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JIS K1556-2006 Polyurethane raw materials -- Testing methods for toluene diisocyanate.pdf

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JIS K1556-2006 Polyurethane raw materials -- Testing methods for toluene diisocyanate.pdf

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໨ç ࣍ ϖʔδ ংจ··············································································································································································· 1 1.ç ద༻ൣғ ································································································································································ 1 2.ç Ҿ༻‫ ································································································································································ ֨ن‬1 3.ç ఆٛ········································································································································································ 2 4.ç ࢼྉͷ࠾औํ๏ ···················································································································································· 2 5.ç ࢼ‫߲ݧ‬໨ ································································································································································ 2 6.ç ࢼ‫ํݧ‬๏ ································································································································································ 2 6.1ç ϋʔθϯ୯Ґ৭਺ ·············································································································································· 2 6.2ç ີ౓······································································································································································ 3 6.3ç ‫ ·································································································································································· ఺ݻڽ‬3 6.4ç ҟੑମൺ཰ ·························································································································································· 4 6.5ç શԘૉྔ ······························································································································································ 8 ෟଐॻ 1ʢࢀߟʣΠιγΞωʔτ‫ؚج‬༗཰ͷࢼ‫ํݧ‬๏ ·······················································································11 ෟଐॻ 2ʢࢀߟʣ๕߳଒ΠιγΞωʔτͷࢎ౓ࢼ‫ํݧ‬๏ ···················································································17 ෟଐॻ 3ʢࢀߟʣՃਫ෼ղੑԘૉͷࢼ‫ํݧ‬๏ ·······································································································22 ೔ຊ޻‫֨نۀ‬ç ç ç JIS K 1556ɿ2006 ϙϦ΢Ϩλϯ‫ݪ‬ྉʵ τϧΤϯδΠιγΞωʔτࢼ‫ํݧ‬๏ Polyurethane raw materials Testing methods for toluene diisocyanate ংจç ͜ͷ‫֨ن‬͸ɼ1968 ೥ʹ੍ఆ͞Εɼࠓ೔ʹࢸ͍ͬͯΔɻͦͷ‫ޙ‬ͷࢼ‫߲ݧ‬໨ͷ௥Ճŋมߋ‫ํݧࢼͼٴ‬๏ ͷվྑʹରԠ͢ΔͨΊʹվਖ਼ͨ͠ɻ ͳ͓ɼࢀߟͱͯ͠ΠιγΞωʔτ‫ؚج‬༗཰ɼࢎ౓‫ͼٴ‬Ճਫ෼ղੑԘૉͷࢼ‫ํݧ‬๏ΛͦΕͧΕෟଐॻ 1ɼ ෟଐॻ 2 ‫ͼٴ‬ෟଐॻ 3 ʹࣔͨ͠ɻΠιγΞωʔτ‫ؚج‬༗཰͸ɼISO 14896:2000ɼPlasticsʵPolyurethane raw materialsʵDetermination of isocyanate content Λ‫ͯ͠ͱૅج‬ɼࢎ౓͸ɼISO 14898:1999ɼPlasticsʵAromatic isocyanates for use in the production of polyurethaneʵDetermination of acidity Λ‫ͯ͠ͱૅج‬ɼՃਫ෼ղੑԘૉ͸ɼ ISO 15028:2004ɼPlasticsʵAromatic isocyanates for use in the production of polyurethanesʵDetermination of hydrolysable chlorine Λ‫ͯ͠ͱૅج‬ɼͦΕͧΕಠཱͨ͠೔ຊ޻‫੍ͯ͠ͱ֨نۀ‬ఆ͞ΕΔ༧ఆͰ͋Δɻ ‫ࠂܯ‬ç ͜ͷ‫֨ن‬Λ࢖༻͢Δऀ͸ɼҰൠతͳࢼ‫ʹ࡞ૢݧ‬ਫ਼௨͍ͯ͠ͳ͚Ε͹ͳΒͳ͍ɻ͜ͷ‫֨ن‬͸ɼ҆શʹ ؔͯ͢͠΂ͯΛఏ‫͍ͯ͠ݴ‬ΔΘ͚Ͱ͸ͳ͍ɻద੾ͳ҆શ‫֬߁݈ͼٴ‬อʹؔ͢ΔखҾ͖ͷ࡞੒ฒͼʹɼ࢖༻ ʹઌ‫ࠃ֤͚ͯۦ‬ͷ‫੍ن‬৚݅ʹద߹͍ͯ͠Δ͜ͱΛ֬ೝ͢Δ͜ͱ͸ɼ͜ͷ‫֨ن‬ͷ࢖༻ऀͷ੹຿Ͱ͋Δɻ 1. ద༻ൣғç ͜ͷ‫֨ن‬͸ɼϙϦ΢Ϩλϯͷ੡଄ʹ࢖༻͢ΔτϧΤϯδΠιγΞωʔτʢҎԼɼTDI ͱ͍ ͏ɻʣͷࢼ‫ํݧ‬๏ʹ͍ͭͯ‫ن‬ఆ͢Δɻ 2. Ҿ༻‫֨ن‬ç ࣍ʹ‫͛ܝ‬Δ‫֨ن‬͸ɼ͜ͷ‫ʹ֨ن‬Ҿ༻͞ΕΔ͜ͱʹΑͬͯɼ͜ͷ‫֨ن‬ͷ‫ن‬ఆͷҰ෦Λߏ੒͢ Δɻ͜ΕΒͷҾ༻‫֨ن‬ͷ͏ͪͰɼൃߦ೥Λ෇‫͋ͯ͠ه‬Δ΋ͷ͸ɼ‫ࡌه‬ͷ೥ͷ൛͚͕ͩ͜ͷ‫֨ن‬ͷ‫ن‬ఆΛߏ ੒͢Δ΋ͷͰ͋ͬͯɼͦͷ‫ޙ‬ͷվਖ਼൛ɾ௥ิʹ͸ద༻͠ͳ͍ɻൃޮ೥Λ෇‫͍ͳ͍ͯ͠ه‬Ҿ༻‫֨ن‬͸ɼͦͷ ࠷৽൛ʢ௥ิΛ‫ؚ‬ΉɻʣΛద༻͢Δɻ JIS B 7410ç ੴ༉ྨࢼ‫༻ݧ‬Ψϥε੡Թ౓‫ܭ‬ JIS B 7411ç Ұൠ༻Ψϥε੡๮ঢ়Թ౓‫ܭ‬ JIS K 0061ç Խֶ੡඼ͷີ౓‫ͼٴ‬ൺॏଌఆํ๏ JIS K 0071-1ç Խֶ੡඼ͷ৭ࢼ‫ํݧ‬๏ʵୈ 1 ෦ɿϋʔθϯ୯Ґ৭਺ʢനۚʵίόϧτεέʔϧʣ JIS K 0113ç ిҐࠩɾిྲྀɾిྔɾΧʔϧϑΟογϟʔణఆํ๏௨ଇ JIS K 1101ç ࢎૉ JIS K 8001ç ࢼༀࢼ‫ํݧ‬๏௨ଇ JIS K 8034ç Ξητϯʢࢼༀʣ JIS K 8464ç γΫϩϔΩαϯʢࢼༀʣ JIS K 8541ç ঳ࢎʢࢼༀʣ 2 K 1556ɿ2006 JIS K 8891ç ϝλϊʔϧʢࢼༀʣ JIS R 3505ç Ψϥε੡ମੵ‫ܭ‬ JIS Z 8401ç ਺஋ͷ‫ؙ‬Ίํ JIS Z 8802ç pH ଌఆํ๏ ISO 3696:1987ɼWater for analytical laboratory useʵSpecification and test methods 3. ఆٛç ͜ͷ‫͍༻Ͱ֨ن‬Δओͳ༻‫ޠ‬ͷఆٛ͸ɼ࣍ʹΑΔɻ a) ҟੑମൺ཰ç TDI ͷҟੑମͰ͋Δ 2,4-TDI ‫ ͼٴ‬2,6-TDI ͷ࣭ྔ෼཰ʢˋʣຢ͸Ϟϧ෼཰ʢˋʣͷ࿨͕ 100 ˋͱͳΔΑ͏ʹɼ2 छͷҟੑମͷൺ཰ΛͦΕͧΕඦ෼཰Ͱදͨ͠΋ͷɻ b) Ճਫ෼ղੑԘૉྔç TDI ੡଄தʹੜ੒͠ɼࢼྉதʹෆ७෺ͱͯ͠‫·ؚ‬ΕΔՄೳੑͷ͋Δ༗‫ͼٴػ‬ແ‫ػ‬ ͷԘԽ෺Ͱ͋ͬͯɼࢼ‫ݧ‬৚݅Լʹ͓͍ͯϝλϊʔϧͱ൓Ԡͯ͠ԘԽਫૉΛൃੜ͢ΔԘԽ෺ྔΛԘૉͷ ࣭ྔ෼཰ʢˋʣͰදͨ͠΋ͷɻ c) શԘૉྔç ࢼྉΛࢎૉதͰ೩মͤͯ͞ੜ੒͢ΔԘԽ෺ྔΛɼࢼྉதͷԘૉͷ࣭ྔ෼཰ʢˋʣͱͯ͠ද ͨ͠΋ͷɻ d) ϙϦ΢Ϩλϯç ༗‫ػ‬δΠιγΞωʔτຢ͸༗‫ػ‬ϙϦΠιγΞωʔτͱɼ2 ‫׭‬ೳຢ͸ͦΕҎ্ͷਫࢎ‫ج‬ Λ΋ͭԽ߹෺ͱͷ൓ԠʹΑͬͯಘΒΕΔϙϦϚʔɻ e) ΠιγΞωʔτ‫ؚج‬༗཰ç ࢼྉதʹଘࡏ͢ΔΠιγΞωʔτ‫ج‬ʢҎԼɼNCO ‫ͱج‬΋͍͏ɻʣͷ࣭ྔ෼ ཰ʢˋʣɻ f) Ξϛϯ౰ྔç δ-n-ϒνϧΞϛϯ 1 g ౰ྔͱ݁߹͢Δࢼྉͷ࣭ྔ gɻ g) ࢎ౓ç ࢼྉͷࢎͷ‫͞ڧ‬Λ HCl ྔͱͯ͠ɼµg/g ຢ͸ˋͰࣔͨ͠΋ͷɻ 4. ࢼྉͷ࠾औํ๏(1)ç ϩοτΛ୅ද͢ΔࢼྉΛ࠾औ͢Δɻಛʹౙ‫ق‬த͸ɼౚ݁‫݁ͼٴ‬থੳग़ͷ͓ͦΕ͕ ͋ΔͷͰ஫ҙΛཁ͢Δɻ݁থੳग़ͷ৔߹͸ɼ40 ˆҎԼͷԹ౓ͰՃԹ͠ɼ‫׬‬શʹ༹ղͨ͠ࢼྉΛ࠾औ͢Δɻ ஫(1) ࢼྉ࠾औͷͱ͖͸ɼอ‫۩ޢ‬ʢखାɼอ‫ڸ؟ޢ‬ɼ๷ಟϚεΫͳͲʣΛண༻͠ɼ‫ؾ׵‬ΛΑ͘͢Δɻ ஠ૉ‫ྲྀؾ‬தͰ࣪‫ؾ‬Λආ͚ͯ࠾औ͢Δɻ ࢼྉอଘͷ৔߹͸ɼ஠ૉຢ͸‫ס‬૩ۭ‫Ͱؾ‬γʔϧ͠ɼີખͯ͠ྫྷ҉ॴʹஷଂ͢Δɻ ࢼྉ͕ਓମʹ෇ணͨ͠৔߹͸ɼ଎΍͔ʹੴ͚ΜਫͰચড়͢Δɻ ഇ‫͢غ‬Δ৔߹͸ɼਫΛຬͨͨ͠։์༰‫ࢼʹث‬ྉΛೖΕɼ2 ೔ؒ์ஔͯ͠෼ղ‫ࣺͯޙ‬Δɻ ࢖༻ࡁΈͷ෼ੳ‫۩ث‬͸ɼϝλϊʔϧதʹ 1 ൩์ஔ͠ɼચড়‫ס‬૩‫ޙ‬ɼ࠶࢖༻͢Δɻ 5. ࢼ‫߲ݧ‬໨ç ࢼ‫߲ݧ‬໨͸ɼ࣍ʹΑΔɻ a) ϋʔθϯ୯Ґ৭਺ç b) ີ౓ç c) ‫఺ݻڽ‬ç d) ҟੑମൺ཰ç e) શԘૉྔç 6. ࢼ‫ํݧ‬๏ç 6.1 ϋʔθϯ୯Ґ৭਺ç ϋʔθϯ୯Ґ৭਺͸ɼJIS K 0071-1 ʹΑͬͯଌఆ͢Δɻͨͩ͠ɼϋʔθϯ୯Ґඪ ४ൺ৭ӷ͸ɼද 1 ʹΑΔɻ 3 K 1556ɿ2006 ඪ४ൺ৭ӷͷ൪߸ 5 10 15 20 25 30 40 50 ද 1ç ϋʔθϯ୯Ґඪ४ൺ৭ӷ ‫ر‬ऍׂ߹ ඪ४ൺ৭ӷ‫ݪ‬ӷྔ mL 1.0 2.0 3.0 4.0 5.0 6.0 8.0 10.0 ਫ mL 99.0 98.0 97.0 96.0 95.0 94.0 92.0 90.0 6.2 ີ౓ç ີ౓͸ɼJIS K 0061 ʹΑͬͯଌఆ͢Δɻ 6.3 ‫఺ݻڽ‬ç 6.3.1 ཁࢫç ࢼྉΛҰఆͷ଎౓Ͱ͔͖·ͥͳ͕ΒɼΏͬ͘Γྫྷ٫͠ɼ͜ͷͱ͖‫ٻ‬ΊΒΕΔ‫ۂ఺ݻڽ‬ઢ͔Β ‫఺ݻڽ‬Λ‫ٻ‬ΊΔɻ‫·͕࢝ݻڽ‬ΔͱԹ౓্ঢ͕֬ೝ͞ΕΔ͕ɼԹ౓্ঢ‫ޙ‬ɼଌఆ༻Թ౓‫ܭ‬ͷࢦ͕ࣔҰఆͱͳ ΔԹ౓ΛಡΈऔΓɼ‫͢ͱ఺ݻڽ‬Δɻ 6.3.2 ૷ஔ‫۩ثͼٴ‬ç ʢਤ 1 ࢀরʣ a) ࢼྉ༰‫ث‬ç ಺‫ ܘ‬25ʶ1 mmɼ௕͞ 280ʶ6 mm ͷΨϥε੡ͷ΋ͷΛ࢖༻͢Δɻ b) ۭ‫֎ؾ‬౵ç ֎‫ ܘ‬50ʶ1 mmɼ௕͞ 175ʶ4 mm ͷΨϥε੡ͷ΋ͷΛ࢖༻͢Δɻ c) δϡϫʔළç ಺‫ ܘ‬85ʶ2 mmɼ௕͞ 180ʶ4 mm ͷ΋ͷΛ࢖༻͢Δɻ d) อ࣋ശç ಺‫ ܘ‬138ʶ3 mmɼߴ͞ 205ʶ5 mm ͷ΋ͷΛ࢖༻͢Δɻ e) ଌఆ༻Թ౓‫ܭ‬ç JIS B 7410 ʹ‫ن‬ఆ͢Δ‫༻఺ݻڽ‬Թ౓‫ ܭ‬SOP57 ‫ܗ‬Λ࢖༻͢Δɻ f) ྫྷഔ༻Թ౓‫ܭ‬ç JIS B 7411 ʹ‫ن‬ఆ͢Δਁ຅ઢ෇͖Թ౓‫Ͱܭ‬ɼద੾ͳԹ౓ൣғͷ΋ͷΛ࢖༻͢Δɻ g) ͔͖ࠞͥ๮ç ௚‫ܘ‬໿ 1 mm ͷ਑ۚͰɼͦͷԼ୺Λ֎‫ ܘ‬18 mm ͷྠঢ়ʹͨ͠΋ͷΛ࢖༻͢Δɻ h) ୤ࢷ໖ɼຢ͸ಉ౳඼ç 6.3.3 ૢ࡞ç ࢼྉΛ‫ס‬૩ͨ͠ࢼྉ༰‫ث‬ʢAʣͷඪઢ·ͰೖΕɼଌఆ༻Թ౓‫ܭ‬ʢEʣ‫͖͔ͥࠞͼٴ‬๮ʢGʣΛ ࠩ͠ࠐΜͰɼખΛ͢Δ(2)ɻ࣍ʹɼ͜ΕΛۭ‫֎ؾ‬౵ʢBʣதʹࠩ͠ࠐΈɼ༧‫͞ظ‬ΕΔ‫఺ݻڽ‬ΑΓ໿ 10 ˆ௿͍ ྫྷഔΛೖΕͨδϡϫʔළʢCʣதʹอ࣋͢ΔɻࢼྉͷԹ౓͕༧‫͞ظ‬ΕΔ‫఺ݻڽ‬ΑΓ໿ 5 ˆߴ͍Թ౓·Ͱྫྷ ٫ͨ͠ͱ͖ɼ͔͖ࠞͥ๮ʢGʣΛຖ෼ 30 ճͷׂ߹ͰΏͬ͘Γ্Լʹಈ͔͠ɼ30 ඵ͝ͱʹଌఆ༻Թ౓‫ܭ‬ʢEʣ ࣔ౓Λάϥϑ༻ࢴʹϓϩοτ͢Δɻ‫·͕࢝ݻڽ‬ΓɼԹ౓্ঢ͕‫ͯͬ͜ى‬΋ɼͳ͓͔͖ࠞͥΛଓ͚ɼগͳ͘ ͱ΋࿈ଓ 5 ఺ͷ‫͕఺ݻڽ‬ಉҰԹ౓ͱͳͬͨͱ͖ͷԹ౓Λ 0.01 ˆ·ͰಡΈऔΔɻ ஫(2) ଌఆ༻Թ౓‫ܭ‬ͷਫۜ‫ٿ‬͸ɼࢼྉ༰‫಺ث‬ͷࢼྉͷதԝʹҐஔ͢ΔΑ͏ʹ͢Δɻ 6.3.4 ਫ਼౓ç ࢼ‫݁ݧ‬Ռͷଥ౰ੑΛ൑அ͢ΔͨΊʹɼ࣍ͷࢦඪΛ༻͍Δɻ ‫ڐ‬༰ࠩʢˆʣ ಉҰਓɾಉҰ૷ஔͷ৔߹ 0.2 ผਓɾผ૷ஔͷ৔߹ 0.6 4 K 1556ɿ2006 6.3.5 ใࠂç ‫఺ݻڽ‬͸ɼ2 ճͷଌఆ݁ՌΛฏ‫ͯ͠ۉ‬ɼJIS Z 8401 ʹΑͬͯখ਺఺ҎԼୈ 1 Ґʹ‫ؙ‬Ίͯใࠂ ͢Δɻ ୯Ґç mm Aɿࢼྉ༰‫ث‬ Bɿۭ‫֎ؾ‬౵ Cɿδϡϫʔළ Dɿอ࣋ശ Eɿଌఆ༻Թ౓‫ܭ‬ Fɿྫྷഔ༻Թ౓‫ܭ‬ Gɿ͔͖ࠞͥ๮ HɿඪઢʢඪઢͷҐஔ͸ఈ͔Β 100 mmʣ Iɿ୤ࢷ໖ຢ͸ಉ౳඼ ਤ 1ç ૷ஔͷҰྫ 6.4 ҟੑମൺ཰ç 6.4.1 ཁࢫç ҟੑମൺ཰ͷଌఆ͸ɼ2,6-ҟੑମൺ཰͕ 5 ˋΛ௒͑ 95 ˋҎԼͷ৔߹ʢA ๏ʣͱɼ0 ˋҎ্ 5 ˋҎԼͷ৔߹ʢB ๏ʣͱʹ෼͚ΔɻͦΕͧΕͷࢼྉΛγΫϩϔΩαϯͰ‫ر‬ऍͨ͠‫ݕ‬ӷΛ੺֎෼ޫޫ౓‫ܭ‬ Λ༻͍ͯଌఆ͠ɼ๕߳଒‫؀‬ͷ C-H ໘֎ৼಈʹ‫ؼ‬ଐ͢Δ 810 cmʵ1ʢ12.35 µmʣ෇ۙ‫ ͼٴ‬780 cmʵ1ʢ12.80 µmʣ ෇ۙͷ‫ٵ‬ऩ‫ۃ‬େͷ‫౓ޫٵ‬Λ‫ٻ‬Ίɼ‫ྔݕ‬ઢΛ༻͍֤ͯҟੑମͷൺ཰Λࢉग़͢Δɻ 6.4.2 ૷ஔ‫۩ثͼٴ‬ç a) ੺֎෼ޫޫ౓‫ܭ‬ç 2,4-ҟੑମͷ 810 cmʵ1ʢ12.35 µmʣ෇ۙͷ‫ٵ‬ऩ‫ۃ‬େ‫ ͼٴ‬2,6-ҟੑମͷ 780 cmʵ1ʢ12.80 5 K 1556ɿ2006 µmʣ෇ۙͷ‫ٵ‬ऩ‫ۃ‬େΛࣝผ͢Δͷʹे෼ͳ෼ղೳΛ΋ͭɼ୯ޫଋ‫ܗ‬ए͘͠͸ෳޫଋ‫ܗ‬ͷ෼ࢄ‫֎੺ܗ‬෼ ޫޫ౓‫ܭ‬ຢ͸ϑʔϦΤม‫֎੺ܗ׵‬෼ޫޫ౓‫ܭ‬ʢFT-IRʣΛ࢖༻͢Δ͜ͱ͕Ͱ͖Δɻ උߟ ੺֎෼ޫޫ౓෼ੳ૷ஔ͸ɼछʑ͋ΔͷͰɼ͜ͷํ๏Ҏ֎ͷଌఆ৚݅Λ༻͍Δ৔߹ʹ͸ɼ͜Εͱ ಉ౳ͷਫ਼౓͕ಘΒΕΔ৚݅Λ৻ॏʹ‫ٻ‬Ίͨ‫ͯ͠༻࠾ޙ‬΋Α͍ɻ b) ηϧç ԘԽφτϦ΢Ϝͷ૭൘Λ࢖ͬͨް͞ 0.2 mmʢA ๏ʣ‫ ͼٴ‬0.1 mmʢB ๏ʣͷηϧΛ༻͍Δɻηϧ ͷް͞͸ɼ‫ׯ‬ব͡·๏ʹΑͬͯଌఆ͢Δɻ c) ‫ڞ‬ખ෇શྔϑϥεί(3)ç 25 mL ຢ͸ 50 mL ஫(3) Ψϥε‫ྨ۩ث‬͸ɼे෼ʹ‫ס‬૩͓͔ͯ͠ͳ͍ͱɼࢼྉ͕࣪෼ͱ༰қʹ൓Ԡ͢ΔͷͰ஫ҙΛཁ͢Δɻ 6.4.3 ࢼༀç a) γΫϩϔΩαϯç JIS K 8464 ʹ‫ن‬ఆ͢ΔγΫϩϔΩαϯɻਫ෼ͷ࣭ྔ෼཰͸ɼ0.02 ˋҎԼͱ͠ɼ830 ʙ770 cmʵ1ʢ12ʙ13 µmʣͷྖҬͰ 0.2 mm ͷηϧͰಁա཰͕ 70 ˋҎ্͋Δ΋ͷɻ b) ඪ४ࢼྉç ७ 2,4-ҟੑମ‫ͼٴ‬७ 2,6-ҟੑମͷඪ४ࢼྉ͸ɼͦΕͧΕ७ਮͷରԠ͢ΔΞϛϯͷϗεήϯ ԽʹΑͬͯ߹੒͠ɼਅۭৠཹʹΑͬͯਫ਼੡ͨ͠΋ͷ(4)ɻ ஫(4) ७ 2,4-ҟੑମ‫ͼٴ‬७ 2,6-ҟੑମ͸ɼۭ‫ؾ‬தͷ࣪෼ͱ൓Ԡ͢ΔͷͰɼஷଂ༰‫ث‬͸‫ס‬૩஠ૉͰஔ‫͠׵‬ ͯɼऔѻ͍΋ಉ͡งғ‫ؾ‬தͰߦ͏ɻ 6.4.4 ૢ࡞ç a) A ๏ç 1) ‫ྔݕ‬ઢͷ࡞੒‫਺܎ޫٵͼٴ‬ͷܾఆç ७ 2,4-ҟੑମ‫ͼٴ‬७ 2,6-ҟੑମͷඪ४ࢼྉΛද 2 ʹैͬͯ 0.01 g ·Ͱਖ਼͘͠͸͔Γɼ25 mL ຢ͸ 50 mL ͷ‫ס‬૩શྔϑϥείதͰγΫϩϔΩαϯͰඪઢ·Ͱਖ਼֬ʹ‫ر‬ ऍͯ͠ 6 छྨͷೱ౓ͷඪ४༹ӷΛ֤ҟੑମʹ͍ͭͯɼ‫ ܭ‬12 ‫ݸ‬ௐ੡͢Δɻ ද 2ç A ๏ඪ४༹ӷ 2,4-ҟੑମඪ४༹ӷೱ౓ ७ 2,4-ҟੑମ࣭ྔ ༹ഔ‫ر‬ऍʹΑͬͯௐ੡͢Δ࠷ऴඪ४༹ӷྔ g/mL g mL 0.040 1.0 25 0.024 0.60 25 0.016 0.40 25 0.008 0 0.20 25 0.004 0 0.10 25 0.002 0 0.10 50 0.040 1.0 25 0.024 0.60 25 0.016 0.40 25 0.008 0 0.20 25 0.004 0 0.10 25 0.002 0 0.10 50 ࣍ʹɼඪ४༹ӷΛॱ࣍ 0.2 mm ͷηϧʹ஫ೖͯ͠೾਺Ҭ 870ʙ740 cmʵ1ʢ೾௕Ҭ 11.5ʙ13.5 µmʣͷ ൣғʹεϖΫτϧΛඳ͔ͤɼඪ४༹ӷ୯ಠͷεϖΫτϧͷ্ʹॏͶͯ‫ه‬࿥͢Δ(5)ɻଓ͍ͯ͜ΕΒε ϖΫτϧਤʹ͍ͭͯ 2,4-ҟੑମͷ 810 cmʵ1ʢ12.35 µmʣ෇ۙͷ‫ٵ‬ऩ‫ۃ‬େ‫ ͼٴ‬2,6-ҟੑମͷ 780 cmʵ1 ʢ12.80 µmʣ෇ۙͷ‫ٵ‬ऩ‫ۃ‬େͷ‫౓ޫٵ‬Λ‫ٻ‬Ίɼೱ౓ͱ‫ͱ౓ޫٵ‬ͷؔ܎Λάϥϑ্ʹϓϩοτ͠ɼ࠷ খೋ৐๏ʹΑͬͯ‫ྔݕ‬ઢΛ࡞੒͢Δɻ͜ͷ‫ྔݕ‬ઢΛ༻͍ͯɼ࣍ͷࣜʹΑͬͯ‫਺܎ޫٵ‬Λ‫ٻ‬ΊΔɻ 6 K 1556ɿ2006 Иa = A ca ⋅ d ͜͜ʹɼ Иa ɿ Aɿ ca ɿ ‫਺܎ޫٵ‬ʦmL /ʢgŋmmʣʧ ඪ४༹ӷͷ‫ ౓ޫٵ‬log 10 I0 / I I0ɿޫ‫౓ڧ‬ʢಁաલʣIɿޫ‫౓ڧ‬ʢಁա‫ޙ‬ʣ ༹ӷͷೱ౓ʢg / mLʣ d ɿ ηϧͷް͞ʢmmʣ ஫(5) Ұ࿈ͷૢ࡞࣮ࢪத͸ɼ੺֎෼ޫޫ౓‫ܭ‬ͷௐ੔Λߦͬͯ͸ͳΒͳ͍ɻ 2) ଌఆç ࢼྉ໿ 1 g Λਖ਼͘͠͸͔Γɼ಺༰ 25 mL ͷ‫ס‬૩શྔϑϥείதʹγΫϩϔΩαϯͰ‫ر‬ऍ͠ɼ ‫ݕ‬ӷΛௐ੡͢Δɻ͜ͷ‫ݕ‬ӷΛ 0.2 mm ͷް͞ͷηϧʹೖΕͯɼ‫ྔݕ‬ઢ࡞੒࣌ͱಉҰ৚݅Ͱ 870ʙ740 cmʵ1 ͷ೾਺Ҭʢ11.5ʙ13.5 µm ͷ೾௕Ҭʣʹ͍ͭͯεϖΫτϧΛ‫ه‬࿥͢Δɻ b) B ๏ç 1) ‫ྔݕ‬ઢͷ࡞੒‫਺܎ޫٵͼٴ‬ͷܾఆç ७ 2,4-ҟੑମ‫ͼٴ‬७ 2,6-ҟੑମͷඪ४ࢼྉΛɼද 3 ʹैͬͯ 0.001 g ͷҐ·Ͱਖ਼͘͠͸͔ͬͯࠞ߹ௐ੡͢Δɻ ද 3ç B ๏ඪ४ӷ 2,6-ҟੑମൺ཰ ˋ ७ 2,4-ҟੑମ࣭ྔ g ७ 2,6-ҟੑମ࣭ྔ g 0.00 4.000 0.000 0.50 3.980 0.020 1.00 3.960 0.040 2.00 3.920 0.080 3.00 3.880 0.120 4.00 3.840 0.160 5.00 3.800 0.200 ް͞ 0.1 mm ͷηϧΛ༻͍ͯɼલ‫ه‬Ұ࿈ͷඪ४ӷͷ 830ʙ740 cmʵ1 ೾਺Ҭʢ12.0ʙ13.5 µm ೾௕Ҭʣ ͷεϖΫτϧΛඳ͔ͤɼͦΕͧΕͷεϖΫτϧਤ͔Β 2,6-ҟੑମͷ 780 cmʵ1ʢ12.80 µmʣ෇ۙʹ͓ ͚Δ‫ٵ‬ऩ‫ۃ‬େͷ‫౓ޫٵ‬ΛϕʔεϥΠϯ๏ʹΑͬͯ‫ٻ‬Ίɼೱ౓ͱ‫ͱ౓ޫٵ‬ͷؔ܎Λάϥϑʹϓϩοτ ͠ɼ࠷খೋ৐๏ʹΑͬͯ‫ྔݕ‬ઢΛ࡞੒͢Δɻ͜ͷ‫ྔݕ‬ઢΛ༻͍ͯɼ࣍ͷࣜʹΑͬͯ‫਺܎ޫٵ‬Λ‫ٻ‬Ί Δɻ Иb = A × 100 cb ×d ͜͜ʹɼ Иb ɿ Aɿ cbɿ dɿ ‫਺܎ޫٵ‬ʢmmʵ1ʣ ඪ४ӷͷ‫ ౓ޫٵ‬log 10 I0 / I I0ɿޫ‫౓ڧ‬ʢಁաલʣIɿޫ‫౓ڧ‬ʢಁա‫ޙ‬ʣ 2,6-ҟੑମൺ཰ʢˋʣ ηϧͷް͞ʢmmʣ 2) ଌఆç ࢼྉΛ 1)Ͱ༻͍ͨް͞ 0.1 mm ͷηϧʹೖΕɼಉ༷ʹͯ͠ 830ʙ740 cmʵ1 ͷ೾਺Ҭʢ12.0ʙ13.5 µm ͷ೾௕Ҭʣʹ͍ͭͯεϖΫτϧΛ‫ه‬࿥͢Δɻ 6.4.5 ‫ࣜࢉܭ‬ç a) A ๏ç 6.4.4 a) 1)ͷૢ࡞ͱಉ༷ʹ֤ͯ͠੒෼ͷ‫౓ޫٵ‬Λ‫ٻ‬ΊΔɻ2,4-ҟੑମ‫ ͼٴ‬2,6-ҟੑମͰ͸ɼೋͭ ͷ‫ٵ‬ऩଳͷΘ͔ͣͳΦʔόʔϥοϓ͕͋ΔͨΊʹɼ࣍ͷࣜʹΑͬͯ 2,4-ҟੑମ‫ ͼٴ‬2,6-ҟੑମͷิਖ਼ ‫౓ޫٵ‬Λ‫͚ͳ͠ࢉܭ‬Ε͹ͳΒͳ͍ɻç A2,6ʹA780ʵ0.043A810 7 K 1556ɿ2006 A2,4ʹA810ʵ0.024A780 ͜͜ʹɼ A2,6ɿ 2,6-ҟੑମͷิਖ਼‫౓ޫٵ‬ A2,4ɿ 2,4-ҟੑମͷิਖ਼‫౓ޫٵ‬ A810ɿ 810 cmʵ1ʢ12.35 µmʣ෇ۙʹ͓͚Δ‫ٵ‬ऩ‫ۃ‬େͷ‫౓ޫٵ‬ A780ɿ 780 cmʵ1ʢ12.80 µmʣ෇ۙʹ͓͚Δ‫ٵ‬ऩ‫ۃ‬େͷ‫౓ޫٵ‬ ࣍ʹɼ͜ΕΒͷิਖ਼‫͔౓ޫٵ‬Β‫ྔݕ‬ઢΛ༻͍ͯ‫਺܎ޫٵ‬Λ‫ٻ‬Ίɼ࣍ͷࣜʹΑ֤ͬͯҟੑମ‫ؚ‬༗཰Λ ࢉग़͢Δɻ 異性体含有率(%) = A ×100 Иa × d × m 25 ͜͜ʹɼ Aɿ Иa ɿ dɿ mɿ 25ɿ ิਖ਼‫ ౓ޫٵ‬log 10 I0 / I I0ɿޫ‫౓ڧ‬ʢಁաલʣIɿޫ‫౓ڧ‬ʢಁա‫ޙ‬ʣ ‫਺܎ޫٵ‬ʦmL /ʢgŋmmʣʧ ηϧͷް͞ʢmmʣ ࢼྉͷ࣭ྔʢgʣ શྔϑϥείͷ༰ੵʢmLʣ ֤ҟੑମൺ཰ͷ߹‫ܭ‬͸ɼ100ʶ3 ˋҎ಺ʹ͠ͳ͚Ε͹ͳΒͳ͍ɻ ͜Ε͸ɼ࣍ͷࣜʹΑͬͯҟੑମ‫ؚ‬༗཰Λิਖ਼͠ɼิਖ਼ 2,4-ҟੑମൺ཰‫ ͼٴ‬2,6-ิਖ਼ҟੑମൺ཰ͱ ͢Δɻ 補正2,4 - 異性体比率(%) ʹ P P+Q ×100 補正2,6 - 異性体比率(%) ʹ100ʵ補正2,4 - 異性体比率(%) ͜͜ʹɼ Pɿ 2,4-ҟੑମ‫ؚ‬༗཰ʢˋʣ Qɿ 2,6-ҟੑମ‫ؚ‬༗཰ʢˋʣ b) B ๏ç 6.4.4 b) 1)ͷૢ࡞ͱಉ༷ʹͯ͠ 2,6-ҟੑମͷ 780 cmʵ1ʢ12.80 µmʣ෇ۙʹ͓͚Δ‫ٵ‬ऩ‫ۃ‬େͷ‫ޫٵ‬ ౓Λ‫ٻ‬Ίɼ‫ྔݕ‬ઢΛ༻͍ͯɼ࣍ͷࣜʹΑͬͯɼ֤੒෼ҟੑମൺ཰Λࢉग़͢Δɻ 2,6 - 異性体比率(%) ʹИb A × d ×100 2,4 - 異性体比率(%) ʹ1ɹ00ʵ2,6 - 異性体比率(%) ͜͜ʹɼ A ɿ 780 cmʵ1ʢ12.80 µmʣ෇ۙʹ͓͚Δ‫ٵ‬ऩ‫ۃ‬େͷ‫ ౓ޫٵ‬log 10 I0 / I I0ɿޫ‫౓ڧ‬ʢಁաલʣIɿޫ‫౓ڧ‬ʢಁա‫ޙ‬ʣ Иb ɿ ‫਺܎ޫٵ‬ʢmmʵ1ʣ d ɿ ηϧͷް͞ʢmmʣ 6.4.6 ਫ਼౓ç ࢼ‫݁ݧ‬Ռͷଥ౰ੑΛ൑அ͢ΔͨΊʹɼ࣍ͷࢦඪΛ༻͍Δɻ ‫ڐ‬༰ࠩʢˋʣ ಉҰਓɾಉҰ૷ஔͷ৔߹ 0.6 ผਓɾผ૷ஔͷ৔߹ 1.5 6.4.7 ใࠂç ҟੑମൺ཰͸ɼ6.4.5 ʹΑͬͯখ਺఺ҎԼୈ 2 Ґ·Ͱࢉग़͠ɼ2 ճͷࢼ‫݁ݧ‬ՌΛฏ‫ ͯ͠ۉ‬JIS Z 8401 ʹΑͬͯখ਺఺ҎԼୈ 1 Ґʹ‫ؙ‬Ίͯใࠂ͢Δɻ 6.5 શԘૉྔç 8 K 1556ɿ2006 6.5.1 ཁࢫç ࢼྉΛγΣχʔήϧ೩মϑϥείʹೖΕࢎૉதͰ೩ম͠ɼੜ੒ͨ͠ԘԽ෺Λਫʹ‫ٵ‬ऩͤ͞ɼ Ξητϯ༹ഔதͰۜʵۜԘԽۜి‫ۃ‬Λ༻͍ɼ঳ࢎ༹ۜӷͰిҐࠩణఆΛ͢ΔɻશԘૉྔ͸ɼࢼྉதͷશԘ ૉʢClʣ෼ΛʢˋʣͰࣔ͢ɻ 6.5.2 ૷ஔ‫۩ثͼٴ‬ç ૷ஔ‫۩ثͼٴ‬͸ɼ࣍ʹΑΔɻ a) ిҐࠩణఆ૷ஔຢ͸ pH ϝʔλç JIS K 0113 ຢ͸ JIS Z 8802 ʹΑΔɻ b) ࢦࣔి‫ۃ‬ʢۜి‫ۃ‬ʣ c) ࢀরి‫ۃ‬ʢۜʵۜԘԽۜి‫ۃ‬ʣ d) ϚάωνοΫελʔϥ e) ࢼྉ࠾औ༻஫ࣹ‫ث‬ç f) γΣχʔήϧ೩মϑϥείç ਤ 3 ʹࣔ͢നۚઢ‫ͼٴ‬ന͔ۚ͝Λ΋ͭɼ‫ڞ‬ખ෇͖ߗ࣭Ψϥε੡ͷ 1 L ϑ ϥείʢਤ 2ʣɻ g) ϏʔΧʔç 100 mL ຢ͸ 200 mL h) ϏϡϨοτç JIS R 3505 ʹ‫ن‬ఆ͢Δ 5 mL Ͱɼ0.02 mL ͝ͱʹࠁ౓ͷ͋Δ΋ͷɻ i) ϐϯηοτç ਤ 2ç γΣχʔήϧ೩মϑϥείͷҰྫ ୯Ґç mm ਤ 3ç γΣχʔήϧϑϥείͷന͔ۚ͝෇͖ખͷҰྫ 6.5.3 ࢼༀç ࢼༀ͸ɼ࣍ʹΑΔɻ a) 0.000 5 mol/L ঳ࢎ༹ۜӷç 0.01 mol/L ঳ࢎۜඪ४༹ӷΛਫͰਖ਼͘͠ 20 ഒʹ‫ر‬ऍ͠ɼௐ੡ͨ͠΋ͷɻ b) Ξητϯç JIS K 8034 ʹ‫ن‬ఆ͢Δ΋ͷɻ 9 K 1556ɿ2006 c) ‫ر‬঳ࢎç JIS K 8541 ʹ‫ن‬ఆ͢Δ঳ࢎΛ౳ྔͷਫͰ‫ر‬ऍͨ͠΋ͷɻ d) ࢎૉç JIS K 1101 ʹ‫ن‬ఆ͢Δѹॖࢎૉɻ e) Ζࢴ(6)ç ෯ 5 mmɼ௕͞ 25 mm ͷ΋ͷɻ f) ୤ࢷ໖ç ୈे࢛վਖ਼೔ຊༀ‫ʹํہ‬ΑΔ΋ͷɻ ஫(6) ੾औΓ‫࡞ૢͼٴ‬த͸ɼಛʹਗ਼ড়ʹऔΓѻ͏ɻ 6.5.4 ૢ࡞ç Ζࢴ‫ͼٴ‬୤ࢷ໖ ໿ 50 mg Λਤ 4 ͷΑ͏ʹന͔ۚ͝ʹೖΕ(7)ɼࢼྉ࠾औ༻஫ࣹ‫ࢼͰث‬ྉ 60 ʙ100 mg Λਖ਼֬ʹ୤ࢷ໖தʹ͸͔ΓࠐΉɻΖࢴʹ఺Րͨ͠‫ޙ‬ɼ͋Β͔͡Ίਫ໿ 15 mL ΛೖΕɼ಺෦Λࢎૉ Ͱஔ‫ͨ͠׵‬೩মϑϥείதʹ଎΍͔ʹࠩ͠ࠐΈɼΖࢴʹਫ͕෇ண͠ͳ͍Α͏ʹ೩মϑϥείΛ੩͔ʹ܏ࣼ ͠ɼਫͰϑϥείͷ‫ޱ‬Λ෧͡Δɻ೩ম͕ऴΘͬͨΒɼϑϥείͷಶΓ͕‫׬‬શʹফࣦ͢Δ·ͰৼΓɼ໿ 5 ෼ ؒ੩ஔͨ͠‫ޙ‬ɼϑϥείͷખͷपғʹগྔͷΞητϯΛೖΕɼ੩͔ʹખΛ֎ͯ͠ΞητϯΛϑϥείதʹ ‫ٵ‬ೖͤ͞Δɻϑϥεί಺ͷ༹ӷΛϏʔΧʹҠ͠ɼϑϥεί಺นΛΞητϯ໿ 30 mL Ͱચ͍ɼ༹ӷ͸ϏʔΧ ʹूΊΔɻ͜ΕΛϚάωνοΫελʔϥͰ͔͘͸Μ͠ͳ͕Β‫ر‬঳ࢎ 2ʙ3 ణΛՃ͑ͯɼࢦࣔి‫ࢀͼٴۃ‬রి ‫ۃ‬ΛೖΕɼిҐࠩణఆ૷ஔຢ͸ pH ϝʔλʹ઀ଓ͠ɼϑϧεέʔϧΛ 100 mV ຢ͸ 250 mV ʹηοτͯ͠ɼ ӷԹΛ໿ 20 ˆʹอͬͨ 0.000 5 mol/L ঳ࢎ༹ۜӷΛ༻͍ͯణఆ͠ɼಘΒΕͨణఆ‫ۂ‬ઢͷม‫఺ۂ‬Λऴ఺ͱ͢ Δ(8)ɻ͜ͷࢼ‫ʹݧ‬͸ಉҰ৚݅Ͱۭࢼ‫ݧ‬Λߦ͏ɻ ஫(7) Ζࢴ‫ͼٴ‬୤ࢷ໖͕‫ʹ׼‬Ԛછ͞ΕΔͱਖ਼͍͠ଌఆ͕Ͱ͖ͳ͍ͷͰബ͍ΰϜखାͳͲΛண༻͠ɼૢ ࡞͸ɼϐϯηοτͰߦ͏ɻ (8) ऴ఺ͷ‫ٻ‬Ίํ͸ɼJIS K 0113 ͷ 5.2.2ʢऴ఺ܾఆํ๏ʣʹΑΔɻ උߟ ೩মૢ࡞ʹ౰ͨͬͯ͸ɼ࣍ͷ఺Λਖ਼͘͠कΒͳ͚Ε͹ͳΒͳ͍ɻ a) ࢼྉɼ୤ࢷ໖‫ͼٴ‬Ζࢴ͸ɼ‫ن‬ఆྔҎ্Λ࢖༻͠ͳ͍ɻ b) ϑϥεί͸ɼৗʹஸೡʹऔΓѻ͍ɼ͖͕ͣ෇͔ͳ͍Α͏ʹ͢Δɻ c) ϑϥεί͸ɼ࢖༻લʹ͖ͣͷͳ͍͜ͱΛ֬ೝͨ͠‫ޙ‬ɼ࢖༻͢Δɻ d) ϑϥεί͸ɼ࢖༻ͷස౓͕ଟ͘ͳΔͱͻͣΈ͕ͰΔͷͰɼద੾ͳ࣌‫ظ‬ʢ໿ 1 ೥ఔ౓ʣʹߋ ৽͢Δ͜ͱ͕๬·͍͠ɻ e) ϑϥείͷ‫ޱ‬ખ෦ʹάϦʔεΛ༻͍ͯ͸ͳΒͳ͍ɻ f) ૢ࡞ʹ͸ɼಁࢹϚεΫɼֵखାͳͲͷอ‫۩ޢ‬Λ༻͍ɼ޲͔͍ଆʹ͸ۚ໢ͷཱ͍ͭͯΛஔ͍ ͯສҰͷഁଛʹඋ͑ɼϑϥείͷఈΛ֎ଆ޲͖ͱͯ͠อ࣋͢Δɻ 10 K 1556ɿ2006 ਤ 4ç ࢼྉ૷ͯΜͷํ๏ 6.5.5 ‫ࣜࢉܭ‬ç શԘૉྔʢˋʣ͸ɼ࣍ͷࣜʹΑͬͯࢉग़͢Δɻ T = 3 545× (VS −VB )× c m ͜͜ʹɼ Tɿ VS ɿ VB ɿ cɿ mɿ શԘૉྔʢˋʣ ࢼ‫ʹݧ‬ཁͨ͠঳ࢎ༹ۜӷͷྔʢmLʣ ۭࢼ‫ʹݧ‬ཁͨ͠঳ࢎ༹ۜӷͷྔʢmLʣ ঳ࢎ༹ۜӷͷਖ਼֬ͳೱ౓ʢmol/Lʣ ࢼ‫ࢼ༻ݧ‬ྉͷ࠾औྔʢmgʣ 6.5.6 ਫ਼౓ç ࢼ‫݁ݧ‬Ռͷଥ౰ੑΛ൑அ͢ΔͨΊʹɼ࣍ͷࢦඪΛ༻͍Δɻ ‫ڐ‬༰ࠩʢˋʣ ಉҰਓɾಉҰ૷ஔͷ৔߹ 0.015 ผਓɾผ૷ஔͷ৔߹ 0.03 6.5.7 ใࠂç શԘૉྔ͸ɼ6.5.5 ʹΑͬͯখ਺఺ҎԼ 3 Ґ·Ͱࢉग़͠ɼ2 ճͷࢼ‫݁ݧ‬ՌΛฏ‫ ͯ͠ۉ‬JIS Z 8401 ʹΑͬͯখ਺఺ҎԼୈ 2 Ґʹ‫ؙ‬Ίͯใࠂ͢Δɻ 11 K 1556ɿ2006 ෟଐॻ 1ʢࢀߟʣΠιγΞωʔτ‫ؚج‬༗཰ͷࢼ‫ํݧ‬๏ ংจç ͜ͷෟଐॻ͸ ISO 14896ɿ2000 ͷؔ࿈͢Δ෦෼Λ຋༁͠ɼࢀߟͱͯ͠௥Ճͨ͠΋ͷͰ‫ن‬ఆͷҰ෦ Ͱ͸ͳ͍ɻ 1. ‫ݪ‬ཧç 1.1 A ๏ç ΠιγΞωʔτࢼྉʹա৒ͷδ-n-ϒνϧΞϛϯͷτϧΤϯ༹ӷΛՃ͑ͯ൓Ԡͤ͞ɼ૬౰͢ Δ೘ૉΛੜ੒ͤ͞ΔɻࣨԹ·Ͱྫྷ٫‫ޙ‬ɼ‫༹ڞ‬ഔͱͯ͠ΞητϯΛఴՃ͢Δɻͦͷ‫ޙ‬ɼԘࢎඪ४ਫ༹ӷΛ ༻͍ͯɼిҐࠩణఆ๏ຢ͸ࢦࣔༀణఆ๏ʹΑͬͯ‫ٯ‬ణఆΛߦ͍ɼऴ఺Λ‫ٻ‬ΊΔɻ 1.2 B ๏ç ΠιγΞωʔτࢼྉʹա৒ͷδ-n-ϒνϧΞϛϯͷτϧΤϯ/τϦΫϩϩϕϯθϯ༹ӷΛՃ͑ ͯ൓Ԡͤ͞ɼ૬౰͢Δ೘ૉΛੜ੒ͤ͞ΔɻࣨԹ·Ͱྫྷ٫‫ޙ‬ɼ൓Ԡ෺ΛϝλϊʔϧͰ‫ر‬ऍ͠ɼԘࢎϝλϊ ʔϧ༹ӷΛ༻͍ͯɼిҐࠩణఆ๏ຢ͸ࢦࣔༀణఆ๏ʹΑͬͯ‫ٯ‬ణఆΛߦ͍ɼऴ఺Λ‫ٻ‬ΊΔɻ 2. ๦֐ࣄ߲ç ԘԽΧϧϘχϧɼΠιγΞωʔτதͷΧϧόϛϯࢎԘԽ෺ɼԘԽਫૉ‫ͼٴ‬ଞͷࢎੑຢ͸ Ԙ‫ج‬ੑԽ߹෺͕ఆྔͷ๦֐ͱͳΔɻ ਫ਼੡ΠιγΞωʔτதͰ͸ɼ͜ΕΒͷෆ७෺͸௨ৗɼগྔ͔͠ଘࡏ͠ͳ͍ͷͰఆྔʹ͸Ө‫͍ͳ͠ڹ‬ɻ ͔͠͠ɼૈ੡ຢ͸มੑΠιγΞωʔτ͸ɼ໿ 0.3 ˋҎ্ͷࢎ౓Λ‫ؚ‬Ή৔߹͕͋Δɻͦͷ৔߹ɼະਫ਼੡ ΠιγΞωʔτͷ NCO ‫ؚ‬༗཰ͷ஋͸ɼࢎ౓ʠิਖ਼ʡຢ͸ʠະิਖ਼ʡͱใࠂ͢Δͷ͕๬·͍͠ɻ 3. ࢼྉͷ࠾औ ༗‫ػ‬ΠιγΞωʔτ͸ɼงғ‫ؾ‬தͷਫ෼ͱ൓Ԡ͢ΔͷͰɼࢼྉͷ࠾औத͸ɼ஫ҙΛ෷ ͏ඞཁ͕͋Δɻ ௨ৗͷࢼྉ࠾औํ๏ʢྫ͑͹ΦʔϓϯυϥϜ͔Βͷࢼྉ࠾औʣ͸ɼ଎΍͔ʹߦΘΕͯ΋ෆ༹ੑ೘ૉʹ ΑΓࢼྉͷԚછΛҾ͖‫͢͜ى‬ɻ͕ͨͬͯ͠ɼৗ࣌ɼ‫ס‬૩ෆ‫׆‬ੑΨεʢྫ͑͹ɼ஠ૉɼΞϧΰϯ͋Δ͍͸ ‫ס‬૩ۭ‫ؾ‬ʣͰࢼྉશମΛ෴͏ɻ ‫ࠂܯ‬çç༗‫ػ‬ΠιγΞωʔτ͸ɼൽෘΛ௨ͯ͠‫ٵ‬ऩຢ͸ৠ‫ؾ‬Λ‫ٵ‬Ҿ͢Δͱ‫͋Ͱݥة‬Δɻç ద੾ͳ‫ؾ׵‬Λߦ͍ɼอ‫ޢ‬खା‫ͼٴ‬อ‫ޢ‬Ί͕ͶΛண༻͢Δɻç ç 4. ࢼ‫ݧ‬৚݅ç ΠιγΞωʔτ͸ɼਫ෼ͱ൓Ԡ͢ΔͨΊɼ࣮‫ࣨݧ‬ͷ࣪౓Λ௿͘อ࣋͢Δɻ૬ର࣪౓ 50 ˋ ҎԼ͕๬·͍͠ɻ 5. ࢼༀç ͢΂ͯͷ෼ੳʹ͓͍ͯɼࢼༀάϨʔυ඼Λ༻͍Δɻಛʹࢦ͕ࣔͳ͚Ε͹ɼISO 6353-1ɼISO 6353-2 ‫ ͼٴ‬ISO 6353-3 ͷ‫͏ैʹࡌه‬ɻे෼ʹ७౓ͷߴ͍΋ͷͰɼଌఆͷਫ਼౓ΛଛͳΘͳ͚Ε͹ɼଞͷά Ϩʔυ඼Λ༻͍ͯ΋Α͍ɻ ಛʹ‫ن‬ఆ͕ͳ͍‫ݶ‬Γɼ͜ͷ‫֨ن‬ͷਫͱ͸ɼISO 3696 ʹΑΔάϨʔυ 3 ͷਫΛࢦ͢ɻ 5.1 Ξητϯç ʢA ๏ʣç 5.2 τϧΤϯç λΠϓ 4A ͷϞϨΩϡϥʔγʔϒͰ୤ਫͨ͠΋ͷɻ 5.3 δ-n-ϒνϧΞϛϯ༹ӷ 1 mol/L ʢA ๏ʣδ-n-ϒνϧΞϛϯ 129 g ΛɼτϧΤϯͰ 1 L ʹ‫ر‬ऍͨ͠ ΋ͷɻ 12 K 1556ɿ2006 5.4 δ-n-ϒνϧΞϛϯ༹ӷ 2 mol/L ʢB ๏ʣδ-n-ϒνϧΞϛϯ 258 g ΛτϧΤϯͰ 1 L ʹ‫ر‬ऍͨ͠΋ ͷɻ 5.5 Ԙࢎਫ༹ӷç 1 mol/L ʢA ๏ʣ1 mol/L Ԙࢎਫ༹ӷΛ४උ͠ɼ0.001 mol/L ·Ͱඪఆͨ͠΋ͷɻ 5.6 Ԙࢎϝλϊʔϧ༹ӷ 1 mol/L ʢB ๏ʣ1 mol/L Ԙࢎϝλϊʔϧ༹ӷΛ४උ͠ɼ0.001 mol/L ·Ͱඪఆ ͨ͠΋ͷɻ ࢀߟ ‫ۉ‬Ұ༹ӷʹ͢ΔͨΊɼԘࢎϝλϊʔϧ༹ӷΛ༻͍Δ͜ͱ͕๬·͍͠ɻࢧো͕ͳ͚Ε͹Ԙࢎਫ ༹ӷΛ༻͍ͯ΋Α͍ɻ͔͠͠ɼଟ͘ͷణఆͰ୙Γ͕ൃੜ͢Δɻ൓Ԡੜ੒෺ͷೋ૚ԽΛ࠷খԽ ͢ΔͨΊʹɼϝλϊʔϧ 200ʙ250 mL Λ௥Ճ͢Δͷ͕Α͍ɻࠞ߹෺͕ɼे෼͔͘͸ΜͰ͖Ε ͹ɼ‫ݧܦ‬తʹෆ‫ۉ‬Ұੑ͸ɼ݁ՌʹѱӨ‫ڐͣͤڹ‬༰Ͱ͖Δɻ 5.7 ϒϩϞϑΣϊʔϧϒϧʔ༹ӷç ࢦࣔༀణఆ༻ɿ0.04 ˋࢼༀ༻ϒϩϞϑΣϊʔϧϒϧʔφτϦ΢Ϝ Ԙਫӷɻຢ͸ɼ0.04 ˋϒϩϞϑΣϊʔϧϒϧʔΞητϯ༹ӷɻ 5.8 1,2,4-τϦΫϩϩϕϯθϯʢTCBʣç λΠϓ 4A ͷϞϨΩϡϥʔγʔϒͰ୤ਫͨ͠΋ͷʢB ๏ʣɻ 5.9 ϝλϊʔϧç ʢB ๏ʣç 6. ૷ஔç 6.1 ిҐࠩణఆ૷ஔຢ͸ pH ϝʔλç ਖ਼֬ʹ 0.1 mV ຢ͸ͦΕҎ্ͷਫ਼౓ͰଌఆͰ͖ɼରి‫ۃ‬ຢ͸ෳ߹ ΨϥεʵΧϩϝϧి‫ۃ‬ʢ1 mol/L ԘԽϦν΢Ϝͷϝλϊʔϧ༹ӷຢ͸ಉ౳༹ӷͰຬͨ͞Εͨ΋ͷʣ‫ͼٴ‬ 20 mL ༰ྔͷϐετϯϏϡϨοτΛ૷උͨ͠૷ஔɻ 6.2 ஫ࣹ‫ث‬ç 2 mL ‫ ͼٴ‬5 mL Ͱ೪ੑϓϨϙϦϚʔΛଌΔͨΊͷɼগͳ͘ͱ΋ 1 mg ͷҧ͍͕ଌఆͰ͖Δ େ‫ܘޱ‬஫ࣹ‫ث‬ɻ 6.3 ϚάωνοΫελʔϥ 6.4 Խֶ͸͔Γç 0.1 mg ͷਫ਼౓Ͱͻΐ͏ྔͰ͖Δ΋ͷɻ 6.5 Α͏ૉϑϥείç ༰ྔ 500 mL ͷ΋ͷɼ‫ڞ‬ખ෇͖ʢA ๏ʣɻ 6.6 ࡾ֯ϑϥείç ༰ྔ 250 mL ͷ΋ͷɻ޿‫ޱ‬ʢB ๏ʣɻ 6.7 શྔϐϖοτç JIS R 3505 ʹ‫ن‬ఆ͢Δɼ༰ྔ 25 mLʢA ๏ʣ‫ ͼٴ‬20 mLʢB ๏ʣͷ΋ͷɻ 6.8 ϝεϐϖοτç JIS R 3505 ʹ‫ن‬ఆ͢Δɼ༰ྔ 1 mL ͷ΋ͷɻ 6.9 ϝεγϦϯμç JIS R 3505 ʹ‫ن‬ఆ͢Δɼ༰ྔ 250 mLʢA ๏ʣ‫ ͼٴ‬100 mLʢB ๏ʣͷ΋ͷɻ 6.10 ϏʔΧʔç ༰ྔ 500 mL ͷ΋ͷɻ 6.11 ϏϡϨοτç ࢦࣔༀణఆ๏Ͱ༻͍ΔɼJIS R 3505 ʹ‫ن‬ఆ͢Δ༰ྔ 50 mL ͷ΋ͷɻ 7. A ๏ʵτϧΤϯ/δ-n-ϒνϧΞϛϯԘࢎਫ༹ӷç 7.1 ૢ࡞ํ๏ç 7.1.1 શྔϐϖοτʢ6.7ʣΛ༻͍ɼ1 mol/L δ-n-ϒνϧΞϛϯ 25 mL ΛΑ͏ૉϑϥείʢ6.5ʣʹఴՃ ͢Δɻ͍࣍ͰɼτϧΤϯʢ5.2ʣ10 mL Ͱϑϥείน໘Λ͙͢͢ɻ 7.1.2 ద੾ͳ஫ࣹ‫ث‬ʢ6.2ʣΛ༻͍ɼ‫׬‬શʹ༹ղ͍ͯ͠ΔࢼྉΛ 0.1 mg ·Ͱͻΐ͏ྔ͢ΔɻΠιγΞω ʔτ͕݁থԽ͍ͯ͠Δ৔߹ɼ‫ۉ‬Ұʹ༹ղ͢ΔΑ͏ʹ৻ॏʹՃ೤͢Δɻࢼྉ m0 άϥϜΛɼΑ͏ૉϑϥεί தͷδ-n-ϒνϧΞϛϯ༹ӷʹఴՃ͠‫ڞ‬ખΛ͢Δɻ ࢼྉͷ࣭ྔʢm0ʣ͸ɼΠιγΞωʔτͷʢ15ʶ5ʣϛϦ౰ྔ‫ؚ‬༗ͱ͢ΔɻTDI ͷ৔߹ɼ໿ 1.5 gɼMDI ͷ৔߹ɼ໿ 2.5 g ͱͳΔɻ ΠιγΞωʔτ౰ྔ͕ɼະ஌ͳ৔߹ɼద౰ͳࢼྉྔͰ༧උࢼ‫ݧ‬Λߦ͏ɻ 13 K 1556ɿ2006 7.1.3 ‫׬‬શ༹ղ‫ޙ‬ɼࣨԹͰ 15 ෼ؒ൓Ԡͤ͞Δɻ൓ԠʹΑ༹ͬͯӷ͸ɼൃ೤͢ΔɻࣨԹʢߋʹ 5 ෼ʙ10 ෼ʣʹ໭Δ·Ͱ์ஔ͢Δɻ 7.1.4 ϝεγϦϯμʢ6.9ʣΛ༻͍ͯΞητϯʢ5.1ʣ150 mL Λϑϥείน໘ʹ஫ҙͯͦͦ͗͠ɼખΛ͢ Δɻ 7.1.5 ࣍ʹࣔ͢ೋͭͷํ๏͍ͣΕ͔Λ༻͍ͯɼա৒ͷδ-n-ϒνϧΞϛϯΛణఆ͢Δɻ 7.1.5.1 ిҐࠩణఆ๏ʢਪ঑ʣç Α͏ૉϑϥείͷ಺༰෺Λణఆ༻ϏʔΧʔʢ6.10ʣʹҠ͠ɼΞητϯ ʢ5.1ʣ25 mL Ͱ͙͢͢ɻϚάωνοΫελʔϥ্ʹϏʔΧʔΛஔ͖ɼ͔͘͸Μ͢Δɻ ి‫ۃ‬Λ൓Ԡࠞ߹෺ʹਁ͠ɼిҐࠩణఆ૷ஔʢ6.1ʣΛ༻͍ͯɼ1 mol/L Ԙࢎਫ༹ӷͰణఆ͠ɼ౰ྔ఺Λ ଌఆ͢Δɻ 7.1.5.2 ࢦࣔༀణఆ๏ç Α͏ૉϑϥείΛϚάωνοΫελʔϥʹஔ͖ɼ൓Ԡࠞ߹෺Λ͔͘͸Μ͢Δɻ ໨੝෇͖ 1 mL ϐϖοτʢ6.8ʣΛ༻͍ɼϒϩϞϑΣϊʔϧϒϧʔ༹ӷʢ5.7ʣ0.8 mL ΛఴՃ͢Δɻ ϏϡϨοτΛ༻͍ɼ1 mol/L Ԙࢎਫ༹ӷͰణఆ͢Δɻࢦࣔༀ͕੨৭͔Βগͳ͘ͱ΋ 15 ඵؒԫ৭͕҆ఆ ͢Δ·ͰణఆΛߦ͏ɻ༹ӷ͸ɼణఆ։࢝ͷ੨৭͔Β੨Έ͕͔ͬͨ྘৭ͷதؒମ৭ʹɼͦͯ͠ऴ఺ͷԫ৭ ʹมΘΔɻऴ఺ͷ൑அ͸ɼ‫ʹݧܦ‬ΑΔ͕ɼ࠷ॳͷԫ৭͕֬ೝ͞ΕΔ·Ͱ͸ૉૣ͘ణఆͰ͖Δɻ͜ͷม৭ ͸ɼ0.2ʙ0.3 mL Ͱ‫ݱ‬ΕΔɻ 7.1.6 ࢼྉΛআ͍ۭͨࢼ‫ݧ‬ΛಉҰ৚݅Ͱ࣮ࢪ͢Δɻç 7.2 ݁Ռͷදࣔç 7.2.1 ΠιγΞωʔτ‫ؚج‬༗཰ʢ%NCOʣ͸ɼ࣍ͷࣜʹΑͬͯࢉग़͢Δɻç %NCO = 4.202× (V1 −V2 )× c m0 ͜͜ʹɼ V1ɿ V2ɿ cɿ m0ɿ 4.202ɿ ۭࢼ‫ʹݧ‬ཁͨ͠ɼ0.01 mL ·Ͱଌఆͨ͠Ԙࢎͷ࢖༻ྔʢmLʣ ࢼྉͷణఆʹཁͨ͠ɼ0.01 mL ·Ͱଌఆͨ͠Ԙࢎͷ࢖༻ྔ ʢmLʣ Ԙࢎͷೱ౓ʢmol/Lʣ ࢼྉͷ࣭ྔʢgʣ 1 000 mg Λ g ʹɼͦͯ͠ඦ෼཰ʹม‫͢׵‬ΔɼNCO ౰ྔʢ42.02 mg/ϛϦ౰ྔʣͷఆ਺ 7.2.2 Ξϛϯ౰ྔ͸ɼ࣍ͷࣜʹΑͬͯࢉग़͢Δɻ Ξϛϯ౰ྔ = 1 000 × m0 (V1 −V2 )× c 7.2.3 ୯Ұҟੑମຢ͸ҟੑମࠞ߹෺ʢྫ͑͹ʠ७ʡTDI ຢ͸ MDIʣʹΑΔΠιγΞωʔτ͸ɼ७౓ͱ͠ ͯɼ࣍ͷࣜʹΑͬͯ%Ͱࢉग़͢Δɻ 純度 = (V1 −V2 )× c × E 1 000 × m0 ×100 ͜͜ʹɼ V1ɿ ۭࢼ‫ʹݧ‬ཁͨ͠ɼ0.01 mL ·Ͱଌఆͨ͠Ԙࢎͷ࢖༻ྔʢmLʣ V2ɿ ࢼྉͷణఆʹཁͨ͠ɼ0.01 mL ·Ͱଌఆͨ͠Ԙࢎͷ࢖༻ྔ ʢmLʣ cɿ Ԙࢎͷೱ౓ʢmol/Lʣ Eɿ ΠιγΞωʔτͷ౰ྔʢ७ TDI ͸ɼ87.08 mgöϛϦ౰ྔɼ७ MDI ͸ɼ125.13 mgöϛϦ౰ྔʣ m0āç ࢼྉͷ࣭ྔʢgʣ 1 000ɿ g ͔Β mg ΁ͷม‫਺܎׵‬ 14 K 1556ɿ2006 100ɿ ύʔηϯτ΁ͷม‫਺܎׵‬ 7.2.4 ΩϩάϥϜ౰ͨΓͷ౰ྔ਺ʢ౰ྔ/kgʣ͸ɼ࣍ͷࣜʹΑͬͯࢉग़͢Δɻ 当量/kg = (V1 −V2 )× c m0 ͜͜ʹɼ V1ɼV2ɼc ‫ ͼٴ‬m0 ͸ 7.2.3 ʹಉ͡ɻ 7.2.5 ਫ਼੡ΠιγΞωʔτதͰ͸ɼࢎੑෆ७෺͸গྔ͔͠‫·ؚ‬Εͳ͍ͨΊɼఆྔ஋ʹ͸Ө‫͍ͳ͠ڹ‬ɻ͠ ͕ͨͬͯɼࢎ౓ิਖ਼ͷඞཁ͸ͳ͍ɻ 7.3 ਫ਼౓‫ͼٴ‬ภΓç 7.3.1 ਫ਼౓ʢਫ਼੡ TDIʣ(1)ç ݁Ռͷଥ౰ੑΛ൑அ͢ΔͨΊʹɼ࣍ͷࢦඪΛ༻͍Δɻ ஫(1) ‫ࢿૅج‬ྉ͸ɼΞϝϦΧϓϥενοΫ‫ڠ‬ٞձϙϦ΢Ϩλϯ‫ݪ‬ྉ෼ੳҕһձʢPURMACʣͰೖख Մೳɻ a) ‫܁‬ฦ͠ਫ਼౓ʢಉҰਓ෼ੳʣç ಉҰਓɼಉҰ೔ɼಉҰ૷ஔͰͷ 2 ఺ͷଌఆ݁Ռͷ͕ࠩࢦࣔༀణఆ๏ͷ ৔߹ɼ૬ରൺ 0.4 ˋʢ95 ˋ৴པ‫ݶ‬քʣ·ͨ͸ɼిҐࠩࣗಈణఆ๏ͷ৔߹ɼ૬ରൺ 0.2 ˋʢ95 ˋ৴ པ‫ݶ‬քʣΛ௒͑Δ৔߹͸ɼٙΘ͍͜͠ͱΛߟྀ͢΂͖Ͱ͋Δɻ b) ࠶‫ݱ‬ਫ਼౓ʢࢼ‫ؒࣨݧ‬ʣç ಉҰࢼྉͷҟͳͬͨࢼ‫Ͱࣨݧ‬ͷ 2 ఺ͷଌఆ݁Ռͷ͕ࠩ૬ରൺ 0.8 ˋʢ95 ˋ ৴པ‫ݶ‬քʣΛ௒͑Δ৔߹͸ɼٙΘ͍͜͠ͱΛߟྀ͢΂͖Ͱ͋Δɻ 7.3.2 ภΓç ภΓ͸ɼࢼ‫݁ݧ‬Ռͷ‫ظ‬଴஋ͱɼ࠾୒͞Εͨࢀর஋ͱͷࠩͰ͋Δɻ͜ͷࢼ‫ํݧ‬๏ͰͷภΓ͸ɼ ֬ఆ͞Ε͍ͯͳ͍ɻ 7.4 ࢼ‫ݧ‬ใࠂç ࢼ‫ݧ‬ใࠂॻ͸ɼ࣍ͷࣄ߲Λ‫͚ͳ·ؚ‬Ε͹ͳΒͳ͍ɻ a) ͜ͷ‫֨ن‬ͷ൪߸ç b) ࢼྉΛ‫׬‬શʹಛఆ͢ΔͨΊͷඞཁͳࣄ߲ c) ࢖༻ͨ͠ణఆํ๏ʢిҐࠩణఆ๏ຢ͸ࢦࣔༀణఆ๏ʣ d) ࢼ‫݁ݧ‬Ռʢ୯ҐͳͲΛද‫͢ه‬Δʣ e) ͜ͷ‫ʹ֨ن‬͸‫ن‬ఆ͞Ε͍ͯͳ͍͕ɼ݁ՌʹӨ‫͕͋ڹ‬Δ͔΋͠Εͳ͍ิ଍ࣄ߲ຢ͸ৄࡉ f) ࢼ‫ݧ‬೔ç 8. B ๏ʵτϧΤϯ/TCB/δ-n-ϒνϧΞϛϯɾԘࢎϝλϊʔϧ༹ӷ๏ç 8.1 ૢ࡞ํ๏ç 8.1.1 ਫɼΞϧίʔϧ‫ߴͼٴ‬७౓ΞητϯͰ࿈ଓͯ͗͢͢͠ɼ100 ˆͰ‫ס‬૩ɼྫྷ٫ͨ͠޿‫֯ࡾޱ‬ϑϥε ί 250 mLʢ6.6 ࢀরʣʹ TCBʢ5.8 ࢀরʣ25 mL ΛೖΕΔɻ δ-n-ϒνϧΞϛϯ༹ӷʢ5.4 ࢀরʣ20 mL ΛશྔϐϖοτͰɼϑϥείʹҠ͢ɻ಺༰෺Λࠞ߹͢Δͨ Ίʹ͔͘͸Μ͢Δɻ 8.1.2 ඞཁͱ͢ΔࢼྉྔΛ 0.001 g ·Ͱ͸͔ΓͱΔɻඞཁͱ͢Δࢼྉྔ͸ɼ࣍ͷࣜʹΑͬͯ‫ٻ‬ΊΔɻ 試料量 = 84 予想する %NCO TDI ͸໿ 1.8 gɼMDI ͸໿ 2.5 g Ͱ͋Δɻ 8.1.3 ϑϥείΛΧόʔ͠ɼ༹ӷ͕‫ۉ‬ҰʹͳΔ·Ͱ͔͘͸Μ͢Δɻ൓Ԡࠞ߹෺͸ɼ໿ 40 ˆʹԹ·Δɻ 8.1.4 ൓Ԡࠞ߹෺͕ɼࣨԹʹ໭Δ·Ͱ์ஔ͢Δɻͦͷ‫ޙ‬ʢ20ʙ25 ෼ؒʣɼϝλϊʔϧ 100 mL ΛఴՃ͢ Δɻ 15 K 1556ɿ2006 8.1.5 pH 4.0 ෇ۙͷม‫ Ͱ·఺ۂ‬1 mol/L Ԙࢎϝλϊʔϧ༹ӷͰిҐࠩణఆΛ͢Δɻ 8.1.6 ࢼྉΛఴՃ͠ͳ͍ۭࢼ‫ݧ‬Λ͢ΔɻpH 4.0 ෇ۙͷม‫ Ͱ·఺ۂ‬1 mol/L Ԙࢎϝλϊʔϧ༹ӷͰిҐࠩ ణఆΛ͢Δɻ 8.1.7 ిҐࠩణఆ૷ஔ͕ೖखͰ͖ͳ͍ͳΒ͹ɼణఆ͸ैདྷͷϏϡϨοτ 50 mLʢ6.11 ࢀরʣΛ༻͍ϒϩ ϞϑΣϊʔϧϒϧʔࢦࣔༀͰߦ͏ɻ ໨੝Γ෇͖ϐϖοτ 1.0 mLʢ6.8 ࢀরʣΛ༻͍ɼణఆ͢Δ༹֤ӷʹϒϩϞϑΣϊʔϧϒϧʔࢦࣔༀʢ5.7 ࢀরʣ0.8 mL ΛఴՃ͢Δɻ 15 ඵؒɼԫ৭͕҆ఆ͢Δ·Ͱۭࢼ‫ࢼͼٴݧ‬ྉ༹ӷͷణఆΛߦ͏ɻ༹ӷ͸ɼణఆ։࢝ͷ੨৭͔Β੨Έ͕ ͔ͬͨ྘৭ͷதؒ৭ʹɼͦͯ͠ɼऴ఺ͷԫ৭ʹมΘΔɻऴ఺ͷ൑அ͸‫ʹݧܦ‬ΑΔ͕ɼణఆӷͷణԼʹΑ Δ࠷ॳͷԫ৭͕֬ೝ͞ΕΔ·Ͱ͸ૉૣ͘ణఆͰ͖Δɻ͜ͷม৭͸ɼ0.2ʙ0.3 mL Ͱ‫ݱ‬ΕΔɻ 8.2 ࢼ‫݁ݧ‬Ռç 8.2.1 ‫ٻ‬ΊΔ %NCOɼΞϛϯ౰ྔຢ͸ΩϩάϥϜ౰ͨΓͷ౰ྔ͸ɼ7.2 ͷࣜʹΑͬͯࢉग़͢Δɻ 8.2.2 ਫ਼੡ΠιγΞωʔτதͰ͸ɼࢎੑෆ७෺͸গྔ͔͠‫·ؚ‬Εͳ͍ͨΊɼఆྔ஋ʹ͸Ө‫͍ͳ͠ڹ‬ɻ͠ ͔͠ɼૈ੡͋Δ͍͸มੑΠιγΞωʔτ͸͔ͳΓͷྔͷࢎੑԽ߹෺Λ‫ؚ‬Ή͔΋͠Εͳ͍ͷͰɼNCO ‫ؚ‬༗ ཰ͷใࠂ஋͸ࢎ౓ʹ͍ͭͯิਖ਼͢Δඞཁ͕͋Δɻ ΠιγΞωʔτࢼྉͷࢎ౓͸ɼதࢎ౓ʙߴࢎ౓ʢ100 µg/g Ҏ্ʣͷ৔߹ɼA ๏Ͱɼຢ͸௿ࢎ౓ʢ100µg/g ະຬʣͷ৔߹ɼB ๏Λ༻͍‫ٻ‬ΊΔɻࢎ౓͸ɼ%HCl Ͱද‫͢ه‬Δɻ ç ࢎ౓ʹΑΔิਖ਼ %NCO ͸ɼ࣍ͷࣜʹΑͬͯࢉग़͢Δɻ %NCO(酸度補正値) = %NCO(未補正値) −ʢ1.152 × %HClʣ 8.2.3 ͜͜ʹɼ 1.152ɿԘԽਫૉͷ౰ྔͰׂͬͨ NCO ౰ྔ %NCOʢະิਖ਼஋ʣɿ8.2.1 Ͱ‫ٻ‬Ίͨ%NCO ࢎ౓ิਖ਼ͨ͠Ξϛϯ౰ྔ͸ɼ࣍ͷࣜʹΑͬͯࢉग़͢Δɻ 1 アミン当量(酸度補正 = 1 値) アミン当量(未補正値 ) − %NCO 3 650 ͜͜ʹɼ Ξϛϯ౰ྔʢະิਖ਼஋ʣɿ8.2.1 ͷΞϛϯ౰ྔ %NCOɿ8.2.2 ͔Βͷ஋ 3 650ɿԘࢎ౰ྔʷ100 8.3 ਫ਼౓‫ͼٴ‬ภΓ(2) ஫(2) ‫ࢿૅج‬ྉ͸ɼASTM ຊ෦͔ΒೖखՄೳɻRR:D20-104 Λཁ‫͢ٻ‬Δ͜ͱɻ ਫ਼౓ͷ֓ࢉ͸ɼLuprinate M20SʢBASFʣɼPAPI 20 ‫ ͼٴ‬Isonate143LʢDowʣɼMondur PFʢMobayɼ ‫ ݱ‬Bayerʣฒͼʹ Rubinate HF185ʢRubiconʣͷͦΕͧΕͷαϯϓϧʹ͍ͭͯɼ1989 ೥ʹ࣮ ࢪͨ͠ࢼ‫Ͱؒࣨݧ‬ͷ‫ͮ͘جʹڀݚ‬ɻ11 ͔ॴͷࢼ‫͕ࣨݧ‬ɼ‫ࢀʹڀݚ‬Ճɻ 8.3.1 ૈ੡ຢ͸มੑΠιγΞωʔτͷ݁Ռͷଥ౰ੑΛධՁ͢ΔͨΊʹɼ࣍ͷࢦඪΛ༻͍Δɻ 8.3.1.1 ‫܁‬ฦ͠ਫ਼౓ʢಉҰਓ෼ੳʣç ಉҰਓɼಉҰ೔‫ͼٴ‬ಉҰ૷ஔͰͷ 2 ఺ͷଌఆ݁Ռͷ͕ࠩɼ૬ରൺ 0.3 ˋʢ95 ˋ৴པ‫ݶ‬քʣΛ௒͑Δ৔߹͸ɼٙΘ͍͜͠ͱΛߟྀ͢΂͖Ͱ͋Δɻ 8.3.1.2 ࠶‫ݱ‬ਫ਼౓ʢࢼ‫ؒࣨݧ‬ʣç ಉҰࢼྉͷҟͳͬͨࢼ‫Ͱࣨݧ‬ͷ 2 ఺ͷଌఆ݁Ռͷ͕ࠩɼ૬ରൺ 2.07 ˋ ʢ95 ˋ৴པ‫ݶ‬քʣΛ௒͑Δ৔߹͸ɼٙΘ͍͜͠ͱΛߟྀ͢΂͖Ͱ͋Δɻ 8.3.2 MDI ҟੑମͷ݁Ռͷଥ౰ੑΛධՁ͢ΔͨΊʹɼ࣍ͷࢦඪΛ༻͍Δɻ 16 K 1556ɿ2006 8.3.2.1 ‫܁‬ฦ͠ਫ਼౓ç ಉҰਓɼಉҰ೔‫ͼٴ‬ಉҰ૷ஔͰͷ 2 ఺ͷଌఆ݁Ռͷ͕ࠩɼ૬ରൺ 0.11 ˋʢ95 ˋ ৴པ‫ݶ‬քʣΛ௒͑Δ৔߹͸ɼٙΘ͍͜͠ͱΛߟྀ͢΂͖Ͱ͋Δɻ 8.3.2.2 ࠶‫ݱ‬ਫ਼౓ç ࢼ‫ؒࣨݧ‬ͷਫ਼౓͸ܾఆͰ͖ͳ͔ͬͨɻ 8.3.3 TDI ҟੑମͰ͸ɼਫ਼౓ΛධՁ͢Δʹ͸ෆे෼Ͱ͋ͬͨɻTDI ҟੑମͷਫ਼౓͸ MDI ͷͦΕʹྨࣅ ͍ͯ͠ΔͱࢥΘΕΔɻ 8.3.4 ภΓ͸ɼଌఆ݁Ռͷ‫ظ‬଴஋ͱɼ࠾୒͞Εͨࢀর஋ͱͷࠩͰ͋Δɻ͜ͷࢼ‫ํݧ‬๏ͰͷภΓ͸ɼ֬ఆ ͞Ε͍ͯͳ͍ɻ 8.4 ࢼ‫ݧ‬ใࠂç ࢼ‫ݧ‬ใࠂॻʹ͸ɼ࣍ͷࣄ߲Λ‫͚ͳ·ؚ‬Ε͹ͳΒͳ͍ɻ a) ͜ͷ‫֨ن‬ͷ൪߸ç b) ࢼྉΛ‫׬‬શʹಛఆ͢ΔͨΊͷඞཁͳࣄ߲ç c) ࢖༻ͨ͠ణఆํ๏ʢిҐࠩణఆ๏ຢ͸ࢦࣔༀణఆ๏ʣç d) ࢼ‫݁ݧ‬Ռʢ୯ҐͳͲΛද‫͢ه‬Δʣç e) ࢎ౓ิਖ਼ͷ༗ແç f) ͜ͷ‫ʹ֨ن‬͸‫ن‬ఆ͞Ε͍ͯͳ͍͕ɼ݁ՌʹӨ‫͕͋ڹ‬Δ͔΋͠Εͳ͍ิ଍ࣄ߲ຢ͸ৄࡉ g) ࢼ‫ݧ‬೔ 17 K 1556ɿ2006 ෟଐॻ 2ʢࢀߟʣ๕߳଒ΠιγΞωʔτͷࢎ౓ࢼ‫ํݧ‬๏ ংจç ͜ͷෟଐॻ͸ ISO 14898ɿ1999 ͷؔ࿈͢Δ෦෼Λ຋༁͠ɼࢀߟͱͯ͠௥Ճͨ͠΋ͷͰ‫ن‬ఆͷҰ෦Ͱ ͸ͳ͍ɻ·ͨɼଆઢͷ͋Δ෦෼͸ɼ‫ʹ֨نࡍࠃݪ‬͸ͳ͍͕ࢀߟͱͯ͠௥Ճͨ͠ࣄ߲Ͱ͋Δɻ 1. ‫ݪ‬ཧç 1.1 A ๏ç ΠιγΞωʔτࢼྉΛɼա৒ͷϝλϊʔϧͱ൓Ԡ༹ͤ͞ࡎதͰ΢ϨλϯԽ͢Δɻࢎ੒෼͸ɼ ΢ϨλϯԽͷաఔʹ༹͓͍ͯࡎதͰ༡཭͢Δɻ༡཭ͨ͠ࢎ੒෼ΛɼਫࢎԽΧϦ΢Ϝϝλϊʔϧ༹ӷͰిҐ ࠩణఆΛߦ͏ɻࢎ౓͸ɼణఆ݁Ռ͔Β‫ٻͰࢉܭ‬ΊΔɻ 1.2 B ๏ç ΠιγΞωʔτࢼྉΛɼա৒ͷࢎੑ 1-ϓϩύϊʔϧͱ༹ࡎதͰ൓Ԡͤ͞Δɻࢎ੒෼͸ɼ΢Ϩ λϯԽͷաఔʹ༹͓͍ͯࡎதͰ༡཭͢Δɻࢎ੒෼͸ɼਫࢎԽΧϦ΢Ϝϝλϊʔϧ༹ӷͰిҐࠩణఆΛߦ͏ɻ ۭࢼ‫༹༻ݧ‬ӷΛಉ༷ʹͯ͠ௐ߹͢Δɻۭࢼ‫ͱݧ‬ణఆ஋ͱͷ͔ࠩΒΠιγΞωʔτࢼྉͷࢎ౓Λ‫͢ࢉܭ‬Δɻ 2. ࢖༻໨తç ͜ͷ‫ٻ‬Ίํ͸ɼϙϦ΢Ϩλϯ༻ΠιγΞωʔτ‫ͼٴ‬ϓϨϙϦϚʔͷ‫ڀݚ‬ฒͼʹ඼࣭؅ཧΛ ໨తͱ͢ΔධՁʹ࢖༻Ͱ͖Δɻ 3. ๦֐ࣄ߲ç ͜ͷ‫ٻ‬Ίํ͸ɼΞϧίʔϧͱͷॳ‫ظ‬൓ԠͷΑ͏ͳൺֱతԺ࿨ͳ৚݅Ͱ༰қʹ༡཭͢Δࢎ੒ ෼Λଌఆ͢Δ΋ͷͰɼ͜ͷࢎ੒෼͸ओʹԘԽਫૉͰ͋Δɻա౓ͷ൓Ԡ‫ͼٴ‬Ճ೤͸ɼଞͷԘૉ‫ؚ‬༗Խ߹෺ͱ ͷ൓ԠΛ‫͜͠ى‬ɼԘԽਫૉΛ༡཭͢Δ͜ͱ͔Βߴ͍ଌఆ஋ͱͳΔɻԘ‫ج‬ੑ੒෼͸ɼΠιγΞωʔτதʹଘ ࡏ͢Δͱ͸ߟ͑ʹ͍͕͘ɼణఆΛ๦֐͢Δɻࢼༀ‫΁۩ثͼٴ‬ͷ‫ൃۮ‬తͳࢎ੒෼ɼԘ‫ج‬ੑ੒෼ͷࠞೖ͸ణఆ ஈ֊ͷ๦֐ͱͳΔɻ 4. ࢼ‫ݧ‬৚݅ç ΠιγΞωʔτ͸ɼਫ෼ͱ൓Ԡ͢ΔͨΊɼ࣮‫ࣨݧ‬ͷ࣪౓͸௿͘อ࣋͢Δɻ૬ର࣪౓ 50 ˋ ҎԼ͕๬·͍͠ɻ 5. ࢼༀç ͢΂ͯͷ෼ੳʹ͓͍ͯɼࢼༀάϨʔυ඼Λ༻͍Δɻಛʹࢦ͕ࣔͳ͚Ε͹ɼࢼༀ͸ɼISO 6353-1ɼ ISO 6353-2 ‫ ͼٴ‬ISO 6353-3 ͷ‫͏ैʹࡌه‬ɻे෼ʹ७౓ͷߴ͍΋ͷͰɼଌఆͷਫ਼౓ΛଛͳΘͳ͚Ε͹ɼଞͷ άϨʔυ඼Λ༻͍ͯ΋Α͍ɻ ಛʹ‫ن‬ఆ͕ͳ͍‫ݶ‬Γɼ͜ͷ‫֨ن‬ͷਫͱ͸ ISO 3696 ʹΑΔάϨʔυ 2 ͷਫΛࢦ͢ɻ 5.1 ਫࢎԽΧϦ΢Ϝ A ๏༻Ͱɼ0.02 mol/L ͷϝλϊʔϧ༹ӷʢ1.12 g ਫࢎԽΧϦ΢Ϝ/1 000 mL ϝλϊ ʔϧʣͰϑλϧࢎਫૉΧϦ΢ϜͰඪఆͨ͠΋ͷɻ 5.2 ਫࢎԽΧϦ΢Ϝ B ๏༻Ͱɼ0.01 mol/L ͷϝλϊʔϧ༹ӷʢ0.56 g ਫࢎԽΧϦ΢Ϝ/1 000 mL ϝλϊ ʔϧʣͰϑλϧࢎਫૉΧϦ΢ϜͰඪఆͨ͠΋ͷɻ 5.3 τϧΤϯ A ๏ɼB ๏༻ͰɼλΠϓ 4A ͷϞϨΩϡϥʔγʔϒͰ୤ਫͨ͠΋ͷɻ 5.4 1,2,4-τϦΫϩϩϕϯθϯʢTCBʣ A ๏ɼB ๏༻ͰɼλΠϓ 4A ͷϞϨΩϡϥʔγʔϒͰ୤ਫͨ͠ ΋ͷɻ 5.5 ϝλϊʔϧ 5.6 ςτϥώυϩϑϥϯ A ๏ɼB ๏༻ 5.7 ࢎੑ 1-ϓϩύϊʔϧ B ๏༻Ͱɼ120 µL ͷೱԘࢎʹ 1-ϓϩύϊʔϧ 4 L ΛՃ͑ͨ΋ͷɻ 18 K 1556ɿ2006 5.8 Τλϊʔϧ ϝλϊʔϧɼ1-ϓϩύϊʔϧͷ୅ΘΓʹ༻͍ͯ΋Α͍ɻมੑΤλϊʔϧ͸ɼࢼ‫݁ݧ‬Ռ ʹӨ‫͕֬ͱ͍͜ͳ͕ڹ‬ೝ͞ΕΕ͹༻͍ͯ΋Α͍ɻ 6. ૷ஔç 6.1 ిҐࠩణఆ૷ஔ 0.1 mV ຢ͸ͦΕҎ্ͷਫ਼౓Λ΋ͭ΋ͷɻద੾ͳి‫ۃ‬ຢ͸ΨϥεʵΧϩϝϧి‫ۃ‬ͷ ૊߹ͤʢ6.2ɼ6.3 ࢀরʣͰɼϚάωνοΫελʔϥΛඋ͑ͨ΋ͷɻ 6.2 ࢀরి‫ ۃ‬Χϩϝϧి‫ۃ‬ɼμϒϧδϟϯΫγϣϯ‫ͼٴ‬εϦʔϒλΠϓͰɼ྆νϟϯόʔ͸ɼԘԽϦ ν΢ϜΤλϊʔϧ༹ӷͰຬͨ͞Ε͍ͯΔ΋ͷɻ 6.3 ଌఆి‫ ۃ‬Ψϥε pH ి‫ۃ‬ɻ 6.4 ͸͔Γç 1 mg ͷਫ਼౓Ͱͻΐ͏ྔͰ͖Δ΋ͷɻ 6.5 ϚάωνοΫελʔϥ 6.6 ࣗಈ෼஫‫ث‬ຢ͸શྔϐϖοτ JIS R 3505 ʹ‫ن‬ఆ͢Δ 20 mL ‫ ͼٴ‬100 mL ͷ΋ͷɻ 6.7 ϏʔΧç 300 mL ͷ΋ͷɻ 6.8 ϝεγϦϯμʔç JIS R 3505 ʹ‫ن‬ఆ͢Δ 50 mL ‫ ͼٴ‬100 mL ͷ΋ͷɻ 6.9 ͻΐ͏ྔ‫۩ث‬ç ϐϖοτຢ͸ӷମαϯϓϧ 1 mg ·Ͱͷࠩҟ͕෼͔Δద੾ͳ‫۩ث‬ɻ 7. A ๏ʵதࢎ౓ʙߴࢎ౓๕߳଒ΠιγΞωʔτʢ100 µg/g Ҏ্ʣଌఆ๏ç 7.1 ૢ࡞ç 7.1.1 2 ͭͷਗ਼ড়Ͱ‫ס‬૩ͨ͠ 300 mL ϏʔΧʔʹࢼྉ໿ 10 g Λ࠾औ͠ 1 mg ·Ͱͻΐ͏ྔ͢Δɻ 7.1.2 50 mL ͷτϧΤϯΛͦΕͧΕͷϏʔΧʔʹՃ͑ɼϚάωνοΫελʔϥͰɼ͔͘͸Μ͠ͳ͕Β༹͔ ͢ɻ උߟ ࢼྉ͕༰қʹ༹ղ͠ͳ͍৔߹͸ɼTCBʢ5.4 ࢀরʣΛτϧΤϯͷ୅ΘΓʹ༻͍ͯ΋Α͍ɻ͜ͷ ํ๏ΛϓϨϙϦϚʔͰ༻͍Δ৔߹͸ɼ༹ղੑΛߴΊΔͨΊʹτϧΤϯͷ୅ΘΓʹςτϥώυ ϩϑϥϯʢ5.6 ࢀরʣΛ༻͍ͯ΋Α͍ɻਫ਼੡ TDIʢτϧΤϯδΠιγΞωʔτʣͰτϧΤϯ͕ ඞཁͳ͍৔߹͸ɼϝλϊʔϧʢ5.5 ࢀরʣΛՃ͑Δ 7.1.3 ʹਐΜͰ΋Α͍ɻ 7.1.3 ͦΕͧΕͷϏʔΧʔʹϝλϊʔϧʢ5.5 ࢀরʣΛ 100 mL Ճ͑Δʢ5.8 ୅ସՄೳͳ༹ࡎࢀরʣɻ 7.1.4 ࣌‫Ͱࡼܭ‬ϏʔΧʔΛ෴͍ɼϚάωνοΫελʔϥʹΑͬͯ 20 ෼͔ؒ͘͸Μ͢Δɻ 7.1.5 6.1 ͷణఆ૷ஔΛ༻͍ɼͦΕͧΕΛ 0.02 mol/L ਫࢎԽΧϦ΢Ϝ༹ӷͰɼpH ͕ 4ʙ9 ؒͷऴ఺·Ͱణ ఆ͢Δɻ 7.2 ‫ࣜࢉܭ‬ç ࢎ౓͸ɼµgʢHClʣ/g ͱͯ࣍͠ʹࣔࣜ͢Ͱ‫͢ࢉܭ‬Δɻ 酸度[µg(HCl)/g] = ɹV × c × F   m ͜͜ʹɼ Vɿ ࢼྉଌఆʹཁͨ͠ਫࢎԽΧϦ΢Ϝ༹ӷͷ༰ྔʢmLʣ cɿ ਫࢎԽΧϦ΢Ϝ༹ӷͷਖ਼֬ͳೱ౓ʢmol/Lʣ Fɿ 36 455ç ʦ36.455ʢԘԽਫૉͷ෼ࢠྔʣ ʷ1 000ʢmg/g Λ µg/g ΁‫͢ࢉ׵‬ΔϑΝΫλʣʧ mɿ ࢼྉͷ࣭ྔʢgʣ ç 19 K 1556ɿ2006 ࢎ౓͸ɼԘԽਫૉͱͯ͠ͷ%ʢ%HClʣͱͯ࣍͠ʹࣔࣜ͢Ͱ‫ͯ͠ࢉܭ‬΋Α͍ɻ %HCl = ɹ3.6455×V × c   m ͜͜ʹɼ Vɿ ࢼྉଌఆʹཁͨ͠ਫࢎԽΧϦ΢Ϝ༹ӷͷ༰ྔʢmLʣ cɿ ਫࢎԽΧϦ΢Ϝ༹ӷͷਖ਼֬ͳೱ౓ʢmol/Lʣ mɿ ࢼྉͷ࣭ྔʢgʣ 7.3 ਫ਼౓‫ͼٴ‬ภΓç 7.3.1 Ұൠç ݁Ռͷଥ౰ੑΛධՁ͢ΔͨΊʹɼ࣍ͷࢦඪΛ༻͍Δɻ උߟ ਫ਼౓͸ɼถࠃϓϥενοΫձٞͷϙϦ΢Ϩλϯ‫ݪ‬ྉ෼ੳҕһձͷ‫ʹڀݚ‬ΑΓಘΒΕͨσʔλʹ ‫͖ͮج‬ɼASTM E 691 ʹΑͬͯ‫ٻ‬Ίͨɻ‫ڀݚ‬ใࠂॻͷίϐʔ͸ɼSPIʢΞϝϦΧϓϥενοΫ޻ ‫ۀ‬ձʣຊ෦͔ΒೖखͰ͖Δɻ 7.3.2 ‫܁‬ฦ͠ਫ਼౓ʢಉҰਓ෼ੳʣç ಉҰਓɼಉҰ೔ʹΑΔ 2 ఺ͷࢼ‫݁ݧ‬Ռ͕ɼ5 µg/gʢ95 ˋ৴པ‫ݶ‬քʣΛ ௒͑Δ৔߹͸ɼٙΘ͍͜͠ͱΛߟྀ͢΂͖Ͱ͋Δɻ 7.3.3 ࠶‫ݱ‬ਫ਼౓ʢࢼ‫ؒࣨݧ‬ʣç ಉҰࢼྉͷҟͳͬͨࢼ‫Ͱࣨݧ‬ͷ 2 ఺ͷࢼ‫݁ݧ‬Ռͷฏ‫ ͕ۉ‬21 µg/gʢ95 ˋ৴ པ‫ݶ‬քʣΛ௒͑Δ৔߹͸ɼٙΘ͍͜͠ͱΛߟྀ͢΂͖Ͱ͋Δɻ 7.3.4 ภΓç ภΓ͸ɼࢼ‫ݧ‬஋ͷ‫ظ‬଴஋ͱ࠾୒͞Εͨࢀর஋ͱͷࠩͰ͋Δɻ͜ͷࢼ‫ํݧ‬๏ͰͷภΓ͸ɼ֬ఆ ͞Ε͍ͯͳ͍ɻ 7.4 ࢼ‫ݧ‬ใࠂç ࢼ‫ݧ‬ใࠂॻ͸ɼ࣍ͷࣄ߲Λ‫͚ͳ·ؚ‬Ε͹ͳΒͳ͍ɻ a) ͜ͷ‫֨ن‬ͷ൪߸ b) ࢼྉΛ‫׬‬શʹಛఆ͢ΔͨΊͷඞཁͳࣄ߲ c) ࢼ‫ํݧ‬๏ʢA ๏ຢ͸ B ๏ʣ d) ࢼ‫݁ݧ‬Ռç 2 ఺ͷฏ‫ۉ‬஋Λ µg/g Ͱ੔਺Ͱࣔ͢ɻ e) ͜ͷ‫ʹ֨ن‬͸‫ن‬ఆ͞Ε͍ͯͳ͍͕ɼ݁ՌʹӨ‫͕͋ڹ‬Δ͔΋͠Εͳ͍ิ଍ࣄ߲ຢ͸ৄࡉ f) ࢼ‫ݧ‬೔ 8. B ๏ʵ௿ࢎ౓๕߳଒ΠιγΞωʔτʢ100 µg/g ະຬʣଌఆ๏ç 8.1 ૢ࡞ç 8.1.1 ి‫ۃ‬Λ pH 4 ‫ ͼٴ‬pH 7 ͷ؇িਫ༹ӷͰߍਖ਼͢Δɻ 8.1.2 ֤ࢼ‫ݧࢼۭʹͱ͝ݧ‬Λ࣮ࢪ͢Δɻۭࢼ‫ݧ‬ͷௐ߹͸ɼࢼ‫ݧ‬ͷखॱʹ४͡Δɻ͢΂ͯͷࢼ‫ݧࢼۭͼٴݧ‬ ͸ɼ2 ճߦ͏ɻ 8.1.3 ࢼྉ໿ 20 g Λ 1 mg ·Ͱ 300 mL ϏʔΧʹͻΐ͏ྔ͢Δɻ 8.1.4 τϧΤϯ 50 mL ΛՃ͑Δɻ උߟ ࢼྉ͕༰қʹ༹ղ͠ͳ͍৔߹͸ɼTCBʢ5.4 ࢀরʣΛτϧΤϯͷ୅ΘΓʹ༻͍ͯ΋Α͍ɻ͜ͷ ํ๏ΛϓϨϙϦϚʔͰ༻͍Δ৔߹͸ɼ༹ղੑΛߴΊΔͨΊʹτϧΤϯͷ୅ΘΓʹςτϥώυ ϩϑϥϯʢ5.6 ࢀরʣΛ༻͍ͯ΋Α͍ɻਫ਼੡ TDI ͰτϧΤϯ͕ඞཁͳ͍৔߹͸ɼTDI ʹ௚઀ ࢎੑ 1-ϓϩύϊʔϧΛՃ͑Δ 8.1.5 ʹਐΜͰ΋Α͍ɻ 8.1.5 શྔϐϖοτʢ6.6 ࢀরʣͰ 100 mL ͷࢎੑ 1-ϓϩύϊʔϧʢ5.7 ࢀরʣΛՃ͑Δʢ5.8 ͷ୅ସ༹ࡎ ࢀরʣɻ 20 K 1556ɿ2006 8.1.6 ࣌‫Ͱࡼܭ‬ϏʔΧΛ෴͍ɼϚάωνοΫελʔϥʹΑͬͯɼ20 ෼͔ؒ͘͸Μ͢Δɻࢼ‫༹ݧ‬ӷ͸ɼణ ఆ·ͰࣨԹʹอͭɻ 8.1.7 0.01 mol/L ਫࢎԽΧϦ΢Ϝϝλϊʔϧ༹ӷʹΑͬͯɼऴ఺Λ௒͑Δ·ͰిҐࠩణఆΛߦ͏ɻణఆ͸ɼ pH 8 Λ௒͑Δ·Ͱ‫ܧ‬ଓ͢Δɻࢦࣔ஋͕ෆ҆ఆͳ৔߹‫ۃిͼٴ‬ͷԠ౴͕஗͍৔߹͸ɼpH ి‫ۃ‬Λ 2:1 ེࢎɼ঳ ࢎࠞ߹ӷʹ 10 ෼ؒਁ͖ͤ͠ɼଓ͍ͯɼਫʹ 20 ෼ؒਁ͖ͤͨ͠‫ޙ‬ɼΞητϯͰચ͏ɻ 8.1.8 ऴ఺·ͰͷణఆӷྔΛ‫ه‬࿥͢ΔɻೋͭҎ্ͷऴ఺͕֬ೝ͞ΕͨΒɼpH 7 ҎԼͰࢎੑ౓͕ɼ࠷΋ߴ ͍ม‫఺ۂ‬Λ‫ه‬࿥͢Δɻ௨ৗɼม‫఺ۂ‬͸ɼpH 4ʙ5 ؒʹ‫ݱ‬ΕΔɻ 8.2 ‫ࣜࢉܭ‬ç ࢎ౓͸ɼʢµgHCl/g ࢼྉʣͱͯ͠ɼ࣍ͷࣜʹΑͬͯࢉग़͢Δɻ 酸度[µg/g] =  (VS-VB ) × c × F   m ͜͜ʹɼ VSɿ VBɿ cɿ Fɿ mɿ ࢼྉଌఆʹཁͨ͠ਫࢎԽΧϦ΢Ϝ༹ӷͷ༰ྔʢmLʣ ۭࢼ‫ʹݧ‬ཁͨ͠ਫࢎԽΧϦ΢Ϝ༹ӷͷ༰ྔʢmLʣ ਫࢎԽΧϦ΢Ϝ༹ӷͷਖ਼֬ͳೱ౓ʢmol/Lʣ 36 455ç ʦ36.455ʢԘԽਫૉͷ෼ࢠྔʣʧ ç ʷʦ1 000ʢmg/g Λ µg/g ΁‫͢ࢉ׵‬ΔϑΝΫλʣʧ ࢼྉͷ࣭ྔʢgʣ ࢎ౓͸ɼHCl ͱͯ͠ͷ%(%HCl)ͱͯ࣍͠ʹࣔࣜ͢Ͱ‫ͯ͠ࢉܭ‬΋Α͍ɻ %HCl =  3.6455× (VS-VB ) × c   m ͜͜ʹɼ VSɿ VBɿ cɿ mɿ ࢼྉଌఆʹཁͨ͠ਫࢎԽΧϦ΢Ϝ༹ӷͷ༰ྔʢmLʣ ۭࢼ‫ʹݧ‬ཁͨ͠ਫࢎԽΧϦ΢Ϝ༹ӷͷ༰ྔʢmLʣ ਫࢎԽΧϦ΢Ϝ༹ӷͷਖ਼֬ͳೱ౓ʢmol/Lʣ ࢼྉͷ࣭ྔʢgʣ 8.3 ਫ਼౓‫ͼٴ‬ภΓç උߟ ࣍ͷਫ਼౓σʔλ͸ɼ1993 ೥ͷϥ΢ϯυϩϏϯςετ݁Ռʹ‫͖ͮج‬ɼASTM E 691 ʹΑͬͯ‫ٻ‬Ί ͨɻ9 ͔ॴͷࢼ‫ࢀʹڀݚ͕ࣨݧ‬Ճ͍ͯ͠Δɻ ද 1ç ϥ΢ϯυϩϏϯࢎ౓σʔλ ୯Ґç µg/gʢHCl ͱͯ͠ʣ ࢼྉ ฏ‫ۉ‬ ซߦ‫ڐ‬༰ࠩç r ࠶‫ڐݱ‬༰ࠩç R ਫ਼੡ TDIç ࢼྉ A ç ç ç 39.47 ç ç ç 4.03 ç ç ç 11.98 ਫ਼੡ TDIç ࢼྉ B ç ç ç 73.81 ç ç ç 8.79 ç ç ç 21.84 TDI ϙϦΤʔςϧϓϨϙϦϚʔ ç ç ç 23.58 ç ç ç 2.77 ç ç ç 11.20 MDI ϙϦΤʔςϧϓϨϙϦϚʔ ç ç ç 3.37 ç ç ç 2.30 ç ç ç 6.36 มੑ MDI ϗϞϙϦϚʔ ç ç ç 1.12 ç ç ç 4.28 ç ç ç 6.75 ਫ਼੡ MDI ç ç ç 1.07 ç ç ç 2.07 ç ç ç 7.08 21 K 1556ɿ2006 8.3.1 ‫܁‬ฦ͠ਫ਼౓ʢಉҰਓʣç ಉҰਓɼಉҰ૷ஔ‫ͼٴ‬ಉҰ೔ʹΑΔ 2 ఺ͷࢼ‫݁ݧ‬Ռ͕ද 1 ʹࣔ͢ r Λ௒͑ Δ৔߹͸ɼٙΘ͍͜͠ͱΛߟྀ͢΂͖Ͱ͋Δɻ 8.3.2 ࠶‫ݱ‬ਫ਼౓ʢࢼ‫ؒࣨݧ‬ʣç ಉҰࢼྉͷҟͳͬͨࢼ‫Ͱࣨݧ‬ͷ 2 ఺ͷࢼ‫݁ݧ‬Ռͷฏ‫͕ۉ‬ɼද 1 ʹࣔ͢ R Λ௒͑Δ৔߹͸ɼٙΘ͍͜͠ͱΛߟྀ͢΂͖Ͱ͋Δɻ 8.3.3 ภΓç ภΓ͸ɼࢼ‫݁ݧ‬Ռͷ‫ظ‬଴஋ͱɼ࠾୒͞Εͨࢀর஋ͱͷࠩͰ͋Δɻ͜ͷࢼ‫ํݧ‬๏ͰͷภΓ͸ɼ ֬ఆ͞Ε͍ͯͳ͍ɻ 8.4 ࢼ‫ݧ‬ใࠂç 7.4 ʹ४͡Δɻ 22 K 1556ɿ2006 ෟଐॻ 3ʢࢀߟʣՃਫ෼ղੑԘૉͷࢼ‫ํݧ‬๏ ংจç ͜ͷෟଐॻ͸ ISO 15028ɿ2004 ͷؔ࿈͢Δ෦෼Λ຋༁͠ɼࢀߟͱͯ͠௥Ճͨ͠΋ͷͰ‫֨ن‬ͷҰ෦Ͱ ͸ͳ͍ɻ 1. ‫ݪ‬ཧç Ճਫ෼ղੑԘૉ͸ϝλϊʔϧͱ൓Ԡͯ͠ԘԽਫૉΛੜ੒͢Δɻ൓Ԡऴྃ‫ʹޙ‬ɼణఆՄೳͳԘૉ Խ߹෺ྔΛɼ঳ࢎۜඪ४༹ӷͰిҐࠩణఆʹΑΓ‫ٻ‬ΊΔɻ 2. ๦֐ࣄ߲ç νΦγΞϯࢎԘɼγΞϯࢎԘɼེԽ෺ɼϤ΢Խ෺ɼ‫ۜͼٴ‬ΠΦϯͱ൓Ԡ͢Δଞͷ෺࣭ɼฒ ͼʹࢎੑ༹ӷதͰۜΠΦϯΛؐ‫͢ݩ‬Δ෺࣭͕ଌఆΛ๦֐͢Δ͜ͱ͕͋Δɻ 3. ࢼྉͷ࠾औç ༗‫ػ‬ΠιγΞωʔτ͸งғ‫ؾ‬தͷਫ෼ͱ൓Ԡ͢ΔͷͰɼࢼྉͷ࠾औத͸஫ҙΛ෷͏ඞཁ ͕͋Δɻ௨ৗͷࢼྉ࠾औํ๏ʢྫ͑͹ɼΦʔϓϯυϥϜ͔Βͷࢼྉ࠾औʣ͸଎΍͔ʹߦΘΕͯ΋ෆ༹ੑ೘ ૉʹΑΓࢼྉͷԚછΛҾ͖‫͢͜ى‬ɻ͕ͨͬͯ͠ɼৗ࣌ɼ‫ס‬૩ෆ‫׆‬ੑΨεʢྫ͑͹ɼ஠ૉΨεɼΞϧΰϯΨ εຢ͸‫ס‬૩ۭ‫ؾ‬ʣͰࢼྉશମΛ෴͏ɻ ‫ࠂܯ‬ç ༗‫ػ‬ΠιγΞωʔτ͸ɼൽෘΛ௨ͯ͠‫ٵ‬ऩຢ͸ৠ‫ؾ‬Λ‫ٵ‬Ҿ͢Δͱ‫͋Ͱݥة‬Δɻద੾ͳ‫ؾ׵‬Λߦ ͍ɼอ‫ޢ‬खା‫ͼٴ‬อ‫ޢ‬Ί͕ͶΛண༻͢Δɻ 4. ࢼༀç ͢΂ͯͷࢼ‫͍͓ͯʹݧ‬ɼࢼༀάϨʔυ඼Λ༻͍Δɻಛʹࢦ͕ࣔͳ͚Ε͹ɼࢼༀ͸ ISO 6353-2 ͷ ‫͏ैʹࡌه‬ɻे෼ʹ७౓ͷߴ͍΋ͷͰɼଌఆͷਫ਼౓ΛଛͳΘͳ͚Ε͹ɼଞͷάϨʔυ඼Λ༻͍ͯ΋Α͍ɻ ಛʹ‫ن‬ఆ͕ͳ͍͔͗Γɼਫͱ͸ ISO 3696 ʹఆٛ͞Ε͍ͯΔάϨʔυ 2 Λࢦ͢ɻ 4.1 ೱ঳ࢎɼHNO3ɼISO 6353-2 ʹ‫ن‬ఆ͢Δൺॏ͕ 1.42 ͷ΋ͷɻ 4.2 ϝλϊʔϧɼCH3OHɼISO 6353-2 ʹ‫ن‬ఆ͢Δ΋ͷɻ 4.3 0.01mol/L ঳ࢎۜඪ४༹ӷç ඪ४ԘࢎΛ༻͍ͯॏྔଌఆ๏ɼຢ͸ిҐࠩଌఆ๏ʹΑͬͯɼ0.000 5 mol/L ͷࠩ·Ͱ‫ݕ‬ग़Ͱ͖ΔΑ͏ʹඪఆͨ͠΋ͷɻ 5. ૷ஔç 5.1 ణఆ૷ஔɼۜʵԘԽۜి‫ۃ‬Λ΋ͭࣗಈణఆ૷ஔʢਪ঑ʣɼຢ͸ۜʵԘԽۜి‫ ͼٴۃ‬ISO 385 ʹ‫ن‬ఆ͢ Δ 50 mL ϏϡϨοτΛ΋ͭखಈణఆ૷ஔɻ 5.2 શྔϐϖοτç JIS R 3505 ʹ‫ن‬ఆ͢Δ༰ྔ 50 mL ͷ΋ͷɻ 5.3 ϏʔΧʔç ISO 4787 ʹ‫ن‬ఆ͢Δ༰ྔ 400 mL ͷ΋ͷɻ 5.4 ϚάωνοΫελʔϥç ͔͘͸Μ๮Λඋ͑ͨϚάωνοΫελʔϥɼຢ͸ಉ౳ͷ΋ͷɻ 5.5 ͸͔Γç 0.01 g ͷਫ਼౓Ͱͻΐ͏ྔͰ͖Δ΋ͷɻ 6. ૢ࡞ç 6.1 ࢼྉ༰‫͔ث‬ΒɼࢼྉΛ 9ʙ11 gʢՃਫ෼ղੑԘૉ͕ 0.01 ˋະຬͱ༧૝͞ΕΔ৔߹͸ɼࢼྉΛ 18ʙ22 gʣ Λਗ਼ড়Ͱ‫ס‬૩ͨ͠ 400 mL ϏʔΧʔʹ 0.01 g ·Ͱਖ਼͘͠͸͔ΓͱΔɻϝλϊʔϧ 50 mL ΛՃ͑ɼ͔͘͸Μ ͢Δɻ͔͘͸ΜΛଓ͚Δͱɼ൓Ԡ͕࢝·ΓɼϏʔΧʔ͕ஆ͔͘ͳΓɼϏʔΧʔͷଆนʹ݁থ͕ੳग़͢Δ(1)ɻ ϏʔΧʔΛਫͰ൒෼·Ͱຬͨ͠ʢ൓Ԡ෺Λ‫ݻ‬Խͤͣ͞ɼ·ͨɼԘԽਫૉͷϩεΛ࠷খʹ͢ΔͨΊʹɼૉૣ 23 K 1556ɿ2006 ͘ਫΛՃ͑Δɻʣɼ30 ෼ؒԺ΍͔ʹࣽ෸͢Δɻ ஫(1)ç ΠιγΞωʔτͷதʹ͸൓Ԡ͠ʹ͘͘ɼগ͠ஆΊΔඞཁ͕͋Δ΋ͷ͕͋ΔɻҰํɼ൓Ԡ͸͢Δ ͕݁থ͕ੳग़͠ͳ͍΋ͷ΋͋Δɻ 6.2 ਫͰ͔͘͸Μ๮Λ͗͢͢ͳ͕Βऔग़͠ɼϏʔΧʔͷ಺นΛચ͏ɻϏʔΧʔΛණཋதͰ໿ 10ˆʹྫྷ٫ ͠ɼ঳ࢎΛ 10 ణՃ͑ΔɻۜʵԘԽۜి‫ۃ‬ʢ5.1ʣΛ༻͍ɼ0.01 mol/L ঳ࢎۜඪ४༹ӷʢ4.3ʣͰ͔͘͸Μ͠ ͳ͕ΒిҐࠩణఆ͢ΔɻՃਫ෼ղੑԘૉ͕ 0.2 ˋΑΓେ͖͍৔߹͸ɼ0.01 mol/L ঳ࢎۜඪ४༹ӷͷ୅ΘΓ ʹ 0.1 mol/L ঳ࢎ༹ۜӷΛ࢖༻͢Δɻ ౷‫ܭ‬σʔλ͸ 10 ˆྫྷ٫৚݅ͷϥ΢ϯυϩϏϯςετʹ‫͍͍ͯͮج‬Δɻ໿ 20 ˆͷྫྷ٫Ͱे෼Ͱ͋Δͱͷ ใࠂ΋͋Δɻ݁Ռ͕ 10 ˆྫྷ٫ͰಘΒΕͨ݁Ռͱ౷‫ܭ‬తʹ͕ࠩͳ͚Ε͹ɼ20 ˆྫྷ٫Ͱ΋Α͍ɻ 7. ݁Ռͷදࣔç Ճਫ෼ղੑԘૉ͸ɼ࣍ͷࣜʹΑ࣭ͬͯྔ෼཰ʢˋʣͰࢉग़͢Δɻ 加水分解性塩素 ʹɹ3.55 ×V m × c   ͜͜ʹɼ Vɿ cɿ mɿ 3.55ɿ ࢼྉͷణఆʹཁͨ͠঳ࢎ༹ۜӷʢmLʣ ঳ࢎ༹ۜӷͷೱ౓ʢmol/Lʣ ࢼྉͷ࣭ྔʢgʣ Ԙૉͷ‫ྔࢠݪ‬ʢ35.5ʣͱ mg ͔Β g ΁ͷม‫܎׵‬ ਺ʢ1 000ʣɼ‫ͼٴ‬ɼ࣭ྔ෼཰ʢˋʣ΁ͷม‫܎׵‬ ਺ʢ100ʣΛ૊Έ߹Θͤͨ܎਺ɻ 8. ਫ਼౓‫ͼٴ‬ภΓç 8.1 ਫ਼౓ç ਫ਼౓ͷ‫ࡌه‬͸ 3 ͔ॴͷࢼ‫͞ࢪ࣮Ͱࣨݧ‬Εͨ‫ݶ‬ఆ͞Εͨϥ΢ϯυϩϏϯςετʹ‫͍͍ͯͮج‬Δɻ ͕ͨͬͯ͠ɼ͜ͷࢼ‫ํݧ‬๏͸܎૪ͷࡍͷ൑ఆʹ͸࢖༻͢΂͖Ͱ͸ͳ͍ɻಉҰਓɼಉҰ೔ɼಉҰ૷ஔͰͷ 2 ఺ͷଌఆ݁Ռͷ͕ࠩɼ0.001 ͔Β 0.2 ˋͷՃਫ෼ղੑԘૉൣғʹ͓͍ͯɼ0.000 5 ˋΛ௒͑Ε͹ɼͦͷ݁Ռ ͸ٙΘ͍͜͠ͱΛߟྀ͢Δ͜ͱ͕๬·͍͠ɻ ҟͳͬͨࢼ‫Ͱࣨݧ‬ͷଌఆ݁Ռͷ͕ࠩɼ0.003 ˋΛ௒͑Ε͹ɼͦͷ݁Ռ͸ٙΘ͍͜͠ͱΛߟྀ͢Δ͜ͱ͕ ๬·͍͠ɻ 8.2 ภΓç ภΓ͸ɼଌఆ݁Ռͷ‫ظ‬଴஋ͱɼ࠾୒͞Εͨࢀর஋ͱͷࠩͰ͋Δɻ͜ͷࢼ‫ํݧ‬๏ͰͷภΓ͸ɼ ֬ఆ͞Ε͍ͯͳ͍ɻ 9. ࢼ‫ݧ‬ใࠂç ࢼ‫ݧ‬ใࠂʹ͸ɼ࣍ͷࣄ߲Λ‫͚ͳ·ؚ‬Ε͹ͳΒͳ͍ɻ a) ͜ͷ‫֨ن‬൪߸ b) ࢼྉΛ‫׬‬શʹಛఆ͢ΔͨΊͷඞཁͳࣄ߲ c) ࢼ‫݁ݧ‬ՌʢՃਫ෼ղੑԘૉ͸ 0.001 ˋ·Ͱ‫͢ࡌه‬Δɻʣ d) ͜ͷ‫ʹ֨ن‬͸‫ن‬ఆ͞Ε͍ͯͳ͍͕ɼ݁ՌʹӨ‫͕͋ڹ‬Δ͔΋͠Εͳ͍ิ଍ࣄ߲ຢ͸ৄࡉ e) ࢼ‫ݧ‬೔ 24 K 1556ɿ2006 ࢀߟจ‫ݙ‬ ISO 385ɼLaboratory glasswareʵBurettes ISO 4787ɼLaboratory glasswareʵVolumetric glasswareʵMethods for use and testing of capacity ISO 6353-1ɼReagents for chemical analysisʵPart 1ɿGeneral test methods ISO 6353-2ɼReagents for chemical analysisʵPart 2ɿSpecificationsʵFirst series ISO 6353-3ɼReagents for chemical analysisʵPart 3ɿSpecificationsʵSecond series ASTM D 4876ɼStandard Test Method for Polyurethane Raw MaterialsʕDetermination of Acidity of Crude or Modified Isocyanates ASTM D 5629ɼStandard Test Method for Polyurethane Raw MaterialsʕDetermination of Acidity in Low-Acidity Aromatic Isocyanates and Polyurethane Prepolymers ASTM E 691ɼStandard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test method

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