用于医药辅助品(pin)、水溶性润(run)滑剂、软化剂、不饱和(he)树脂等。

聚(ju)氧(yang)(yang)化(hua)(hua)乙(yi)(yi)烯(25322-68-3)的(de)(de)(de)(de)制(zhi)(zhi)备(bei)(bei)(bei)方法： 由(you)乙(yi)(yi)二(er)(er)(er)醇(chun)(chun)(chun)缩聚(ju)或(huo)(huo)由(you)环氧(yang)(yang)乙(yi)(yi)烷与水(shui)加(jia)(jia)(jia)(jia)聚(ju)而得。 鉴别试(shi)(shi)(shi)(shi)验(yan)： 溶(rong)(rong)(rong)解性：表观分(fen)子(zi)(zi)(zi)量(liang)(liang)在(zai)1000(或(huo)(huo)以(yi)上(shang)(shang)(shang))的(de)(de)(de)(de)聚(ju)乙(yi)(yi)二(er)(er)(er)醇(chun)(chun)(chun)，极易溶(rong)(rong)(rong)于(yu)(yu)(yu)水(shui)。聚(ju)乙(yi)(yi)二(er)(er)(er)醇(chun)(chun)(chun)溶(rong)(rong)(rong)于(yu)(yu)(yu)许多有(you)(you)机溶(rong)(rong)(rong)剂(ji)，包括脂(zhi)(zhi)肪族酮类和(he)(he)(he)醛类、三(san)氯甲(jia)(jia)烷、乙(yi)(yi)二(er)(er)(er)醇(chun)(chun)(chun)醚、酯类及芳香(xiang)族碳氢(qing)化(hua)(hua)合(he)(he)(he)(he)物；不(bu)溶(rong)(rong)(rong)于(yu)(yu)(yu)乙(yi)(yi)醚和(he)(he)(he)大多数(shu)脂(zhi)(zhi)肪族碳氢(qing)化(hua)(hua)合(he)(he)(he)(he)物。在(zai)水(shui)和(he)(he)(he)有(you)(you)机溶(rong)(rong)(rong)剂(ji)中(zhong)(zhong)(zhong)(zhong)(zhong)(zhong)溶(rong)(rong)(rong)解度(du)(du)随着分(fen)子(zi)(zi)(zi)量(liang)(liang)的(de)(de)(de)(de)提高而降(jiang)低。表观分(fen)子(zi)(zi)(zi)量(liang)(liang)：表观分(fen)子(zi)(zi)(zi)量(liang)(liang)低于(yu)(yu)(yu)1000者，为(wei)申报(bao)值(zhi)的(de)(de)(de)(de)95.0%～105.0%；表观分(fen)子(zi)(zi)(zi)量(liang)(liang)在(zai)1000～7000者，为(wei)申报(bao)值(zhi)的(de)(de)(de)(de)90.0%～110.0%；高于(yu)(yu)(yu)7000者，为(wei)申报(bao)值(zhi)的(de)(de)(de)(de)87.5%～112.5%。 质量(liang)(liang)指(zhi)标(biao)分(fen)析： 1.酸(suan)(suan)度(du)(du)(以(yi)醋酸(suan)(suan)计(ji))取(qu)试(shi)(shi)(shi)(shi)样(yang)6g，放(fang)入(ru)(ru)-250ml三(san)角烧(shao)瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)(zhong)(zhong)，加(jia)(jia)(jia)(jia)酚(fen)酞试(shi)(shi)(shi)(shi)液(ye)(ye)(ye)(TS-167)数(shu)滴(di)(di)和(he)(he)(he)中(zhong)(zhong)(zhong)(zhong)(zhong)(zhong)性乙(yi)(yi)醇(chun)(chun)(chun)50ml，用(yong)(yong)(yong)(yong)0.1mol/L氢(qing)氧(yang)(yang)化(hua)(hua)钾(jia)乙(yi)(yi)醇(chun)(chun)(chun)液(ye)(ye)(ye)滴(di)(di)定(ding)至(zhi)(zhi)(zhi)粉红色(se)(se)，并维持(chi)15s。滴(di)(di)定(ding)时(shi)的(de)(de)(de)(de)耗用(yong)(yong)(yong)(yong)量(liang)(liang)不(bu)得超(chao)(chao)过(guo)(guo)0.5ml。 2.氧(yang)(yang)化(hua)(hua)乙(yi)(yi)烯按下述方法测定(ding)。 (1)吗(ma)(ma)啉(lin)(lin)溶(rong)(rong)(rong)液(ye)(ye)(ye)的(de)(de)(de)(de)制(zhi)(zhi)备(bei)(bei)(bei)：由(you)一(yi)(yi)份重蒸吗(ma)(ma)啉(lin)(lin)和(he)(he)(he)九份无水(shui)甲(jia)(jia)醇(chun)(chun)(chun)混(hun)合(he)(he)(he)(he)而成。 (2)混(hun)合(he)(he)(he)(he)指(zhi)示剂(ji)的(de)(de)(de)(de)制(zhi)(zhi)备(bei)(bei)(bei)：取(qu)4，4′-双-(氨基-1-萘偶(ou)氮2，2′-均(jun)(jun)二(er)(er)(er)苯代乙(yi)(yi)烯磺酸(suan)(suan))0.050g和(he)(he)(he)亮黄0.010g，放(fang)入(ru)(ru)一(yi)(yi)60ml管形瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)(zhong)(zhong)。加(jia)(jia)(jia)(jia)入(ru)(ru)0.1mol/L氢(qing)氧(yang)(yang)化(hua)(hua)钠(na)1.5ml，混(hun)合(he)(he)(he)(he)。加(jia)(jia)(jia)(jia)水(shui)3.5ml后混(hun)合(he)(he)(he)(he)。用(yong)(yong)(yong)(yong)45ml甲(jia)(jia)醇(chun)(chun)(chun)将上(shang)(shang)(shang)述混(hun)合(he)(he)(he)(he)物洗人贮(zhu)藏瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)(zhong)(zhong)，混(hun)合(he)(he)(he)(he)后备(bei)(bei)(bei)用(yong)(yong)(yong)(yong)。 ??? (3)标(biao)准(zhun)(zhun)(zhun)(zhun)盐(yan)酸(suan)(suan)甲(jia)(jia)醇(chun)(chun)(chun)液(ye)(ye)(ye)的(de)(de)(de)(de)制(zhi)(zhi)备(bei)(bei)(bei)：取(qu)盐(yan)酸(suan)(suan)8．5ml，与1000ml无水(shui)甲(jia)(jia)醇(chun)(chun)(chun)混(hun)合(he)(he)(he)(he)。取(qu)该液(ye)(ye)(ye)9．00ml，加(jia)(jia)(jia)(jia)酚(fen)酞试(shi)(shi)(shi)(shi)液(ye)(ye)(ye)(TS-167)数(shu)滴(di)(di)，用(yong)(yong)(yong)(yong)0.1mol/L氢(qing)氧(yang)(yang)化(hua)(hua)钠(na)液(ye)(ye)(ye)进行标(biao)定(ding)。超(chao)(chao)过(guo)(guo)48h后需重新进行标(biao)定(ding)。 ??? (4)操(cao)作(zuo)：取(qu)无水(shui)甲(jia)(jia)醇(chun)(chun)(chun)50ml，放(fang)入(ru)(ru)-250ml锥形烧(shao)瓶(ping)(ping)。加(jia)(jia)(jia)(jia)上(shang)(shang)(shang)述混(hun)合(he)(he)(he)(he)指(zhi)示剂(ji)4～6滴(di)(di)，用(yong)(yong)(yong)(yong)上(shang)(shang)(shang)述标(biao)准(zhun)(zhun)(zhun)(zhun)盐(yan)酸(suan)(suan)甲(jia)(jia)醇(chun)(chun)(chun)液(ye)(ye)(ye)滴(di)(di)定(ding)至(zhi)(zhi)(zhi)纯蓝色(se)(se)。加(jia)(jia)(jia)(jia)试(shi)(shi)(shi)(shi)样(yang)约(yue)25g(准(zhun)(zhun)(zhun)(zhun)确称重)，以(yi)作(zuo)为(wei)空(kong)白(bai)试(shi)(shi)(shi)(shi)样(yang)液(ye)(ye)(ye)，摇(yao)(yao)振至(zhi)(zhi)(zhi)完全(quan)(quan)溶(rong)(rong)(rong)解。用(yong)(yong)(yong)(yong)标(biao)准(zhun)(zhun)(zhun)(zhun)盐(yan)酸(suan)(suan)甲(jia)(jia)醇(chun)(chun)(chun)液(ye)(ye)(ye)滴(di)(di)定(ding)至(zhi)(zhi)(zhi)纯蓝色(se)(se)，临(lin)将滴(di)(di)定(ding)终(zhong)点时(shi)应(ying)(ying)小心地少(shao)量(liang)(liang)滴(di)(di)加(jia)(jia)(jia)(jia)。 (5)取(qu)吗(ma)(ma)啉(lin)(lin)溶(rong)(rong)(rong)液(ye)(ye)(ye)50ml，放(fang)入(ru)(ru)一(yi)(yi)耐热耐压(ya)瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)(zhong)(zhong)，而取(qu)等(deng)量(liang)(liang)的(de)(de)(de)(de)吗(ma)(ma)啉(lin)(lin)溶(rong)(rong)(rong)液(ye)(ye)(ye)放(fang)入(ru)(ru)一(yi)(yi)较小的(de)(de)(de)(de)瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)(zhong)(zhong)，以(yi)此作(zuo)为(wei)试(shi)(shi)(shi)(shi)剂(ji)空(kong)白(bai)液(ye)(ye)(ye)。在(zai)第一(yi)(yi)只瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)(zhong)(zhong)加(jia)(jia)(jia)(jia)入(ru)(ru)试(shi)(shi)(shi)(shi)样(yang)约(yue)25g(准(zhun)(zhun)(zhun)(zhun)确称重)，摇(yao)(yao)振至(zhi)(zhi)(zhi)完全(quan)(quan)溶(rong)(rong)(rong)解。密(mi)塞，将瓶(ping)(ping)牢(lao)固裹(guo)缠后放(fang)入(ru)(ru)布(bu)袋中(zhong)(zhong)(zhong)(zhong)(zhong)(zhong)。将两只瓶(ping)(ping)子(zi)(zi)(zi)紧挨着一(yi)(yi)起放(fang)入(ru)(ru)98℃±2℃的(de)(de)(de)(de)水(shui)浴中(zhong)(zhong)(zhong)(zhong)(zhong)(zhong)。维持(chi)30min，水(shui)浴中(zhong)(zhong)(zhong)(zhong)(zhong)(zhong)的(de)(de)(de)(de)水(shui)位(wei)应(ying)(ying)略(lve)高于(yu)(yu)(yu)瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)(zhong)(zhong)液(ye)(ye)(ye)位(wei)。取(qu)出后于(yu)(yu)(yu)空(kong)气中(zhong)(zhong)(zhong)(zhong)(zhong)(zhong)放(fang)冷至(zhi)(zhi)(zhi)室温(wen)。松开裹(guo)带(dai)，去盖以(yi)放(fang)余压(ya)，然(ran)后取(qu)掉裹(guo)带(dai)。在(zai)每只瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)(zhong)(zhong)缓慢(man)加(jia)(jia)(jia)(jia)入(ru)(ru)醋酐(gan)20ml，摇(yao)(yao)至(zhi)(zhi)(zhi)完全(quan)(quan)溶(rong)(rong)(rong)解。然(ran)后于(yu)(yu)(yu)室温(wen)下放(fang)置15min。如瓶(ping)(ping)子(zi)(zi)(zi)仍显(xian)温(wen)热，则需冷至(zhi)(zhi)(zhi)室温(wen)。于(yu)(yu)(yu)每只瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)(zhong)(zhong)加(jia)(jia)(jia)(jia)混(hun)合(he)(he)(he)(he)指(zhi)示剂(ji)4～6滴(di)(di)，然(ran)后用(yong)(yong)(yong)(yong)标(biao)准(zhun)(zhun)(zhun)(zhun)的(de)(de)(de)(de)盐(yan)酸(suan)(suan)甲(jia)(jia)醇(chun)(chun)(chun)液(ye)(ye)(ye)滴(di)(di)定(ding)至(zhi)(zhi)(zhi)纯蓝色(se)(se)，临(lin)近终(zhong)点时(shi)需缓慢(man)少(shao)量(liang)(liang)滴(di)(di)加(jia)(jia)(jia)(jia)。 3.乙(yi)(yi)二(er)(er)(er)醇(chun)(chun)(chun)和(he)(he)(he)二(er)(er)(er)甘(gan)(gan)醇(chun)(chun)(chun)的(de)(de)(de)(de)测定(ding)：表观分(fen)子(zi)(zi)(zi)量(liang)(liang)低于(yu)(yu)(yu)450的(de)(de)(de)(de)聚(ju)乙(yi)(yi)二(er)(er)(er)醇(chun)(chun)(chun)试(shi)(shi)(shi)(shi)样(yang)。 ??? ①仪(yi)(yi)器(qi)：选用(yong)(yong)(yong)(yong)一(yi)(yi)适(shi)当的(de)(de)(de)(de)气相色(se)(se)谱(pu)仪(yi)(yi)，接有(you)(you)一(yi)(yi)氢(qing)焰离子(zi)(zi)(zi)化(hua)(hua)检测器(qi)，用(yong)(yong)(yong)(yong)一(yi)(yi)15m×3mm(内径)的(de)(de)(de)(de)不(bu)锈钢柱；用(yong)(yong)(yong)(yong)60/80目(mu)未(wei)酸(suan)(suan)洗过(guo)(guo)的(de)(de)(de)(de)硅藻(zao)土(Chromosorb W或(huo)(huo)相似品(pin))作(zuo)为(wei)载(zai)体(ti)，用(yong)(yong)(yong)(yong)12%(重量(liang)(liang)计(ji))山梨醇(chun)(chun)(chun)作(zuo)为(wei)流动相。 ②基本操(cao)作(zuo)条(tiao)件：柱温(wen)165℃；载(zai)气为(wei)氨(或(huo)(huo)其他惰性气体(ti))流量(liang)(liang)为(wei)70ml/min；记(ji)录器(qi)：-0.5～+1.05mV，满刻度(du)(du)响应(ying)(ying)时(shi)间ls；燃烧(shao)时(shi)的(de)(de)(de)(de)氢(qing)和(he)(he)(he)空(kong)气流应(ying)(ying)保证获(huo)得最大灵敏(min)度(du)(du)。 ③标(biao)准(zhun)(zhun)(zhun)(zhun)溶(rong)(rong)(rong)液(ye)(ye)(ye)的(de)(de)(de)(de)制(zhi)(zhi)备(bei)(bei)(bei)：备(bei)(bei)(bei)准(zhun)(zhun)(zhun)(zhun)确称取(qu)预经重蒸的(de)(de)(de)(de)乙(yi)(yi)二(er)(er)(er)醇(chun)(chun)(chun)和(he)(he)(he)二(er)(er)(er)甘(gan)(gan)醇(chun)(chun)(chun)适(shi)量(liang)(liang)，溶(rong)(rong)(rong)于(yu)(yu)(yu)水(shui)，以(yi)制(zhi)(zhi)备(bei)(bei)(bei)成色(se)(se)谱(pu)标(biao)准(zhun)(zhun)(zhun)(zhun)，两标(biao)准(zhun)(zhun)(zhun)(zhun)液(ye)(ye)(ye)的(de)(de)(de)(de)浓度(du)(du)各(ge)为(wei)1～6mg/ml。 ? ④试(shi)(shi)(shi)(shi)样(yang)液(ye)(ye)(ye)的(de)(de)(de)(de)制(zhi)(zhi)备(bei)(bei)(bei)：准(zhun)(zhun)(zhun)(zhun)确称取(qu)试(shi)(shi)(shi)(shi)样(yang)约(yue)4g，放(fang)入(ru)(ru)一(yi)(yi)10ml容(rong)量(liang)(liang)瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)(zhong)(zhong)，用(yong)(yong)(yong)(yong)水(shui)定(ding)容(rong)后混(hun)合(he)(he)(he)(he)备(bei)(bei)(bei)用(yong)(yong)(yong)(yong)。 ??? ⑤操(cao)作(zuo)：取(qu)上(shang)(shang)(shang)述两标(biao)准(zhun)(zhun)(zhun)(zhun)液(ye)(ye)(ye)各(ge)2μl，注入(ru)(ru)色(se)(se)谱(pu)仪(yi)(yi)，并各(ge)取(qu)得色(se)(se)谱(pu)图。在(zai)标(biao)准(zhun)(zhun)(zhun)(zhun)条(tiao)件下，乙(yi)(yi)二(er)(er)(er)醇(chun)(chun)(chun)的(de)(de)(de)(de)滞(zhi)留时(shi)间平均(jun)(jun)为(wei)2min，二(er)(er)(er)甘(gan)(gan)醇(chun)(chun)(chun)为(wei)6.5min。量(liang)(liang)取(qu)峰高，并记(ji)录以(yi)下各(ge)值(zhi)：乙(yi)(yi)二(er)(er)(er)醇(chun)(chun)(chun)的(de)(de)(de)(de)峰高A，mm；标(biao)准(zhun)(zhun)(zhun)(zhun)液(ye)(ye)(ye)中(zhong)(zhong)(zhong)(zhong)(zhong)(zhong)乙(yi)(yi)二(er)(er)(er)醇(chun)(chun)(chun)的(de)(de)(de)(de)浓度(du)(du)B，mg/ml；二(er)(er)(er)甘(gan)(gan)醇(chun)(chun)(chun)的(de)(de)(de)(de)峰高C，mm；标(biao)准(zhun)(zhun)(zhun)(zhun)液(ye)(ye)(ye)中(zhong)(zhong)(zhong)(zhong)(zhong)(zhong)二(er)(er)(er)甘(gan)(gan)醇(chun)(chun)(chun)的(de)(de)(de)(de)浓度(du)(du)D，mg/ml。