仪器分析第四版课后题第三章答案.doc

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1、第三章思考题解答1.从分离原理、仪器构造及应用范围上简要比较气相色谱及液相色谱的异同点。解:二者都是根据样品组分与流动相和固定相相互作用力的差别进行分离的。从仪器构造上看,液相色谱需要增加高压泵以提高流动相的流动速度,克服阻力。同时液相色谱所采用的固定相种类要比气相色谱丰富的多,分离方式也比较多样。气相色谱的检测器主要采用热导检测器、氢焰检测器和火焰光度检测器等。而液相色谱则多使用紫外检测器、荧光检测器及电化学检测器等。但是二者均可与MS等联用。二者均具分离能力高、灵敏度高、分析速度快,操作方便等优点,但沸点太高的物质或热稳定性差的物质难以用气相色谱进行分析。而只要试样能够制成溶液,既可用于H

2、PLC分析,而不受沸点高、热稳定性差、相对分子量大的限制。2.液相色谱中影响色谱峰展宽的因素有哪些? 与气相色谱相比较, 有哪些主要不同之处?解:液相色谱中引起色谱峰扩展的主要因素为涡流扩散、流动的流动相传质、滞留的流动相传质以及柱外效应。在气相色谱中径向扩散往往比较显著,而液相色谱中径向扩散的影响较弱,往往可以忽略。另外,在液相色谱中还存在比较显著的滞留流动相传质及柱外效应。3. 在液相色谱中, 提高柱效的途径有哪些?其中最有效的途径是什么?解:液相色谱中提高柱效的途径主要有:1.提高柱内填料装填的均匀性;2.改进固定相 减小粒度; 选择薄壳形担体; 选用低粘度的流动相; 适当提高柱温其中,

3、减小粒度是最有效的途径.4. 液相色谱有几种类型?它们的保留机理是什么? 在这些类型的应用中,最适宜分离的物质是什么?解:液相色谱有以下几种类型:液-液分配色谱; 液-固吸附色谱; 化学键合色谱;离子交换色谱; 离子对色谱; 空间排阻色谱等.其中;液-液分配色谱的保留机理是通过组分在固定相和流动相间的多次分配进行分离的。可以分离各种无机、有机化合物。液-固吸附色谱是通过组分在两相间的多次吸附与解吸平衡实现分离的.最适宜分离的物质为中等相对分子质量的油溶性试样,凡是能够用薄层色谱分离的物质均可用此法分离。化学键合色谱中由于键合基团不能全部覆盖具有吸附能力的载体,所以同时遵循吸附和分配的机理,最适

4、宜分离的物质为与液-液色谱相同。离子交换色谱和离子色谱是通过组分与固定相间亲合力差别而实现分离的.各种离子及在溶液中能够离解的物质均可实现分离,包括无机化合物、有机物及生物分子,如氨基酸、核酸及蛋白质等。在离子对色谱色谱中,样品组分进入色谱柱后,组分的离子与对离子相互作用生成中性化合物,从而被固定相分配或吸附进而实现分离的.各种有机酸碱特别是核酸、核苷、生物碱等的分离是离子对色谱的特点。空间排阻色谱是利用凝胶固定相的孔径与被分离组分分子间的相对大小关系,而分离、分析的方法。最适宜分离的物质是:另外尚有手性色谱、胶束色谱、环糊精色谱及亲合色谱等机理。5. 在液-液分配色谱中,为什么可分为正相色谱

5、及反相色谱?解:采用正相及反相色谱是为了降低固定液在流动相中的溶解度从而避免固定液的流失。6.何谓化学键合固定相?它有什么突出的优点?解:利用化学反应将固定液的官能团键合在载体表面形成的固定相称为化学键合固定相.优点:固定相表面没有液坑,比一般液体固定相传质快的多. 无固定相流失,增加了色谱柱的稳定性及寿命. 可以键合不同的官能团,能灵活地改变选择性,可应用与多种色谱类型及样品的分析. 有利于梯度洗提,也有利于配用灵敏的检测器和馏分的收集.7. 何谓化学抑制型离子色谱及非抑制型离子色谱?试述它们的基本原理.解:在离子色谱中检测器为电导检测器,以电解质溶液作为流动相,为了消除强电解质背景对电导检

6、测器的干扰,通常除了分析柱外,还增加一根抑制柱,这种双柱型离子色谱法称为化学抑制型离子色谱法.例如为了分离阴离子,常使用NaOH溶液为流动相,钠离子的干扰非常严重,这时可在分析柱后加一根抑制柱,其中装填高容量H+型阳离子交换树脂,通过离子交换,使NaOH转化为电导值很小的H2O,从而消除了背景电导的影响但是如果选用低电导的流动相(如10- 5 10-4M的苯甲酸盐或邻苯二甲酸盐),则由于背景电导较低,不干扰样品的检测,这时候不必加抑制柱,只使用分析柱,称为非抑制型离子色谱法何谓梯度洗提?它与气相色谱中的程序升温有何异同之处?解:在一个分析周期内,按一定程序不断改变流动相的组成或浓度配比,称为梯

7、度洗提是改进液相色谱分离的重要手段梯度洗提与气相色谱中的程序升温类似,但是前者连续改变的是流动相的极性、pH或离子强度,而后者改变的温度程序升温也是改进气相色谱分离的重要手段高效液相色谱进样技术与气相色谱进样技术有和不同之处?解:在液相色谱中为了承受高压,常常采用停流进样与高压定量进样阀进样的方式10以液相色谱进行制备有什么优点?解:以液相色谱进行制备时,分离条件温和,分离检测中不会导致试样被破坏,切易于回收原物11.在毛细管中实现电泳分离有什么优点?解:毛细管由于散热效率很高,可以减少因焦耳热效应造成的区带展宽,因而可以采用较高的电压,克服了传统电泳技术的局限,极大地提高分离效率,而且分离时

8、间缩短,试样分析范围宽,检测限低对于大分子的分离往往比色谱方法具有更高的柱效12.试述CZE, CGE,MECC的基本原理毛细管区带电泳(CZE)是在指外加电场的作用下,溶质在毛细管内的背景电解质溶液中以一定速度迁移而形成一个一个独立的溶质带的电泳模式,其分离基础是淌度的差别因为中性物质的淌度差为零,所以不能分离中性物质。带电粒子的迁移速度为电泳速度与电渗流的矢量和在缓冲溶液中带正电的粒子由于迁移方向与电渗流相同,流动速度最快,最先流出,负电荷粒子的运动方向与电渗流相反,最后流出,中性粒子的电泳速度与电渗流相同,因而迁移速度介于二者之间这样各种粒子因差速迁移而达到区带分离,这就是CZE的分离原

9、理毛细管凝胶电泳(CGE) 是毛细管内填充凝胶或其他筛分介质,如交联或非交联的聚丙烯酰胺。荷质比相等,但分子的大小不同的分子,在电场力的推动下在凝胶聚合物构成的网状介质中电泳,其运动受到网状结构的阻碍。大小不同的分子经过网状结构时受到的阻力不同,大分子受到的阻力大,在毛细管中迁移的速度慢;小分子受到的阻力小,在毛细管中迁移的速度快,从而使它们得以分离。这就是CGE的分离原理胶束电动色谱(MECC)是以胶束为假固定相的一种电动色谱,是电泳技术与色谱技术的结合。多数MECC在毛细管中完成,故又称为胶束电动毛细管色谱 。MECC是在电泳缓冲液中加入表面活性剂,当溶液中表面活性剂浓度超过临界胶束浓度时

10、,表面活性剂分子之间的疏水基因聚集在一起形成胶束(假固定相),溶质不仅可以由于淌度差异而分离,同时又可基于在水相和胶束相之间的分配系数不同而得到分离,这样一般毛细管电泳中不能分离的中性化合物在MECC中可以分离以下是大学体验英语综合教程2(第三版)课后翻译答案Unit11. 任何年满18岁的人都有资格投票。(be eligible to, vote)Answer:Anyone over the age of 18 is eligible to vote.2. 每学期开学前,这些奖学金的申请表格就会由学校发给每一个学生。(apply for, scholarship)Answer:A form

11、to apply for these scholarships is sent by the university to every student before the start of every semester.3. 遵照医生的建议,我决定戒烟。(on the advice of)Answer:On the advice of my doctor, I decided to give up smoking.4. 公园位于县城的正中央。(be located in)Answer:The park is located right in the center of town.5. 这所大学

12、提供了我们所需的所有材料和设备。(facilities)Answer:The university provides all the materials and facilities we desire.1. 他们花了多年的时间寻找内心的平静,但是收效甚微。(search for)Answer:They spent many years searching for peace of mind, but with little success.2. 这种新药的成功研制已经使许多疾病的治疗发生了根本性的变革。(revolutionize)Answer:The successful developm

13、ent of the new drug has revolutionized the treatment of many diseases.3. 由于这个国家的经济不景气,这家公司濒于破产。(on the edge of)Answer:The company is on the edge of bankruptcy due to the economic depression in the country.4. 大学毕业后他成为了一名护士。他认为护士这一职业可能很有发展前途。(rewarding)Answer:He became a nurse after college. He though

14、t nursing could be a very rewarding career.5. 他像往常一样在文件上签了名。(just as)Answer:He signed his name on the paper just as he has always done it.Unit21. 警察们正忙着填写关于这场事故的各种表格。(fill out)Answer:The policemen are busy fi lling out forms about the accident.2. 我想在还车之前把油箱加满。(fill up, fuel tank)Answer:I want to fi

15、ll up the fuel tank before returning the car.3. 如果你要投诉,最好遵循正确的程序。(follow the procedure)Answer:If you want to make a complaint, youd better follow the correct procedure.4. 要不是约翰帮忙,我们绝不会这么快就完成实验。(without)Answer:We couldnt have fi nished the experiment so soon without Johns help.5. 暴风雨之后,岸边的人们焦急地搜索湖面以期

16、发现小船的踪迹。(scan for)Answer:After the storm, the people on the shore anxiously scanned the lake for any sign of the boat.1. 这个国家不大,但是在国际事务中它却发挥着重要作用。(play a role)Answer:This country is not big, but it plays an important role in international affairs.2. 正是在我叔叔的帮助下,我得以克服困难,按时完成了任务。(it is . that)Answer:It

17、 was with the help of my uncle that I overcame the difficulty and completed the assignment in time.3. 毕业时他决定留在北京,而他最好的朋友却选择了去西藏。(while)Answer:While he decided to stay in Beijing upon graduation, his best friend chose to go to Tibet.4. 在这次校园英语演讲比赛中,我们班的玛丽获得了第三名。(come in)Answer:In this Campus English

18、Speaking Contest, Mary from our class came in third.5. 你应该知道学习弹钢琴需要有时间,有金钱,还要有毅力。(as well as)Answer:You should know that it takes time, money as well as perseverance to learn to play the piano.Unit31. 我发现量入为出地过日子越来越难了。(increasingly)Answer:I find it increasingly difficult to live within my income.2.

19、现代政治家们都试图以电视讲话来影响普通百姓。(reach out)Answer:Modern politicians try to reach out to ordinary people in their TV speeches.3. 应该帮助学生对人生采取积极的态度。(adopt)Answer:Pupils should be helped to adopt a positive attitude to life.4. 希望全班同学参加这些讨论。(participate in)Answer:Everyone in the class is expected to participate i

20、n these discussions.5. 如果你犯了罪就必须受到惩罚。(crime)Answer:If you commit a crime you must expect to be punished.1.儿子的死让老妇人变得麻木痴呆了。(numb)Answer:The old woman was numbed by her sons death.2.身处所有这些烦恼之中,他依然能保持乐观。(in the midst)Answer:In the midst of all troubles, he managed to remain cheerful.3. 虽有困难,他们还是设法坚持试验下

21、去。(carry on)Answer:They managed to carry on their experiments in spite of the difficulties.4.我们必须淘汰不合格的申请人。(weed out)Answer:We have to weed out unqualified applicants.5. 医生要他减少抽烟。(cut down on)Answer:The doctor told him to cut down on smoking.Unit41.她在公共汽车站一直等到末班车进站。(come in)Answer:She waited at the

22、bus stop until the last bus came in.2.如果我们能帮得上忙,尽管和我们联系。(contact)Answer:If there is any way we can be of assistance, please do not hesitate to contact us.3 .他需要多少船务人员才能使他的游艇航行?(crew, yacht)Answer:How many crew does he need to sail his yacht?4 .虽然她的新书没有上一本好,但是我还是喜欢它。(not quite as)Answer:I enjoyed her

23、 new book though its not quite as good as her last one.5 .我从未遇到过如此善良的人。(never before)Answer:Never before have I met such a kind person.1.公共汽车放慢速度并停下,让那位乘客上车。(slow down)Answer:The bus slowed down and stopped to allow the passenger to get on board.2.许多车子都驶过去了,可是没有一辆愿意让我们搭便车。(roll by)Answer:Many vehicl

24、es rolled by, but no one offered us a ride.3 .请勿践踏草地。(get off)Answer:Please get off the grass.4.他按妻子的吩咐,一下班就去了市场。(make ones way)Answer:He made his way to the marketplace right after work, as his wife had asked him to do.5 .值得庆幸的是,史蒂夫 (Steve) 从自行车上摔下来时没有摔断骨头。(luckily)Answer:Luckily, Steve didnt break

25、 any bones when he fell off his bike.Unit51. 我们得把感情放在一边,从专业的角度来对待这件事。(from a professional standpoint)Answer:We have to put aside our emotions and take it from a professional standpoint.2. 这部戏非常精彩,我很快就沉浸于激动人心的剧情之中。(lose oneself in)Answer:The play was so wonderful that I soon lost myself in the excite

26、ment of it.3 .她没有什么爱好除非你把看电视也算是一种爱好。(unless)Answer:She hasnt got any hobbies unless you call watching TV a hobby.4. 他说他是直接从市长本人那里得到这个信息的。(first-hand)Answer:He said that he had got the information first-hand from the Mayor himself.5 .既然你不能回答这个问题,我们最好问问别人。(since)Answer:Since you cant answer the questi

27、on, perhaps wed better ask someone else.1. 由于公共汽车司机突然刹车,旅客们都不由自主地向前摔倒。(brake, pitch forward)Answer:All the passengers pitched forward because the bus driver braked sharply.2. 这个协议将冲破对自由贸易设置的障碍。(break through, obstacle)Answer:This agreement will break through the obstacles to free trade.3 .我刚放下叫出租车的电

28、话,车就来了。(soon after)Answer:The taxi arrived soon after I rang for it.4. 在过去,不管我什么时候到家,我父母总会等我。(no matter)Answer:My parents always waited up for me no matter what time I got home.5 .由于没有一方愿意让步,两个公司之间的对话完全破裂了。(break down)Answer:Talks between the two companies completely broke down, because neither of t

29、hem wanted to give in.Unit61. 那件工作很难做,不过我想试试看。(have a shot)Answer:Its a difficult job, but Id like to have a shot.2. 这是一本关于商务实践而非理论的书。(as opposed to)Answer:This is a book about business practice as opposed to theory.3. 社会活动从未耽误她的学习。(in the way)Answer:Social activities never get in the way of her stu

30、dies.4. 直到1911年人们才发现第一种维生素。(It is not until . that)Answer:It was not until 1911 that the first of the vitamins was identified.5. 尽管年事已高,爷爷每天还帮忙做家务。(despite)Answer:Despite advanced years, Grandpa helps do housework every day.1. 我们的婚姻很幸福,但我们也曾经历过许多坎坷。(ups and downs)Answer:Our marriage is happy but wev

31、e had many ups and downs.2. 许多外语教师常常在课堂上自顾自地讲得太多。(be inclined to)Answer:Many teachers of foreign languages are inclined to talk too much themselves in class.3. 那位著名演员每天早晨锻炼一小时以保持健康。(work out)Answer:The famous actor keeps fit by working out for an hour every morning.4. 与他促膝长谈之后,她的怀疑消失了。(melt away)Ans

32、wer:After a long heart-to-heart talk with him, her suspicion melted away.5. 目前我们没有职位空缺,但我们肯定会记住您的申请。(keep in mind)Answer:We have no vacancies now, but well certainly keep your application in mind.Unit71. 他并不后悔说过的话,只是觉得他完全可以不用这种方式表达。(could have done)Answer:He did not regret what he had said but felt

33、that he could have expressed it differently.2. 我们最好等到12月14日。那时大卫已考完试,就能和我们一起去度假了。(will have done)Answer:Wed better wait till 14 December. David will have had his exam by then, so hell be able to go on holiday with us.3. 他正在做一个新项目,年底前必须完成。(work on)Answer:Hes working on a new project which has to be f

34、inished by the end of the year.4. 他们让我们使用他们的实验室,作为回报,我们则让他们分享研究成果。(in return)Answer:They are letting us use their lab, and in return, we are sharing with them the results of our research.5. 诸如打电话、听电话一类的事情占用了这位秘书的大部分时间。(take up)Answer:Such things as making and answering telephone calls take up most o

35、f the secretarys time.1. 他们把房子卖了后就到加拿大和女儿住在一起。(go off) Answer:They sold their house and went off to live in Canada with their daughter.2. 你下星期这个时候会在干什么?还是像平常一样干活。(will be doing)Answer:What will you be doing this time next week?Ill be working as usual.3. 他既聪明又勤奋,不久就接管了杂志的编辑工作。(editing; before long)An

36、swer:He was intelligent and hard-working and before long he took over the editing of the magazine.4. 你话还没说完别人就挂断电话,难道你不恼火吗?(hang up)Answer:Dont you hate it when someone hangs up on you before you finish speaking?5. 让他们感到惊恐的是,他们的房顶着火了。(to ones horror)Answer:To their horror, the roof of their house caught fire.

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