《濾棒中三乙酸甘油酯施加量均勻性的測(cè)定實(shí)驗(yàn)報(bào)告》

PAGEPAGE2 《濾棒中三乙酸甘油酯施加量均勻性的測(cè)定》實(shí)驗(yàn)報(bào)告《濾棒中三乙酸甘油酯施加量均勻性的測(cè)定》標(biāo)準(zhǔn)項(xiàng)目組2012年9月PAGEI目錄TOC\o"1-1"\h\z\u1立項(xiàng)背景 12實(shí)驗(yàn)方案 23濾棒樣品選擇 54濾棒樣品分切條件的確定 55濾棒中三乙酸甘油酯施加量均勻性的表征方法 326濾棒樣品取樣次數(shù)的確定 337取樣間隔時(shí)間的確定 368重復(fù)性試驗(yàn) 379樣品普查 3910比對(duì)試驗(yàn) 4011結(jié)論 41《濾棒中三乙酸甘油酯施加量均勻性的測(cè)定》技術(shù)報(bào)告1立項(xiàng)背景濾棒是指以過(guò)濾材料為原料，加工卷制而成的具有過(guò)濾性能并有一定長(zhǎng)度的圓形棒。濾棒分切后接裝在卷煙煙支的抽吸端，對(duì)卷煙煙氣中某些物質(zhì)（如焦油、煙堿等）起到過(guò)濾作用，是濾嘴卷煙的一個(gè)組成部分。卷煙濾嘴對(duì)煙氣粒相物有一定的過(guò)濾作用，可部分地濾去煙氣中的某些成分，如焦油、煙堿等，減少煙氣中的有害物質(zhì)，從而緩解吸煙與健康的矛盾。消費(fèi)者接受濾嘴卷煙的另一個(gè)原因是濾嘴避免了煙末粘在嘴唇上所引起的不適感。對(duì)于卷煙企業(yè)，則可以借接裝濾嘴減少單箱煙葉消耗，提高產(chǎn)品質(zhì)量檔次和價(jià)值，從而獲得較大的經(jīng)濟(jì)效益。世界上最早出現(xiàn)的濾嘴卷煙是1931年本森·海格公司生產(chǎn)的以紙為濾嘴的“議會(huì)”(Parliament)牌卷煙。醋酸纖維濾嘴出現(xiàn)于二十世紀(jì)50年代，1951年美國(guó)Brown＆Williamson生產(chǎn)的“總督”（Viceroy）牌卷煙最先使用了以醋酸纖維為濾材的濾嘴。1954年英國(guó)皇家醫(yī)學(xué)會(huì)發(fā)表了“吸煙與健康”報(bào)告以后，世界性吸煙與健康的爭(zhēng)論不斷升級(jí)，加速了濾嘴卷煙的發(fā)展。至1976年濾嘴卷煙已達(dá)世界總產(chǎn)量的40％左右，二十世紀(jì)80年代末，主要生產(chǎn)卷煙國(guó)的濾嘴卷煙平均已達(dá)85％左右。其中日本、英國(guó)為98％，美國(guó)、原聯(lián)邦德國(guó)95％，韓國(guó)、埃及、阿根廷等國(guó)家已達(dá)100％。我國(guó)濾嘴卷煙生產(chǎn)起步較晚，1973年青島卷煙廠(chǎng)生產(chǎn)的“大前門(mén)”牌卷煙最早接裝了紙質(zhì)濾嘴，到二十世紀(jì)80年代初期濾嘴卷煙只占我國(guó)總產(chǎn)量的3％。隨著我國(guó)煙草行業(yè)的崛起，1985年以后濾嘴卷煙急速發(fā)展，1990年上升到50％，1996年末卷煙接嘴率達(dá)到了93%，1998年已達(dá)97.3％，至今無(wú)嘴卷煙的生產(chǎn)已寥寥無(wú)幾。隨著濾棒生產(chǎn)技術(shù)的發(fā)展和卷煙新產(chǎn)品的開(kāi)發(fā)，濾嘴不僅在數(shù)量上滿(mǎn)足了卷煙廠(chǎng)的需要，而且在品種上也開(kāi)始按卷煙的功能和香味，采用多種材料、多種形態(tài)。目前世界上生產(chǎn)的卷煙濾棒主要采用醋酸纖維絲束施加增塑劑成型后用紙卷制而成。在煙用醋酸纖維濾棒的成型工藝中，大多采用三乙酸甘油酯作為增塑劑，以改善濾棒與卷煙的接裝特性，提高濾棒的抗熱塌陷性能。為了達(dá)到足夠的硬度,三乙酸甘油酯的目標(biāo)用量一般為整個(gè)濾棒重量的6%～10%。當(dāng)用量少于6%時(shí)，濾棒硬度達(dá)不到生產(chǎn)要求，大于10%時(shí)，對(duì)濾棒硬度不產(chǎn)生明顯影響，但會(huì)使三乙酸甘油酯向煙支內(nèi)部轉(zhuǎn)移，從而影響卷煙的抽吸質(zhì)量。目前涉及到煙用三乙酸甘油酯的標(biāo)準(zhǔn)主要有《YC/T144-2008煙用三乙酸甘油酯》、《YC/T331-2010醋酸纖維濾棒中三乙酸甘油酯的測(cè)定氣相色譜法》《YC/T420-2011煙用三乙酸甘油酯純度的測(cè)定氣相色譜法》以及CORESTA第59號(hào)推薦方法《DeterminationofTriacetininFilterRodsbyGasChromatographic》。煙草行業(yè)涉及到均勻性測(cè)定的標(biāo)準(zhǔn)主要有《YC/T353-2010卷煙加料均勻性的測(cè)定》、《YC/T366-2010打葉煙葉烤煙質(zhì)量均勻性評(píng)價(jià)》以及《YC/T426-2012煙草混合均勻度的測(cè)定》。“濾棒中三乙酸甘油酯施加量均勻性的測(cè)定”是《YC/Z240-2008煙草及煙草制品標(biāo)準(zhǔn)體系》明確提出的制定標(biāo)準(zhǔn)，濾棒中三乙酸甘油酯施加均勻性的測(cè)定對(duì)于穩(wěn)定煙草制品質(zhì)量有著重要的意義，通過(guò)該標(biāo)準(zhǔn)的制定能夠提高濾棒成型工藝水平，滿(mǎn)足煙草行業(yè)特色工藝加工精細(xì)化的要求。有鑒于此，福建中煙工業(yè)有限責(zé)任公司于2010年10月申報(bào)了《濾棒中三乙酸甘油酯施加量均勻性的測(cè)定》的煙草行業(yè)標(biāo)準(zhǔn)，2011年4月該項(xiàng)目進(jìn)入國(guó)家煙草專(zhuān)賣(mài)局下達(dá)的2011年度煙草行業(yè)標(biāo)準(zhǔn)制修訂項(xiàng)目計(jì)劃（國(guó)煙科[2011]165號(hào)文件）本項(xiàng)目了通過(guò)試驗(yàn)建立了濾棒中三乙酸甘油酯施加量均勻性的測(cè)定方法，并經(jīng)過(guò)福建中煙工業(yè)有限責(zé)任公司、川渝中煙工業(yè)有限責(zé)任公司、紅云紅河煙草（集團(tuán)）有限責(zé)任公司、深圳煙草工業(yè)有限責(zé)任公司等單位的驗(yàn)證，完成了本標(biāo)準(zhǔn)方法的實(shí)驗(yàn)室間比對(duì)實(shí)驗(yàn)。2實(shí)驗(yàn)方案《濾棒中三乙酸甘油酯施加量均勻性的測(cè)定》標(biāo)準(zhǔn)主要適用于濾棒中三乙酸甘油酯均勻性的測(cè)定，本標(biāo)準(zhǔn)的研究?jī)?nèi)容主要包括：（1）濾棒樣品選擇目前卷煙濾棒主要由卷煙企業(yè)成型車(chē)間自行生產(chǎn)，主要的濾棒成型機(jī)有KDF2、KDF4兩種機(jī)型，絲束中三乙酸甘油酯的施加方式主要由噴嘴、刷涂?jī)煞N方式，本標(biāo)準(zhǔn)項(xiàng)目開(kāi)展必須選擇能夠涵蓋上述條件的濾棒樣品。（2）濾棒樣品分切條件的確定將濾棒樣品沿徑向、軸向進(jìn)行分切，其中徑向的分切長(zhǎng)度分別為80、60、40、20、10mm，軸向的分切比例分別為1、1/2、1/4、1/8、1/16，徑向、軸向的分切水平按照L25(52)正交設(shè)計(jì)表進(jìn)行組合。濾棒進(jìn)行軸向、徑向分切后，參照《YC/T331-2010醋酸纖維濾棒中三乙酸甘油酯的測(cè)定氣相色譜法》規(guī)定的方法進(jìn)行檢測(cè)，L25(52)正交設(shè)計(jì)共有25種分切方式，每種分切方式檢測(cè)30個(gè)樣品，為評(píng)定檢測(cè)結(jié)果的準(zhǔn)確性，對(duì)其測(cè)量的不確定度和標(biāo)準(zhǔn)偏差進(jìn)行分析，剔除標(biāo)準(zhǔn)偏差小于不確定度3倍的條件，進(jìn)一步采用一般線(xiàn)性模型中的單因變量多因素方差分析確定合適的濾棒分切條件。（3）濾棒中三乙酸甘油酯施加量均勻性評(píng)價(jià)方法的確定通過(guò)文獻(xiàn)調(diào)研考察現(xiàn)有的國(guó)家標(biāo)準(zhǔn)、行業(yè)標(biāo)準(zhǔn)及地方標(biāo)準(zhǔn)中涉及到均勻性評(píng)價(jià)的方法，確定濾棒中三乙酸甘油酯施加量均勻性的評(píng)價(jià)方法。（4）濾棒樣品取樣量的確定于濾棒成型車(chē)間分別取相同濾棒成型機(jī)臺(tái)生產(chǎn)的同批次的濾棒樣品10、20、30、40、60個(gè)，檢測(cè)其中的三乙酸甘油酯含量后采用統(tǒng)計(jì)分析的單因變量單因素方差分析比較不同取樣量濾棒樣品中三乙酸甘油酯含量的差異性。（5）濾棒樣品取樣間隔時(shí)間的確定于濾棒成型機(jī)濾棒出口處等時(shí)間間隔進(jìn)行取樣，時(shí)間間隔分別為30、60、90、120s，按照確定的取樣量進(jìn)行取樣后檢測(cè)其中三乙酸甘油酯的含量，采用統(tǒng)計(jì)分析中的單因變量單因素方差分析比較不同時(shí)間間隔濾棒樣品中三乙酸甘油酯含量的差異性。（6）不同批次濾棒樣品三乙酸甘油酯施加量均勻性的重復(fù)性檢驗(yàn)于濾棒成型車(chē)間取相同濾棒成型機(jī)臺(tái)生產(chǎn)的相同規(guī)格的不同批次的樣品，檢測(cè)其中的三乙酸甘油酯含量后采用統(tǒng)計(jì)分析中的單因變量單因素方差分析比較不同批次濾棒樣品中三乙酸甘油酯含量的差異性。（7）樣品普查將建立的方法普查福建中煙及其他煙草工業(yè)企業(yè)在產(chǎn)的濾棒產(chǎn)品中三乙酸甘油酯施加量的均勻性，計(jì)算均勻系數(shù)。（8）比對(duì)試驗(yàn)將建立的方法分別于不同的實(shí)驗(yàn)室間開(kāi)展標(biāo)準(zhǔn)方法的比對(duì)試驗(yàn)，以驗(yàn)證方法的可行性。本標(biāo)準(zhǔn)項(xiàng)目開(kāi)展的技術(shù)路線(xiàn)如圖1。確定樣品取樣時(shí)間間隔確定樣品取樣時(shí)間間隔確定施加量均勻性的表征方法方法的重復(fù)性檢驗(yàn)濾棒樣品分切方式確定確定濾棒樣品的取樣量濾棒中三乙酸甘油酯施加量均勻性的測(cè)定樣品選擇樣品普查比對(duì)實(shí)驗(yàn)建立標(biāo)準(zhǔn)圖1技術(shù)路線(xiàn)圖3濾棒樣品選擇卷煙濾棒產(chǎn)品主要由卷煙企業(yè)成型車(chē)間自行生產(chǎn)，主要的濾棒成型機(jī)有KDF2、KDF4兩種機(jī)型，絲束中三乙酸甘油酯的施加方式主要由噴嘴、刷涂?jī)煞N方式，本標(biāo)準(zhǔn)項(xiàng)目開(kāi)展選擇了兩個(gè)廠(chǎng)家、四種規(guī)格的樣品（表1）。表1樣品信息編號(hào)廠(chǎng)家絲束規(guī)格成型紙壓降（mmH2O）機(jī)型施加方式1龍巖煙草工業(yè)有限責(zé)任公司3.0/32000高透成型紙310KDF2刷涂2龍巖煙草工業(yè)有限責(zé)任公司3.0/32000高透成型紙310KDF4噴嘴3龍巖煙草工業(yè)有限責(zé)任公司3.9/31000普通成型紙280KDF2噴嘴4廈門(mén)煙草工業(yè)有限責(zé)任公司3.0/32000普通成型紙420KDF4噴嘴4濾棒樣品分切條件的確定將濾棒樣品沿徑向、軸向進(jìn)行分切，其中徑向的分切長(zhǎng)度分別為80、60、40、20、10mm，軸向的分切比例分別為1、1/2、1/4、1/8、1/16，徑向、軸向的分切水平按照L25(52)正交設(shè)計(jì)表進(jìn)行組合。濾棒進(jìn)行軸向、徑向分切后，參照《YC/T331-2010醋酸纖維濾棒中三乙酸甘油酯的測(cè)定氣相色譜法》規(guī)定的方法進(jìn)行檢測(cè)，L25(52)正交設(shè)計(jì)共有25種分切方式，每種分切方式檢測(cè)30個(gè)樣品，為評(píng)定檢測(cè)結(jié)果的準(zhǔn)確性，對(duì)其測(cè)量的不確定度和標(biāo)準(zhǔn)偏差進(jìn)行分析，剔除標(biāo)準(zhǔn)偏差小于不確定度3倍的條件，進(jìn)一步采用一般線(xiàn)性模型中的單因變量多因素方差分析確定合適的濾棒分切條件。4.1不確定度評(píng)定的原理為評(píng)定檢測(cè)結(jié)果的準(zhǔn)確性，對(duì)其測(cè)量的不確定度進(jìn)行分析。4.1.1不確定度來(lái)源分析影響濾棒中三乙酸甘油酯含量的測(cè)量結(jié)果的各個(gè)不確定度分量可從測(cè)量過(guò)程（圖2）和數(shù)學(xué)模型中分析其來(lái)源，最終的不確定度來(lái)源分析見(jiàn)圖3。開(kāi)始開(kāi)始制樣稱(chēng)重萃取氣相色譜法測(cè)定按公式計(jì)算結(jié)果制備標(biāo)準(zhǔn)溶液結(jié)束樣品質(zhì)量（m）樣品質(zhì)量（m）天平稱(chēng)量允差天平分辨率萃取液體積（v）定量加液器校準(zhǔn)溫度三甘酯純度標(biāo)準(zhǔn)物質(zhì)質(zhì)量天平稱(chēng)量允差天平分辨率儲(chǔ)備液體積定量加液器校準(zhǔn)溫度標(biāo)線(xiàn)擬合儲(chǔ)備液稀釋1mL移液管（m）溫度校準(zhǔn)溫度校準(zhǔn)5mL移液管（m）2mL移液管（m）溫度校準(zhǔn)重復(fù)性三乙酸甘油酯含量濃度測(cè)量（c）圖3濾棒中三乙酸甘油酯含量測(cè)定的不確定度來(lái)源分析圖測(cè)量重復(fù)性與測(cè)量結(jié)果直接相關(guān)的重復(fù)性測(cè)量過(guò)程包括樣品的均勻性、氣相色譜的進(jìn)樣量等，這一分量可由測(cè)量結(jié)果的重復(fù)性表示。4.1.來(lái)源于天平的稱(chēng)量允差、天平的分辨率以及稱(chēng)量時(shí)浮力的影響。4.1.主要有三個(gè)影響因素：(1)定量加液器校準(zhǔn)；（2）測(cè)量時(shí)溫度的變化4.1.濃度測(cè)量不確定度來(lái)源于：（1）標(biāo)準(zhǔn)物質(zhì)質(zhì)量引入的不確定度分量；（2）標(biāo)準(zhǔn)儲(chǔ)備液體積引入的不確定度分量，包括定量加液器校準(zhǔn)引入的不確定度分量和溫度引入的不確定度分量；（3）標(biāo)準(zhǔn)物質(zhì)純度引入的不確定度分量；（4）標(biāo)準(zhǔn)儲(chǔ)備液稀釋引入的不確定度分量，包括：定量加液器校準(zhǔn)引入的不確定度分量、定容體積溫度引入的不確定度分量、分度吸量管引入的不確定度分量、移出液體溫度引入的不確定度分量和工作曲線(xiàn)擬合引入的不確定度分量。.2.1測(cè)量結(jié)果重復(fù)性引入的的相對(duì)標(biāo)準(zhǔn)不確定度EMBEDEquation.DSMT4將處理好的試樣連續(xù)進(jìn)樣7次，每次進(jìn)樣1μL，進(jìn)行平行測(cè)量，測(cè)量重復(fù)性引入的標(biāo)準(zhǔn)不確定去由7次測(cè)量結(jié)果的平均值的標(biāo)準(zhǔn)差表示，：重復(fù)性測(cè)量的標(biāo)準(zhǔn)差相對(duì)標(biāo)準(zhǔn)不確定度：測(cè)量結(jié)果的平均值樣品質(zhì)量m引入的相對(duì)標(biāo)準(zhǔn)不確定度EMBEDEquation.DSMT44.1.天平計(jì)量檢定證書(shū)標(biāo)明其稱(chēng)量的最大允差為0.5mg，假定為矩形分布，換算為標(biāo)準(zhǔn)不確定度為：樣品凈重為兩次稱(chēng)量所得，每一次稱(chēng)重均為獨(dú)立觀(guān)測(cè)結(jié)果，故計(jì)算兩次.2由天平的檢定證書(shū)可知其分辨率為0.1mg，假定為矩形分布，換算成標(biāo)準(zhǔn)不確定度為：樣品凈重為兩次稱(chēng)量操作所得，每一次稱(chēng)重均為獨(dú)立觀(guān)察結(jié)果，故計(jì)算兩次：4.1.2由于樣品稱(chēng)量時(shí)均是按常規(guī)在空氣中進(jìn)行的，因此不考慮浮力修正，故該項(xiàng)不確定度在此忽略不計(jì)。4.1.2稱(chēng)量樣品的質(zhì)量為m，相對(duì)不確定度為：萃取液體積測(cè)量引入的相對(duì)不確定度分量EMBEDEquation.DSMT4.1定量加液器校準(zhǔn)引入的標(biāo)準(zhǔn)不確定度分量EMBEDEquation.DSMT4由自校獲取，定量加液器在20℃條件下，定量加入20mL乙醇，乙醇的體積為（20±.2溫度波動(dòng)引入的標(biāo)準(zhǔn)不確定度分量EMBEDEquation.DSMT4定量加液器在20℃校準(zhǔn)、實(shí)驗(yàn)室溫度在20±5℃之間變動(dòng)，乙醇的體積膨脹系數(shù)為0.00109mL/.3將上述與萃取液體積v相關(guān)的分量合成，即得到樣品萃取液體積為20mL，萃取液體積引入的相對(duì)不確定度為：萃取液體積為20mL，萃取液體積引入的相對(duì)不確定度為：樣品濃度測(cè)量引入的相對(duì)不確定度分量EMBEDEquation.DSMT4.1標(biāo)準(zhǔn)物質(zhì)質(zhì)量引入的不確定度分量EMBEDEquation.DSMT4計(jì)量檢定證書(shū)給出天平稱(chēng)量質(zhì)量在（0～5×104mg）時(shí)最大允差0.5mg，分辨率為0.1mg，按矩形分布及標(biāo)準(zhǔn)物質(zhì)的稱(chēng)量質(zhì)量m1估計(jì)，則：.2稱(chēng)取三乙酸甘油酯標(biāo)準(zhǔn)物質(zhì)后，在50mL容量瓶中定容。計(jì)量檢定證書(shū)給出50mL容量瓶的最大允差0.05mL，按三角形分布估計(jì)，則50mL容量瓶校準(zhǔn)引入的相對(duì)不確定度為：溫度波動(dòng)引入的標(biāo)準(zhǔn)不確定度：容量瓶在20℃校準(zhǔn)、實(shí)驗(yàn)室溫度在20±5℃之間變動(dòng)，乙醇的體積膨脹系數(shù)為0.00109mL/合成標(biāo)準(zhǔn)儲(chǔ)備液體積引入的不確定度分量，.3三乙酸甘油酯純度引入的相對(duì)不確定度分量EMBEDEquation.DSMT4三乙酸甘油酯的純度（99.80±0.12）%，按均勻分布估計(jì)，則.4標(biāo)準(zhǔn)儲(chǔ)備液稀釋引入的不確定度分量EMBEDEquation.3由于標(biāo)準(zhǔn)儲(chǔ)備液及萃取液中加入內(nèi)標(biāo)，所以標(biāo)準(zhǔn)儲(chǔ)備液稀釋引入的不確定度分量主要受分度吸量管校準(zhǔn)和移出液體溫度影響，而與定量加液器的體積無(wú)關(guān)。（1）分度吸量管校準(zhǔn)引入的不確定度分量EMBEDEquation.DSMT4計(jì)量檢定證書(shū)給出1mL分度吸量管的最大允差0.008mL，2mL分度吸量管的最大允差0.012mL，按三角形分布估計(jì)按三角形分布估計(jì)則1mL分度吸量管2mL分度吸量管（2）分度吸量管移出液體溫度引入的不確定度分量分度吸量管在20℃校準(zhǔn)，實(shí)驗(yàn)室溫度在20±5℃之間變動(dòng)，乙醇體積膨脹系數(shù)為0.00109mL/（3）工作標(biāo)準(zhǔn)溶液配制過(guò)程引入的相對(duì)不確定定分量工作標(biāo)準(zhǔn)溶液配制過(guò)程是分別移取0.1、0.2、0.4、0.8、1.2、1.6、2.0mL的儲(chǔ)備液后，采用定量加液器加入20mL的萃取液,用到1mL分度吸量管4次，2mL分度吸量管3次。.5工作曲線(xiàn)擬合引入的不確定度分量EMBEDEquation.DSMT4三乙酸甘油酯的工作曲線(xiàn)采用最小二乘法擬合，則式中—校準(zhǔn)曲線(xiàn)的標(biāo)準(zhǔn)差—樣品溶液的測(cè)定次數(shù)；—標(biāo)準(zhǔn)溶液的測(cè)定總次數(shù)；—標(biāo)準(zhǔn)曲線(xiàn)的斜率；—標(biāo)準(zhǔn)曲線(xiàn)的截距；—由校準(zhǔn)曲線(xiàn)方程求得的樣品溶液中三乙酸甘油酯的濃度；—不同校準(zhǔn)標(biāo)準(zhǔn)溶液中三乙酸甘油酯的濃度的平均值；—不同校準(zhǔn)標(biāo)準(zhǔn)溶液的濃度配制值；—標(biāo)準(zhǔn)溶液的測(cè)定值—單次標(biāo)準(zhǔn)溶液峰面積的測(cè)定值.6合成樣品濃度測(cè)量引入的相對(duì)不確定度分量EMBEDEquation.DSMT4合成不確定度將各不確定度分量進(jìn)行合成樣品中三乙酸甘油酯含量的測(cè)定結(jié)果為x，因此4.2濾棒樣品分切后三乙酸甘油酯含量的檢測(cè)及分析將兩個(gè)廠(chǎng)家的四種規(guī)格的濾棒樣品（表1）沿徑向、軸向進(jìn)行分切后，參照《YC/T331-2010醋酸纖維濾棒中三乙酸甘油酯的測(cè)定氣相色譜法》規(guī)定的方法進(jìn)行檢測(cè)，對(duì)其測(cè)量的不確定度和標(biāo)準(zhǔn)偏差進(jìn)行分析，剔除標(biāo)準(zhǔn)偏差小于不確定度3倍的條件，進(jìn)一步采用一般線(xiàn)性模型中的單因變量多因素方差分析確定合適的濾棒分切條件。4.2.11＃樣品分析1＃樣品取自龍巖煙草工業(yè)有限責(zé)任公司濾棒成型車(chē)間，成型機(jī)型為KDF2，三乙酸甘油酯的施加方式為刷涂（表1），將1#樣品沿徑向、軸向進(jìn)行分切，徑向、軸向的分切水平按照L25(52)正交設(shè)計(jì)表進(jìn)行組合，L25(52)正交設(shè)計(jì)共有25種分切方式，每種分切方式檢測(cè)30個(gè)樣品（表2）。，，表21#濾棒樣品分切后三乙酸甘油酯的含量軸向分切比例11/21/41/81/1611/21/41/81/1611/21/41/81/1611/21/41/81/1611/21/41/81/16徑向分切長(zhǎng)度（mm）808080808060606060604040404040202020202010101010107.346.237.128.717.686.938.326.518.988.797.238.648.438.554.357.607.676.265.957.907.985.918.324.888.527.388.607.426.926.947.517.157.396.847.697.076.818.878.795.057.477.038.806.577.498.087.085.485.437.047.627.018.026.168.267.197.627.277.857.847.007.366.786.635.336.746.715.916.968.487.447.106.315.029.667.557.576.466.968.147.298.425.949.308.147.327.676.965.244.157.388.307.428.018.957.847.077.055.257.657.078.268.366.698.066.948.626.898.367.347.577.189.025.154.757.397.697.077.238.227.647.996.674.697.187.266.586.175.818.067.147.859.786.255.677.188.646.448.207.167.117.276.658.066.777.616.689.235.128.697.246.878.287.937.677.056.277.229.059.437.537.196.557.984.887.397.057.117.467.128.157.506.905.507.507.107.396.796.327.757.286.857.207.856.627.507.758.068.524.977.156.388.465.627.767.896.626.325.115.737.236.196.578.679.017.008.088.928.309.787.168.298.965.254.467.467.267.746.156.737.588.197.425.356.816.986.758.639.128.617.077.856.506.379.327.737.597.076.525.547.017.605.826.127.517.486.777.325.0810.017.308.538.017.308.967.127.127.128.188.626.938.686.356.924.947.218.487.649.056.517.486.626.816.026.107.267.537.318.138.366.657.526.498.747.207.117.768.088.335.637.286.626.879.345.907.887.566.295.648.887.397.418.776.948.517.228.198.157.715.847.596.078.787.455.517.176.748.208.425.267.647.858.305.509.537.488.197.457.718.677.738.636.046.687.716.938.497.427.824.746.798.557.259.005.947.276.068.314.979.017.156.787.925.745.747.106.647.586.007.647.286.566.378.984.607.537.425.226.565.787.626.436.555.359.117.167.997.407.567.127.147.208.587.977.957.547.197.989.275.007.218.277.818.846.628.007.187.195.037.607.077.228.876.418.077.248.166.206.108.037.497.997.596.155.727.087.165.204.977.827.107.295.534.909.036.937.806.178.397.506.848.167.248.787.097.008.147.126.155.797.057.887.505.438.357.766.868.245.337.927.247.448.627.238.987.198.466.285.426.857.267.735.717.305.667.617.116.998.917.617.697.418.625.457.087.138.257.998.628.937.277.378.516.377.077.516.618.325.955.527.556.867.457.826.917.456.447.555.065.967.468.247.068.458.227.178.577.427.035.037.586.925.888.245.717.136.676.609.038.317.706.906.545.015.657.086.587.189.007.797.036.598.526.235.997.197.6110.118.225.137.838.036.806.718.347.747.295.514.638.967.376.825.726.958.117.108.756.086.315.397.437.566.727.976.066.586.407.307.997.727.756.577.155.388.037.488.007.966.358.546.918.596.117.865.087.467.737.846.655.298.008.038.157.056.817.838.245.395.338.237.147.237.508.966.577.057.198.468.957.827.206.937.597.715.187.046.947.066.006.347.636.485.766.387.747.368.438.406.507.417.176.147.385.999.407.348.429.426.384.557.318.125.626.245.617.687.316.285.786.247.258.388.067.087.617.118.825.956.718.247.296.968.328.355.157.187.617.296.127.597.607.366.895.949.287.077.216.418.418.517.377.948.268.738.187.187.916.229.694.837.667.526.867.027.367.547.038.515.138.157.078.308.247.566.277.187.087.366.789.197.518.158.627.434.777.317.048.255.297.587.496.926.615.307.126.977.457.436.046.497.047.958.176.114.537.086.787.934.614.357.408.268.035.849.537.398.036.565.747.17PAGE PAGE14表31#濾棒樣品分切后三乙酸甘油酯含量分析軸向分切比例徑向分切長(zhǎng)度mm）標(biāo)準(zhǔn)偏差不確定度標(biāo)準(zhǔn)偏差/不確定度正態(tài)檢驗(yàn)（Shapiro-Wilk）檢驗(yàn)統(tǒng)計(jì)量P1800.1800.1131.593//1/2800.7130.1136.3320.9490.1611/4800.8510.1167.3350.9610.3281/8801.0340.1228.5020.9470.1401/16800.8450.1864.5310.9350.0681600.2000.1131.770//1/2600.7710.1136.8220.9440.1151/4601.0120.1188.5700.9430.1081/8601.1630.1826.3850.9210.0291/16601.4270.1867.6780.9600.3071400.2200.1121.970//1/2400.6900.1235.5940.9710.5761/4401.1190.1229.1740.9780.7751/8401.3260.1807.3660.9650.4151/16400.6170.2632.346//1200.3100.1162.668//1/2200.6370.1225.2440.9590.3001/4200.9220.1825.0700.9690.5061/8201.2940.2335.5660.9440.1141/16201.0290.7291.412//1100.2330.1251.864//1/2100.5970.1723.4640.9780.7571/4101.0320.2264.5660.9520.1941/8100.3930.3691.064//1/16101.2240.6801.799//L25(52)正交設(shè)計(jì)共有25種分切方式，評(píng)定了每種分切方式的不確定度，分析了每種分切方式檢測(cè)的30個(gè)樣品的標(biāo)準(zhǔn)偏差，結(jié)果表明濾棒樣品分切后體積（質(zhì)量）大的樣品其標(biāo)準(zhǔn)偏差較小，標(biāo)準(zhǔn)偏差與不確定度的比值較小，進(jìn)一步說(shuō)明不確定度對(duì)樣品中三乙酸甘油酯含量的檢測(cè)影響較大，剔除了標(biāo)準(zhǔn)偏差小于不確定度3倍的9種分切方式，保留了標(biāo)準(zhǔn)偏差大于不確定度3倍的16種分切方式（表3）。正態(tài)檢驗(yàn)（Shapiro-Wilk）結(jié)果表明：保留分切方式樣品中三乙酸甘油酯的含量分布滿(mǎn)足正態(tài)分布（p>0.05）(表3)。Levene方差齊性檢驗(yàn)結(jié)果表明：1#樣品保留分切方式檢測(cè)結(jié)果的方差不具備齊性（p<0.05）（表4）。表41#樣品保留分切方式檢測(cè)結(jié)果的方差齊性檢驗(yàn)檢驗(yàn)方法檢驗(yàn)統(tǒng)計(jì)量P差異顯著性L(fǎng)evene檢驗(yàn)5.0140.000顯著表51#樣品保留分切方式檢測(cè)結(jié)果的方差分析變異來(lái)源III型方差SS自由度均方MS統(tǒng)計(jì)量FP值校正的模型27.362151.8241.8400.027截距23264.578123264.57823467.0420.000軸向分切比例5.13631.7121.7270.161徑向分切長(zhǎng)度15.65343.9133.9470.004軸向分切比例*徑向分切長(zhǎng)度5.15580.6440.6500.736誤差459.9974640.991合計(jì)26844.635480校正的合計(jì)487.359479進(jìn)一步采用一般線(xiàn)性模型中的單因變量多因素方差分析確定合適的濾棒分切條件，由于樣品的方差不齊，在多重比較時(shí)選擇方差不具有齊性的“Tamhane’sT2”法進(jìn)行比較。方差分析的結(jié)果表明：1#樣品在軸向分切比例水平上不存在差異性（p>0.05），在徑向分切長(zhǎng)度的不同水平上存在差異（p<0.05）（表5）。進(jìn)一步的“Tamhane’sT2”法多重比較結(jié)果表明：在軸向1/2、1/4、1/8、1/16的分切比例的檢測(cè)結(jié)果不存在差異（p>0.05），徑向分切長(zhǎng)度80、60、40、20mm間的檢測(cè)結(jié)果不存在差異（p>0.05），徑向分切長(zhǎng)度80、60、40mm的檢測(cè)結(jié)果與10mm的檢測(cè)結(jié)果存在差異（p<0.05），徑向分切長(zhǎng)度20、10mm檢測(cè)結(jié)果間不存在差異（p>0.05）（表6、表7）。表61#樣品保留分切方式中軸向分切比例間的多重比較軸向分切比例軸向分切比例均值差值標(biāo)準(zhǔn)誤差P1/21/40.1450.1010.6261/80.1450.1240.8101/16-0.2000.1630.7821/41/2-0.1450.1010.6261/80.0000.1371.0001/16-0.3450.1740.2631/81/2-0.1450.1240.8101/40.0000.1371.0001/16-0.3460.1880.3471/161/20.2000.1630.7821/40.3450.1740.2631/80.3460.1880.347表71#樣品保留分切方式中徑向分切長(zhǎng)度間的多重比較徑向分切長(zhǎng)度(mm)徑向分切長(zhǎng)度(mm)均值差值標(biāo)準(zhǔn)誤差p1020-0.1810.1500.92840-0.4860.1570.02360-0.4360.1490.03880-0.5500.1340.00120100.1810.1500.92840-0.3050.1540.39260-0.2550.1460.57180-0.3700.1310.05340100.4860.1570.023200.3050.1540.392600.0500.1521.00080-0.0640.1391.00060100.4360.1490.038200.2550.1460.57140-0.0500.1521.00080-0.1140.1300.99180100.5500.1340.001200.3700.1310.053400.0640.1391.000600.1140.1300.9914.2.22＃樣品分析2＃樣品取自龍巖煙草工業(yè)有限責(zé)任公司濾棒成型車(chē)間，成型機(jī)型為KDF4，三乙酸甘油酯的施加方式為噴嘴（表1），將1#樣品沿徑向、軸向進(jìn)行分切，徑向、軸向的分切水平按照L25(52)正交設(shè)計(jì)表進(jìn)行組合，L25(52)正交設(shè)計(jì)共有25種分切方式，每種分切方式檢測(cè)30個(gè)樣品（表8）。表92#濾棒樣品分切后三乙酸甘油酯含量分析軸向分切比例徑向分切長(zhǎng)度mm）標(biāo)準(zhǔn)偏差不確定度標(biāo)準(zhǔn)偏差/不確定度正態(tài)檢驗(yàn)（Shapiro-Wilk）檢驗(yàn)統(tǒng)計(jì)量P1800.2090.0852.459//1/2800.2980.0873.4250.9790.8001/4800.4670.0935.0220.9920.9981/8800.5020.1104.5640.9820.8721/16800.4420.1303.4000.9750.6811600.2460.0793.1140.9450.1281/2600.2970.0893.3370.9740.6441/4600.2730.0903.0330.9500.1691/8600.4800.1114.3240.9580.2711/16600.5120.1643.1220.9620.3391400.2680.0803.3500.9670.4601/2400.2330.0713.2820.9710.5701/4400.4470.0934.8060.9630.3641/8400.4690.1553.0260.9770.7521/16400.4050.1772.288//1200.2450.0813.0250.9560.2511/2200.3630.0904.0330.9450.1281/4200.3440.1073.2150.9840.9261/8200.4270.1772.412//1/16200.4150.3131.326//1100.3890.1033.7770.9630.3751/2100.3860.1033.7480.9830.9071/4100.4230.1353.1330.9790.8101/8100.5390.3361.604//1/16100.4380.6620.662//軸向分切比例11/21/41/81/1611/21/41/81/1611/21/41/81/1611/21/41/81/1611/21/41/81/16徑向分切長(zhǎng)度（mm）808080808060606060604040404040202020202010101010105.485.654.866.185.975.186.495.725.086.655.695.775.175.635.615.466.105.954.375.536.235.795.486.195.616.465.464.795.665.525.016.625.585.565.825.165.934.725.216.515.184.956.036.125.745.545.676.755.744.856.155.365.146.535.585.795.215.655.184.924.985.535.474.435.496.406.225.355.315.805.524.645.845.285.895.374.705.415.535.785.005.485.785.464.835.054.706.805.425.855.676.215.095.325.625.875.056.006.045.865.755.515.175.456.224.845.155.306.796.475.345.515.116.045.685.096.305.335.375.644.774.654.985.514.555.375.526.255.365.524.495.065.435.406.045.936.035.465.465.715.185.845.556.004.746.085.095.395.914.855.875.125.714.605.875.065.515.475.186.555.784.315.375.166.045.205.035.195.385.565.174.855.535.505.264.826.145.874.185.485.206.475.475.745.675.935.495.405.125.525.766.396.315.175.475.075.334.535.144.546.215.675.545.755.835.165.375.825.714.975.305.175.635.475.875.255.575.345.384.885.885.755.145.355.226.315.255.325.566.075.535.065.705.495.665.305.755.865.636.024.935.285.875.575.145.416.045.056.285.236.905.425.056.025.925.015.435.615.584.885.425.775.955.755.164.985.535.505.065.975.355.765.325.235.396.265.385.895.836.065.735.225.875.655.585.535.685.386.015.225.875.535.665.295.254.756.535.834.955.866.945.365.5014.905.375.565.576.025.285.895.425.346.185.325.755.405.755.435.515.304.835.736.515.595.795.115.315.455.555.405.514.406.385.535.675.295.835.485.115.475.285.405.125.684.475.066.096.855.405.496.015.815.565.225.535.384.605.065.465.265.734.955.274.915.795.985.635.775.574.795.215.966.645.945.726.345.405.455.525.785.675.074.865.756.026.124.985.305.345.694.755.474.915.794.745.084.706.095.445.945.506.445.235.665.425.296.066.435.305.635.295.575.125.525.744.755.365.195.505.225.575.306.205.594.9005.495.626.035.186.015.536.056.435.105.465.045.394.786.546.535.905.445.515.726.075.705.625.325.885.865.485.235.665.926.365.505.525.416.185.585.505.505.215.515.585.644.685.515.166.305.025.716.175.535.685.295.355.825.836.325.255.445.265.455.575.266.384.966.135.445.644.715.405.306.125.705.845.965.686.125.536.085.395.835.685.765.505.495.455.575.335.274.985.465.545.435.055.775.816.145.585.624.556.094.955.585.815.734.985.914.815.574.755.405.105.375.704.735.065.325.864.834.965.786.375.845.365.426.285.835.405.755.874.705.845.005.756.434.934.835.545.275.145.865.295.554.674.936.526.805.435.825.365.775.774.195.535.575.515.705.495.415.645.935.456.135.325.924.414.564.726.605.666.025.275.574.625.075.426.144.615.445.605.705.734.586.174.865.935.025.725.576.035.014.504.956.825.205.075.735.605.015.145.676.176.095.565.665.205.905.144.875.635.9024.865.325.835.406.775.215.946.725.275.035.325.905.484.985.605.855.796.374.505.246.035.414.605.025.356.104.605.775.986.525.745.465.816.024.944.695.505.745.106.455.235.385.064.934.925.375.494.265.374.475.544.785.565.216.615.245.625.865.674.815.535.776.415.016.065.655.525.615.094.585.485.334.955.715.205.335.045.364.885.63表82#濾棒樣品分切后三乙酸甘油酯的含量PAGE PAGE19L25(52)正交設(shè)計(jì)共有25種分切方式，評(píng)定了每種分切方式的不確定度，分析了每種分切方式檢測(cè)的30個(gè)樣品的標(biāo)準(zhǔn)偏差，結(jié)果表明濾棒樣品分切后體積（質(zhì)量）大的樣品其標(biāo)準(zhǔn)偏差較小，標(biāo)準(zhǔn)偏差與不確定度的比值較小，進(jìn)一步說(shuō)明不確定度對(duì)樣品中三乙酸甘油酯含量的檢測(cè)影響較大，剔除了標(biāo)準(zhǔn)偏差小于不確定度3倍的6種分切方式，保留了標(biāo)準(zhǔn)偏差大于不確定度3倍的19種分切方式（表9）。正態(tài)檢驗(yàn)（Shapiro-Wilk）結(jié)果表明：保留分切方式樣品中三乙酸甘油酯的含量分布滿(mǎn)足正態(tài)分布（p>0.05）(表10)。Levene方差齊性檢驗(yàn)結(jié)果表明：2#樣品保留分切方式檢測(cè)結(jié)果的方差不具備齊性（p<0.05）（表11）。表112#樣品保留分切方式檢測(cè)結(jié)果的方差齊性檢驗(yàn)檢驗(yàn)方法檢驗(yàn)統(tǒng)計(jì)量P差異顯著性L(fǎng)evene檢驗(yàn)3.4720.000顯著表122#樣品保留分切方式檢測(cè)結(jié)果的方差分析變異來(lái)源III型方差SS自由度均方MS統(tǒng)計(jì)量FP值校正的模型41.484182.30516.1590.000截距15468.774115468.774108454.1980.000軸向分切比例1.17740.2942.0620.084徑向分切長(zhǎng)度7.72641.93213.5420.000軸向分切比例*徑向分切長(zhǎng)度32.951103.29523.1030.000誤差78.5895510.143合計(jì)17365.943570校正的合計(jì)120.073569進(jìn)一步采用一般線(xiàn)性模型中的單因變量多因素方差分析確定合適的濾棒分切條件，由于樣品的方差不齊，在多重比較時(shí)選擇方差不具有齊性的“Tamhane’sT2”法進(jìn)行比較。方差分析的結(jié)果表明：2#樣品在軸向分切比例水平上不存在差異性（p>0.05），在徑向分切長(zhǎng)度的不同水平上存在差異（p<0.05）（表12）。進(jìn)一步的“Tamhane’sT2”法多重比較結(jié)果表明：在軸向1、1/2、1/4、1/8、1/16的分切比例的檢測(cè)結(jié)果不存在差異（p>0.05），徑向分切長(zhǎng)度80、60、40間的檢測(cè)結(jié)果不存在差異（p>0.05），徑向分切長(zhǎng)度80、60、40mm的檢測(cè)結(jié)果與20mm的檢測(cè)結(jié)果存在差異（p<0.05），徑向分切長(zhǎng)度20、10mm檢測(cè)結(jié)果間不存在差異（p>0.05）（表13、表14）。表132#樣品保留分切方式中軸向分切比例間的多重比較軸向分切比例軸向分切比例均值差值標(biāo)準(zhǔn)誤差P11/2-0.0180.0471.0001/40.0130.0511.0001/80.0010.0661.0001/16-0.1180.0750.7191/210.0180.0471.0001/40.0300.0521.0001/80.0190.0681.0001/16-0.1010.0760.8791/41-0.0130.0511.0001/2-0.0300.0521.0001/8-0.0110.0701.0001/16-0.1310.0780.6431/81-0.0010.0661.0001/2-0.0190.0681.0001/40.0110.0701.0001/16-0.1200.0890.8671/1610.1180.0750.7191/20.1010.0760.8791/40.1310.0780.6431/80.1200.0890.867表142#樣品保留分切方式中徑向分切長(zhǎng)度間的多重比較徑向分切長(zhǎng)度(mm)徑向分切長(zhǎng)度(mm)均值差值標(biāo)準(zhǔn)誤差p1020-0.0160.0701.00040-0.1860.0660.05760-0.1990.0680.03680-0.3150.0700.00020100.0160.0701.00040-0.1700.0550.02360-0.1830.0560.01380-0.2990.0590.00040100.1860.0660.057200.1700.0550.02360-0.0140.0511.00080-0.1290.0540.16560100.1990.0680.036200.1830.0560.013400.0140.0511.00080-0.1150.0560.32980100.3150.0700.000200.2990.0590.000400.1290.0540.165600.1150.0560.3294.2.33＃樣品分析3＃樣品取自龍巖煙草工業(yè)有限責(zé)任公司濾棒成型車(chē)間，成型機(jī)型為KDF2，三乙酸甘油酯的施加方式為噴嘴（表1），將3#樣品沿徑向、軸向進(jìn)行分切，徑向、軸向的分切水平按照L25(52)正交設(shè)計(jì)表進(jìn)行組合，L25(52)正交設(shè)計(jì)共有25種分切方式，每種分切方式檢測(cè)30個(gè)樣品（表15）。表163#濾棒樣品分切后三乙酸甘油酯含量分析軸向分切比例徑向分切長(zhǎng)度mm）標(biāo)準(zhǔn)偏差不確定度標(biāo)準(zhǔn)偏差/不確定度正態(tài)檢驗(yàn)（Shapiro-Wilk）檢驗(yàn)統(tǒng)計(jì)量P1800.5560.0916.1010.9620.3521/2800.7520.07010.7540.9350.0671/4800.4890.1114.4200.9750.6901/8800.7680.0908.5150.9400.0911/16800.5060.1044.8580.9770.7341600.4330.0636.8910.9540.2201/2600.5310.0757.1190.9700.5471/4600.8400.07611.0980.9370.0771/8600.7630.0839.1650.9760.7061/16600.5690.1204.7290.9760.7101400.2580.0703.6830.9580.2681/2400.5740.0688.4400.9540.2181/4400.5790.1045.5600.9750.6871/8400.7090.1076.6340.9650.4151/16400.5440.1383.9450.9490.1561200.2980.0664.5360.9420.1021/2200.4810.0825.8860.9830.8911/4200.5100.1074.7610.9680.4841/8200.7890.1724.5860.9710.5661/16200.6900.2832.441//1100.4400.0845.2450.9580.2781/2100.4220.0954.4240.9760.7251/4100.5790.1384.1900.9720.5901/8100.6830.3072.223//1/16100.5500.8190.672//表153#濾棒樣品分切后三乙酸甘油酯的含量軸向分切比例11/21/41/81/1611/21/41/81/1611/21/41/81/1611/21/41/81/1611/21/41/81/16徑向分切長(zhǎng)度（mm）808080808060606060604040404040202020202010101010104.824.084.854.943.945.024.703.383.705.233.914.314.014.513.244.093.714.374.084.734.654.014.424.726.004.064.654.894.724.254.034.254.624.314.274.433.933.665.344.164.264.823.344.224.874.453.973.595.245.364.795.134.524.824.273.925.073.623.373.744.244.404.444.054.443.954.783.564.325.464.734.333.824.465.264.715.853.814.744.104.324.164.453.683.544.413.685.344.533.284.514.964.135.445.184.673.304.254.836.194.304.055.375.885.374.535.044.193.323.534.544.464.605.203.903.844.603.595.105.554.933.964.656.195.375.585.534.534.414.724.894.213.503.763.514.824.634.894.583.824.653.854.133.244.894.854.534.684.454.104.104.684.784.564.423.974.363.644.473.284.554.484.964.593.254.684.734.044.814.534.683.384.264.695.814.975.454.724.504.344.245.024.584.713.464.003.854.803.533.154.475.084.724.334.914.564.345.064.246.104.945.714.323.323.674.533.715.054.833.404.624.734.233.034.123.994.052.843.976.024.793.855.164.885.844.084.304.563.124.474.585.255.804.623.894.324.714.694.154.324.714.273.303.056.314.294.314.744.915.754.653.814.063.315.244.875.124.932.902.994.324.685.104.723.943.925.283.663.644.834.843.514.534.745.855.134.633.985.004.864.793.723.893.663.374.684.804.545.063.734.194.063.543.036.014.294.083.975.125.894.894.804.394.964.724.993.775.523.634.494.413.684.823.923.764.515.614.584.796.104.573.835.783.915.144.055.023.922.904.494.863.516.192.964.494.644.504.152.933.703.995.273.245.145.254.114.834.354.416.055.535.593.594.284.484.243.985.004.004.054.294.693.914.343.494.554.404.434.484.644.243.794.144.465.284.683.563.843.154.243.744.745.602.854.404.093.784.874.923.943.844.184.723.313.684.284.684.744.155.775.454.244.833.103.784.944.265.033.955.044.713.993.564.363.423.825.273.284.664.394.193.803.373.755.854.753.674.293.753.535.194.565.504.664.904.154.034.345.083.824.244.864.214.423.573.894.783.554.516.154.304.114.534.444.663.974.125.664.664.634.075.504.703.283.924.084.823.544.603.814.953.963.696.425.303.813.784.074.864.634.473.625.494.934.124.105.965.653.103.684.584.124.254.644.234.373.624.124.985.144.633.773.703.693.704.704.434.306.224.114.163.664.183.704.584.544.453.883.704.675.173.713.935.095.304.804.233.924.933.874.894.203.745.244.434.534.444.693.273.764.414.474.133.164.624.684.763.944.573.795.024.385.064.643.955.243.814.434.074.374.464.544.535.403.634.184.914.464.044.504.894.173.304.655.964.643.654.313.644.304.954.474.224.764.604.695.273.654.155.384.344.603.415.174.935.324.554.636.005.863.563.264.415.024.085.223.843.494.524.414.754.435.374.074.914.284.693.464.064.604.824.054.715.845.964.243.475.273.003.404.464.133.624.394.704.103.615.744.674.844.325.313.934.954.925.174.504.085.045.833.673.703.523.543.384.253.263.304.153.904.084.845.515.114.763.894.504.335.333.885.334.193.684.815.804.113.733.964.183.473.924.163.833.794.024.354.444.623.924.593.754.973.915.164.485.053.514.233.725.063.784.354.844.114.014.203.453.694.134.754.755.114.713.783.844.435.434.036.264.684.584.183.383.585.693.773.314.564.374.174.554.454.345.334.334.225.153.984.074.043.814.804.784.884.776.064.304.534.665.52PAGE PAGE23L25(52)正交設(shè)計(jì)共有25種分切方式，評(píng)定了每種分切方式的不確定度，分析了每種分切方式檢測(cè)的30個(gè)樣品的標(biāo)準(zhǔn)偏差，結(jié)果表明濾棒樣品分切后體積（質(zhì)量）大的樣品其標(biāo)準(zhǔn)偏差較小，標(biāo)準(zhǔn)偏差與不確定度的比值較小，進(jìn)一步說(shuō)明不確定度對(duì)樣品中三乙酸甘油酯含量的檢測(cè)影響較大，剔除了標(biāo)準(zhǔn)偏差小于不確定度3倍的3種分切方式，保留了標(biāo)準(zhǔn)偏差大于不確定度3倍的22種分切方式（表16）。正態(tài)檢驗(yàn)（Shapiro-Wilk）結(jié)果表明：保留分切方式樣品中三乙酸甘油酯的含量分布滿(mǎn)足正態(tài)分布（p>0.05）(表10)。Levene方差齊性檢驗(yàn)結(jié)果表明：3#樣品保留分切方式檢測(cè)結(jié)果的方差不具備齊性（p<0.05）（表17）。表173#樣品保留分切方式檢測(cè)結(jié)果的方差齊性檢驗(yàn)檢驗(yàn)方法檢驗(yàn)統(tǒng)計(jì)量P差異顯著性L(fǎng)evene檢驗(yàn)4.5060.000顯著表183#樣品保留分切方式檢測(cè)結(jié)果的方差分析變異來(lái)源III型方差SS自由度均方MS統(tǒng)計(jì)量FP值校正的模型28.970211.3804.0570.000截距11565.744111565.74434016.1910.000軸向分切比例9.26542.3166.8130.000徑向分切長(zhǎng)度0.73240.1830.5380.708軸向分切比例*徑向分切長(zhǎng)度19.604131.5084.4350.000誤差216.9246380.340合計(jì)12618.517660校正的合計(jì)245.894659進(jìn)一步采用一般線(xiàn)性模型中的單因變量多因素方差分析確定合適的濾棒分切條件，由于樣品的方差不齊，在多重比較時(shí)選擇方差不具有齊性的“Tamhane’sT2”法進(jìn)行比較。方差分析的結(jié)果表明：3#樣品在軸向分切比例水平上存在差異性（p<0.05），在徑向分切長(zhǎng)度的不同水平上不存在差異（p>0.05）（表18）。進(jìn)一步的“Tamhane’sT2”法多重比較結(jié)果表明：在徑向80、60、40、20、10mm的分切長(zhǎng)度的檢測(cè)結(jié)果不存在差異（p>0.05），軸向分切比例1、1/2、1/4間的檢測(cè)結(jié)果不存在差異（p>0.05），軸向分切比例1與1/8、1/16間檢測(cè)結(jié)果存在差異（p<0.05），軸向分切比例1/2與1/16間檢測(cè)結(jié)果存在差異（p<0.05），軸向分切比例1/4、1/8、1/16間的檢測(cè)結(jié)果不存在差異（p>0.05）（表19、20）。表193#樣品保留分切方式中軸向分切比例間的多重比較軸向分切比例軸向分切比例均值差值標(biāo)準(zhǔn)誤差P11/20.1070.0600.5411/40.1510.0640.1761/80.2230.0780.0451/160.3700.0680.0001/21-0.1070.0600.5411/40.0430.0721.0001/80.1150.0840.8481/160.2620.0750.0061/41-0.1510.0640.1761/2-0.0430.0721.0001/80.0720.0870.9951/160.2190.0780.0521/81-0.2230.0780.0451/2-0.1150.0840.8481/4-0.0720.0870.9951/160.1470.0890.6561/161-0.3700.0680.0001/2-0.2620.0750.0061/4-0.2190.0780.0521/8-0.1470.0890.656表203#樣品保留分切方式中徑向分切長(zhǎng)度間的多重比較徑向分切長(zhǎng)度(mm)徑向分切長(zhǎng)度(mm)均值差值標(biāo)準(zhǔn)誤差p10200.0380.0801.000400.0120.0751.000600.0300.0791.000800.0160.0771.0002010-0.0380.0801.00040-0.0260.0731.00060-0.0080.0771.00080-0.0220.0761.0004010-0.0120.0751.000200.0260.0731.000600.0180.0721.000800.0040.0701.0006010-0.0300.0791.000200.0080.0771.00040-0.0180.0721.00080-0.0140.0741.0008010-0.0160.0771.000200.0220.0761.00040-0.0040.0701.000600.0140.0741.0004.2.44＃樣品分析4＃樣品取自廈門(mén)煙草工業(yè)有限責(zé)任公司濾棒成型車(chē)間，成型機(jī)型為KDF4，三乙酸甘油酯的施加方式為噴嘴（表1），將4#樣品沿徑向、軸向進(jìn)行分切，徑向、軸向的分切水平按照L25(52)正交設(shè)計(jì)表進(jìn)行組合，L25(52)正交設(shè)計(jì)共有25種分切方式，每種分切方式檢測(cè)30個(gè)樣品（表21）。表224#濾棒樣品分切后三乙酸甘油酯含量分析軸向分切比例徑向分切長(zhǎng)度mm）標(biāo)準(zhǔn)偏差不確定度標(biāo)準(zhǔn)偏差/不確定度正態(tài)檢驗(yàn)（Shapiro-Wilk）檢驗(yàn)統(tǒng)計(jì)量P1800.1620.0831.952//1/2800.5950.0906.6110.9460.1291/4800.4200.0934.5160.9780.7841/8800.4950.1263.9290.9600.3011/16800.7090.1674.2460.9490.1581600.1930.0971.990//1/2600.4820.0984.9180.9410.0951/4600.6360.1056.0570.9840.9101/8600.5060.1483.4190.9790.7861/16600.5310.1743.0520.9490.1591400.1970.0952.074//1/2400.5220.1025.1180.9430.1081/4400.5200.1114.6850.9700.5501/8400.7150.1544.6430.9810.8401/16400.7030.2662.643//1200.2380.0902.644//1/2200.4160.1103.7820.9540.2121/4200.3780.1203.1500.9520.1931/8200.6620.2103.1520.9760.7241/16200.8590.3222.668//1100.1790.1101.627//1/2100.5130.1403.6640.9520.1871/4100.6350.2043.1130.9810.8511/8100.8310.2972.798//1/16101.3710.6012.281//表214#濾棒樣品分切后三乙酸甘油酯的含量軸向分切比例11/21/41/81/1611/21/41/81/1611/21/41/81/1611/21/41/81/1611/21/41/81/16徑向分切長(zhǎng)度（mm）808080808060606060604040404040202020202010101010106.605.716.437.376.846.267.467.986.836.586.316.768.036.375.815.647.076.406.135.655.896.766.646.066.787.437.216.076.326.136.516.485.497.015.576.366.536.686.876.075.927.205.579.006.866.426.566.586.506.026.116.016.376.916.698.575.606.