbing resin that has absorbed the liquid for subsequent pulverization or the like. However, white carbon is easier to stir than the water-absorbent resin, and the particles of each white carbon are easier to disperse. Therefore, white carbon can be produced with excellent production efficiency without performing a step of extending or pulverizing.
［収容工程］
さらに、本願は、このように調整された検出材等を、容器に収容する収容工程を有する検出用具の製造方法とすることができる。本発明の検出材は、流動性に優れているため、容器へ収容させやすく、効率よく検出用具を製造することができる。収容においては、所定の量容器に加えるための操作としても取り扱いやすく、容器内で蓋を設けるために所定の形状として広げる際にも取り扱いやすい。吸水性樹脂に加工をしないため、粉粒の状態で使用できる。ホワイトカーボンも粉粒状のため、流動性があるため、充填が容易になった。
[Containment process]
Furthermore, the present application can be a method for manufacturing a detection tool having a housing step of housing a detection material or the like adjusted in such a manner in a container. Since the detection material of the present invention has excellent fluidity, it can be easily stored in a container, and a detection tool can be manufactured efficiently. In the storage, it is easy to handle as an operation for adding a predetermined amount to the container, and it is easy to handle when expanding the container to a predetermined shape to provide a lid in the container. Since the water-absorbent resin is not processed, it can be used in the form of powder. Since the white carbon is also in the form of powder and granules, it has fluidity, so that the filling becomes easy.
［検出用具］
本発明の検出用具は、ホワイトカーボンに発色剤を担持させた試薬担持ホワイトカーボンと、吸水性樹脂とを容器に収容させたものである。この検出用具は、容器内に、試験対象の液を加えることで検出材がその液の成分に反応し、発色剤の発色の有無で検査することができる。容器に検出材が含まれた状態のままで検査することもでき取り扱いやすい。検出用具への、試薬担持ホワイトカーボンと吸水性樹脂との収容は、これらを予め混合した状態で容れてもよいし、これらをそれぞれ別々に収容してもよい。容器内に収容し、密閉した状態で振るなどの操作により混合させることができる。
[Detection tool]
The detection tool of the present invention is a container in which a reagent-supporting white carbon in which a color former is supported on white carbon and a water-absorbing resin are contained in a container. In this detection tool, when a liquid to be tested is added to a container, the detection material reacts to the components of the liquid, and it can be inspected by the presence or absence of coloring of the coloring agent. Inspection can be performed with the container containing the detection material, which is easy to handle. The detection tool may contain the reagent-carrying white carbon and the water-absorbing resin in a state where they are mixed in advance, or they may be stored separately. It can be contained in a container and mixed by an operation such as shaking in a sealed state.
容器は、検出材を収容できる任意のものを用いることができる。好ましくは、容器内に円滑に試験対象の液を加えることができるように容器内の容量に空きがあるようにしたり、液を収容して容量が広がる袋状のものなどを用いる。このために、容器には容器内に液を加えるための開口部や、開口させるための易割部、開閉を調整できる開閉部、液のみを通過させる通液部などを設けることが好ましい。 Any container that can accommodate the detection material can be used as the container. It is preferable to use a bag or the like which has an empty space in the container or has a large capacity to accommodate the liquid so that the liquid to be tested can be smoothly added to the container. For this purpose, it is preferable that the container is provided with an opening for adding a liquid into the container, an easy-to-open part for opening, an opening / closing part capable of adjusting opening and closing, a liquid passing part for passing only the liquid, and the like.
検出用具は、例えば、検出材を内包させた包装構造を有する検出用具であり、前記包装構造の第一の面として懸濁物質の通過を抑制し通液性を有する多孔質材の層を有し、前記包装構造の第二の面として透明樹脂製の透明層を有し、第一の面と第二の面との周囲に接着部を有する包装構造である検出用具のような構造とすることができる。この構造は、特許第６２９２６４７号公報を適宜参照して作製してもよい。このような検出用具とすれば、多孔質材の層から液を選択的に吸液して検出用具内の検出材がその液と接触する。そして反応の有無を確認するときは、この透明層から観察することができる。 The detection tool is, for example, a detection tool having a packaging structure in which a detection material is included, and has a layer of a porous material that suppresses the passage of suspended substances and has liquid permeability as a first surface of the packaging structure. Then, the second surface of the packaging structure has a transparent layer made of a transparent resin, and has a structure like a detection tool which is a packaging structure having an adhesive portion around the first surface and the second surface. be able to. This structure may be manufactured by appropriately referring to Japanese Patent No. 6292647. With such a detection tool, the liquid is selectively absorbed from the porous material layer, and the detection material in the detection tool comes into contact with the liquid. When confirming the presence or absence of a reaction, observation can be made from this transparent layer.
また、検出用具には、色見本部を設けてもよい。この色見本と比較して、発色剤が反応する対象の物質が試験対象に含まれているか判別することができる。 The detection tool may be provided with a color sample section. By comparing with the color sample, it is possible to determine whether or not the test target contains a substance to which the color former reacts.
［実施形態］
図１は、本発明の検出用具の実施形態の一例を示すものである。検出用具１は、透明容器３と不織布４とによる容器内に、検出材２が収容されている。なお、透明容器３と不織布４とは、溶着部５によりその周囲が接着させてある。この不織布４側から、試験対象の液が選択的に検出用具１内に通液し、検出材２に吸液され、発色剤の検出対象が含まれている場合、その呈色が生じる。この呈色は、透明容器３を用いていることから目視等で直ちに観察することができる。
[Embodiment]
FIG. 1 shows an example of an embodiment of the detection tool of the present invention. The detection tool 1 has a detection material 2 housed in a container formed of a transparent container 3 and a nonwoven fabric 4. In addition, the periphery of the transparent container 3 and the nonwoven fabric 4 are adhered to each other by a welding portion 5. From the nonwoven fabric 4 side, the liquid to be tested selectively flows into the detection tool 1 and is absorbed by the detection material 2, and when the detection target of the color former is included, its coloration occurs. This coloration can be immediately observed visually or the like since the transparent container 3 is used.
図２は、本発明の検出用具を製造する工程を説明するための図である。試薬担持ホワイトカーボン２１と、吸水性樹脂２２とをそれぞれ所定の量を調整する（ａ）。その後、これらを混合した検出材２として、透明容器３に収容する（ｂ）。そして、透明容器３内で揺らすなどして検出材２を透明容器３内に広げて、不織布４で蓋をする（ｃ）。不織布４と透明容器３との周囲を溶着して溶着部５を設けて密閉することで検出用具１が得られる（ｄ）。 FIG. 2 is a diagram for explaining a step of manufacturing the detection tool of the present invention. A predetermined amount of each of the reagent-carrying white carbon 21 and the water-absorbing resin 22 is adjusted (a). Thereafter, the mixture is contained in the transparent container 3 as the detection material 2 obtained by mixing them (b). Then, the detection material 2 is spread in the transparent container 3 by shaking or the like in the transparent container 3 and covered with the nonwoven fabric 4 (c). The periphery of the nonwoven fabric 4 and the transparent container 3 are welded to each other to provide a welded portion 5 and hermetically seal to obtain the detection tool 1 (d).
［環境汚染物質の評価］
本発明の検出材は、環境汚染物質の有無の評価検出に用いることができる。環境汚染物質は、主に無機化合物系のものと有機化合物系のものとがあるが、本発明においては、本発明の基材として用いるホワイトカーボンに担持される発色剤が反応することができるものであればいずれも評価対象とすることができる。特に、弱酸性〜弱アルカリ性の水系のものを対象とすることが好ましく、例えば、フッ素、鉛、ホウ素、クロム等を評価対象の環境汚染物質とすることができる。
[Evaluation of environmental pollutants]
The detection material of the present invention can be used for evaluation detection of the presence or absence of environmental pollutants. Environmental pollutants are mainly classified into inorganic compound-based substances and organic compound-based substances. In the present invention, those in which a color former supported on white carbon used as a substrate of the present invention can react. Any of them can be evaluated. In particular, it is preferable to use a weakly acidic to weakly alkaline water-based one. For example, fluorine, lead, boron, chromium, and the like can be environmental pollutants to be evaluated.
本発明は、前述した本発明の検出材を用いて、環境汚染物質の有無を評価する方法とすることができる。すなわち、土壌中や水中の汚染物質の有無、またはさらにその濃度を評価する評価方法としても達成することができる。 The present invention can be a method for evaluating the presence or absence of environmental pollutants using the above-described detection material of the present invention. That is, the present invention can also be achieved as an evaluation method for evaluating the presence or absence of contaminants in soil or water, or the concentration thereof.
例えば、土壌を評価する方法の場合は、必要に応じて適宜土壌を水で湿潤させる等した状態で、検出材を直接接触させることで土壌中に、検出材の発色剤が反応して発色する対象となる汚染物質が存在するか否かを評価することができる。また、評価対象が水中の環境汚染物質の場合、その試験対象とする水に、本発明の検出材を直接接触させ、呈色反応の有無から環境汚染物質の有無を評価することができる。 For example, in the case of a method for evaluating soil, if necessary, in a state where the soil is appropriately wetted with water, and by directly contacting the detection material, the color forming agent of the detection material reacts and develops color in the soil. It can be evaluated whether or not the target pollutant exists. When the evaluation target is an environmental pollutant in water, the detection material of the present invention can be directly contacted with water to be tested, and the presence or absence of an environmental pollutant can be evaluated based on the presence or absence of a color reaction.
この評価方法は、前述のように検出材を土壌に直接接触させることで行ってもよい。また、直接接触させず、ろ紙等の吸水性物質を介在させて行うこともでき、ろ紙等を用いる場合、測定後の検出材の回収が容易であり、また、ろ紙を介することで土壌中の水分が検出材に直接吸い上げられ、着色の有無を観察しやすくすることができる。また、検出用具の状態で試験対象に接触させて評価してもよい。 This evaluation method may be performed by bringing the detection material into direct contact with the soil as described above. In addition, without direct contact, it can be carried out with a water-absorbing substance such as filter paper interposed.When filter paper or the like is used, recovery of the detection material after measurement is easy, and in the soil through the filter paper, Moisture is directly sucked into the detection material, which makes it easy to observe the presence or absence of coloring. The evaluation may be performed by bringing the detection tool into contact with the test object.
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、その要旨を変更しない限り以下の実施例に限定されるものではない。 Hereinafter, the present invention will be described in more detail with reference to examples, but the present invention is not limited to the following examples unless the gist is changed.
［評価項目］
［安息角］
安息角の測定は、注入法により測定した。注入法は、検出材を容器に容れて自然落下させたとき、落下して平面に堆積した検出材がなす角度を測定するものである。検出材は、試料９．０ｇを用いて、注入法を行う容器として傾斜６３度、排出口幅φ２３ｍｍのプラスチック製の漏斗を用いて、漏斗出口から平面までの距離を６０ｍｍとして測定する。３回測定した平均値を用いる。
[Evaluation item]
[Angle of repose]
The angle of repose was measured by an injection method. In the injection method, when the detection material is allowed to fall naturally in a container, the angle formed by the detection material that has fallen and deposited on a flat surface is measured. The detection material is measured using 9.0 g of the sample, using a plastic funnel having an inclination of 63 degrees and a discharge port width of 23 mm as a container for performing the injection method, and setting the distance from the funnel outlet to the plane at 60 mm. The average value measured three times is used.
［含水率］
水分計（Ｓａｒｔｏｒｉｕｓ製「ＭＡ３５」）を用いて、秤量した吸水性樹脂（０．５ｇ〜１ｇ）等の測定の対象を、１００℃で１０分間加熱処理する乾燥により、その対象が吸水していた水を乾燥させ、その乾燥の前後の重量比から、減少した重量が水分として、ＪＩＳ Ｋ００６８（２００１）に準じて、含水率を測定した。
含水率（％）＝（（乾燥前の対象の重量Ｘ０（ｇ）−乾燥後の対象の重量Ｘ１（ｇ））／乾燥前の対象の重量Ｘ０（ｇ））×１００
[Moisture content]
Using a moisture meter (“MA35” manufactured by Sartorius), a measurement target such as a water-absorbent resin (0.5 g to 1 g) weighed was dried by heat treatment at 100 ° C. for 10 minutes. The water was dried, and the water content was measured according to JIS K0068 (2001), based on the weight ratio before and after the drying, with the reduced weight as the moisture.
Water content (%) = ((weight of subject before drying X 0 (g) −weight of subject after drying X 1 (g)) / weight of subject before drying X 0 (g)) × 100
［試薬］
［発色剤］
・ランタン−アリザレンコンプレキソン発色剤（発色剤Ｆ−ａ）
ランタン−アリザリンコンプレキソンを用いたフッ素検出用試薬であるアルフッソン（登録商標）（同仁化学製）を用いた。
・ジフェニルカルバジド（発色剤Ｃｒ−ａ）
ジフェニルカルバジド（和光純薬製）を用いた。
・アゾメチンＨ（発色剤Ｂ−ａ）
アゾメチンＨ（和光純薬製、“８−ヒドロキシ−１−（サリチリデンアミノ）−３，６−ナフタレンジスルホン酸・２ナトリウム塩”）を用いた。
[reagent]
[Coloring agent]
-Lanthanum-alizaren complexone color former (color former Fa)
Alfusson (registered trademark) (manufactured by Dojindo Chemical Co., Ltd.), which is a fluorine detection reagent using lanthanum-alizarin complexone, was used.
・ Diphenylcarbazide (coloring agent Cr-a)
Diphenylcarbazide (manufactured by Wako Pure Chemical Industries) was used.
Azomethine H (color former Ba)
Azomethine H (manufactured by Wako Pure Chemical Industries, "8-hydroxy-1- (salicylideneamino) -3,6-naphthalenedisulfonic acid disodium salt") was used.
［ホワイトカーボン］
・ホワイトカーボン（１）
基材として、ホワイトカーボンである“ゼオシール １１００Ｖ”（多木化学社製）を用いた。
[White carbon]
・ White carbon (1)
As a base material, “ZEOSeal 1100V” (manufactured by Taki Chemical Co., Ltd.), which is white carbon, was used.
［吸水性樹脂］
・吸水性樹脂（１）
変性ポリアルキレンオキサイド／ノニオン型熱可塑性吸水性樹脂である“アクアコーク（登録商標） ＴＷＢ−Ｐ”（住友精化社製）を吸水性樹脂（１）として用いた。
・吸水性樹脂（２）
ポリアクリル酸ナトリウム系吸水性樹脂である“アクアキープ（登録商標） ＳＡ−６０”（住友精化社製）を吸水性樹脂（２）として用いた。
[Water absorbent resin]
・ Water absorbent resin (1)
"Aquacork (registered trademark) TWB-P" (manufactured by Sumitomo Seika), which is a modified polyalkylene oxide / nonionic thermoplastic water-absorbing resin, was used as the water-absorbing resin (1).
・ Water absorbent resin (2)
"Aquakeep (registered trademark) SA-60" (manufactured by Sumitomo Seika), which is a sodium polyacrylate-based water-absorbing resin, was used as the water-absorbing resin (2).
［実施例１］ 検出材（Ｆ−ａ１） 混合試験
１） 発色試薬として、発色剤（Ｆ−ａ）０．５ｇを、純水１２．５ｇに溶解させて発色剤溶液（Ｆ−１）を調整した。
２）ホワイトカーボン（１）と、発色剤溶液（Ｆ−１）とを、質量比１：１で混合して吸液ホワイトカーボンとした。
３）吸液ホワイトカーボンを含水率５％以下まで乾燥して、試薬担持ホワイトカーボン（ＷＣ（Ｆ−１））を得た。
４）前述のＷＣ（Ｆ−１）１０質量部と、予め乾燥した状態で保管した吸水性樹脂（１）６質量部とを混合して検出材（Ｆ−ａ１）を得た。
[Example 1] Detection material (F-a1) Mixing test 1) As a color-forming reagent, 0.5 g of a color-forming agent (F-a) was dissolved in 12.5 g of pure water to prepare a color-forming agent solution (F-1). It was adjusted.
2) White carbon (1) and the color former solution (F-1) were mixed at a mass ratio of 1: 1 to obtain a liquid-absorbing white carbon.
3) The liquid-absorbing white carbon was dried to a water content of 5% or less to obtain a reagent-supporting white carbon (WC (F-1)).
4) The detection material (F-a1) was obtained by mixing 10 parts by mass of the WC (F-1) described above and 6 parts by mass of the water-absorbent resin (1) stored in a dried state in advance.
［製造例１］ 検出材（Ｆ´−ａ１）
１）前述の発色剤溶液（Ｆ−１）１００質量部と、吸水性樹脂（１）１００質量部とを混合して、吸液吸水性樹脂とした。この吸液吸水性樹脂は、シート状である。
２）シート状の吸液吸水性樹脂を含水率５％以下まで乾燥して、１ｍｍ〜３ｍｍ程度の大きさのフレーク状に粉砕し検出材（Ｆ´−ａ１）を得た。
[Production Example 1] Detection material (F'-a1)
1) 100 parts by mass of the above-described color former solution (F-1) and 100 parts by mass of the water-absorbent resin (1) were mixed to obtain a liquid-absorbent water-absorbent resin. This liquid-absorbent water-absorbent resin is in the form of a sheet.
2) The sheet-shaped liquid-absorbent water-absorbent resin was dried to a moisture content of 5% or less and pulverized into flakes having a size of about 1 mm to 3 mm to obtain a detection material (F′-a1).
［製造例２］ 検出材（Ｆ´−ａ２）
発色剤（Ｆ−ａ１）１／２６質量部と、ホワイトカーボン（１）１質量部と、吸水性樹脂（１）６／１０質量部とを乾燥状態で混合し、検出材（Ｆ´−ａ２）とした。
[Production Example 2] Detection material (F′-a2)
1/26 parts by mass of the color former (F-a1), 1 part by mass of white carbon (1), and 6/10 parts by mass of the water-absorbent resin (1) were mixed in a dry state, and the detection material (F′-a2) was mixed. ).
［安息角の測定］
図３は、検出材（Ｆ−ａ１）と、検出材（Ｆ´−ａ１）の安息角を測定した結果である。
検出材（Ｆ−ａ１）は、安息角２２度であり、流動性に優れたものであった。一方、吸水性樹脂に吸液させて製造する検出材（Ｆ´−ａ１）は、安息角６３度であり、流動性が低く、取り扱いしにくいものであった。
[Measurement of angle of repose]
FIG. 3 shows the result of measuring the angle of repose of the detection material (F-a1) and the detection material (F′-a1).
The detection material (F-a1) had an angle of repose of 22 degrees and was excellent in fluidity. On the other hand, the detection material (F′-a1) manufactured by absorbing the liquid in the water-absorbent resin had a repose angle of 63 degrees, low fluidity, and was difficult to handle.
［水と接触したときの外観］
検出材（Ｆ−ａ１）０．２ｇ、試薬担持ＷＣ（Ｆ−１）０．１ｇ、検出材（Ｆ´−ａ１）０．２ｇ、検出材（Ｆ´−ａ２）０．２ｇを、それぞれ水５ｍＬに混合して静置したときの状態を、図４に示す。
図４（ａ）は、検出材（Ｆ−ａ１）の試験結果である。吸水性樹脂が液を吸収し全体を高粘度の組成物状とし、吸水性樹脂が隣接する試薬担持ホワイトカーボンに液が展開したり、ホワイトカーボンから試薬が滲みだし、全体として均一な外観であった。
図４（ｂ）は、試薬担持ＷＣ（Ｆ−１）の試験結果である。試薬担持ホワイトカーボン（ＷＣ）が、沈降し、ホワイトカーボン層と、水層とが分離した状態となり、色もばらつきがあった。
図４（ｃ）は、検出材（Ｆ´−ａ１）の試験結果である。吸水性樹脂が吸液しにくい状態となっており、さらに、吸水性樹脂から発色剤の展開が生じにくいと考えられ、色ムラが大きいものとなった。
図４（ｄ）は、検出材（Ｆ´−ａ２）の試験結果である。発色剤が溶液中に溶けきれないと考えられ沈降し、さらに吸水性樹脂が吸液して固化し、色ムラも大きいものとなった。
[Appearance when in contact with water]
0.2 g of the detection material (F-a1), 0.1 g of the reagent-supporting WC (F-1), 0.2 g of the detection material (F′-a1), and 0.2 g of the detection material (F′-a2) FIG. 4 shows a state in which the mixture is left standing after mixing with 5 mL.
FIG. 4A shows a test result of the detection material (F-a1). The water-absorbent resin absorbs the liquid to form a high-viscosity composition as a whole, and the liquid-absorbent resin spreads on the adjacent reagent-supporting white carbon or the reagent oozes out of the white carbon, resulting in a uniform appearance as a whole. Was.
FIG. 4B shows the test results of the reagent-supporting WC (F-1). The reagent-carrying white carbon (WC) settled, and the white carbon layer and the aqueous layer were separated, and the color also varied.
FIG. 4C shows a test result of the detection material (F′-a1). The water-absorbent resin was in a state where it was difficult to absorb liquid, and it was considered that the development of the color-forming agent from the water-absorbent resin was unlikely to occur, resulting in large color unevenness.
FIG. 4D shows a test result of the detection material (F′-a2). The coloring agent was considered to be insoluble in the solution and settled, and the water-absorbing resin absorbed and solidified, resulting in large color unevenness.
［発色までの時間］
・検出材（Ｆ−ａ１）０．２ｇを、カップ状のφ４０ｍｍ・深さ４ｍｍのＰＥＴ製の透明樹脂容器に容れて、不織布で開口部に蓋をし、透明樹脂容器と不織布との周囲を溶着させて、検出用具（Ｆ−ａ１）を得た。
・検出材（Ｆ−ａ１）に代え、検出材（Ｆ´−ａ１）（発色剤を担持させた吸水性樹脂である検出材（Ｆ´−ａ１）を用いた検出材）を用いて、検出用具（Ｆ−ａ１）と同様に製造し検出用具（Ｆ´−ａ１）を得た。
これらの検出用具を、フッ素を含有する溶液の上に静置したときの外観の経時変化を図５に示す。検出材（Ｆ−ａ１）は約５分程度で液を吸水し、約２０分程度でフッ素と反応した呈色が明確に確認できる状態となった。一方、検出材（Ｆ´−ａ１）は、吸液し呈色を確認できるまで約４０分程度要し、均一性はやや低い状態であった。
[Time to color development]
-0.2 g of the detection material (F-a1) is placed in a cup-shaped PET transparent resin container having a diameter of 40 mm and a depth of 4 mm, and the opening is covered with a nonwoven fabric. By welding, a detection tool (F-a1) was obtained.
-Detection is performed by using a detection material (F'-a1) (a detection material using a detection material (F'-a1) that is a water-absorbing resin supporting a coloring agent) instead of the detection material (F-a1). The detection tool (F'-a1) was obtained in the same manner as the tool (F-a1).
FIG. 5 shows changes over time in the appearance when these detection tools were allowed to stand on a solution containing fluorine. The detection material (F-a1) absorbed the liquid in about 5 minutes, and was in a state where the coloration reacted with fluorine was clearly confirmed in about 20 minutes. On the other hand, it took about 40 minutes for the detection material (F′-a1) to absorb the liquid and confirm the coloration, and the uniformity was slightly low.
［実施例２］ 検出材（Ｆ−ａ２） 混合比の検討
１） 発色試薬として、発色剤（Ｆ−ａ）１．５ｇを、純水１２．５ｇに溶解させて発色剤溶液（Ｆ−２）を調整した。
２）ホワイトカーボン（１）と、発色剤溶液（Ｆ−２）とを、質量比３：１０で混合して吸液ホワイトカーボンとした。
３）吸液ホワイトカーボンを含水率５％以下まで乾燥して、試薬担持ホワイトカーボン（Ｆ−２）を得た。この試薬担持ホワイトカーボンに担持されている発色剤量（発色剤／ホワイトカーボン）は、３５７ｍｇ／ｇである。
４）試薬担持ホワイトカーボン（Ｆ−２）と、吸水性樹脂（１）との混合比率を変更し、検出材を調製した。混合比率は、試薬担持ホワイトカーボン：吸水性樹脂として、１００：１〜１：２０で段階的に変更して、それぞれ別の容器にいれた。これに、フッ素含有溶液を添加して呈色の状態を確認した。図６は、試験結果を示す写真であり、左側に混合比率を説明するための表を、右側にそれと対応する評価結果を示す。いずれも均一に呈色し、発色剤の呈色を確認することができた。試薬担持ホワイトカーボン量が多い、すなわち、発色剤が多いほどより濃い呈色となった。なお、特に、試薬担持ホワイトカーボン：吸水性樹脂を１：２．５で混合したものが最も観察しやすい状態であった。
[Example 2] Detection material (F-a2) Examination of mixing ratio 1) As a coloring agent, 1.5 g of coloring agent (Fa) was dissolved in 12.5 g of pure water to form a coloring agent solution (F-2). ) Was adjusted.
2) White carbon (1) and the color former solution (F-2) were mixed at a mass ratio of 3:10 to obtain a liquid-absorbing white carbon.
3) The liquid-absorbing white carbon was dried to a water content of 5% or less to obtain a reagent-supporting white carbon (F-2). The amount of the color former supported on the reagent-supported white carbon (color former / white carbon) was 357 mg / g.
4) The mixing ratio between the reagent-supporting white carbon (F-2) and the water-absorbent resin (1) was changed to prepare a detection material. The mixing ratio was changed stepwise from 100: 1 to 1:20 as a reagent-supporting white carbon: water-absorbent resin, and put in separate containers. To this was added a fluorine-containing solution, and the state of coloration was confirmed. FIG. 6 is a photograph showing the test results. A table for explaining the mixing ratio is shown on the left, and the corresponding evaluation results are shown on the right. In each case, the color was uniform, and the color of the color former could be confirmed. The more the amount of the reagent-supporting white carbon, that is, the more the color former, the deeper the color. In particular, a mixture of the reagent-supporting white carbon and the water-absorbing resin at a ratio of 1: 2.5 was the most easily observable state.
［実施例３］ 検出材（Ｆ−ａ３）、（Ｆ−ａ４）
１） [実施例１]に係る試薬担持ＷＣ（Ｆ−１）に、水を追加して、含水率１３．４％の試薬担持ホワイトカーボン（ＷＣ（Ｆ−３））を作製した。
２−１） 前述のＷＣ（Ｆ−３）：１質量部に対して、含水率５．６％とした吸水性樹脂（１）：２質量部を、混合して、検出材（Ｆ−ａ３）を作製した。
２−２） 前述のＷＣ（Ｆ−３）：１質量部に対して、含水率３８．６％とした吸水性樹脂（１）：２質量部を混合して、検出材（Ｆ−ａ４）を作製した。
[Example 3] Detection materials (F-a3), (F-a4)
1) Water was added to the reagent-carrying WC (F-1) according to Example 1 to prepare a reagent-carrying white carbon (WC (F-3)) having a water content of 13.4%.
2-1) The above-mentioned WC (F-3): 1 part by mass, 2 parts by mass of the water-absorbing resin (1) having a water content of 5.6%, are mixed, and the detection material (F-a3) is mixed. ) Was prepared.
2-2) Detecting material (F-a4) by mixing 2 parts by weight of water-absorbent resin (1) having a water content of 38.6% with respect to 1 part by weight of WC (F-3) described above. Was prepared.
［実施例４］ 検出材（Ｃｒ−ａ１）〜（Ｃｒ−ａ３）
１） ジフェニルカルバジドをアセトンに溶解させてジフェニルカルバジド溶液を調製した。これをホワイトカーボン（１）に吸液させ、乾燥させたあと、水と１０ｗｔ％硫酸を添加して、含水率２１．９％の試薬担持ホワイトカーボン（ＷＣ（Ｃｒ−１））を作製した。
２−１） 前述のＷＣ（Ｃｒ−１）：１質量部に対して、含水率１．０％とした吸水性樹脂（１）：２質量部を、混合して、検出材（Ｃｒ−ａ１）を作製した。
２−２） 前述のＷＣ（Ｃｒ−１）：１質量部に対して、含水率５．６％とした吸水性樹脂（１）：２質量部を、混合して、検出材（Ｃｒ−ａ２）を作製した。
２−３） 前述のＷＣ（Ｃｒ−ａ１）：１質量部に対して、含水率３８．６％とした吸水性樹脂（１）：２質量部を、混合して、検出材（Ｃｒ−ａ３）を作製した。
[Example 4] Detection materials (Cr-a1) to (Cr-a3)
1) Diphenylcarbazide was dissolved in acetone to prepare a diphenylcarbazide solution. This was absorbed in white carbon (1) and dried, and then water and 10 wt% sulfuric acid were added to prepare a reagent-supporting white carbon (WC (Cr-1)) having a water content of 21.9%.
2-1) 2 parts by mass of the water-absorbent resin (1) having a water content of 1.0% was mixed with 1 part by mass of the above-mentioned WC (Cr-1) to form a detection material (Cr-a1). ) Was prepared.
2-2) 2 parts by weight of the water-absorbent resin (1) having a water content of 5.6% with respect to 1 part by weight of the above-mentioned WC (Cr-1), and mixed with the detection material (Cr-a2). ) Was prepared.
2-3) The above-mentioned WC (Cr-a1): 1 part by mass was mixed with 2 parts by mass of a water-absorbing resin (1) having a water content of 38.6% to form a detection material (Cr-a3). ) Was prepared.
［実施例５］ 検出材（Ｂ−ａ１）〜（Ｂ−ａ３）
１） アゾメチンＨ（和光純薬製）１．０ｇとＬ−アスコルビン酸（昭和製薬株式会社製）３ｇとを秤量し、純水で２５ｍＬにメスアップした。
２） 酢酸アンモニウム５０ｇ、クエン酸一水和物０．２ｇ、ＥＤＴＡ・２Ｎａ０．２ｇ、純水５０ｍＬを混合し、さらに硫酸３ｍＬ、リン酸１ｍＬを混合し、加熱しながら溶解させた。
３） 前述の１）の液と、２）の液とを、等体積比（２５ｍＬ：２５ｍＬ）で混合することで、０．５ｇ−アゾメチンＨ／１００ｍＬ溶液を作製し、これを発色剤溶液とした。
４） ３）の発色剤溶液１０ｇをホワイトカーボン（１）２ｇに吸液させて、乾燥させ含水率１３．３％の試薬担持ホワイトカーボン（ＷＣ（Ｂ−１））を作製した。
５−１） 前述のＷＣ（Ｂ−１）：１質量部に対して、含水率１６．７％とした吸水性樹脂（２）：２質量部を、混合して、検出材（Ｂ−ａ１）を作製した。
５−２） 前述のＷＣ（Ｂ−１）：１質量部に対して、含水率２７．０％とした吸水性樹脂（２）：２質量部を、混合して、検出材（Ｂ−ａ２）を作製した。
５−３） 前述のＷＣ（Ｂ−１）：１質量部に対して、含水率４０．９％とした吸水性樹脂（２）：２質量部を、混合して、検出材（Ｂ−ａ３）を作製した。
[Example 5] Detection materials (B-a1) to (B-a3)
1) 1.0 g of azomethine H (manufactured by Wako Pure Chemical Industries, Ltd.) and 3 g of L-ascorbic acid (manufactured by Showa Pharmaceutical Co., Ltd.) were weighed and made up to 25 mL with pure water.
2) 50 g of ammonium acetate, 0.2 g of citric acid monohydrate, 0.2 g of EDTA · 2Na, and 50 mL of pure water were mixed, and 3 mL of sulfuric acid and 1 mL of phosphoric acid were mixed and dissolved while heating.
3) The solution of 1) and the solution of 2) are mixed at an equal volume ratio (25 mL: 25 mL) to prepare a 0.5 g-azomethine H / 100 mL solution, which is then referred to as a color former solution. did.
4) 10 g of the color former solution of 3) was absorbed into 2 g of white carbon (1), and dried to prepare a reagent-supporting white carbon (WC (B-1)) having a water content of 13.3%.
5-1) The above-mentioned WC (B-1): 1 part by mass was mixed with 2 parts by mass of a water-absorbent resin (2) having a water content of 16.7%, and mixed with the detection material (B-a1). ) Was prepared.
5-2) 2 parts by mass of the water-absorbent resin (2) having a water content of 27.0% with respect to 1 part by mass of the above-mentioned WC (B-1), and mixed with the detection material (B-a2). ) Was prepared.
5-3) The above-mentioned WC (B-1): 1 part by mass was mixed with 2 parts by mass of a water-absorbent resin (2) having a water content of 40.9%, and mixed with the detection material (B-a3). ) Was prepared.
［発色試験］
・六価クロム検出試験
実施例４で製造した検出材を用いて、六価クロム濃度０ｐｐｍ、０．１ｐｐｍ、２．０ｐｐｍの水溶液を検液として評価した結果を図７に示す。容器に、検出材を０．２ｇ配置し、各六価クロム濃度の水溶液（０ｐｐｍは水単独）５ｍＬを添加して発色の有無を評価した。
いずれのサンプルも六価クロム濃度に応じた発色が確認された。濃度０ｐｐｍ（水）では、ほぼ無色であるが、濃度０．１ｐｐｍの液と接すると淡いピンク色が確認でき、濃度２．０ｐｐｍの液と接するとより濃いピンク色が確認できる。なお、検出材（Ｃｒ−ａ１）や検出材（Ｃｒ−ａ２）の方が、検出材（Ｃｒ−ａ３）よりも濃いピンク色が確認できる。
[Color test]
-Hexavalent chromium detection test FIG. 7 shows the results of using the detection material manufactured in Example 4 and evaluating aqueous solutions having hexavalent chromium concentrations of 0 ppm, 0.1 ppm, and 2.0 ppm as test solutions. 0.2 g of the detection material was placed in a container, and 5 mL of an aqueous solution (0 ppm was water alone) at each hexavalent chromium concentration was added to evaluate the presence or absence of color development.
Color development corresponding to the hexavalent chromium concentration was confirmed in all samples. At a concentration of 0 ppm (water), it is almost colorless, but a light pink color can be confirmed when it comes into contact with a liquid having a concentration of 0.1 ppm, and a deeper pink color can be confirmed when it comes into contact with a solution having a concentration of 2.0 ppm. It should be noted that the detection material (Cr-a1) and the detection material (Cr-a2) can confirm a deeper pink color than the detection material (Cr-a3).
・ホウ素検出試験
実施例５で製造した検出材を用いて、０ｐｐｍ、２ｐｐｍ、１０ｐｐｍの水溶液を検液として評価した結果を図８に示す。容器に、検出材を０．１ｇ配置し、各ホウ素濃度の水溶液（０ｐｐｍは水単独）５ｍＬを添加して発色の有無を評価した。
ホウ素濃度に応じた発色が確認された。濃度０ｐｐｍ（水）では、ほぼ無色から淡いピンク色であるが、濃度２ｐｐｍの液と接すると薄い黄色が確認でき、濃度１０ｐｐｍの液と接するとより濃い黄色が確認できる。特に、吸水性樹脂（２）の含水率が低い検出材（Ｂ−ａ１）の方が、発色を確認しやすかった。一方、吸水性樹脂（２）の含水率が高い検出材（（Ｂ−３）は０ｐｐｍや、２ｐｐｍの低濃度の検液に対して、やや発色が不安定な挙動を示した。
-Boron detection test FIG. 8 shows the results of using the detection material produced in Example 5 and evaluating 0 ppm, 2 ppm, and 10 ppm aqueous solutions as test solutions. 0.1 g of the detection material was placed in a container, and 5 mL of an aqueous solution of each boron concentration (0 ppm was water alone) was added to evaluate the presence or absence of color development.
Color development corresponding to the boron concentration was confirmed. At a concentration of 0 ppm (water), the color is almost colorless to pale pink, but when it comes into contact with a solution having a concentration of 2 ppm, a pale yellow color can be confirmed, and when it comes into contact with a solution having a concentration of 10 ppm, a deeper yellow color can be confirmed. In particular, the detection material (B-a1) having a low water content of the water-absorbent resin (2) was easier to confirm color development. On the other hand, the detection material ((B-3)) having a high water content of the water-absorbent resin (2) showed a somewhat unstable behavior in color development with respect to a test solution having a low concentration of 0 ppm or 2 ppm.
［含水率の影響］
実施例３〜５により製造した検出材の、安息角を測定した。また、検出用具とするための容器への充填しやすさを検討した。評価結果を表１に示す。安息角が、４０度以下のとき、特に充填しやすい程度の流動性を有することが確認された。
[Effect of moisture content]
The angle of repose of the detection materials manufactured according to Examples 3 to 5 was measured. In addition, the ease of filling into a container for use as a detection tool was examined. Table 1 shows the evaluation results. When the angle of repose was 40 degrees or less, it was confirmed that the composition had fluidity such that it could be easily filled.
本発明の検出材や検出用具は、土壌などの環境汚染物質の検出に利用することができ、産業上有用である。 INDUSTRIAL APPLICABILITY The detection material and the detection tool of the present invention can be used for detecting environmental pollutants such as soil, and are industrially useful.
１ 検出用具
２ 検出材
２１ 試薬担持ホワイトカーボン
２２ 吸水性樹脂
３ 透明容器
４ 不織布
５ 溶着部
DESCRIPTION OF SYMBOLS 1 Detection tool 2 Detecting material 21 Reagent-supporting white carbon 22 Water-absorbing resin 3 Transparent container 4 Nonwoven fabric 5 Welding part
Claims (7)
前記吸液ホワイトカーボンを乾燥させて試薬担持ホワイトカーボンを得る乾燥工程と、
前記試薬担持ホワイトカーボンと、吸水性樹脂とを混合して検出材を得る混合工程と、を有する検出材の製造方法。 Contacting white carbon with a color former solution containing a color former to obtain a liquid-absorbing white carbon absorbing the color former solution,
A drying step of drying the liquid-absorbing white carbon to obtain a reagent-carrying white carbon,
A method for producing a detection material, comprising: a mixing step of mixing the reagent-supporting white carbon with a water-absorbing resin to obtain a detection material.
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