JIS K6910-2007 Testing methods for phenolic resins.pdf

K 6910：2007 （1） 規格，工業標準化法第 14 条準用第 12 条第 1 項規定基，合成樹脂工業協会 (JTPIA)，日本工業連盟(JPIF)及財団法人日本規格協会(JSA)，工業標準原案具日 本工業規格改正申出，日本工業標準調査会審議経，経済産業大臣改正日 本工業規格。 ，JIS K 6910:1999 改正，規格置換。 規格，著作権法保護対象著作物。 規格一部，特許権，出願公開後特許出願，実用新案権又出願公開後実用新案登録出願 抵触可能性注意喚起。経済産業大臣及日本工業標準調査会，特許 権，出願公開後特許出願，実用新案権又出願公開後実用新案登録出願係確認，責任 。 JIS K 6910 ，次示附属書。 附属書（参考）JIS 対応国際規格対比表 免费标准下载网( w w w . f r e e b z . n e t ) 免费标准下载网( w w w . f r e e b z . n e t ) 无需注册, 即可下载 K 6910：2007 目 次 序文···············································································································································································1 1. 適用範囲································································································································································1 2. 引用規格································································································································································1 3. 定義········································································································································································3 4. 試験項目································································································································································3 5. 試験方法································································································································································4 5.1 色相······································································································································································4 5.2 密度······································································································································································6 5.3 粘度······································································································································································6 5.4 pH·········································································································································································8 5.5 混和性··································································································································································8 5.6 不揮発分······························································································································································9 5.7 融点（法）·················································································································11 5.8 軟化点（環球法）·············································································································································12 5.9 残·····························································································································································12 5.10 見掛密度·······················································································································································14 5.11 流···································································································································································14 5.12 含有量（法） ···············································································18 5.13 外観···································································································································································19 5.14 化時間·······················································································································································19 5.15 性物質···················································································································································24 5.16 遊離···············································································································································25 5.17 遊離（塩化法）································································31 5.18 水分（自動容量滴定法） ···························································································32 5.19 電気伝導度·······················································································································································32 5.20 固定炭素分·······················································································································································33 5.21 酸硬化時発熱最高温度及到達時間·······································································································34 5.22 液体分離···········································································································36 5.23 示差走査熱量測定反応熱及反応温度 ···························································································41 附属書（参考）JIS 対応国際規格対比表····························································································44 免费标准下载网( w w w . f r e e b z . n e t ) 免费标准下载网( w w w . f r e e b z . n e t ) 无需注册, 即可下载 著作権法無断複製，転載等禁止。 日本工業規格 JIS K 6910：2007 樹脂試験方法 Testing methods for phenolic resins 序文 規格， 1999年第2版発行ISO 10082， PlasticsPhenolic resinsClassification and test methods 翻訳，技術的内容変更作成日本工業規格。 ，規格側線又点線下線施箇所，原国際規格変更事項。変 更一覧表説明付，附属書（参考）示。 1. 適用範囲 規格，樹脂(1)試験方法規定。 注(1) 樹脂，類，類主剤縮合反応 得熱硬化性樹脂（含。 ）及又他成分含。 備考 規格対応国際規格，次示。 ，対応程度表記号，ISO/IEC Guide 21 基，IDT（一致） ，MOD （修正） ，NEQ（同等）。 ISO 10082:1999，PlasticsPhenolic resinsClassification and test methods (MOD) 2. 引用規格 次掲規格，規格引用，規格規定一部構成 。引用規格，発行年付記，記載年版規格規定構 成，後改正版追補適用。発効年付記引用規格，最 新版（追補含。 ）適用。 JIS K 0061 化学製品密度及比重測定方法 JIS K 0071-2 化学製品色試験方法第 2 部：色数 JIS K 0113 電位差電流電量滴定方法通則 備考 ISO 760:1978 Determination of waterKarl Fischer method (General method)引用事項， 規格該当事項同等。 JIS K 0127 分析通則 JIS K 2425 油，加工及試験方法 JIS K 5601-2-2 塗料成分試験方法第 2 部：溶剤可溶物中成分分析第 2 節：軟化点（環球法） JIS K 6900 用語 備考 ISO 472:1988 PlasticsVocabulary ，規格一致。 JIS K 7112 非発泡密度及比重測定方法 JIS K 7117-1 液状， 乳濁状又分散状樹脂形回転粘度計 見掛粘度測定方法 備考 ISO 2555:1989 PlasticsResins in the liquid state or as emulsions or dispersionsDetermination 免费标准下载网( w w w . f r e e b z . n e t ) 免费标准下载网( w w w . f r e e b z . n e t ) 无需注册, 即可下载 2 K 6910：2007 of apparent viscosity by the Brookfield Test method 引用事項，規格該当事項同 等。 JIS K 7117-2 液状， 乳濁状又分散状樹脂回転粘度計定断速度粘 度測定方法 備考 ISO 3219:1993 PlasticsPolymers/resins in the liquid state or as emulsions or dispersions Determination of viscosity using a rotational viscometer with defined shear rate 引用事項， 規格該当事項同等。 JIS K 7365 規定漏斗注材料見掛密度求方 備考 ISO 60:1977 PlasticsDetermination of apparent density of material that can be poured from a specified funnel ，規格一致。 JIS K 8034 （試薬） JIS K 8101 （99.5） （試薬） JIS K 8129 塩化（）六水和物（試薬） JIS K 8142 塩化鉄（）六水和物（試薬） JIS K 8180 塩酸（試薬） JIS K 8201 塩化（試薬） JIS K 8576 水酸化（試薬） JIS K 8598 （試薬） JIS K 8839 2-（試薬） JIS K 8896 （試薬） JIS K 8891 （試薬） JIS K 8897 （試薬） JIS K 8951 硫酸（試薬） JIS K 8983 硫酸銅（）五水和物（試薬） JIS K 8986 硫酸十水和物（試薬） JIS R 1301 化学分析用磁器 JIS Z 8801-1 試験用第 1 部：金属製網 JIS Z 8802 pH 測定方法 ISO 3146:2000 PlasticsDetermination of melting behaviour (melting temperature or melting range) of semi-crystalline polymers by capillary tube and polarizing-microscope methods ISO 4610:2001 PlasticsVinyl chloride homopolymer and copolymer resinsSieve analysis using air-jet sieve apparatus ISO 8618: 1995 PlasticsLiquid phenolic resinsConventional determination of non-volatile matter ISO 8619:2003 PlasticsPhenolic resin powderDetermination of flow distance on a heated glass plate ISO 8974:2002 PlasticsPhenolic resinsDetermination of residual phenol content by gas chromatography ISO 8975:1989 PlasticsPhenolic resinsDetermination of pH ISO 8987:1995 PlasticsPhenolic resinsDetermination of reactivity on a B-transformation test plate ISO 8988:2006 PlasticsPhenolic resinsDetermination of hexamethylenetetramine contentKjeldahl method, perchloric acid method and hidrochloric acid method ISO 8989:1995 PlasticsLiquid phenolic resinsDetermination of water miscibility 免费标准下载网( w w w . f r e e b z . n e t ) 免费标准下载网( w w w . f r e e b z . n e t ) 无需注册, 即可下载 3 K 6910：2007 ISO 9396:1997 PlasticsPhenolic resinsDetermination of the gel time of resols under specific conditions using automatic apparatus ISO 9771:1995 PlasticsPhenolic resinsDetermination of the pseudo-adiabatic temperature rise of liquid resols when cured under acid conditions ISO 9944:1990 PlasticsPhenolic resinsDetermination of electrical conductivity of resin extracts ISO 11401:1993 PlasticsPhenolic resinsSeparation by liquid chromatography ISO 11402:2004 Phenolic, amino and condensation resinsDetermination of free-formaldehyde content ISO 11409:1993 PlasticsPhenolic resinsDetermination of heats and temperatures of reaction by differential scanning calorimetry ISO 12058-1:1997 PlasticsDetermination of viscosity using a falling-ball viscometerPart 1: Inclined-tube method 3. 定義 規格用主用語定義，JIS K 6900 ，次。 a) 混和性 樹脂水加，発生必要水添加量質量分率表 。 b) 不揮発分 液体樹脂蒸発又乾燥残量質量分率表。 c) 流 試料斜面化流長。 d) 性物質 交換水樹脂中抽出及塩素 。 e) 遊離 樹脂中残存未反応。 f) 遊離 樹脂中残存未反応。 g) 電気伝導度 交換水樹脂中抽出液電気伝導度。 h) 固定炭素量 還元雰囲気，焼成加熱，炭化残留物灰分差引値。 4. 試験項目 試験項目，表 1 。 表 1 樹脂試験方法 試料形態 試験項目 試験箇条 色相 A 法（溶液法） B 法（板法） 5.1.1 5.1.2 密度 A 法（浮法） B 法（比重瓶法） 5.2.1 5.2.2 粘度 A 法（形回転粘度計） B 法（円平板形回転粘度計） C 法（落球粘度計） 5.3.1 5.3.2 5.3.3 pH 5.4 混和性 5.5 液体 不揮発分 5.6 融点（法） 5.7 軟化点（環球法） 5.8 残 A 法（法） B 法（法） 5.9.1 5.9.2 固体 見掛密度 5.10 免费标准下载网( w w w . f r e e b z . n e t ) 免费标准下载网( w w w . f r e e b z . n e t ) 无需注册, 即可下载 4 K 6910：2007 表 1 樹脂試験方法（続） 試料形態 試験項目 試験箇条 流 A 法 B 法 5.11.1 5.11.2 固体 含有量（法） 5.12 外観 5.13 化時間 A 法（付熱板法） B 法（平板法） C 法（自動装置試験管法） D 法（手動試験管法） 5.14.1 5.14.2 5.14.3 5.14.4 性物質 5.15 遊離 5.16 遊離（塩化法） 5.17 水分（自動容量滴定法） 5.18 電気伝導度 5.19 固定炭素分 5.20 液体固体共通 酸硬化時発熱最高温度及到達時間 5.21 5. 試験方法 5.1 色相 5.1.1 色相 A 法（溶液法） 5.1.1.1 試薬標準液 a) 希塩酸 JIS K 8180 規定試薬特級塩酸 1±0.1 部（質量）水 17±0.1 部（質量）溶 。 b) 塩化第二鉄溶液 JIS K 8142 規定試薬特級塩化鉄（）六水和物 5±0.1 部（質量）希塩酸 1.2 ±0.1 部（質量）溶。溶液，硫酸（比重 1.840）100 ml 重酸 3± 0.01 g 溶溶液色調合。 c) 塩化溶液 JIS K 8129 規定試薬特級塩化（）六水和物 1±0.01 部（質量） 希塩酸 3±0.01 部溶。 d) 標準液(2) 表 2 組成溶液調製，JIS K 0071-2 規定試料管詰 密栓。 注(2) 色相標準溶液，安定，常用標準液別，一部冷暗室保管 。少 3 月常用標準液冷暗室保管標準液比較，色変化 確。変化，新調製。 免费标准下载网( w w w . f r e e b z . n e t ) 免费标准下载网( w w w . f r e e b z . n e t ) 无需注册, 即可下载 5 K 6910：2007 表 2 標準液調製表 単位 ml 色数標準液 番号 塩化第二鉄溶液 塩化溶液 希塩酸 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 000.13 000.19 000.29 000.43 000.65 001.00 001.70 002.50 003.80 005.10 007.50 010.80 016.60 022.20 029.40 037.80 051.30 100.00 00.19 00.29 00.43 00.65 00.91 01.30 01.70 02.00 03.00 03.60 05.30 07.60 10.00 13.30 17.60 22.80 25.60 00.00 99.68 99.52 99.28 98.92 98.35 97.70 96.60 95.50 93.20 91.30 87.20 81.60 73.40 64.50 53.00 39.40 23.10 00.00 備考 番号 18 調製方法，規格用。 5.1.1.2 操作 a) 試料管試料(3)入，標準液両者平行並。 注(3) 試料完全透明状態測定。雑物存在濁 ，乾燥紙過試料。 b) 北側自然光線又昼光色，標準液色比較。測定温度 25±5 。 5.1.1.3 報告 a) 規格番号 b) 試料内容 c) 測定結果 d) 測定日 5.1.2 色相 B 法法（比色計法） 5.1.2.1 装置器具 a) 比色計(4) 注(4) 比色計 a) 1 使場合（色数 19）下窓， 2 使場合（色数 918）上 窓読取。 b) 比色計箱裏，光線直角。 c) 自然光見北向望，直射日光避。昼光色測定 ，室中行。 免费标准下载网( w w w . f r e e b z . n e t ) 免费标准下载网( w w w . f r e e b z . n e t ) 无需注册, 即可下载 6 K 6910：2007 5.1.2.2 操作 a) 試料管試料入，比色計。 b) 比色板回転，自然光又昼光色光試料色比色一致窓現数 字読取。，測定温度 25±5 。 5.1.2.3 報告 a) 規格番号 b) 試料内容 c) 測定結果 d) 測定日 5.2 密度 5.2.1 密度 A 法（浮法） 測定，JIS K 0061 行。 5.2.2 密度 B 法（比重瓶法） 測定，JIS K 7112 行。 5.2.3 報告 a) 規格番号 b) 試料内容 c) 測定結果 d) 測定日 5.3 粘度 5.3.1 粘度 A 法（形回転粘度計） 測定，JIS K 7117-1 行。 5.3.2 粘度 B 法（円平板形回転粘度計） 測定，JIS K 7117-2 行。 5.3.3 粘度 C 法（落球粘度計） 詳細，ISO 12058-1:1997 。次，ISO 12058-1:1997 概要示。 5.3.3.1 装置器具 a) 落球粘度計 図 1 参照。装置，3.3×106 1膨張係数，校正酸 作製，液体満傾斜試料管（落球管）表 3 示 11.015.81 mm 直 径 6 種類球。誤差最少，試料管球，付 。表 3 ，各球性状，定数及測定可能粘度範囲示。 免费标准下载网( w w w . f r e e b z . n e t ) 免费标准下载网( w w w . f r e e b z . n e t ) 无需注册, 即可下载 7 K 6910：2007 単位 mm 図 1 落球粘度計 表 3 試料管内径 15.94 mm 落球粘度計用球 球 No. 材質 密度 g/cm3 直径 mm 円形許容範囲 mm 定数 K （近似値） mPas2cm3/g 測定範囲 mPas 1 酸 2.4 15.81±0.01 ±0.000 5 0.007 0.610 2 酸 2.4 15.6±0.05 ±0.000 5 0.09 7130 3 鉄 8.1 15.6±0.05 ±0.001 0.09 30700 4 鉄 8.1 15.2±0.1 ±0.001 0.7 2004 800 5 鉄又鋼 7.18.1 14.0±0.5 ±0.001 7 1 50045 000 6 鋼 7.77.8 11±1 ±0.002 35 7 500 b) 温度計 最少目盛，0.1 小，±0.03 誤差測定。 c) 温度調節器 1080 範囲，±0.05 誤差制御。 5.3.3.2 測定 液体試料管注，球入。試料管上端栓装着。球 気泡付注意。測定温度少 15 分間保持。測定前，液混合目的 一度球試料管中回転。後，球試料管二線間通過時間測定。 5.3.3.3 結果 動粘度，次式算出。 ()tK 21 = ， ：粘度 (mPas) K：装置定数（表 3 参照）mPascm3/(g) 1 ：測定温度球密度 (g/cm3) 2 ：測定温度試験液体密度 (g/cm3) t：試料管二線間球通過要時間 (s) 3 回測定行，3 個測定値平均。 免费标准下载网( w w w . f r e e b z . n e t ) 免费标准下载网( w w w . f r e e b z . n e t ) 无需注册, 即可下载 8 K 6910：2007 5.3.3.4 報告 a) 規格番号 b) 試料内容 c) 測定結果 d) 測定日 5.4 pH 詳細 ISO 8975:1989 。次 ISO 8975:1989 概要示。 5.4.1 試薬標準液 分析，分析用試薬，蒸留水又純水用。標準液，国家標準 標準液（計量標準供給制度基供給 JCSS Japan Calibration Service System 付証明書付）又，標準液場合，一般的市販標準液 用，次。 a) 酸塩標準液 b) 中性酸塩標準液 c) 四酸（砂）標準液 5.4.2 装置器具 JIS Z 8802 規定。 5.4.3 操作 JIS Z 8802 規定操作行。 5.4.4 測定 詳細，ISO 8975:1989 。次 ISO 8975:1989 概要示。 a) 試料溶液調製 受渡当事者間合意場合， 試料水加直接測定。 1) 測定温度 23±0.5 安定試料温度調整。 2) 水試料質量分率 50 試料溶液調製。液 2 層分離場合，水層測定必要十 分量待，分液漏斗分離，水層測定。 b) pH 測定 1) 一度装置調整，電極，測定用容器水洗浄，後，試料溶液洗浄。 2) 試料溶液混，測定用容器（他清潔，乾燥容器用。 ）適量注， 試料溶液温度 23±0.5 後，電極浸。 3) pH 計指示値安定確認，記録。 4) 試料溶液新，操作繰返。 pH 計新指示値前値差 0.