JP2011179887A - Reagent and method for simply measuring concentration of industrial medical agent - Google Patents
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- 239000003153 chemical reaction reagent Substances 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims description 9
- 239000003795 chemical substances by application Substances 0.000 title abstract description 3
- 239000002736 nonionic surfactant Substances 0.000 claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 15
- ZMZDMBWJUHKJPS-UHFFFAOYSA-M Thiocyanate anion Chemical compound [S-]C#N ZMZDMBWJUHKJPS-UHFFFAOYSA-M 0.000 claims abstract description 8
- 150000001868 cobalt Chemical class 0.000 claims abstract description 8
- ZMZDMBWJUHKJPS-UHFFFAOYSA-N hydrogen thiocyanate Natural products SC#N ZMZDMBWJUHKJPS-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000012086 standard solution Substances 0.000 claims abstract description 5
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 12
- 239000002738 chelating agent Substances 0.000 claims description 11
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- DBVJJBKOTRCVKF-UHFFFAOYSA-N Etidronic acid Chemical compound OP(=O)(O)C(O)(C)P(O)(O)=O DBVJJBKOTRCVKF-UHFFFAOYSA-N 0.000 claims description 7
- 239000003317 industrial substance Substances 0.000 claims description 7
- 235000006408 oxalic acid Nutrition 0.000 claims description 4
- 238000005259 measurement Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 239000003171 wood protecting agent Substances 0.000 abstract description 30
- 239000007864 aqueous solution Substances 0.000 abstract description 8
- 238000002835 absorbance Methods 0.000 abstract 1
- 239000002023 wood Substances 0.000 description 12
- 239000003755 preservative agent Substances 0.000 description 11
- -1 iron ion Chemical class 0.000 description 8
- 239000004480 active ingredient Substances 0.000 description 7
- 238000004040 coloring Methods 0.000 description 7
- 239000003085 diluting agent Substances 0.000 description 7
- 238000011161 development Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000010790 dilution Methods 0.000 description 5
- 239000012895 dilution Substances 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 150000002989 phenols Chemical class 0.000 description 5
- 230000002335 preservative effect Effects 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000000417 fungicide Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- JWZXKXIUSSIAMR-UHFFFAOYSA-N methylene bis(thiocyanate) Chemical compound N#CSCSC#N JWZXKXIUSSIAMR-UHFFFAOYSA-N 0.000 description 3
- SOIFLUNRINLCBN-UHFFFAOYSA-N ammonium thiocyanate Chemical compound [NH4+].[S-]C#N SOIFLUNRINLCBN-UHFFFAOYSA-N 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 230000000855 fungicidal effect Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000000691 measurement method Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- GOSHEZZPLYXNIQ-UHFFFAOYSA-N (5-bromo-2,5-diiodopent-3-enyl) hydrogen carbonate Chemical compound C(C(C=CC(Br)I)I)OC(=O)O GOSHEZZPLYXNIQ-UHFFFAOYSA-N 0.000 description 1
- TUBQDCKAWGHZPF-UHFFFAOYSA-N 1,3-benzothiazol-2-ylsulfanylmethyl thiocyanate Chemical compound C1=CC=C2SC(SCSC#N)=NC2=C1 TUBQDCKAWGHZPF-UHFFFAOYSA-N 0.000 description 1
- HGUFODBRKLSHSI-UHFFFAOYSA-N 2,3,7,8-tetrachloro-dibenzo-p-dioxin Chemical compound O1C2=CC(Cl)=C(Cl)C=C2OC2=C1C=C(Cl)C(Cl)=C2 HGUFODBRKLSHSI-UHFFFAOYSA-N 0.000 description 1
- AVGVFDSUDIUXEU-UHFFFAOYSA-N 2-octyl-1,2-thiazolidin-3-one Chemical compound CCCCCCCCN1SCCC1=O AVGVFDSUDIUXEU-UHFFFAOYSA-N 0.000 description 1
- 229940099451 3-iodo-2-propynylbutylcarbamate Drugs 0.000 description 1
- WYVVKGNFXHOCQV-UHFFFAOYSA-N 3-iodoprop-2-yn-1-yl butylcarbamate Chemical compound CCCCNC(=O)OCC#CI WYVVKGNFXHOCQV-UHFFFAOYSA-N 0.000 description 1
- GQXPKSRYYSBMLT-UHFFFAOYSA-N 4-(4,5-dichlorooctyl)-1,2-thiazolidin-3-one Chemical compound CCCC(Cl)C(Cl)CCCC1CSNC1=O GQXPKSRYYSBMLT-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 241000218631 Coniferophyta Species 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229920001214 Polysorbate 60 Polymers 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- 239000007983 Tris buffer Substances 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000007059 acute toxicity Effects 0.000 description 1
- 231100000403 acute toxicity Toxicity 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 150000005215 alkyl ethers Chemical class 0.000 description 1
- 125000005037 alkyl phenyl group Chemical group 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- 239000003429 antifungal agent Substances 0.000 description 1
- 229940121375 antifungal agent Drugs 0.000 description 1
- 239000004599 antimicrobial Substances 0.000 description 1
- TWFZGCMQGLPBSX-UHFFFAOYSA-N carbendazim Chemical compound C1=CC=C2NC(NC(=O)OC)=NC2=C1 TWFZGCMQGLPBSX-UHFFFAOYSA-N 0.000 description 1
- 230000007665 chronic toxicity Effects 0.000 description 1
- 231100000160 chronic toxicity Toxicity 0.000 description 1
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000011121 hardwood Substances 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- WJCNZQLZVWNLKY-UHFFFAOYSA-N thiabendazole Chemical compound S1C=NC(C=2NC3=CC=CC=C3N=2)=C1 WJCNZQLZVWNLKY-UHFFFAOYSA-N 0.000 description 1
- 239000010875 treated wood Substances 0.000 description 1
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Description
本発明は、非イオン系界面活性剤を含有する工業用薬剤、またはその水希釈液の濃度を簡易的に測定し、管理するための方法に関する。 The present invention relates to a method for simply measuring and managing the concentration of an industrial chemical containing a nonionic surfactant or its water dilution.
工業用薬剤を水で希釈し、使用する例として木材保存剤、除草剤がある。木材保存剤の使用にあたっては、処理を行う季節、木材の樹種などによって木材保存剤の濃度を調整するため、木材保存剤の濃度を定期的に測定する必要がある。 Examples of using industrial chemicals diluted with water include wood preservatives and herbicides. When using wood preservatives, it is necessary to measure the concentration of wood preservatives periodically in order to adjust the concentration of wood preservatives depending on the season of treatment, the wood species, etc.
木材保存剤の有効成分は、従来ハロゲン化フェノール化合物が主として用いられていた。ハロゲン化フェノールは２価の銅イオンと錯体を形成し茶色に発色するため、硫酸銅や塩化銅を含有させた試験紙を用いて簡易に濃度を測定することが可能であった。 Conventionally, halogenated phenol compounds have been mainly used as the active ingredient of wood preservatives. Since the halogenated phenol forms a complex with a divalent copper ion and develops a brown color, it was possible to easily measure the concentration using a test paper containing copper sulfate or copper chloride.
近年、ハロゲン化フェノール化合物は急性及び慢性毒性が強く、また難分解性であることから、蓄積による二次公害の懸念があり、また処理された木材を焼却することによってダイオキシンの発生の危険性があり、環境汚染に対する配慮から使用が敬遠され、代替剤が望まれていた。 In recent years, halogenated phenolic compounds have strong acute and chronic toxicity and are hardly degradable. Therefore, there are concerns about secondary pollution due to accumulation, and there is a risk of dioxin generation by incinerating treated wood. The use was avoided from consideration for environmental pollution, and an alternative was desired.
このような理由から、近年ハロゲン化フェノール化合物を含まない薬剤が次々と開発され、使用されている。これらの非ハロゲン化フェノール製剤を使用する場合にも簡易に濃度を測定する必要がある。例えば、メチレンビスチオシアネートを有効成分とする木材防カビ剤希釈液の濃度測定方法として、前処理試薬に水酸化ナトリウム等アルカリ性試薬または亜硫酸塩等の還元性試薬、発色試薬として３価の鉄イオンを含有する試薬を用いる方法が提案されている。しかし本法は、メチレンビスチオシアネートを有効成分とする木材防カビ剤にのみ適用できるものであった。
また、リン酸塩をインジケーターとして簡易に木材防カビ剤の濃度を測定することが提案されているが、発色が明瞭ではなく、汚れがある液体では発色の程度が確認できないという問題があった。
For these reasons, drugs that do not contain halogenated phenol compounds have been developed and used one after another. Even when these non-halogenated phenol preparations are used, it is necessary to easily measure the concentration. For example, as a method for measuring the concentration of a wood fungicide diluted solution containing methylenebisthiocyanate as an active ingredient, an alkaline reagent such as sodium hydroxide or a reducing reagent such as sulfite is used as a pretreatment reagent, and a trivalent iron ion is used as a coloring reagent. A method using a contained reagent has been proposed. However, this method was applicable only to wood fungicides containing methylene bis-thiocyanate as an active ingredient.
Further, it has been proposed to simply measure the concentration of the wood fungicide using phosphate as an indicator, but there is a problem that the color development is not clear and the degree of color development cannot be confirmed in a liquid with dirt.
非ハロゲン化フェノール系の木材保存剤成分は多くの種類があり、それらは一種または二種以上の有効成分を含有している。しかし、これらの成分を簡易に測定することは非常に困難であり、有効成分毎に簡易濃度測定方法を開発する必要があった。 There are many types of non-halogenated phenol-based wood preservative components, which contain one or more active ingredients. However, it is very difficult to easily measure these components, and it is necessary to develop a simple concentration measurement method for each active component.
また、木材保存剤の希釈液を採取し、保存剤のメーカーに送付し、濃度分析方法として高速液体クロマトグラフ装置（ＨＰＬＣ）やガスクロマトグラフ装置（ＧＣ）等の機器を用いて分析する方法が行われているが、結果が迅速に得られず、しかも手間とコストがかかるものである。分析結果を得られることが遅いと木材保存剤の濃度を補正するのが遅れ、濃度低下によるカビの発生等の障害が起こりやすい。 In addition, a method of collecting a diluted solution of wood preservative, sending it to the manufacturer of the preservative, and analyzing the concentration using a device such as a high performance liquid chromatograph (HPLC) or gas chromatograph (GC) is performed. However, the results cannot be obtained quickly, and it takes time and money. If the analysis result is slow to be obtained, the correction of the concentration of the wood preservative is delayed, and troubles such as mold generation due to the decrease in the concentration are likely to occur.
工業用薬剤、特に木材保存剤希釈液の処理槽における濃度を、簡易かつ迅速に測定することが、本発明の課題である。 It is an object of the present invention to easily and quickly measure the concentration of industrial chemicals, particularly wood preservative diluents in treatment tanks.
本発明者は鋭意研究を重ねた結果、木材保存剤中に配合されている非イオン系界面活性剤を木材保存剤のインジケーターとして簡易に測定することによって、木材保存剤の濃度を迅速に見積もることができることを見出し、本発明を完成させた。 As a result of extensive research, the present inventor can quickly estimate the concentration of a wood preservative by simply measuring the nonionic surfactant contained in the wood preservative as an indicator of the wood preservative. The present invention has been completed.
すなわち本発明は、呈色試薬としてチオシアン酸塩およびコバルト塩を含有する水溶液を用いることを特徴とする、非イオン系界面活性剤を含有する木材保存剤の濃度測定試薬であり、また希釈液中の木材保存剤の濃度をこの呈色試薬を用いて発色させ、これを同様にして発色させた標準液と比色することにより、木材保存剤の濃度を決定することを特徴とする濃度測定方法である。また、実際に製材工場などで木材を浸漬処理し、木材の抽出物や金属イオンの混入により着色した木材保存剤希釈液では、呈色試薬としてチオシアン酸塩およびコバルト塩を含有する水溶液のみを用いた場合に、着色により判定しづらい場合があるが、シュウ酸や１−ヒドロキシエタン−１，１−ジホスホン酸を含有する溶液を用いることで着色を低減させ比色しやすくするものである。 That is, the present invention is a reagent for measuring the concentration of a wood preservative containing a nonionic surfactant, characterized by using an aqueous solution containing a thiocyanate and a cobalt salt as a color reagent, A concentration measuring method characterized in that the concentration of the wood preservative is determined by color-developing the concentration of the wood preservative using the coloring reagent and color-matching it with a standard solution colored in the same manner. It is. In addition, for wood preservative dilutions that have been dipped in wood at a sawmill, etc., and colored by mixing wood extracts and metal ions, only aqueous solutions containing thiocyanate and cobalt salts are used as color reagents. In some cases, it may be difficult to determine by coloring, but by using a solution containing oxalic acid or 1-hydroxyethane-1,1-diphosphonic acid, coloring is reduced and colorimetry is facilitated.
本発明の試薬または方法を用いることにより、非イオン系界面活性剤を含有する工業用薬剤剤、特に木材保存剤希釈液の処理槽における濃度を、簡易かつ迅速に測定することができる。 By using the reagent or method of the present invention, the concentration of an industrial chemical agent containing a nonionic surfactant, particularly a wood preservative diluent, in a treatment tank can be measured easily and rapidly.
木材保存剤の希釈液における非イオン系界面活性剤の濃度は木材保存剤の濃度と比例するため、非イオン系界面活性剤濃度を測定することによって間接的に木木材保存剤の濃度を求めることができる。 Since the concentration of nonionic surfactant in the dilution of wood preservative is proportional to the concentration of wood preservative, the concentration of wood preservative should be determined indirectly by measuring the concentration of nonionic surfactant. Can do.
本発明の呈色試薬は、チオシアン酸塩およびコバルト塩の水溶液で、非イオン系界面活性剤と反応し呈色させるために用いられる。
チオシアン酸塩は、アルカリ金属イオンやアンモニウムイオン等いずれの塩を用いても差し支えなく、通常はチオシアン酸アンモニウムを用いることができる。コバルト塩については、硝酸イオンや硫酸イオン等いずれの塩を用いても差し支えない。チオシアン酸塩とコバルト塩の水溶液はチオシアン酸塩とコバルト塩の重量比率が、１０：１〜１：１０となるように、加温しながら水に溶解することが望ましい。
The color reagent of the present invention is an aqueous solution of thiocyanate and cobalt salt and is used for reacting with a nonionic surfactant to cause coloration.
As the thiocyanate, any salt such as alkali metal ion or ammonium ion may be used, and usually ammonium thiocyanate can be used. As for the cobalt salt, any salt such as nitrate ion or sulfate ion may be used. The aqueous solution of thiocyanate and cobalt salt is preferably dissolved in water while heating so that the weight ratio of thiocyanate and cobalt salt is 10: 1 to 1:10.
濃度を測定される木材保存剤は非イオン系界面活性剤を含有するものであれば特に制限はなく、どのような製剤でも良い。例えば水溶製剤、乳剤またはフロアブル製剤でも差し支えない。非イオン系界面活性剤は特に限定するものではないが、例えば、ポリオキシエチレンアルキルフェニルエーテル、ポリオキシエチレンスチリルフェニルエーテル、ポリオキシエチレンアルキルエーテル、ソルビタン脂肪酸エステル、ポリオキシエチレンソルビタン脂肪酸エステルなどが挙げられる。また、これらのノニオン系界面活性剤は一種を単独に用いても二種以上を併用してもよく、製剤に対して重量％で０．０００５〜５０％添加することが望ましい。また、アニオン系界面活性剤と併用することも可能である。 The wood preservative whose concentration is measured is not particularly limited as long as it contains a nonionic surfactant, and any preparation may be used. For example, an aqueous preparation, an emulsion or a flowable preparation may be used. The nonionic surfactant is not particularly limited, and examples thereof include polyoxyethylene alkyl phenyl ether, polyoxyethylene styryl phenyl ether, polyoxyethylene alkyl ether, sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester and the like. It is done. Moreover, these nonionic surfactants may be used individually by 1 type, or may use 2 or more types together, It is desirable to add 0.0005-50% by weight with respect to a formulation. It can also be used in combination with an anionic surfactant.
木材保存剤として用いられる有効成分には特に制限はないが、３−ヨード−２−プロピニルブチルカーバメート、４−クロロフェニル−３−ヨードプロパギルホルマール、メチレンビスチオシアネート、ジヨードメチルパラトリルスルホン、３−ブロモ−２，３−ジヨード−２−プロペニルエチルカルボナート、２−ｎ−オクチルイソチアゾリン−３−オン、４，５−ジクロロ−ｎ−オクチルイソチアゾリン−３−オン、２−チオシアノメチルチオベンゾチアゾール、トリス−Ｎ−シクロヘキシルジアゼニウムジオキシ−アルミニウム塩及びカリウム塩、２−（４−チアゾリル）ベンズイミダゾール、２−ベンズイミダゾールカルバミン酸メチルなどの防腐・防カビ剤等が挙げられる。
The active ingredient used as a wood preservative is not particularly limited, but 3-iodo-2-propynyl butyl carbamate, 4-chlorophenyl-3-iodopropargyl formal, methylene bis thiocyanate, diiodomethyl paratolyl sulfone, 3- Bromo-2,3-diiodo-2-propenylethyl carbonate, 2-n-octylisothiazolin-3-one, 4,5-dichloro-n-octylisothiazolin-3-one, 2-thiocyanomethylthiobenzothiazole, Tris Examples thereof include antiseptic and antifungal agents such as -N-cyclohexyldiazenium dioxy-aluminum salt and potassium salt, 2- (4-thiazolyl) benzimidazole, methyl 2-benzimidazolecarbamate and the like.
木材保存剤が鉄汚染などにより着色する場合があり、上記の呈色試薬を添加したときに試料液の濃度を測定するのに障害となる場合がある。このような場合には呈色試薬と合わせて、金属キレート剤を添加し、鉄汚染などによる着色を生じないようにすることができる。添加されるキレート剤に特に制限はないが、５％シュウ酸水溶液であれば重量％で０．０００５〜１０％添加することが望ましく、１−ヒドロキシエタン−１，１−ジホスホン酸の場合ＤＥＱＵＥＳＴ２０１０（ソルーシア・ジャパン製、１−ヒドロキシエタン−１，１−ジホスホン酸の６０％水溶液）のような市販品が使用できる。 The wood preservative may be colored due to iron contamination or the like, which may be an obstacle to measuring the concentration of the sample solution when the color reagent is added. In such a case, a metal chelating agent can be added together with the color reagent to prevent coloring due to iron contamination or the like. There is no particular limitation on the chelating agent to be added, but if it is a 5% oxalic acid aqueous solution, it is desirable to add 0.0005 to 10% by weight. In the case of 1-hydroxyethane-1,1-diphosphonic acid, DEQUEST 2010 ( A commercially available product such as 60% aqueous solution of 1-hydroxyethane-1,1-diphosphonic acid manufactured by Solusia Japan) can be used.
本発明の測定方法を利用して希釈液中の保存剤の濃度を求めるには、本発明の呈色試薬を用いて発色させた保存剤希釈液と、標準となる保存剤の希釈液を発色させた液の呈色を比色することによって、保存剤の濃度を求めることができる。比色する希釈液の濃度については、日本工業規格ＪＩＳ Ｚ ８７２１のマンセル表色系において、色相１０ＲＰ〜１０Ｂを示すように採取する希釈液の量および添加する呈色試薬の量を調整することが可能である。 In order to determine the concentration of the preservative in the diluent using the measurement method of the present invention, the preservative diluent developed using the color reagent of the present invention and the standard preservative diluent are colored. The concentration of the preservative can be determined by colorimetric coloration of the liquid. Regarding the concentration of the diluent to be colorimetrically adjusted, the amount of the diluent to be collected and the amount of the coloring reagent to be added can be adjusted so as to show the hues 10RP to 10B in the Munsell color system of Japanese Industrial Standard JIS Z 8721. Is possible.
次に本発明の実施例及び試験例をあげて説明するが、本発明はこれらに限定されるものではない。 Next, although the Example and test example of this invention are given and demonstrated, this invention is not limited to these.
（呈色試薬）
チオシアン酸アンモニウム３１０ｇと硝酸コバルト６水和物を１４０ｇ秤量し、少量の水で溶解する。加温しながらイオン交換水を加えて液量を１０００ｍＬとした呈色液とした。
（金属キレート剤１）
シュウ酸５ｇ水９５ｇに溶解させ金属キレート剤溶液とした。
（金属キレート剤２）
１−ヒドロキシエタン−１，１−ジホスホン酸６０％水溶液（ＤＥＱＵＥＳＴ２０１０：ソルーシア・ジャパン製）を用いた。
(Coloring reagent)
Weigh 140 g of ammonium thiocyanate 310 g and cobalt nitrate hexahydrate and dissolve with a small amount of water. While heating, ion exchange water was added to obtain a color solution having a liquid volume of 1000 mL.
(Metal chelating agent 1)
A metal chelating agent solution was prepared by dissolving in 5 g of oxalic acid 5 g and water 95 g.
(Metal chelating agent 2)
A 60% aqueous solution of 1-hydroxyethane-1,1-diphosphonic acid (DEQUEST 2010: manufactured by Solusia Japan) was used.
前記呈色液と金属キレート剤を用いて表１の組合せで試験を実施した。
The test was carried out with the combinations shown in Table 1 using the color developer and metal chelating agent.
（試験例１）
非イオン系界面活性剤を含む木材保存剤（ネオシントールＷ−５２００、住化エンビロサイエンス株式会社製）の希釈液を用い、これらの処理液１ｍＬに前記表１の組合せで示す呈色試薬を０．１ｇ、金属キレート剤を０．０２ｇ添加し発色させた。発色程度を表１に示す。表１より本発明の測定条件での発色は、日本工業規格ＪＩＳ Ｚ ８７２１のマンセル表色系において、色相１０ＲＰ〜１０Ｂを示した。
(Test Example 1)
Using a diluted solution of a wood preservative containing a nonionic surfactant (Neosynthol W-5200, manufactured by Sumika Enviro Science Co., Ltd.), 0 mL of the color reagent shown in the combination of Table 1 is added to 1 mL of these treatment solutions. 0.1 g, 0.02 g of metal chelating agent was added to cause color development. Table 1 shows the degree of color development. From Table 1, the color development under the measurement conditions of the present invention showed hues 10RP to 10B in the Munsell color system of Japanese Industrial Standard JIS Z 8721.
（試験例２）
針葉樹を主に製材する製材所において使用されている非イオン系界面活性剤を含む木材保存剤（ネオシントールＷ−５２００、住化エンビロサイエンス株式会社製）の処理液（６点）を採取し、これらの処理液１ｍＬに前記表１の組合せで呈色試薬０．１ｇ、金属キレート剤０．０２ｇを添加し発色させた。これを発色させた木材保存剤の標準液と比較し木材保存剤の濃度を求めた。また、液体クロマトグラフ装置（ＨＰＬＣ）を用いて有効成分の濃度を測定し、木材保存剤の濃度を求めた。結果を表２に示す。
(Test Example 2)
Sample a processing solution (6 points) of a wood preservative (Neosintole W-5200, manufactured by Sumika Enviro Science Co., Ltd.) containing a nonionic surfactant used in sawmills mainly sawing conifers, In 1 mL of these treatment solutions, 0.1 g of a color reagent and 0.02 g of a metal chelating agent were added in the combinations shown in Table 1 to develop a color. The density | concentration of the wood preservative was calculated | required by comparing this with the standard solution of the wood preservative which made it color. Moreover, the density | concentration of the active ingredient was measured using the liquid chromatograph apparatus (HPLC), and the density | concentration of the wood preservative was calculated | required. The results are shown in Table 2.
（試験例３）
広葉樹を主に製材する製材所において使用されている非イオン系界面活性剤を含む木材保存剤（ネオシントールＷ−１５００、住化エンビロサイエンス株式会社製）の処理液（３点）を採取し、これらの処理液１ｍＬに前記実施例に示す呈色試薬を０．１ｇ、金属キレート剤を０．０２ｇ添加し発色させた。これを同様に発色させた木材保存剤の標準液と比較し木材保存剤の濃度を求めた。また、液体クロマトグラフ装置（ＨＰＬＣ）を用いて有効成分の濃度を測定し、木材保存剤の濃度を求めた。結果を表３に示す。
(Test Example 3)
Collect processing solutions (3 points) of wood preservatives (Neosintole W-1500, manufactured by Sumika Enviro Science Co., Ltd.) containing nonionic surfactants used in sawmills mainly sawing hardwood, To 1 mL of these treatment solutions, 0.1 g of the color reagent shown in the above Example and 0.02 g of metal chelating agent were added to cause color development. The concentration of the wood preservative was determined by comparing this with a standard solution of wood preservative that was similarly developed. Moreover, the density | concentration of the active ingredient was measured using the liquid chromatograph apparatus (HPLC), and the density | concentration of the wood preservative was calculated | required. The results are shown in Table 3.
本発明の試薬を用いて木材保存剤希釈液の濃度を簡易かつ迅速に測定することができ、希釈倍率の管理を簡便に行うことができる。 Using the reagent of the present invention, the concentration of the wood preservative dilution can be measured easily and quickly, and the dilution ratio can be easily managed.
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| JP2017161416A (en) * | 2016-03-10 | 2017-09-14 | 日本メジフィジックス株式会社 | Quantitative method of polyoxyethylene-based nonionic surfactant, and manufacturing method of radioactive pharmaceutical preparation |
| KR20200101617A (en) * | 2019-02-20 | 2020-08-28 | 충남대학교산학협력단 | Method for measuring concentration of wood preservative using electrical conductivity |
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| JP2003252705A (en) * | 2002-02-27 | 2003-09-10 | Shinto Fine Co Ltd | Wood preservative composition |
| JP2005047056A (en) * | 2003-07-30 | 2005-02-24 | Shinto Fine Co Ltd | Wood preservative composition, method for preserving wood against decay and wood subjected to preservative treatment |
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| JPH08219974A (en) * | 1995-02-17 | 1996-08-30 | Nec Corp | Method and apparatus for analyzing surface-active substance |
| JP2002502032A (en) * | 1998-01-28 | 2002-01-22 | クラリアント・インターナシヨナル・リミテッド | Method for measuring nonionic surfactants in alkaline aqueous solutions |
| WO2002086492A1 (en) * | 2001-04-17 | 2002-10-31 | Chugai Seiyaku Kabushiki Kaisha | Method of quantifying surfactant |
| JP2003252705A (en) * | 2002-02-27 | 2003-09-10 | Shinto Fine Co Ltd | Wood preservative composition |
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| JP2017161416A (en) * | 2016-03-10 | 2017-09-14 | 日本メジフィジックス株式会社 | Quantitative method of polyoxyethylene-based nonionic surfactant, and manufacturing method of radioactive pharmaceutical preparation |
| KR20200101617A (en) * | 2019-02-20 | 2020-08-28 | 충남대학교산학협력단 | Method for measuring concentration of wood preservative using electrical conductivity |
| KR102177989B1 (en) | 2019-02-20 | 2020-11-12 | 대한민국(산림청 국립산림과학원장) | Method for measuring concentration of wood preservative using electrical conductivity |
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