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Polymer characterization and testing 聚合物特征和試驗 Testing and characterization (generally 3 categories) 試驗和特征(通常可分為三類) ? Production lab testing for polymer QA release ? 為發(fā)放聚合物質(zhì)量保證書而進(jìn)行的生產(chǎn)實驗室試驗 – Mfr, solubles, additives, etc, – 熔體流動速率( MFR)、可溶性和添加劑等 ? Nonroutine polymer structure testing ? 非常規(guī)的聚合物結(jié)構(gòu)試驗 – MWD, tacticity, melting behavior, – 分子量分布( MWD)、立構(gòu)規(guī)正度、熔融特性 ? Application testing (how does it perform post processing) ? 應(yīng)用試驗(在后加工過程中表現(xiàn)的特性) – Tensiles, HDT, flex mod, impact, etc, – 拉伸強(qiáng)度、熱變形溫度( HDT)、彎曲模量、抗沖擊強(qiáng)度等 – Testing of molded parts (microscopy, gloss, etc), – 對模塑零件進(jìn)行的試驗(顯微鏡試驗、表面光澤等) Production testing 生產(chǎn)試驗 ? Mfr,熔體流動速率( MFR) ? Additive content,添加劑含量 ? Ethylene content,乙烯含量 ? Hexane extractables,己烷可抽提物 ? Decalin solubles,十氫化萘可溶物 ? Xylene extractables,二甲苯可抽提物 ? Volatiles,揮發(fā)份 ? Yellowness index,黃度指數(shù) ? Pellet size,塑料粒子尺寸 ? Powder particle size distribution,粉體顆粒度分布 ? Powder metals analysis,粉體金屬含量分析 ? Dirt / contamination / pellet appearance test,雜質(zhì)/污染物以及粒子的外觀試驗 ? Filter pressure rise / gel test,過濾器壓力升高/凝膠試驗 Mfr 熔體流動速率 ? ASTM D1238 ? 美國材料實驗協(xié)會- ASTM D1238( 試驗方法的標(biāo)準(zhǔn)) ? Measures viscosity of PP melt (a function of Mw) ? 測量聚丙烯熔體的粘度(是分子量的函數(shù)) ? Samples size from to grams (higher MFR requires more sample because more flows through machine during test) ? 樣品重量 ( MFR較高的樣品,由于在試驗中流經(jīng)測試儀器的流量較大,所以需要更多試樣量) ? Cylindrical chamber filled with resin and piston set in place ? 將被測樹脂填滿圓筒形的測試管,將活塞安放就位 ? After 4 minute preheat, weight placed on piston and piston pushed to calibration mark (6 minutes) ? 預(yù)熱 4分鐘后,將 ,并將活塞推到校準(zhǔn)的標(biāo)記位置( 6分鐘) ? Cut extrudate start timer. At end of time period, cut extrudate ? 切斷熔體的擠出條,按動秒表計時,在定時周期結(jié)束時,再次切斷熔體的擠出條 Mfr continued 熔體流動速率( MFR)(續(xù)) ? Mfr (gms/10 minutes) = weight of extrudate / time interval ? MFR(克/ 10分鐘)= 擠出條的重量/時間間隔 ? Generally an automated process ? 通常是一個自動進(jìn)行的測試過程 ? Customers often have only 1 plastometer。 may not agree with our lab ? 客戶通常只有一臺塑性計,有可能和我們實驗室儀器的型號不同 ? Tinius Olsen MP600 = ? 右圖為 Tinius Olsen MP600 型 ? Multiple extrusions / MFR testing measures additive package effectiveness ? 多次擠出/熔體流動速率測試,測量添加劑配比的有效性 Additive content 添加劑含量 ? Only one “key additive” is measured in the pellet ? 只測定塑料顆粒中 “關(guān)鍵添加劑”的含量 ? The key additive level is used as an indicator of total additive level and other additive levels. ? 根據(jù)各項添加劑的添加比例,用這項關(guān)鍵添加劑的含量來表示總的添加劑含量以及其它添加劑含量 ? Method depends on the additive Masterbatch being correct! ? 本方法取決于添加劑母料混合物的配方比例必須是正確的 ? Some additives are easier to measure with precision than others (typical key additives are phenolics, phosphites, and CaSt or DHT). ? 某些添加劑要比其它添加劑更容易精確測定(常用的關(guān)鍵添加劑有酚醛樹脂、磷酸酯,和硬脂酸鈣或二丁基羥甲苯( DHT)) ? Specific tests used to determine additive level include FTIR and XRF ? 用于測定添加劑含量的特殊試驗方法包括富利埃變換紅外光譜法(FTIR)和 X射線熒光分析法( XRF) FTIR 富利埃變換紅外光譜 ? “ Fourier Transform InfraRed” Spectroscopy ? “富利埃變換紅外 ”光譜 ? Good for Phenolics, Hindered Phenols (Primary stabilizers and UV Stabilizers), and similar molecules ? 適合于酚醛樹脂、受阻酚 (主要的穩(wěn)定劑和紫外光穩(wěn)定劑 )以及類似分子的檢測 ? Common Key additives include Irganox 1010/3114, DGMS, and Tinuvin 622, and Sodium Benzoate ? 常用的關(guān)鍵添加劑包括 Irganox 1010/311 DGMS 以及 Tinuvin 622 和苯甲酸鈉 ? Pellets are pression molded into sheet, which is inserted into machine ? 先將樣品塑料粒子壓制成薄片,然后將樣片插入到檢測儀器中 ? Calibration curve needed to calculate additive level ? 需要用校正曲線來計算添加劑的含量 XRF: XRay Fluorescence Spectrometer XRF: X射線熒光光譜儀 ? Good for additives containing Calcium, Phosphorus, Sodium, Sulfur, Zinc ? 適合于檢測含有鈣、磷、鈉、硫、鋅的添加劑 ? Pellets pressed into plaque and inserted into machine ? 先將試樣塑料粒子壓制成型為樣板,然后將樣板插入檢測儀器 ? Need to have a calibration curve for additive ? 必須先建立一條添加劑含量的校正曲線 A D D IT IV E E L E M E N TC a s t ( S T ) C a l c i u m ( C a )DHT M a g n e s i u m ( M g )U l t r a n o x 6 2 6 ( U L ) P h o s p h o r u s ( P )W e s t o n 6 1 9 (