聚(ju)(ju)(ju)(ju)氧(yang)(yang)(yang)化(hua)(hua)乙(yi)(yi)(yi)烯(25322-68-3)的(de)(de)(de)(de)(de)(de)制(zhi)备(bei)(bei)方(fang)法(fa)： 由乙(yi)(yi)(yi)二(er)(er)醇(chun)(chun)(chun)(chun)缩(suo)聚(ju)(ju)(ju)(ju)或(huo)(huo)(huo)由环(huan)氧(yang)(yang)(yang)乙(yi)(yi)(yi)烷与(yu)水(shui)(shui)(shui)(shui)加(jia)聚(ju)(ju)(ju)(ju)而(er)(er)得。 鉴别试(shi)(shi)验： 溶(rong)(rong)(rong)(rong)解(jie)(jie)性(xing)：表(biao)观(guan)(guan)分(fen)(fen)(fen)子(zi)量(liang)(liang)(liang)在(zai)1000(或(huo)(huo)(huo)以(yi)(yi)上)的(de)(de)(de)(de)(de)(de)聚(ju)(ju)(ju)(ju)乙(yi)(yi)(yi)二(er)(er)醇(chun)(chun)(chun)(chun)，极易(yi)溶(rong)(rong)(rong)(rong)于(yu)(yu)(yu)水(shui)(shui)(shui)(shui)。聚(ju)(ju)(ju)(ju)乙(yi)(yi)(yi)二(er)(er)醇(chun)(chun)(chun)(chun)溶(rong)(rong)(rong)(rong)于(yu)(yu)(yu)许多(duo)有机溶(rong)(rong)(rong)(rong)剂，包括脂肪族酮(tong)类(lei)(lei)和(he)(he)(he)(he)醛类(lei)(lei)、三氯甲(jia)烷、乙(yi)(yi)(yi)二(er)(er)醇(chun)(chun)(chun)(chun)醚(mi)、酯类(lei)(lei)及芳香族碳(tan)氢(qing)(qing)化(hua)(hua)合(he)(he)物(wu)；不溶(rong)(rong)(rong)(rong)于(yu)(yu)(yu)乙(yi)(yi)(yi)醚(mi)和(he)(he)(he)(he)大多(duo)数脂肪族碳(tan)氢(qing)(qing)化(hua)(hua)合(he)(he)物(wu)。在(zai)水(shui)(shui)(shui)(shui)和(he)(he)(he)(he)有机溶(rong)(rong)(rong)(rong)剂中(zhong)(zhong)(zhong)(zhong)溶(rong)(rong)(rong)(rong)解(jie)(jie)度(du)(du)(du)(du)随着分(fen)(fen)(fen)子(zi)量(liang)(liang)(liang)的(de)(de)(de)(de)(de)(de)提高(gao)而(er)(er)降低。表(biao)观(guan)(guan)分(fen)(fen)(fen)子(zi)量(liang)(liang)(liang)：表(biao)观(guan)(guan)分(fen)(fen)(fen)子(zi)量(liang)(liang)(liang)低于(yu)(yu)(yu)1000者(zhe)，为(wei)(wei)申(shen)报值(zhi)的(de)(de)(de)(de)(de)(de)95.0%～105.0%；表(biao)观(guan)(guan)分(fen)(fen)(fen)子(zi)量(liang)(liang)(liang)在(zai)1000～7000者(zhe)，为(wei)(wei)申(shen)报值(zhi)的(de)(de)(de)(de)(de)(de)90.0%～110.0%；高(gao)于(yu)(yu)(yu)7000者(zhe)，为(wei)(wei)申(shen)报值(zhi)的(de)(de)(de)(de)(de)(de)87.5%～112.5%。 质量(liang)(liang)(liang)指(zhi)标(biao)(biao)(biao)(biao)分(fen)(fen)(fen)析： 1.酸(suan)(suan)(suan)度(du)(du)(du)(du)(以(yi)(yi)醋酸(suan)(suan)(suan)计)取(qu)(qu)试(shi)(shi)样(yang)(yang)6g，放(fang)(fang)(fang)(fang)入(ru)(ru)-250ml三角烧(shao)瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)，加(jia)酚(fen)酞试(shi)(shi)液(ye)(ye)(ye)(TS-167)数滴(di)(di)和(he)(he)(he)(he)中(zhong)(zhong)(zhong)(zhong)性(xing)乙(yi)(yi)(yi)醇(chun)(chun)(chun)(chun)50ml，用(yong)(yong)(yong)(yong)(yong)(yong)(yong)0.1mol/L氢(qing)(qing)氧(yang)(yang)(yang)化(hua)(hua)钾乙(yi)(yi)(yi)醇(chun)(chun)(chun)(chun)液(ye)(ye)(ye)滴(di)(di)定(ding)(ding)至(zhi)(zhi)粉(fen)红(hong)色(se)(se)(se)，并(bing)维持(chi)15s。滴(di)(di)定(ding)(ding)时的(de)(de)(de)(de)(de)(de)耗用(yong)(yong)(yong)(yong)(yong)(yong)(yong)量(liang)(liang)(liang)不得超过(guo)0.5ml。 2.氧(yang)(yang)(yang)化(hua)(hua)乙(yi)(yi)(yi)烯按下述(shu)方(fang)法(fa)测(ce)定(ding)(ding)。 (1)吗(ma)(ma)啉(lin)溶(rong)(rong)(rong)(rong)液(ye)(ye)(ye)的(de)(de)(de)(de)(de)(de)制(zhi)备(bei)(bei)：由一份重(zhong)(zhong)(zhong)(zhong)蒸吗(ma)(ma)啉(lin)和(he)(he)(he)(he)九份无水(shui)(shui)(shui)(shui)甲(jia)醇(chun)(chun)(chun)(chun)混(hun)合(he)(he)而(er)(er)成。 (2)混(hun)合(he)(he)指(zhi)示剂的(de)(de)(de)(de)(de)(de)制(zhi)备(bei)(bei)：取(qu)(qu)4，4′-双-(氨(an)基(ji)-1-萘偶氮2，2′-均二(er)(er)苯代乙(yi)(yi)(yi)烯磺酸(suan)(suan)(suan))0.050g和(he)(he)(he)(he)亮黄0.010g，放(fang)(fang)(fang)(fang)入(ru)(ru)一60ml管形瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)。加(jia)入(ru)(ru)0.1mol/L氢(qing)(qing)氧(yang)(yang)(yang)化(hua)(hua)钠1.5ml，混(hun)合(he)(he)。加(jia)水(shui)(shui)(shui)(shui)3.5ml后混(hun)合(he)(he)。用(yong)(yong)(yong)(yong)(yong)(yong)(yong)45ml甲(jia)醇(chun)(chun)(chun)(chun)将(jiang)(jiang)(jiang)(jiang)上述(shu)混(hun)合(he)(he)物(wu)洗(xi)人贮藏瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)，混(hun)合(he)(he)后备(bei)(bei)用(yong)(yong)(yong)(yong)(yong)(yong)(yong)。 ??? (3)标(biao)(biao)(biao)(biao)准(zhun)(zhun)(zhun)(zhun)盐(yan)酸(suan)(suan)(suan)甲(jia)醇(chun)(chun)(chun)(chun)液(ye)(ye)(ye)的(de)(de)(de)(de)(de)(de)制(zhi)备(bei)(bei)：取(qu)(qu)盐(yan)酸(suan)(suan)(suan)8．5ml，与(yu)1000ml无水(shui)(shui)(shui)(shui)甲(jia)醇(chun)(chun)(chun)(chun)混(hun)合(he)(he)。取(qu)(qu)该液(ye)(ye)(ye)9．00ml，加(jia)酚(fen)酞试(shi)(shi)液(ye)(ye)(ye)(TS-167)数滴(di)(di)，用(yong)(yong)(yong)(yong)(yong)(yong)(yong)0.1mol/L氢(qing)(qing)氧(yang)(yang)(yang)化(hua)(hua)钠液(ye)(ye)(ye)进(jin)行标(biao)(biao)(biao)(biao)定(ding)(ding)。超过(guo)48h后需(xu)重(zhong)(zhong)(zhong)(zhong)新进(jin)行标(biao)(biao)(biao)(biao)定(ding)(ding)。 ??? (4)操(cao)作：取(qu)(qu)无水(shui)(shui)(shui)(shui)甲(jia)醇(chun)(chun)(chun)(chun)50ml，放(fang)(fang)(fang)(fang)入(ru)(ru)-250ml锥形烧(shao)瓶(ping)(ping)。加(jia)上述(shu)混(hun)合(he)(he)指(zhi)示剂4～6滴(di)(di)，用(yong)(yong)(yong)(yong)(yong)(yong)(yong)上述(shu)标(biao)(biao)(biao)(biao)准(zhun)(zhun)(zhun)(zhun)盐(yan)酸(suan)(suan)(suan)甲(jia)醇(chun)(chun)(chun)(chun)液(ye)(ye)(ye)滴(di)(di)定(ding)(ding)至(zhi)(zhi)纯蓝(lan)色(se)(se)(se)。加(jia)试(shi)(shi)样(yang)(yang)约25g(准(zhun)(zhun)(zhun)(zhun)确(que)称重(zhong)(zhong)(zhong)(zhong))，以(yi)(yi)作为(wei)(wei)空(kong)白试(shi)(shi)样(yang)(yang)液(ye)(ye)(ye)，摇振至(zhi)(zhi)完(wan)全(quan)溶(rong)(rong)(rong)(rong)解(jie)(jie)。用(yong)(yong)(yong)(yong)(yong)(yong)(yong)标(biao)(biao)(biao)(biao)准(zhun)(zhun)(zhun)(zhun)盐(yan)酸(suan)(suan)(suan)甲(jia)醇(chun)(chun)(chun)(chun)液(ye)(ye)(ye)滴(di)(di)定(ding)(ding)至(zhi)(zhi)纯蓝(lan)色(se)(se)(se)，临将(jiang)(jiang)(jiang)(jiang)滴(di)(di)定(ding)(ding)终点时应小(xiao)心地少量(liang)(liang)(liang)滴(di)(di)加(jia)。 (5)取(qu)(qu)吗(ma)(ma)啉(lin)溶(rong)(rong)(rong)(rong)液(ye)(ye)(ye)50ml，放(fang)(fang)(fang)(fang)入(ru)(ru)一耐(nai)热(re)耐(nai)压瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)，而(er)(er)取(qu)(qu)等量(liang)(liang)(liang)的(de)(de)(de)(de)(de)(de)吗(ma)(ma)啉(lin)溶(rong)(rong)(rong)(rong)液(ye)(ye)(ye)放(fang)(fang)(fang)(fang)入(ru)(ru)一较小(xiao)的(de)(de)(de)(de)(de)(de)瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)，以(yi)(yi)此作为(wei)(wei)试(shi)(shi)剂空(kong)白液(ye)(ye)(ye)。在(zai)第一只(zhi)(zhi)瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)加(jia)入(ru)(ru)试(shi)(shi)样(yang)(yang)约25g(准(zhun)(zhun)(zhun)(zhun)确(que)称重(zhong)(zhong)(zhong)(zhong))，摇振至(zhi)(zhi)完(wan)全(quan)溶(rong)(rong)(rong)(rong)解(jie)(jie)。密塞，将(jiang)(jiang)(jiang)(jiang)瓶(ping)(ping)牢固裹缠后放(fang)(fang)(fang)(fang)入(ru)(ru)布袋中(zhong)(zhong)(zhong)(zhong)。将(jiang)(jiang)(jiang)(jiang)两只(zhi)(zhi)瓶(ping)(ping)子(zi)紧挨着一起放(fang)(fang)(fang)(fang)入(ru)(ru)98℃±2℃的(de)(de)(de)(de)(de)(de)水(shui)(shui)(shui)(shui)浴中(zhong)(zhong)(zhong)(zhong)。维持(chi)30min，水(shui)(shui)(shui)(shui)浴中(zhong)(zhong)(zhong)(zhong)的(de)(de)(de)(de)(de)(de)水(shui)(shui)(shui)(shui)位(wei)应略高(gao)于(yu)(yu)(yu)瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)液(ye)(ye)(ye)位(wei)。取(qu)(qu)出后于(yu)(yu)(yu)空(kong)气中(zhong)(zhong)(zhong)(zhong)放(fang)(fang)(fang)(fang)冷(leng)至(zhi)(zhi)室温(wen)(wen)。松开裹带(dai)，去盖以(yi)(yi)放(fang)(fang)(fang)(fang)余压，然后取(qu)(qu)掉(diao)裹带(dai)。在(zai)每只(zhi)(zhi)瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)缓慢加(jia)入(ru)(ru)醋酐(gan)20ml，摇至(zhi)(zhi)完(wan)全(quan)溶(rong)(rong)(rong)(rong)解(jie)(jie)。然后于(yu)(yu)(yu)室温(wen)(wen)下放(fang)(fang)(fang)(fang)置15min。如瓶(ping)(ping)子(zi)仍显温(wen)(wen)热(re)，则需(xu)冷(leng)至(zhi)(zhi)室温(wen)(wen)。于(yu)(yu)(yu)每只(zhi)(zhi)瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)加(jia)混(hun)合(he)(he)指(zhi)示剂4～6滴(di)(di)，然后用(yong)(yong)(yong)(yong)(yong)(yong)(yong)标(biao)(biao)(biao)(biao)准(zhun)(zhun)(zhun)(zhun)的(de)(de)(de)(de)(de)(de)盐(yan)酸(suan)(suan)(suan)甲(jia)醇(chun)(chun)(chun)(chun)液(ye)(ye)(ye)滴(di)(di)定(ding)(ding)至(zhi)(zhi)纯蓝(lan)色(se)(se)(se)，临近终点时需(xu)缓慢少量(liang)(liang)(liang)滴(di)(di)加(jia)。 3.乙(yi)(yi)(yi)二(er)(er)醇(chun)(chun)(chun)(chun)和(he)(he)(he)(he)二(er)(er)甘(gan)醇(chun)(chun)(chun)(chun)的(de)(de)(de)(de)(de)(de)测(ce)定(ding)(ding)：表(biao)观(guan)(guan)分(fen)(fen)(fen)子(zi)量(liang)(liang)(liang)低于(yu)(yu)(yu)450的(de)(de)(de)(de)(de)(de)聚(ju)(ju)(ju)(ju)乙(yi)(yi)(yi)二(er)(er)醇(chun)(chun)(chun)(chun)试(shi)(shi)样(yang)(yang)。 ??? ①仪(yi)器：选用(yong)(yong)(yong)(yong)(yong)(yong)(yong)一适(shi)当(dang)的(de)(de)(de)(de)(de)(de)气相色(se)(se)(se)谱(pu)(pu)仪(yi)，接(jie)有一氢(qing)(qing)焰离子(zi)化(hua)(hua)检(jian)测(ce)器，用(yong)(yong)(yong)(yong)(yong)(yong)(yong)一15m×3mm(内径)的(de)(de)(de)(de)(de)(de)不锈钢柱(zhu)；用(yong)(yong)(yong)(yong)(yong)(yong)(yong)60/80目未(wei)酸(suan)(suan)(suan)洗(xi)过(guo)的(de)(de)(de)(de)(de)(de)硅藻土(Chromosorb W或(huo)(huo)(huo)相似品(pin))作为(wei)(wei)载体，用(yong)(yong)(yong)(yong)(yong)(yong)(yong)12%(重(zhong)(zhong)(zhong)(zhong)量(liang)(liang)(liang)计)山(shan)梨(li)醇(chun)(chun)(chun)(chun)作为(wei)(wei)流动相。 ②基(ji)本操(cao)作条件：柱(zhu)温(wen)(wen)165℃；载气为(wei)(wei)氨(an)(或(huo)(huo)(huo)其他惰性(xing)气体)流量(liang)(liang)(liang)为(wei)(wei)70ml/min；记(ji)录(lu)(lu)器：-0.5～+1.05mV，满(man)刻度(du)(du)(du)(du)响应时间ls；燃烧(shao)时的(de)(de)(de)(de)(de)(de)氢(qing)(qing)和(he)(he)(he)(he)空(kong)气流应保证(zheng)获得最大灵敏度(du)(du)(du)(du)。 ③标(biao)(biao)(biao)(biao)准(zhun)(zhun)(zhun)(zhun)溶(rong)(rong)(rong)(rong)液(ye)(ye)(ye)的(de)(de)(de)(de)(de)(de)制(zhi)备(bei)(bei)：备(bei)(bei)准(zhun)(zhun)(zhun)(zhun)确(que)称取(qu)(qu)预(yu)经重(zhong)(zhong)(zhong)(zhong)蒸的(de)(de)(de)(de)(de)(de)乙(yi)(yi)(yi)二(er)(er)醇(chun)(chun)(chun)(chun)和(he)(he)(he)(he)二(er)(er)甘(gan)醇(chun)(chun)(chun)(chun)适(shi)量(liang)(liang)(liang)，溶(rong)(rong)(rong)(rong)于(yu)(yu)(yu)水(shui)(shui)(shui)(shui)，以(yi)(yi)制(zhi)备(bei)(bei)成色(se)(se)(se)谱(pu)(pu)标(biao)(biao)(biao)(biao)准(zhun)(zhun)(zhun)(zhun)，两标(biao)(biao)(biao)(biao)准(zhun)(zhun)(zhun)(zhun)液(ye)(ye)(ye)的(de)(de)(de)(de)(de)(de)浓度(du)(du)(du)(du)各为(wei)(wei)1～6mg/ml。 ? ④试(shi)(shi)样(yang)(yang)液(ye)(ye)(ye)的(de)(de)(de)(de)(de)(de)制(zhi)备(bei)(bei)：准(zhun)(zhun)(zhun)(zhun)确(que)称取(qu)(qu)试(shi)(shi)样(yang)(yang)约4g，放(fang)(fang)(fang)(fang)入(ru)(ru)一10ml容量(liang)(liang)(liang)瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)，用(yong)(yong)(yong)(yong)(yong)(yong)(yong)水(shui)(shui)(shui)(shui)定(ding)(ding)容后混(hun)合(he)(he)备(bei)(bei)用(yong)(yong)(yong)(yong)(yong)(yong)(yong)。 ??? ⑤操(cao)作：取(qu)(qu)上述(shu)两标(biao)(biao)(biao)(biao)准(zhun)(zhun)(zhun)(zhun)液(ye)(ye)(ye)各2μl，注(zhu)入(ru)(ru)色(se)(se)(se)谱(pu)(pu)仪(yi)，并(bing)各取(qu)(qu)得色(se)(se)(se)谱(pu)(pu)图。在(zai)标(biao)(biao)(biao)(biao)准(zhun)(zhun)(zhun)(zhun)条件下，乙(yi)(yi)(yi)二(er)(er)醇(chun)(chun)(chun)(chun)的(de)(de)(de)(de)(de)(de)滞留时间平(ping)均为(wei)(wei)2min，二(er)(er)甘(gan)醇(chun)(chun)(chun)(chun)为(wei)(wei)6.5min。量(liang)(liang)(liang)取(qu)(qu)峰高(gao)，并(bing)记(ji)录(lu)(lu)以(yi)(yi)下各值(zhi)：乙(yi)(yi)(yi)二(er)(er)醇(chun)(chun)(chun)(chun)的(de)(de)(de)(de)(de)(de)峰高(gao)A，mm；标(biao)(biao)(biao)(biao)准(zhun)(zhun)(zhun)(zhun)液(ye)(ye)(ye)中(zhong)(zhong)(zhong)(zhong)乙(yi)(yi)(yi)二(er)(er)醇(chun)(chun)(chun)(chun)的(de)(de)(de)(de)(de)(de)浓度(du)(du)(du)(du)B，mg/ml；二(er)(er)甘(gan)醇(chun)(chun)(chun)(chun)的(de)(de)(de)(de)(de)(de)峰高(gao)C，mm；标(biao)(biao)(biao)(biao)准(zhun)(zhun)(zhun)(zhun)液(ye)(ye)(ye)中(zhong)(zhong)(zhong)(zhong)二(er)(er)甘(gan)醇(chun)(chun)(chun)(chun)的(de)(de)(de)(de)(de)(de)浓度(du)(du)(du)(du)D，mg/ml。