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專題16化學(xué)實驗探究綜合/r/n1.(山東泰安市/r/n高三模擬/r/n)/r/n葡萄糖酸鈣是一種常用的藥物,臨床上用于治療骨質(zhì)疏松癥。某實驗室對葡萄糖酸鈣的制備工藝進行研究,先以葡萄糖/r/n[CH/r/n2/r/nOH(CHOH)/r/n4/r/nCHO]/r/n和/r/nH/r/n2/r/nO/r/n2/r/n為原料制備葡萄糖酸/r/n[CH/r/n2/r/nOH(CHOH)/r/n4/r/nCOOH]/r/n,再用葡萄糖酸與碳酸鈣反應(yīng)制備葡萄糖酸鈣。已知:/r/n30/r/n%/r/nH/r/n2/r/nO/r/n2/r/n溶液的密度為/r/n1.1g·cm/r/n-3/r/n,回答下列問題:/r/nI./r/n制備葡萄糖酸/r/n(/r/n裝置如圖所示/r/n)/r/n。/r/n(1)/r/n儀器/r/nX/r/n的名稱為/r/n___________/r/n,/r/nY/r/n處為冷凝回流裝置,下列儀器使用正確且效果最好的是/r/n___________(/r/n填字母/r/n)/r/n。/r/n(2)/r/n滴入雙氧水,水浴加熱一段時間后,得到無色透明的葡萄糖酸溶液。反應(yīng)的化學(xué)方程式為/r/n___________/r/n。/r/nⅡ./r/n測定葡萄糖的轉(zhuǎn)化率,確定合適的反應(yīng)溫度。/r/n(3)/r/n用移液管取出三口燒瓶中的反應(yīng)液/r/n2.00mL/r/n置于錐形瓶中,以酚酞作為指示劑并加/r/n20mL/r/n蒸餾水稀釋,用/r/n0.04mol·L/r/n-1/r/nNaOH/r/n標準溶液滴定。/r/n①滴定管使用的正確的操作順序為蒸餾水洗滌/r/n→/r/n標準液潤洗/r/n→___________→___________→___________→___________→/r/n洗凈/r/n→/r/n放回滴定管架/r/n(/r/n填字母/r/n)/r/n。/r/na./r/n滴定結(jié)束后,記錄刻度/r/nb./r/n調(diào)節(jié)液面至/r/n0/r/n刻度或/r/n0/r/n刻度略靠下,記錄刻度/r/nc./r/n裝入標準液并排凈尖嘴處的氣泡/r/nd./r/n將未滴定完的標準液回收/r/n②達到滴定終點時的現(xiàn)象為/r/n___________/r/n。/r/n③滴定過程消耗/r/nNaOH/r/n標準溶液的體積為/r/nV/r/n0/r/nmL/r/n,反應(yīng)后三口燒瓶內(nèi)溶液的體積為/r/nV/r/n1/r/nmL/r/n,實驗條件下葡萄糖的轉(zhuǎn)化率為/r/n___________(/r/n用含/r/nV/r/n0/r/n和/r/nV/r/n1/r/n的代數(shù)式表示/r/n)/r/n。/r/n④若滴定終點時俯視讀數(shù),對轉(zhuǎn)化率的影響為/r/n___________(/r/n填/r/n“/r/n偏高/r/n”“/r/n偏低/r/n”/r/n或/r/n“/r/n無影響/r/n”)/r/n。/r/nⅢ./r/n制備葡萄糖酸鈣。/r/n將/r/nCaCO/r/n3/r/n分散于適量蒸餾水中形成濁液,加入葡萄糖酸,至無/r/nCO/r/n2/r/n氣體放出為止,煮沸,并趁熱采用下圖裝置抽濾,濾掉未反應(yīng)的/r/nCaCO/r/n3/r/n,得到澄清透明的葡萄糖酸鈣溶液。/r/n(4)/r/n抽濾時自來水流的作用是使瓶內(nèi)與大氣形成壓強差,與普通過濾操作相比,抽濾的優(yōu)點是/r/n___________/r/n。/r/n(1)/r/n恒壓滴液漏斗/r/nA(2)CH/r/n2/r/nOH(CHOH)/r/n4/r/nCHO+H/r/n2/r/nO/r/n2/r/n/r/nH/r/n2/r/nO+CH/r/n2/r/nOH(CHOH)/r/n4/r/nCOOH(3)cbad/r/n當?shù)稳胱詈笠坏?r/nNaOH/r/n標準溶液時,溶液由無色變?yōu)榉奂t色,且半分鐘內(nèi)不褪色/r/n/r/n×100/r/n%/r/n/r/n偏低/r/n(4)/r/n過濾速度快/r/n/r/n【分析】/r/n本實驗的目的是制備葡萄糖酸鈣,首先利用雙氧水氧化葡萄糖得到葡萄糖酸,為提高葡萄糖的利用率,反應(yīng)過程中利用球形冷凝管冷凝回流;將/r/nCaCO/r/n3/r/n分散于適量蒸餾水中形成濁液,加入葡萄糖酸,至無/r/nCO/r/n2/r/n氣體放出為止,煮沸,為防止葡萄糖酸鈣析出,趁熱抽濾,得到澄清透明的葡萄糖酸鈣溶液;/r/n測定葡萄糖的轉(zhuǎn)化率時,利用/r/nNaOH/r/n標準液滴定葡萄糖酸,葡萄糖酸為一元酸,與/r/nNaOH/r/n發(fā)生中和反應(yīng)。/r/n(1)/r/n根據(jù)儀器/r/nX/r/n的結(jié)構(gòu)特點可知其為恒壓滴液漏斗;冷凝回流應(yīng)選用球形冷凝管,冷凝水下進上出,故選/r/nA/r/n;/r/n(2)/r/n雙氧水將葡萄糖中的醛基氧化為羧基,得到葡萄糖酸,化學(xué)方程式為/r/nCH/r/n2/r/nOH(CHOH)/r/n4/r/nCHO+H/r/n2/r/nO/r/n2/r/n/r/nH/r/n2/r/nO+CH/r/n2/r/nOH(CHOH)/r/n4/r/nCOOH/r/n;/r/n(3)/r/n①滴定管使用時應(yīng)先用蒸餾水洗滌,為防止稀釋標準液,再用標準液洗滌,然后裝入標準液并排凈尖嘴處的氣泡,并調(diào)節(jié)液面至/r/n0/r/n刻度或/r/n0/r/n刻度略靠下,記錄刻度,然后開始滴定,滴定結(jié)束后,記錄刻度,將未滴定完的標準液回收,再洗凈滴定管放回管架,所以順序為/r/nc→b→a→d/r/n;/r/n②滴定過程中葡萄糖酸與/r/nNaOH/r/n溶液發(fā)生中和反應(yīng),滴定終點時/r/nNaOH/r/n稍過量,溶液顯堿性,指示劑為酚酞,所以溶液會變?yōu)榉奂t色,所以達到滴定終點時的現(xiàn)象為:當?shù)稳胱詈笠坏?r/nNaOH/r/n標準溶液時,溶液由無色變?yōu)榉奂t色,且半分鐘內(nèi)不褪色;/r/n③/r/n30/r/n%/r/nH/r/n2/r/nO/r/n2/r/n溶液中含有/r/nn(H/r/n2/r/nO/r/n2/r/n)=/r/n=0.19mol/r/n,所用/r/nn(/r/n葡萄糖/r/n)=/r/n=0.1mol/r/n,則理論上葡萄糖可以完全反應(yīng),消耗/r/nNaOH/r/n標準溶液的體積為/r/nV/r/n0/r/nmL/r/n,則/r/n2.00mL/r/n反應(yīng)液中/r/nn(/r/n葡萄糖酸/r/n)=0.04V/r/n0/r/n×10/r/n-3/r/nmol/r/n,所以/r/nV/r/n1/r/nmL/r/n反應(yīng)液中/r/nn(/r/n葡萄糖酸/r/n)=0.01V/r/n0/r/n×/r/n×10/r/n-3/r/nmol/r/n,則實際上消耗/r/n0.04V/r/n0/r/n×/r/n×10/r/n-3/r/nmol/r/n葡萄糖,其轉(zhuǎn)化率為/r/n×100/r/n%/r/n=/r/n×100/r/n%;/r/n④若滴定終點時俯視讀數(shù),則/r/nV/r/n0/r/n偏小,根據(jù)計算式可知結(jié)果會偏低;/r/n(4)/r/n抽濾時形成負壓,水流的更快,所以與普通過濾操作相比,抽濾過濾速度快,可以減少因溶液溫度較低而析出的葡萄糖酸鈣。/r/n2.(湖南邵陽市/r/n高三模擬/r/n)/r/n氧化亞銅在強酸性溶液中發(fā)生歧化反應(yīng),某小組同學(xué)設(shè)計如下實驗制備氧化亞銅并測定其純度。/r/n(1)/r/n該小組同學(xué)利用葡萄糖還原/r/nCuSO/r/n4/r/n溶液制備氧化亞銅。/r/n①配制/r/n0.l0.l0.lmol·L/r/n-/r/n1/r/nCuSO/r/n4/r/n溶液,需要稱取膽礬晶體的質(zhì)量為/r/n___________/r/n,完成該實驗操作需要的玻璃儀器除膠頭滴管外還要/r/n___________/r/n。/r/n②該反應(yīng)最適宜溫度為/r/n80/r/n~/r/n90℃/r/n,為探究反應(yīng)發(fā)生的最低溫度,應(yīng)選用的加熱方式為/r/n_______/r/n。/r/n(2)/r/n某同學(xué)為檢驗/r/nCu/r/n2/r/nO/r/n樣品中是否含有/r/nCuO/r/n,設(shè)計如下實驗方案:將/r/nCu/r/n2/r/nO/r/n樣品與足量稀硫酸反應(yīng),觀察到溶液呈藍色。即得出結(jié)論:樣品中含有/r/nCuO/r/n雜質(zhì)。若探究該同學(xué)的方案和結(jié)論是否合理,需用化學(xué)方程式/r/n___________/r/n來進行解釋。/r/n(3)/r/n該小組取含有少量/r/nCuO/r/n雜質(zhì)的/r/nCu/r/n2/r/nO/r/n進行如下實驗,以測定氧化亞銅的純度,/r/n①裝置/r/na/r/n中所加的酸是/r/n___________(/r/n填化學(xué)式/r/n)/r/n。/r/n②通過測定下列物理量,能達到實驗?zāi)康氖?r/n___________(/r/n填字母/r/n)/r/n。/r/nA/r/n.反應(yīng)前后裝置/r/na/r/n的質(zhì)量/r/nB/r/n.裝置/r/nc/r/n充分反應(yīng)后所得固體的質(zhì)量/r/nC/r/n.反應(yīng)前后裝置/r/nd/r/n的質(zhì)量/r/nD/r/n.反應(yīng)前后裝置/r/ne/r/n的質(zhì)量/r/n③驗純后點燃裝置/r/nc/r/n中酒精燈之前,對/r/nK/r/n1/r/n、/r/nK/r/n2/r/n進行的操作是/r/n____________________/r/n。/r/n④若缺少裝置/r/ne/r/n,則氧化亞銅的純度/r/n___________(/r/n填/r/n“/r/n偏高/r/n”“/r/n偏低/r/n”/r/n或/r/n“/r/n無影響/r/n”)/r/n。/r/n(1)12.5g/r/n燒杯、玻璃棒、/r/n500mL/r/n容量瓶/r/n/r/n水浴加熱/r/n(/r/n2/r/n)Cu/r/n2/r/nO+H/r/n2/r/nSO/r/n4/r/n=CuSO/r/n4/r/n+Cu+H/r/n2/r/nO(3)H/r/n2/r/nSO/r/n4/r/nBC/r/n打開/r/nK/r/n2/r/n關(guān)閉/r/nK/r/n1/r/n/r/n偏低/r/n/r/n【分析】/r/n配制/r/n490mL0.1mol?L/r/n-1/r/nCuSO/r/n4/r/n溶液,容量瓶無此規(guī)格,需要在/r/n500mL/r/n容量瓶中配制,據(jù)此計算溶質(zhì),配制溶液的步驟為:計算、量取、稀釋、冷卻、移液、洗滌、定容、搖勻,結(jié)合步驟和操作選擇需要的玻璃儀器。測定氧化亞銅的純度:/r/na/r/n防止酸的揮發(fā),應(yīng)選用難揮發(fā)性的酸,/r/nb/r/n干燥氫氣,/r/nc/r/n還原,/r/nd/r/n測定產(chǎn)生的水,/r/ne/r/n防止空氣中的水和二氧化碳進入/r/nd/r/n,/r/nf/r/n處理尾氣。測定原理是根據(jù)氫氣還原氧化亞銅反應(yīng)后所得固體質(zhì)量或生成水的質(zhì)量來求氧化亞銅的質(zhì)量分數(shù);驗純后應(yīng)保持氣體能通過/r/nd/r/n裝置,使生成的水全部被/r/nd/r/n裝置吸收;若缺少裝置/r/ne/r/n,/r/nd/r/n吸收水的質(zhì)量增加,測定氧化銅質(zhì)量增大。/r/n(1)/r/n①配制/r/n0.l0.l0.lmol·L/r/n-/r/n1/r/nCuSO/r/n4/r/n溶液,容量瓶無此規(guī)格,需要在/r/n500mL/r/n容量瓶中配制,配制/r/n500mL0.1mol?L/r/n-1/r/nCuSO/r/n4/r/n溶液,需要稱取膽礬晶體的質(zhì)量/r/n=0.5L×0.1mol/L×250g/mol=12.5g/r/n,需要稱取膽礬晶體的質(zhì)量為/r/n12.5g/r/n,完成該實驗操作需要的玻璃儀器除膠頭滴管外還要燒杯、玻璃棒、/r/n500mL/r/n容量瓶。故/r/n12.5g/r/n;燒杯、玻璃棒、/r/n500mL/r/n容量瓶;/r/n②該反應(yīng)最適宜溫度為/r/n80/r/n~/r/n90℃/r/n,可知低于/r/n100℃/r/n的溫度,為探究反應(yīng)發(fā)生的最低溫度,應(yīng)選用的加熱方式為水浴加熱。故水浴加熱;/r/n(2)/r/n檢驗/r/nCu/r/n2/r/nO/r/n樣品中是否含有/r/nCuO/r/n,將/r/nCu/r/n2/r/nO/r/n樣品與足量稀硫酸反應(yīng),觀察到溶液呈藍色。即得出結(jié)論:樣品中含有/r/nCuO/r/n雜質(zhì)。若探究該同學(xué)的方案和結(jié)論是否合理,需用化學(xué)方程式/r/nCu/r/n2/r/nO+H/r/n2/r/nSO/r/n4/r/n=CuSO/r/n4/r/n+Cu+H/r/n2/r/nO/r/n來進行解釋。/r/n/r/n(3)/r/n①/r/nd/r/n裝置中的堿石灰會吸收水和酸性氣體,防止/r/na/r/n中酸揮發(fā),故選難揮發(fā)性酸硫酸,裝置/r/na/r/n中所加的酸是/r/nH/r/n2/r/nSO/r/n4/r/n。/r/n/r/n②測定原理是根據(jù)氫氣還原氧化亞銅反應(yīng)后所得固體質(zhì)量或生成水的質(zhì)量來求氧化亞銅的質(zhì)量分數(shù),故/r/nBC/r/n;/r/n③驗純后應(yīng)保持氣體能通過/r/nd/r/n裝置,使生成的水全部被/r/nd/r/n裝置吸收,對/r/nK/r/n1/r/n、/r/nK/r/n2/r/n進行的操作是打開/r/nK/r/n2/r/n關(guān)閉/r/nK/r/n1/r/n。/r/n/r/n④若缺少裝置/r/ne/r/n,/r/nd/r/n吸收水的質(zhì)量增加,測定氧化銅質(zhì)量增大,則氧化亞銅的純度偏低/r/n/r/n3.(山東濟南市/r/n高三/r/n二模)/r/n某活動小組的同學(xué)對甲烷還原氧化銅進行了探究,回答下列問題:/r/n查閱資料得:實驗室制取甲烷常用的方法為無水醋酸鈉/r/n與氫氧化鈉在二氧化錳作催化劑的條件下共熱,產(chǎn)物中有少量的副產(chǎn)物丙酮/r/n,丙酮可與水混溶。/r/n(1)/r/n組裝好儀器后,首先進行的操作是/r/n___________/r/n,實驗中先點燃/r/n___________(/r/n填“/r/nA/r/n”或“/r/nD/r/n”/r/n)/r/n處酒精燈,此時/r/n、/r/n的狀態(tài)為/r/n___________(/r/n填標號/r/n)/r/n。/r/nA/r/n./r/n關(guān)閉、/r/n關(guān)閉/r/nB/r/n./r/n關(guān)閉、/r/n打開/r/nC/r/n./r/n打開、/r/n打開/r/nD/r/n./r/n打開、/r/n關(guān)閉/r/n(2)/r/n裝置/r/nA/r/n中主要發(fā)生反應(yīng)的化學(xué)方程式為/r/n___________/r/n,試管內(nèi)壁加一層鋁箔不僅能使藥品受熱均勻,還能/r/n___________/r/n。/r/n(3)/r/n裝置/r/nB/r/n中盛裝的試劑為/r/n___________/r/n。/r/n(4)/r/n實驗過程中記錄的實驗數(shù)據(jù)如下:/r/n實驗前裝置總質(zhì)量/r/n/g/r/nD/r/nE/r/nF/r/nG/r/n實驗后裝置總質(zhì)量/r/n/g/r/n180.0/r/n277.8/r/n311.5/r/n301.0/r/n實驗前裝置總質(zhì)量/r/n/g/r/n177.2/r/n279.6/r/n312.6/r/n301.0/r/n若裝置/r/nD/r/n中的氧化銅全部被還原成銅,則氣球中收集到的由/r/nD/r/n中反應(yīng)產(chǎn)生的氣體在標準狀況下的體積為/r/n___________L/r/n,此條件下,裝置/r/nD/r/n中發(fā)生反應(yīng)的化學(xué)方程式為/r/n___________/r/n。/r/n(1)/r/n檢查裝置的氣密性/r/nAD(2)/r/n/r/n保護試管,使反應(yīng)混合物不黏附在試管壁上/r/n(3)/r/n水/r/n(4)0.56/r/n/r/n【分析】/r/n加熱裝置/r/nA/r/n、乙酸鈉和氫氧化鈉在催化劑作用下反應(yīng)產(chǎn)生甲烷,甲烷和空氣的混合氣體點燃易爆炸,故需用產(chǎn)生的甲烷排凈空氣,/r/nB/r/n中用水除去副產(chǎn)物丙酮、經(jīng)/r/nC/r/n處濃硫酸干燥后,進入/r/nD/r/n中,甲烷和氧化銅發(fā)生反應(yīng),/r/nE/r/n吸收反應(yīng)生成的水、用/r/nF/r/n中氫氧化鈉溶液吸收生成的二氧化碳,/r/nG/r/n用于檢驗二氧化碳是否吸收完全,氣球用于收集生成的/r/nCO/r/n,據(jù)此回答;/r/n(1)/r/n有氣體參與的實驗,在進行實驗前都要檢查裝置的氣密性。故組裝好儀器后,首先進行的操作是檢查裝置的氣密性,實驗中先點燃/r/nA/r/n處酒精燈,使反應(yīng)發(fā)生生成甲烷、甲烷和空氣的混合氣體點燃易爆炸,故用產(chǎn)生的甲烷驅(qū)趕裝置內(nèi)的空氣/r/n(/r/n從/r/nT/r/n型管口排出/r/n)/r/n,排凈空氣后再加熱/r/nD/r/n處酒精燈,則此時/r/n、/r/n的狀態(tài)為/r/n打開、/r/n關(guān)閉,選/r/nD/r/n;/r/n(2)/r/n裝置/r/nA/r/n中產(chǎn)生甲烷,主要發(fā)生反應(yīng)的化學(xué)方程式為/r/n,鋁箔易導(dǎo)熱,能使藥品受熱均勻,且將氫氧化鈉與試管隔離,避免高溫下氫氧化鈉對試管的腐蝕,也可使反應(yīng)后的試管更容易清洗。故保護試管,使反應(yīng)混合物不黏附在試管壁上;/r/n(3)/r/n產(chǎn)物中有少量的副產(chǎn)物丙酮/r/n,丙酮可與水混溶。故裝置/r/nB/r/n中裝水,用來除去甲烷中的丙酮。/r/n(4)/r/n裝置/r/nD/r/n中減少的質(zhì)量為氧元素的質(zhì)量,即參與反應(yīng)的/r/n,裝置/r/nE/r/n中增加的是水的質(zhì)量,即/r/n,裝置/r/nF/r/n中增加的是/r/n的質(zhì)量,即/r/n,依據(jù)得失電子守恒和質(zhì)量守恒可知,氣球中收集到的是/r/nCO/r/n,其體積為/r/n,則/r/n,物質(zhì)的量之比即化學(xué)計量數(shù)之比、結(jié)合元素質(zhì)量守恒,氧化銅和甲烷反應(yīng)的化學(xué)方程式為/r/n。/r/n4.(湖南永州市/r/n高三模擬/r/n)/r/n過氧乙酸是具有重要用途的有機合成氧化劑和化工原料,實驗室擬合成過氧乙酸并測定其含量。/r/n(1)/r/n濃縮/r/n在圖示裝置/r/n(/r/n加熱裝置已省略/r/n)/r/n中,由分液漏斗向冷凝管/r/n1/r/n中滴加/r/n30%/r/n溶液,最終得到質(zhì)量分數(shù)約/r/n68%/r/n的/r/n溶液。/r/n
/r/n冷凝管/r/n1/r/n、冷凝管/r/n2/r/n中進水接口依次為/r/n___________/r/n、/r/n___________(/r/n填字母/r/n)/r/n。/r/n②加熱溫度不宜超過/r/n60℃/r/n的原因是/r/n___________/r/n。/r/n(2)/r/n合成過氧乙酸/r/n向帶有攪拌裝置及溫度計的/r/n500mL/r/n三口燒瓶中先加入/r/n16g/r/n冰醋酸,在攪拌下滴加/r/n90g68%/r/n溶液,最后加入/r/n4.1mL/r/n濃硫酸,攪拌/r/n5h/r/n,靜置/r/n20h/r/n。/r/n(/r/n已知:/r/nCH/r/n3/r/nCOOH+H/r/n2/r/nO/r/n2/r/n+H/r/n2/r/nO)/r/n①用濃縮的/r/n68%/r/n溶液代替常見的/r/n30%/r/n溶液的目的是/r/n___________/r/n。/r/n②充分攪拌的目的是/r/n___________/r/n。/r/n(3)/r/n過氧乙酸含量的測定/r/n步驟/r/na/r/n:稱取/r/n5.0g/r/n過氧乙酸試樣/r/n(/r/n液體/r/n)/r/n,配制成/r/n100mL/r/n溶液/r/nA/r/n。/r/n步驟/r/nb/r/n:在碘量瓶中加入/r/n5.0mL/r/n溶液、/r/n3/r/n滴/r/n溶液、/r/n5.0mL/r/n溶液/r/nA/r/n,搖勻,用/r/n0.01mol/L/r/n的/r/n溶液滴定至溶液呈微紅色。/r/n步驟/r/nc/r/n:向滴定后的溶液中再加/r/n1.0gKI(/r/n)/r/n,搖勻,置于暗處/r/n5min/r/n,用蒸餾水沖洗瓶蓋及四周,加鉬酸銨催化劑/r/n20mL/r/n,搖勻,用淀粉溶液作指示劑,用/r/n0.05mol/L/r/n的/r/n標準溶液滴定至藍色剛好褪去/r/n(/r/n)/r/n。重復(fù)步驟/r/nb/r/n,步驟/r/nc/r/n三次,測得平均消耗/r/n標準溶液的體積為/r/n20.00mL/r/n。/r/n①步驟/r/na/r/n中配制溶液/r/nA/r/n時,需要用到的玻璃儀器除燒杯、/r/n100mL/r/n容量瓶,玻璃棒和量筒外,還需要/r/n___________/r/n②設(shè)計步驟/r/nb/r/n的目的是/r/n___________/r/n③過氧乙酸的質(zhì)量分數(shù)為/r/n___________%/r/n。/r/n(1)bd/r/n溫度超過/r/n60℃/r/n,/r/n會分解/r/n(2)/r/n增大過氧化氫濃度有利于平衡向生成過氧乙酸的方向移動/r/n/r/n使反應(yīng)物充分接觸,提高原料利用率/r/n(3)/r/n膠頭滴管/r/n/r/n除去其中的/r/n15.2/r/n(1)/r/n①冷凝水下進上出,則冷凝管1、冷凝管2中進水接口依次為/r/nb/r/n、/r/nd/r/n。/r/n②升溫會加快/r/n分解速率,溫度超過/r/n60/r/n℃,/r/n會分解。/r/n(2)/r/n①該反應(yīng)為可逆反應(yīng),增大反應(yīng)物的濃度,平衡向正反應(yīng)方向移動,用/r/n68%/r/n的/r/nH/r/n2/r/nO/r/n2/r/n溶液代替/r/n30%/r/n的/r/nH/r/n2/r/nO/r/n2/r/n溶液,可增大過氧化氫的濃度,有利于平衡向生成過氧乙酸的方向移動;/r/n②充分攪拌,能使反應(yīng)物充分接觸,提高提高原料利用率;/r/n(3)/r/n①配制/r/n100mL/r/n過氧乙酸溶液,配制步驟為:計算、稱量(量取)、溶解、冷卻、轉(zhuǎn)移、洗滌、定容,稱量時用到儀器是天平,溶解時用到燒杯、玻璃棒、量筒,轉(zhuǎn)移溶液時用到燒杯、玻璃棒、100mL容量瓶,定容時還需膠頭滴管,其中屬于玻璃儀器的是/r/n100mL/r/n容量瓶、玻璃棒、燒杯、膠頭滴管、量筒,故還需要的玻璃儀器有膠頭滴管;/r/n②設(shè)計步驟/r/nb/r/n的目的是除去其中的/r/n;/r/n③由/r/n得:/r/n。/r/n5.(江蘇徐州市/r/n高三模擬/r/n)/r/n高鐵酸鉀/r/n(K/r/n2/r/nFeO/r/n4/r/n)/r/n為紫色固體,微溶于/r/nKOH/r/n溶液,具有強氧化性,在酸性或中性溶液中產(chǎn)生/r/nO/r/n2/r/n,在堿性溶液中較穩(wěn)定。/r/n(1)/r/n用如圖所示的裝置制備/r/nK/r/n2/r/nFeO/r/n4/r/n。/r/n①/r/nA/r/n為/r/nCl/r/n2/r/n發(fā)生裝置,裝置/r/nB/r/n的作用是/r/n_______/r/n。/r/n②裝置/r/nC/r/n中發(fā)生反應(yīng)的離子方程式為/r/n_______/r/n。/r/n③當裝置/r/nC/r/n中得到大量紫色固體時立即停止通入/r/nCl/r/n2/r/n,原因是/r/n_______/r/n。/r/n(2)/r/n某鐵礦石的主要成分為/r/nFe/r/n2/r/nO/r/n3/r/n和少量/r/nAl/r/n2/r/nO/r/n3/r/n、/r/nSiO/r/n2/r/n,請補充完整由該鐵礦石制得高純度/r/nFe(OH)/r/n3/r/n的實驗方案:/r/n_______(/r/n實驗中須使用的試劑:稀鹽酸、/r/nNaOH/r/n溶液、/r/nAgNO/r/n3/r/n溶液/r/n)/r/n。/r/n(3)/r/n通過以下方法測定高鐵酸鉀樣品的純度:稱取/r/n0.6000g/r/n高鐵酸鉀樣品,完全溶解于濃/r/nKOH/r/n溶液中,再加入足量亞鉻酸鉀{/r/nK[Cr(OH)/r/n4/r/n]/r/n}反應(yīng)后配成/r/n100.00mL/r/n溶液;取上述溶液/r/n20.00mL/r/n于錐形瓶中,加入稀硫酸調(diào)至/r/npH=2/r/n,用/r/n0.1000mol·L/r/n-1/r/n硫酸亞鐵銨溶液滴定,消耗標準硫酸亞鐵銨溶液/r/n15.00mL/r/n。/r/n測定過程中發(fā)生反應(yīng):/r/nCr(OH)/r/n+/r/n=Fe(OH)/r/n3/r/n+/r/n+OH/r/n-/r/n2/r/n+2H/r/n+/r/n=/r/n+H/r/n2/r/nO/r/n+Fe/r/n2+/r/n+H/r/n+/r/n→Cr/r/n3+/r/n+Fe/r/n3+/r/n+H/r/n2/r/nO(/r/n未配平/r/n)/r/n計算/r/nK/r/n2/r/nFeO/r/n4/r/n樣品的純度/r/n(/r/n寫出計算過程/r/n)/r/n:/r/n_______/r/n。/r/n(1)/r/n除去氣體中的/r/nHCl3Cl/r/n2/r/n+2Fe(OH)/r/n3/r/n+10OH/r/n-/r/n=2/r/n+6Cl/r/n-/r/n+8H/r/n2/r/nO/r/n過量氯氣使溶液顯酸性,在酸性溶液中/r/nK/r/n2/r/nFeO/r/n4/r/n產(chǎn)生/r/nO/r/n2/r/n,在堿性溶液中較穩(wěn)定/r/n(2)/r/n將鐵礦石粉碎,邊攪拌邊加入鹽酸至礦石不再溶解,過濾,向濾液中加入/r/nNaOH/r/n溶液至不再產(chǎn)生沉淀,過濾,洗滌至洗滌濾液滴加硝酸銀不產(chǎn)生沉淀,干燥/r/n(3)n(/r/n硫酸亞鐵銨/r/n)=0.1000mol·L/r/n-1/r/n×15×10/r/n-3/r/nL=1.5×10/r/n-3/r/nmol/r/n,/r/n根據(jù)關(guān)系式2FeO/r/n4/r/n2-/r/n~2CrO/r/n4/r/n2-/r/n~Cr/r/n2/r/nO/r/n7/r/n2-/r/n~6Fe/r/n2+/r/n;/r/nn(K/r/n2/r/nFeO/r/n4/r/n)=/r/n5×10/r/n-4/r/nmol/r/nK/r/n2/r/nFeO/r/n4/r/n產(chǎn)品的純度/r/n=/r/n82.50%/r/n【分析】/r/n高錳酸鉀和濃鹽酸反應(yīng)制取氯氣,用飽和食鹽水除去氯氣中的氯化氫,氯氣、/r/nFe(OH)/r/n3/r/n、過量/r/nKOH/r/n溶液在/r/nC/r/n中反應(yīng)生成/r/nK/r/n2/r/nFeO/r/n4/r/n,/r/nD/r/n裝置吸收剩余氯氣,防止污染。/r/n(1)/r/n①/r/nA/r/n中高錳酸鉀和濃鹽酸反應(yīng)制取氯氣,用/r/nB/r/n中的飽和食鹽水除去氯氣中的氯化氫;/r/n②裝置/r/nC/r/n中氯氣、/r/nFe(OH)/r/n3/r/n、過量/r/nKOH/r/n溶液發(fā)生反應(yīng)制備/r/nK/r/n2/r/nFeO/r/n4/r/n,根據(jù)電子守恒配平離子方程式為/r/n3Cl/r/n2/r/n+2Fe(OH)/r/n3/r/n+10OH/r/n-/r/n=2/r/n+6Cl/r/n-/r/n+8H/r/n2/r/nO/r/n;/r/n③過量氯氣使溶液顯酸性,在酸性溶液中/r/nK/r/n2/r/nFeO/r/n4/r/n產(chǎn)生/r/nO/r/n2/r/n,在堿性溶液中較穩(wěn)定,所以當裝置/r/nC/r/n中得到大量紫色固體時立即停止通入/r/nCl/r/n2/r/n;/r/n(2)/r/n將鐵礦石粉碎,邊攪拌邊加入鹽酸至礦石不再溶解,過濾,向濾液中加入/r/nNaOH/r/n溶液至不再產(chǎn)生沉淀,過濾,洗滌至洗滌濾液滴加硝酸銀不產(chǎn)生沉淀,干燥制得高純度/r/nFe(OH)/r/n3/r/n;/r/n(3)/r/n根據(jù)/r/nCr(OH)/r/n+/r/n=Fe(OH)/r/n3/r/n+/r/n+OH/r/n-/r/n、/r/n2/r/n+2H/r/n+/r/n=/r/n+H/r/n2/r/nO/r/n、/r/n+6Fe/r/n2+/r/n+14H/r/n+/r/n→2Cr/r/n3+/r/n+6Fe/r/n3+/r/n+7H/r/n2/r/nO/r/n得關(guān)系式/r/n2FeO/r/n4/r/n2-/r/n~2CrO/r/n4/r/n2-/r/n~Cr/r/n2/r/nO/r/n7/r/n2-/r/n~6Fe/r/n2+/r/n;/r/nn(/r/n硫酸亞鐵銨/r/n)=0.1000mol·L/r/n-1/r/n×15×10/r/n-3/r/nL=1.5×10/r/n-3/r/nmol/r/n,/r/n根據(jù)關(guān)系式/r/n2FeO/r/n4/r/n2-/r/n~2CrO/r/n4/r/n2-/r/n~Cr/r/n2/r/nO/r/n7/r/n2-/r/n~6Fe/r/n2+/r/n;/r/nn(K/r/n2/r/nFeO/r/n4/r/n)=/r/n5×10/r/n-4/r/nmol/r/nK/r/n2/r/nFeO/r/n4/r/n產(chǎn)品的純度/r/n=/r/n82.50%/r/n;/r/n6.(山東青島市/r/n高三模擬/r/n)/r/n丙烯酸酯類聚合物能降低原油的凝點,改善其低溫流動性,實現(xiàn)自動化輸油。實驗室合成降凝劑所需的丙烯酸十八酯的裝置如圖,可能用到的有關(guān)數(shù)據(jù)如表。/r/n十八醇/r/n丙烯酸/r/n甲苯/r/n丙烯酸十八酯/r/n相對分子質(zhì)量/r/n270/r/n72/r/n92/r/n324/r/n密度/r/n/g?cm/r/n-3/r/n0.81/r/n1.05/r/n0.90/r/n0.80/r/n沸點/r/n//r/n℃/r/n210/r/n141/r/n110.6/r/n402/r/n說中溶解度/r/n難溶/r/n可溶/r/n難溶/r/n難溶/r/n實驗步驟:/r/nⅠ/r/n./r/n向儀器甲中依次加入十八醇/r/n(C/r/n18/r/nH/r/n37/r/nOH)/r/n、阻凝劑、攜水分/r/n劑,安裝好其他儀器。/r/nⅡ/r/n./r/n攪拌、加熱,瓶內(nèi)試劑完全溶解后加入丙烯酸、催化劑,加熱至回流溫度/r/n115/r/n~/r/n120/r/n℃,待分水器水量達到理論量時停止甲加熱。/r/nⅢ/r/n./r/n取甲中產(chǎn)物倒入分液漏斗中,先后用/r/n5%Na/r/n2/r/nCO/r/n3/r/n溶液和蒸餾水多次洗滌,分液后有機層加入無水/r/nMgSO/r/n4/r/n,靜置、過濾,得粗產(chǎn)品,進一步提純,得純凈產(chǎn)品。/r/n回答下列問題:/r/n(1)/r/n儀器甲名稱/r/n___/r/n,儀器乙的作用為/r/n____/r/n。/r/n(2)/r/n步驟Ⅱ生成丙烯酸十八酯的反應(yīng)方程式為/r/n___/r/n,保持回流溫度恒定可采用的加熱方式為/r/n___(/r/n填標號/r/n)/r/na./r/n沸水浴/r/nb./r/n鹽浴/r/nc./r/n電加熱套/r/nd./r/n油浴/r/n(3)/r/n為將反應(yīng)生成的水及時移出,需加入攜水劑。實驗選用甲苯做攜水劑的原因/r/n__/r/n。/r/n(4)/r/n用/r/n5%Na/r/n2/r/nCO/r/n3/r/n溶液水洗的目的/r/n___/r/n,加入無水/r/nMgSO/r/n4/r/n的目的/r/n____/r/n。/r/n(5)/r/n步驟Ⅲ進一步提純,在該提純步驟中會用到的儀器有/r/n____(/r/n填標號/r/n)/r/n。/r/n(1)/r/n三頸燒瓶/r/n/r/n冷凝回流/r/n(2)CH/r/n2/r/n=CHCOOH+C/r/n18/r/nH/r/n37/r/nOH/r/nCH/r/n2/r/n=CHCOOC/r/n18/r/nH/r/n37/r/n+H/r/n2/r/nObcd(3)/r/n甲苯的沸點和水的沸點相差小于/r/n30/r/n℃,且甲苯不溶于水,所以甲苯可作攜水劑/r/n(4)/r/n除去剩余的丙烯酸/r/n/r/n干燥有機物/r/n(5)bcf/r/n(1)/r/n根據(jù)裝置圖分析可以知道儀器甲為三頸燒瓶,儀器乙為冷凝管,其作用為冷凝回流,故三頸燒瓶;冷凝回流;/r/n(2)/r/n丙烯酸和十八醇/r/n(C/r/n18/r/nH/r/n37/r/nOH)/r/n在催化劑、加熱條件下發(fā)生酯化反應(yīng)生成丙烯酸十八酯和水,反應(yīng)方程式為/r/nCH/r/n2/r/n=CHCOOH+C/r/n18/r/nH/r/n37/r/nOH/r/nCH/r/n2/r/n=CHCOOC/r/n18/r/nH/r/n37/r/n+H/r/n2/r/nO/r/n;該反應(yīng)溫度為/r/n115/r/n~/r/n120/r/n℃,超過了水的沸點,故不能用沸水浴,若要保持回流溫度恒定可采用的加熱方式可以為鹽浴、電加熱套、油浴,故選/r/nbcd/r/n,故/r/nCH/r/n2/r/n=CHCOOH+C/r/n18/r/nH/r/n37/r/nOH/r/nCH/r/n2/r/n=CHCOOC/r/n18/r/nH/r/n37/r/n+H/r/n2/r/nO/r/n;/r/nbcd/r/n;/r/n(3)/r/n由于甲苯的沸點和水的沸點相近,因此甲苯和水產(chǎn)生共沸,與水一起蒸出,然后在分水器中分層,因此可作為攜水劑,故甲苯的沸點和水的沸點相差小于/r/n30/r/n℃,且甲苯不溶于水,所以甲苯可作攜水劑;/r/n(4)/r/n由于反應(yīng)后還會存在多余的反應(yīng)物丙烯酸,因此要采用弱堿性的/r/n5%Na/r/n2/r/nCO/r/n3/r/n溶液來中和;由于水洗后的有機物中會存在少量水分,加入無水/r/nMgSO/r/n4/r/n來作為吸水劑干燥除水,故除去剩余的丙烯酸;干燥有機物;/r/n(5)/r/n產(chǎn)物經(jīng)過洗滌干燥,混有的丙烯酸和水已被除去,主要雜質(zhì)還有十八醇,為了提高產(chǎn)物的純度需要進行蒸餾,蒸餾需要用到的儀器有蒸餾燒瓶、直形冷凝管和酒精燈,不能用到的是分液漏斗、球形冷凝管和恒壓分液漏斗,故選/r/nbcf/r/n,故/r/nbcf/r/n。/r/n8.(山東煙臺市/r/n高三/r/n三模)CuCl/r/n是一種重要化工原料,常用作催化劑、殺菌劑?;瘜W(xué)小組利用下圖裝置/r/n(/r/n部分夾持裝置略去/r/n)/r/n制備氯化亞銅。/r/n已知:/r/n①CuCl/r/n為白色固體,微溶于水,不溶于酒精,在空氣中能被迅速氧化。/r/n②CuCl/r/n能溶于氨水,/r/n[Cu(NH/r/n3/r/n)/r/n2/r/n]/r/n+/r/n無色/r/n實驗步驟:/r/nI./r/n向/r/n的/r/nCuCl/r/n2/r/n溶液中,加入/r/n的/r/nNaOH/r/n溶液/r/n30mL/r/n;打開/r/nA/r/n中分液漏斗的活塞產(chǎn)生/r/nSO/r/n2/r/n氣體,一段時間后/r/nC/r/n中產(chǎn)生白色固體。/r/nII./r/n將/r/nC/r/n中混合物過濾、洗滌、干燥得/r/nCuCl/r/n產(chǎn)品。/r/n回答下列問題:/r/n(1)/r/n儀器/r/na/r/n的名稱/r/n_____/r/n,裝置/r/nB/r/n的作用是/r/n_____/r/n。/r/n(2)/r/n步驟/r/nI/r/n中通入/r/nSO/r/n2/r/n發(fā)生反應(yīng)的離子方程式/r/n____/r/n。/r/n(3)/r/n步驟/r/nII/r/n采用抽濾法快速過濾,防止濾渣被空氣氧化為/r/nCu/r/n2/r/n(OH)/r/n3/r/nCl/r/n。/r/nCuCl/r/n被氧化為/r/nCu/r/n2/r/n(OH)/r/n3/r/nCl/r/n的化學(xué)方程式為/r/n___/r/n;用/r/n95%/r/n的乙醇代替蒸餾水洗滌的優(yōu)點是/r/n____/r/n。/r/n(4)/r/n判斷/r/nCuCl/r/n沉淀洗滌干凈的實驗方案是/r/n___/r/n。/r/n(5)CuCl/r/n樣品加氨水溶解后露置于空氣中迅速得到深藍色溶液,深藍色是由于溶液中陽離子/r/n__(/r/n填化學(xué)式/r/n)/r/n呈現(xiàn)的。/r/n(6)/r/n準確稱取所制備的氯化亞銅樣品/r/nmg/r/n,將其置于過量的/r/nFeCl/r/n3/r/n溶液中,待樣品完全溶解后,加入適量稀硫酸,用/r/namol·L/r/n-1/r/n的/r/nK/r/n2/r/nCr/r/n2/r/nO/r/n7/r/n溶液滴定到終點,消耗/r/nK/r/n2/r/nCr/r/n2/r/nO/r/n7/r/n溶液/r/nbmL/r/n,反應(yīng)中/r/n被還原為/r/nCr/r/n3+/r/n(/r/n該條件下/r/nCl/r/n-/r/n不反應(yīng)/r/n)/r/n,樣品中/r/nCuCl/r/n的質(zhì)量分數(shù)為/r/n___/r/n。/r/n(1)/r/n蒸餾燒瓶/r/n/r/n作為安全瓶,防止倒吸,并可以降低二氧化硫在溶液中的溶解度/r/n(2)/r/n(3)/r/nCuCl/r/n難溶于乙醇,且乙醇易揮發(fā)/r/n(4)/r/n取最后一次洗滌液于試管中,向其中滴加硝酸銀溶液,若無白色沉淀生成,則洗滌干凈/r/n(5)[Cu(NH/r/n3/r/n)/r/n4/r/n]/r/n2+/r/n(6)/r/n/r/n【分析】/r/nA中亞硫酸鈉與濃硫酸反應(yīng)制取二氧化硫,B中亞硫酸氫鈉能除去水,二氧化硫不溶于亞硫酸鈉溶液,B中長頸漏斗與外界連通可以平衡內(nèi)外的氣壓,起到防倒吸的作用,同時飽和亞硫酸氫鈉溶液可以降低二氧化硫在水中的溶解度,減少二氧化硫的損失,C中在氯化銅溶液中滴加氫氧化鈉反應(yīng)生成氫氧化銅,氫氧化銅懸濁液中通入二氧化硫,發(fā)生氧化還原反應(yīng)得到氯化亞銅,D中用來吸收尾氣,據(jù)此分析解題。/r/n(1)/r/n由儀器/r/na/r/n的構(gòu)造可知/r/na/r/n為蒸餾燒瓶,/r/nB/r/n中長頸漏斗與外界連通可以平衡內(nèi)外的氣壓,起到防倒吸的作用,同時飽和亞硫酸氫鈉溶液可以降低二氧化硫在水中的溶解度,減少二氧化硫的損失,故蒸餾燒瓶;作為安全瓶,防止倒吸,并可以降低二氧化硫在溶液中的溶解度;/r/n(2)/r/n步驟/r/nI/r/n中在氯化銅溶液中滴加氫氧化鈉反應(yīng)生成氫氧化銅,氫氧化銅懸濁液中通入二氧化硫,發(fā)生氧化還原反應(yīng)得到氯化亞銅,反應(yīng)的方程式為:/r/n;故/r/n;/r/n(3)CuCl/r/n被氧氣氧化為/r/nCu/r/n2/r/n(OH)/r/n3/r/nCl/r/n,反應(yīng)的方程式為:/r/n;/r/nCuCl/r/n不溶于酒精,用/r/n95%/r/n的乙醇代替蒸餾水洗滌可減少/r/nCuCl/r/n的損失,且乙醇易揮發(fā),固體上的乙醇容易分離,故/r/n;/r/nCuCl/r/n難溶于乙醇,且乙醇易揮發(fā);/r/n(4)/r/n判斷/r/nCuCl/r/n沉淀洗滌干凈需檢驗洗滌液中是否存在氯離子,取最后一次的洗滌液加硝酸銀溶液觀察是否生成白色的氯化銀沉淀,故取最后一次洗滌液于試管中,向其中滴加硝酸銀溶液,若無白色沉淀生成,則洗滌干凈;/r/n(5)CuCl/r/n在空氣中迅速被氧化成/r/nCuCl/r/n2/r/n,加氨水后會形成四氨合銅離子,為深藍色的溶液,故/r/n[Cu(NH/r/n3/r/n)/r/n4/r/n]/r/n2+/r/n;/r/n(6)/r/n過程中的發(fā)生的反應(yīng)有:/r/n、/r/n,可知:/r/n,樣品中/r/nCuCl/r/n的質(zhì)量分數(shù)為/r/n=/r/n,故/r/n;/r/n9.(江蘇南通市/r/n高三模擬/r/n)/r/n三氯化六氨合鈷/r/n(III){[Co(NH/r/n3/r/n)/r/n6/r/n]Cl/r/n3/r/n}/r/n是制備其它三價鈷配合物的重要試劑。實驗室以活性炭為催化劑,合成三氯化六氨合鈷/r/n(III)/r/n晶體的流程如圖/r/n已知:①/r/nCo/r/n2+/r/n不易被氧化,/r/nCo/r/n3+/r/n具有強氧化性;/r/n[Co(NH/r/n3/r/n)/r/n6/r/n]/r/n2+/r/n具有較強還原性,/r/n[Co(NH/r/n3/r/n)/r/n6/r/n]/r/n3+/r/n性質(zhì)穩(wěn)定。/r/n②/r/n[Co(NH/r/n3/r/n)/r/n6/r/n]Cl/r/n3/r/n·6H/r/n2/r/nO/r/n在水中的溶解度隨溫度的升高而增大,加入濃鹽酸有利于晶體析出。/r/n(1)“/r/n混合/r/n”/r/n時加入的/r/nNH/r/n4/r/nCl/r/n溶液有利于后續(xù)/r/nCo/r/n2+/r/n與/r/nNH/r/n3/r/n的配合反應(yīng),其原理是/r/n_______/r/n。/r/n(2)/r/n在如圖所示實驗裝置的三頸燒瓶中,發(fā)生/r/n“/r/n配合、氧化/r/n”/r/n。/r/n①控制三頸燒瓶中溶液溫度為/r/n60℃/r/n的原因是/r/n_______/r/n。/r/n②/r/n“/r/n配合/r/n”/r/n步驟安排在/r/n“/r/n氧化/r/n”/r/n步驟之前的目的是/r/n_______/r/n。/r/n③向三頸燒瓶中滴加氨水的實驗操作為/r/n_______/r/n。加入/r/nH/r/n2/r/nO/r/n2/r/n溶液時發(fā)生反應(yīng)的離子方程式為/r/n_______/r/n。/r/n(3)/r/n設(shè)計由過濾后的濾渣獲?。?r/nCo(NH/r/n3/r/n)/r/n6/r/n]Cl/r/n3/r/n·6H/r/n2/r/nO/r/n的實驗方案:向濾渣中加入/r/n80℃/r/n左右的熱水,/r/n_______/r/n,低溫干燥。/r/n(/r/n實驗中須使用的試劑:濃鹽酸、無水乙醇/r/n)/r/n(1)/r/n抑制/r/nNH/r/n3/r/n·H/r/n2/r/nO/r/n的電離和/r/nCo/r/n2+/r/n的水解/r/n(2)/r/n保證較快的反應(yīng)速率,同時減少氨的揮發(fā)/r/n/r/n將不易被氧化的/r/nCo/r/n2+/r/n轉(zhuǎn)化為具有較強還原性的/r/n[Co(NH/r/n3/r/n)/r/n6/r/n]/r/n2+/r/n/r/n打開分液漏斗上口塞子/r/n(/r/n或?qū)⑷由系陌疾叟c瓶口上的小孔對齊/r/n)/r/n,旋開分液漏斗的/r/n/r/n旋塞,逐滴滴加/r/n2[Co(NH/r/n3/r/n)/r/n6/r/n]/r/n2+/r/n+H/r/n2/r/nO/r/n2/r/n+2NH/r/n=2[Co(NH/r/n3/r/n)/r/n6/r/n]/r/n3+/r/n+2NH/r/n3/r/n·H/r/n2/r/nO(3)/r/n充分攪拌后,趁熱過濾,冷卻后向濾液中加入少量濃鹽酸,邊加邊攪拌,充分靜置后過/r/n/r/n濾,用無水乙醇洗滌晶體/r/n2~3/r/n次/r/n/r/n【分析】/r/n將/r/nCoCl/r/n2/r/n?6H/r/n2/r/nO/r/n、/r/nNH/r/n4/r/nCl/r/n溶液、活性炭混合,加入氨水得到/r/n[Co(NH/r/n3/r/n)/r/n6/r/n]Cl/r/n2/r/n,再加入/r/nH/r/n2/r/nO/r/n2/r/n的水溶液,在活性炭的催化作用下,溶液中/r/nCo(II)/r/n被氧化為/r/nCo(Ⅲ)/r/n,生成/r/n[Co(NH/r/n3/r/n)/r/n6/r/n]Cl/r/n3/r/n和活性炭的濁液,過濾,得到濾渣中含有/r/n[Co(NH/r/n3/r/n)/r/n6/r/n]Cl/r/n3/r/n和活性炭,向濾渣中加入/r/n80℃/r/n左右的熱水,充分攪拌后,趁熱過濾,冷卻后向濾液中加入少量濃鹽酸,邊加邊攪拌,充分靜置后過/r/n/r/n濾,用無水乙醇洗滌晶體/r/n2~3/r/n次,低溫干燥得到產(chǎn)品。/r/n(1)NH/r/n4/r/nCl/r/n能抑制/r/nNH/r/n3/r/n·H/r/n2/r/nO/r/n的電離,防止氫氧化根離子與/r/nCo/r/n2+/r/n結(jié)合,同時/r/nNH/r/n4/r/nCl/r/n溶液顯酸性,能抑制/r/nCo/r/n2+/r/n的水解。/r/n(2)/r/n①控制三頸燒瓶中溶液溫度為/r/n60℃/r/n的原因是既能保證較快的反應(yīng)速率,同時減少氨的揮發(fā)。/r/n②根據(jù)已知①,/r/n“/r/n配合/r/n”/r/n步驟安排在/r/n“/r/n氧化/r/n”/r/n步驟之前的目的是將不易被氧化的/r/nCo/r/n2+/r/n轉(zhuǎn)化為具有較強還原性的/r/n[Co(NH/r/n3/r/n)/r/n6/r/n]/r/n2+/r/n。/r/n③向三頸燒瓶中滴加氨水的實驗操作為打開分液漏斗上口塞子/r/n(/r/n或?qū)⑷由系陌疾叟c瓶口上的小孔對齊/r/n)/r/n,旋開分液漏斗的旋塞,逐滴滴加。加入/r/nH/r/n2/r/nO/r/n2/r/n溶液時發(fā)生反應(yīng)的離子方程式為/r/n2[Co(NH/r/n3/r/n)/r/n6/r/n]/r/n2+/r/n+H/r/n2/r/nO/r/n2/r/n+2NH/r/n=2[Co(NH/r/n3/r/n)/r/n6/r/n]/r/n3+/r/n+2NH/r/n3/r/n·H/r/n2/r/nO/r/n。/r/n(3)[Co(NH/r/n3/r/n)/r/n6/r/n]Cl/r/n3/r/n·6H/r/n2/r/nO/r/n在水中的溶解度隨溫度的升高而增大,加入濃鹽酸有利于晶體析出,故實驗方案為:向濾渣中加入/r/n80℃/r/n左右的熱水,充分攪拌后,趁熱過濾,冷卻后向濾液中加入少量濃鹽酸,邊加邊攪拌,充分靜置后過/r/n/r/n濾,用無水乙醇洗滌晶體/r/n2~3/r/n次,低溫干燥。/r/n10.(山東濰坊市/r/n高三/r/n三模)/r/n亞硝酰硫酸/r/n(NOSO/r/n4/r/nH)/r/n是一種淺黃色液體,遇水易分解,溶于濃硫酸,主要用于染料、醫(yī)藥領(lǐng)域的重氮化反應(yīng)。實驗室用如圖裝置/r/n(/r/n夾持裝置略/r/n)/r/n制備少量/r/nNOSO/r/n4/r/nH/r/n,并測定產(chǎn)品中雜質(zhì)硝酸的含量。/r/n回答下列問題:/r/n(1)/r/n裝置/r/nA/r/n中盛裝/r/nNa/r/n2/r/nSO/r/n3/r/n固體的儀器名稱是/r/n_______/r/n,裝置/r/nD/r/n最好選用/r/n_______(/r/n填序號/r/n)/r/n。/r/n(2)/r/n裝置/r/nC/r/n中濃/r/nHNO/r/n3/r/n與/r/nSO/r/n2/r/n在濃/r/nH/r/n2/r/nSO/r/n4/r/n作用下反應(yīng)制得/r/nNOSO/r/n4/r/nH/r/n。/r/n①裝置/r/nC/r/n中溫度過高產(chǎn)率降低的原因是/r/n_______/r/n。/r/n②開始通/r/nSO/r/n2/r/n時,反應(yīng)緩慢,待生成少量/r/nNOSO/r/n4/r/nH/r/n后,溫度變化不大,但反應(yīng)速率明顯加快,其原因是/r/n_______/r/n。/r/n(3)/r/n測定亞硝酰硫酸產(chǎn)品中雜質(zhì)硝酸的含量。/r/n稱取/r/n1.400g/r/n產(chǎn)品放入/r/n250mL/r/n錐形瓶中,加/r/n80mL/r/n濃硫酸,用/r/n標準溶液滴定,消耗標準溶液/r/n20.00mL/r/n。/r/n已知:/r/n可與/r/nNO/r/n生成粉紅色的/r/nFeSO/r/n4/r/n·NO/r/n。/r/n①錐形瓶中加入濃硫酸的作用是/r/n_______/r/n。/r/n②判斷滴定達到終點的現(xiàn)象是/r/n_______/r/n。/r/n(1)/r/n蒸餾燒瓶/r/nb(2)/r/n濃硝酸分解,二氧化硫逸出/r/n/r/n生成的/r/nNOSO/r/n4/r/nH/r/n作為該反應(yīng)的催化劑/r/n(3)/r/n作溶劑,同時作吸水劑,防止亞硝酰硫酸遇水分解/r/n/r/n滴入最后一滴/r/n(NH/r/n4/r/n)/r/n2/r/nFe(SO/r/n4/r/n)/r/n2/r/n標準液,溶液突變?yōu)榉奂t色,且/r/n30s/r/n內(nèi)不變色/r/n/r/n【分析】/r/n裝置/r/nA/r/n中/r/nNa/r/n2/r/nSO/r/n3/r/n固體與濃硫酸反應(yīng)產(chǎn)生/r/nSO/r/n2/r/n,經(jīng)過裝置/r/nB/r/n干燥/r/nSO/r/n2/r/n,/r/nSO/r/n2/r/n進入/r/nC/r/n中與濃硝酸濃硫酸反應(yīng)生成亞硝酰硫酸,裝置/r/nD/r/n為尾氣處理裝置,且由于產(chǎn)品遇水易分解,故裝置/r/nD/r/n還需防止空氣中水蒸氣進入/r/nC/r/n中,故裝置/r/nD/r/n可以為盛有堿石灰的裝置。/r/n(1)/r/n該儀器為帶支管的燒瓶,故為蒸餾燒瓶;由分析知,裝置/r/nD/r/n可以為盛有堿石灰的裝置,故選擇/r/nb/r/n;/r/n(2)/r/n①由于反應(yīng)物濃硝酸受熱易揮發(fā)易分解,且溫度高不利于/r/nSO/r/n2/r/n溶解,故此處填:溫度過高,濃硝酸分解,/r/nSO/r/n2/r/n溶解度下降逸出;/r/n②由于/r/nSO/r/n2/r/n通入速率不變,且溫度變化不大,但反應(yīng)速率明顯加快,考慮可能是因為反應(yīng)受到了催化,由于是生成少量/r/nNOSO/r/n4/r/nH/r/n后反應(yīng)明顯加快,故此時起催化作用的物質(zhì)應(yīng)該為/r/nNOSO/r/n4/r/nH/r/n,故此處填:生成的/r/nNOSO/r/n4/r/nH/r/n作為該反應(yīng)的催化劑;/r/n(3)/r/n①濃硫酸可將產(chǎn)品溶解,同時起到吸水的目的,防止產(chǎn)品/r/nNOSO/r/n4/r/nH/r/n遇水分解,故此處填:作溶劑,同時作吸水劑,防止/r/nNOSO/r/n4/r/nH/r/n遇水分解;/r/n②當?shù)味ㄟ_終點后,再加入標準液,此時過量的/r/nFe/r/n2+/r/n會與反應(yīng)生成的/r/nNO/r/n結(jié)合生成粉紅色/r/nFeSO/r/n4/r/n·/r/nNO/r/n,故此處填:滴入最后一滴/r/n(NH/r/n4/r/n)/r/n2/r/nFe(SO/r/n4/r/n)/r/n2/r/n標準液,溶液突變?yōu)榉奂t色,且/r/n30s/r/n內(nèi)不變色;/r/n11.(遼寧高三三模)/r/n溴化亞鐵/r/n(FeBr/r/n2/r/n)/r/n是棕黃色易潮解的固體,/r/nFe/r/n與/r/nHBr/r/n在高溫下反應(yīng)可以生成/r/nFeBr/r/n2/r/n。某研究性學(xué)習(xí)小組設(shè)計實驗制備少量的/r/nFeBr/r/n2/r/n固體,涉及的裝置如圖所示/r/n(/r/n部分夾持裝置和加熱裝置略/r/n)/r/n:/r/n已知:①/r/nNaBr+H/r/n2/r/nSO/r/n4/r/nNaHSO/r/n4/r/n+HBr↑/r/n;②高溫時,/r/nFeBr/r/n3/r/n會分解為/r/nFeBr/r/n2/r/n。/r/n回答下列問題:/r/n(1)/r/n制備/r/nHBr/r/n時濃硫酸除了體現(xiàn)難揮發(fā)性還體現(xiàn)/r/n____/r/n性,儀器/r/nB/r/n的名稱是/r/n___/r/n。/r/n(2)/r/n裝置/r/nC/r/n中堿石灰的作用有①/r/n___/r/n②/r/n___/r/n。/r/n(3)/r/n實驗時裝置的連接順序是/r/na→____(/r/n按氣流從左到右的方向,填儀器接口小寫字母/r/n)/r/n。/r/n(4)/r/n若反應(yīng)溫度過高,裝置/r/nE/r/n中溶液變?yōu)槌赛S色,寫出可能發(fā)生的化學(xué)反應(yīng)方程式:/r/n___/r/n,該反應(yīng)對/r/nFeBr/r/n2/r/n產(chǎn)品純度沒有影響,可能的原因是/r/n___/r/n。/r/n(5)/r/n實驗結(jié)束后,某同學(xué)取少量上述產(chǎn)品配成/r/nFeBr/r/n2/r/n溶液,向其中滴加少量新制的氯水,振蕩后發(fā)現(xiàn)溶液呈黃色。寫出該反應(yīng)的化學(xué)方程式/r/n___/r/n;繼續(xù)滴加氯水,當/r/nFeBr/r/n2/r/n與/r/nCl/r/n2/r/n物質(zhì)的量相等時反應(yīng)的化學(xué)方程式為/r/n___/r/n。/r/n(1)/r/n強酸/r/n(/r/n球形/r/n)/r/n干燥管/r/n(2)/r/n吸收尾氣中的/r/nHBr/r/n等酸性氣體/r/n/r/n防止空氣中的水蒸氣進入裝置/r/nF(3)fghibcjk(kj)d(e)(4)2NaBr+2H/r/n2/r/nSO/r/n4/r/n(/r/n濃/r/n)/r/nSO/r/n2/r/n↑+Br/r/n2/r/n↑+2H/r/n2/r/nO+Na/r/n2/r/nSO/r/n4/r/nBr/r/n2/r/n與/r/nFe/r/n反應(yīng)生成/r/nFeBr/r/n3/r/n,高溫下/r/nFeBr/r/n3/r/n分解為/r/nFeBr/r/n2/r/n(5)6FeBr/r/n2/r/n+3Cl/r/n2/r/n=2FeCl/r/n3/r/n+4FeBr/r/n3/r/n6FeBr/r/n2/r/n+6Cl/r/n2/r/n=4FeCl/r/n3/r/n+2FeBr/r/n3/r/n+3Br/r/n2/r/n/r/n【分析】/r/n本實驗的目的是利用/r/nHBr/r/n和/r/nFe/r/n高溫下反應(yīng)制備少量的/r/nFeBr/r/n2/r/n固體,/r/nFeBr/r/n2/r/n易被氧化,所以可以先利用稀鹽酸和石灰石反應(yīng)生成二氧化碳,將裝置中的空氣排盡,生成的/r/nCO/r/n2/r/n中含有/r/nHCl/r/n氣體,可以利用飽和碳酸氫鈉溶液除去,之后通入反應(yīng)裝置中排空氣,實驗過程中利用濃硫酸和/r/nNaBr/r/n反應(yīng)制取/r/nHBr/r/n,然后利用裝置/r/nB/r/n干燥/r/nCO/r/n2/r/n和/r/nHBr/r/n,之后再裝置/r/nF/r/n中制取/r/nFeBr/r/n2/r/n,裝置/r/nC/r/n吸收尾氣并防止空氣中的水蒸氣進入裝置/r/nF/r/n使/r/nFeBr/r/n2/r/n水解。/r/n(1)/r/n由于反應(yīng)生成了硫酸氫鈉,該反應(yīng)過程中也體現(xiàn)了硫酸的強酸性;根據(jù)儀器/r/nB/r/n的結(jié)構(gòu)特點可知其為/r/n(/r/n球形/r/n)/r/n干燥管;/r/n(2)/r/n根據(jù)分析可知裝置/r/nC/r/n應(yīng)在最后,可以吸收尾氣中的/r/nHBr/r/n等酸性氣體,同時也可以防止空氣中的水蒸氣進入裝置/r/nF/r/n,使/r/nFeBr/r/n2/r/n水解;/r/n(3)/r/n實驗開始時先用/r/nCO/r/n2/r/n排除裝置內(nèi)的空氣,實驗結(jié)束后,繼續(xù)通入/r/nCO/r/n2/r/n可以使殘留的/r/nHBr/r/n被充分吸收,裝置/r/nA/r/n可以制取/r/nCO/r/n2/r/n,裝置/r/nD/r/n可以除去/r/nCO/r/n2/r/n中混有的/r/nHCl/r/n,裝置/r/nE/r/n制取/r/nHBr/r/n,裝置/r/nB/r/n干燥/r/nCO/r/n2/r/n和/r/nHBr/r/n,之后再裝置/r/nF/r/n中制取/r/nFeBr/r/n2/r/n,裝置/r/nC/r/n吸收尾氣并防止空氣中的水蒸氣進入裝置,所以連接順序為/r/nafghibcjk(kj)d(e)/r/n;/r/n(4)/r/n濃硫酸具有強氧化性,可以將/r/nBr/r/n-/r/n氧化為/r/nBr/r/n2/r/n,/r/nBr/r/n2/r/n的水溶液呈橙黃色,根據(jù)電子守恒和元素守恒可知該反應(yīng)的化學(xué)方程式為/r/n2NaBr+2H/r/n2/r/nSO/r/n4/r/n(/r/n濃/r/n)/r/nSO/r/n2/r/n↑+Br/r/n2/r/n↑+2H/r/n2/r/nO+Na/r/n2/r/nSO/r/n4/r/n;/r/nSO/r/n2/r/n與/r/nFe/r/n不反應(yīng),/r/nBr/r/n2/r/n與/r/nFe/r/n反應(yīng)生成/r/nFeBr/r/n3/r/n,高溫下/r/nFeBr/r/n3/r/n分解為/r/nFeBr/r/n2/r/n,所以對產(chǎn)品純度沒有影響;/r/n(5)/r/n振蕩后發(fā)現(xiàn)溶液呈黃色,說明氯水將/r/nFe/r/n2+/r/n氧化為/r/nFe/r/n3+/r/n,化學(xué)方程式為/r/n6FeBr/r/n2/r/n+3Cl/r/n2/r/n=2FeCl/r/n3/r/n+4FeBr/r/n3/r/n;/r/nFeBr/r/n2/r/n與/r/nCl/r/n2/r/n物質(zhì)的量相等時,不妨設(shè)均為/r/n1mol/r/n,則氧化/r/n1molFe/r/n2+/r/n消耗/r/n0.5mol/r/n氯氣,剩余/r/n0.5mol/r/n氯氣可以氧化/r/n1molBr/r/n-/r/n,所以化學(xué)方程式應(yīng)為/r/n6FeBr/r/n2/r/n+6Cl/r/n2/r/n=4FeCl/r/n3/r/n+2FeBr/r/n3/r/n+3Br/r/n2/r/n。/r/n12.(天津高三二模)/r/n磷化氫/r/n(/r/n)/r/n常用于縮合催化劑、磷的有機化合物制備等。實驗室用白磷/r/n(/r/n)/r/n與濃/r/n(/r/n過量/r/n)/r/n加熱制備/r/n同時得到次磷酸鈉/r/n(/r/n)/r/n裝置如下圖。/r/n已知:/r/n是無色有毒氣體,有強還原性,易自燃。/r/n(1)/r/n儀器/r/na/r/n的名稱為/r/n_______/r/n,/r/nB/r/n應(yīng)選用下圖中裝置/r/n_______/r/n。/r/n(2)/r/n實驗操作有如下步驟:/r/n①打開/r/n,通入/r/n一段時間/r/n②檢查裝置氣密性/r/n③關(guān)閉/r/n,打開磁力加熱攪拌器加熱至/r/n50/r/n℃/r/n~60/r/n℃,滴加燒堿溶液/r/n④在/r/nA/r/n中加入丁醇和白磷。則正確的操作順序是/r/n_______/r/n。/r/n(3)/r/n裝置/r/nA/r/n中發(fā)生反應(yīng)的化學(xué)方程式為/r/n_______/r/n,已知/r/n水溶液/r/n,水溶液/r/n的原因/r/n_______/r/n。/r/n(4)/r/n反應(yīng)結(jié)束后也要打開/r/n,繼續(xù)通入/r/n的目的是/r/n_____/r/n,裝置/r/nD/r/n的作用是/r/n_____/r/n。/r/n(5)/r/n測定/r/n純度。/r/n提純/r/nA/r/n中反應(yīng)后的混合物,得到/r/n(/r/n)/r/n粗品,取/r/n1.00g/r/n配成/r/n溶液,取/r/n于錐形瓶中,酸化后加入/r/n碘水,充分反應(yīng),以淀粉溶液作指示劑,用/r/n溶液滴定至終點,平均消耗/r/n。則產(chǎn)品純度為/r/n_____/r/n。/r/n用/r/n溶液滴定時尖嘴處開始有氣泡,達到滴定終點時無氣泡,則測定結(jié)果/r/n____(“/r/n偏大/r/n”/r/n、/r/n“/r/n偏小/r/n”/r/n或/r/n“/r/n無影響/r/n”)/r/n。/r/n(/r/n相關(guān)反應(yīng)為/r/n,/r/n)/r/n(1)/r/n分液漏斗/r/n/r/n丙/r/n(2)/r/n②④①③/r/n(3)/r/n↑(4)/r/n水解顯堿性或/r/n/r/n防止/r/n被氧化/r/n/r/n吸收多余的/r/n,防止污染空氣/r/n(5)88.0%/r/n偏小/r/n/r/n【分析】/r/n檢漏后打開/r/nK/r/n1/r/n,通入/r/nN/r/n2/r/n一段時間,目的是將裝置中空氣排出,防止/r/nPH/r/n3/r/n被氧化;在/r/nA/r/n中加入丁醇和白磷,關(guān)閉/r/nK/r/n1/r/n,打開磁力加熱攪拌器加熱至/r/n50/r/n℃~/r/n60/r/n℃,滴加燒堿溶液,根據(jù)題干信息知,在加熱條件下,白磷/r/n(P/r/n4/r/n)/r/n與濃/r/nNaOH/r/n反應(yīng)生成/r/nPH/r/n3/r/n,同時得到次磷酸鈉/r/n(NaH/r/n2/r/nPO/r/n2)/r/n,/r/nPH/r/n3/r/n是無色有毒氣體,且具有還原性,所以應(yīng)該用強氧化性物質(zhì)氧化而防止污染大氣,且要防止倒吸,/r/nB/r/n用于收集/r/nPH/r/n3/r/n,/r/nC/r/n裝置是安全瓶/r/n(/r/n防止倒吸/r/n)/r/n,/r/nD/r/n裝置是吸收尾氣。/r/n(1)/r/n儀器/r/na/r/n的名稱為分液漏斗;/r/nPH/r/n3/r/n密度大于氮氣,所以應(yīng)該采用向上排氮氣的方法收集,故/r/nB/r/n應(yīng)選用裝置丙;/r/n(2/r/n實驗前應(yīng)該檢驗裝置是否漏氣,然后向/r/nA/r/n加入丁醇和白磷,再通入氮氣將裝置中空氣排盡,防止/r/nPH/r/n3/r/n被氧化,最后滴加/r/nNaOH/r/n溶液,所以正確的操作順序是②④①③;/r/n(3)/r/n通過以上分析知,裝置/r/nA/r/n中發(fā)生反應(yīng)的化學(xué)方程式為/r/nP/r/n4/r/n+3NaOH+3H/r/n2/r/nO/r/n3NaH/r/n2/r/nPO/r/n2/r/n+PH/r/n3/r/n↑/r/n;/r/n為弱酸酸式根,在溶液中會發(fā)生水解而使溶液顯堿性,故此處填:/r/n水解顯堿性(或/r/n+H/r/n2/r/nO/r/nH/r/n3/r/nPO/r/n2/r/n+OH/r/n-/r/n);/r/n(4)/r/n反應(yīng)結(jié)束后也要打開/r/nK/r/n1/r/n,繼續(xù)通入/r/nN/r/n2/r/n的目的是防止/r/nPH/r/n3/r/n被氧化;/r/nPH/r/n3/r/n是無色有毒氣體且易被氧化,為防止污染空氣,應(yīng)該用強氧化性物質(zhì)吸收,所以/r/nD/r/n的作用是吸收尾氣,防止污染空氣;/r/n(5)c/r/n中生成/r/nNaH/r/n2/r/nPO/r/n2/r/n和/r/nNaCl/r/n,從表知:/r/nNaH/r/n2/r/nPO/r/n2/r/n的溶解度隨溫度升高而急劇增大、而/r/nNaCl/r/n的溶解度隨溫度變化不大,故充分反應(yīng)后/r/nc/r/n中分離出/r/nNaH/r/n2/r/nPO/r/n2/r/n粗產(chǎn)品的操作是蒸發(fā)濃縮、趁熱過濾得氯化鈉晶體、濾液冷卻結(jié)晶過濾得/r/nNaH/r/n2/r/nPO/r/n2/r/n、經(jīng)洗滌后干燥;/r/n(7)/r/n/r/n,根據(jù)方程式/r/n/r/n知:/r/nNa/r/n2/r/nS/r/n2/r/nO/r/n3/r/n消耗的/r/n/r/n,則/r/nNaH/r/n2/r/nPO/r/n2/r/n消耗的/r/n/r/n,根據(jù)方程式/r/n知,/r/n/r/n,則/r/n100mL/r/n溶液中/r/n,/r/n,/r/nNaH/r/n2/r/nPO/r/n2/r/n純度/r/n;由題意知,滴定后尖嘴處充滿標準液,實際尖嘴處的標準液未參與反應(yīng),故所計標準液體積偏大,導(dǎo)致測出的剩余/r/nI/r/n2/r/n的量偏大,則算出與樣品反應(yīng)的/r/nI/r/n2/r/n偏少,故所測結(jié)果偏小。/r/n13.(江蘇南京市·南京師大附中高三/r/n模擬/r/n)/r/n工業(yè)上常利用含硫廢水生產(chǎn)/r/nNa/r/n2/r/nS/r/n2/r/nO/r/n3/r/n·/r/n5H/r/n2/r/nO/r/n,某小組同學(xué)用如下圖裝置/r/n(/r/n略去加熱儀器等/r/n)/r/n模擬生產(chǎn)過程。/r/n已知:/r/ni./r/n燒瓶/r/nC/r/n中發(fā)生反應(yīng)如下:/r/nNa/r/n2/r/nS(aq)/r/n+/r/nH/r/n2/r/nO(l)/r/n+/r/nSO/r/n2/r/n(g)=Na/r/n2/r/nSO/r/n3/r/n(aq)/r/n+/r/nH/r/n2/r/nS(aq)/r/n/r/n(a)/r/n2H/r/n2/r/nS(aq)/r/n+/r/nSO/r/n2/r/n(g)=3S(s)/r/n+/r/n2H/r/n2/r/nO(l)/r/n/r/n(b)/r/nS(s)/r/n+/r/nNa/r/n2/r/
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