高效液相色谱单项选择及思考题试卷 及答案

高效液相色谱单项选择及思考题试卷 及答案
高效液相色谱单项选择及思考题试卷 及答案

高效液相色谱习题及参考答案

一、单项选择题

1. 在液相色谱法中,按分离原理分类,液固色谱法属于()。

A、分配色谱法

B、排阻色谱法

C、离子交换色谱法

D、吸附色谱法2. 在高效液相色谱流程中,试样混合物在()中被分离。

A、检测器

B、记录器

C、色谱柱

D、进样器

3. 液相色谱流动相过滤必须使用何种粒径的过滤膜?

A、0.5μm

B、0.45μm

C、0.6μm

D、0.55μm

4. 在液相色谱中,为了改变色谱柱的选择性,可以进行如下哪些操作?

A、改变流动相的种类或柱子

B、改变固定相的种类或柱长

C、改变固定相的种类和流动相的种类

D、改变填料的粒度和柱长

5. 一般评价烷基键合相色谱柱时所用的流动相为()

A、甲醇/水(83/17)

B、甲醇/水(57/43)

C、正庚烷/异丙醇(93/7)

D、乙腈/水(1.5/98.5)

6. 下列用于高效液相色谱的检测器,()检测器不能使用梯度洗脱。

A、紫外检测器

B、荧光检测器

C、蒸发光散射检测器

D、示差折光检测器

7. 在高效液相色谱中,色谱柱的长度一般在()范围内。

A 、10~30cm B、20~50m C 、1~2m D、2~5m

8. 在液相色谱中, 某组分的保留值大小实际反映了哪些部分的分子间作用力

()

A、组分与流动相

B、组分与固定相

C、组分与流动相和固定相

D、组分与组分

9. 在液相色谱中,为了改变柱子的选择性,可以进行()的操作

A、改变柱长

B、改变填料粒度

C、改变流动相或固定相种类

D、改变流动相的流速

10. 液相色谱中通用型检测器是()

A、紫外吸收检测器

B、示差折光检测器

C、热导池检测器

D、氢焰检测器

11. 在环保分析中,常常要监测水中多环芳烃,如用高效液相色谱分析,应选用下述哪种检波器

A、荧光检测器

B、示差折光检测器

C、电导检测器

D、紫外吸收检测器

12. 在液相色谱法中,提高柱效最有效的途径是()

A、提高柱温

B、降低板高

C、降低流动相流速

D、减小填料粒

13. 在液相色谱中,不会显著影响分离效果的是()

A、改变固定相种类

B、改变流动相流速

C、改变流动相配比

D、改变流动相种类

14. 不是高液相色谱仪中的检测器是()

A、紫外吸收检测器

B、红外检测器

C、差示折光检测

D、电导检测器

15. 高效液相色谱仪与气相色谱仪比较增加了()

A、恒温箱

B、进样装置

C、程序升温

D、梯度淋洗装置

16. 在高效液相色谱仪中保证流动相以稳定的速度流过色谱柱的部件是()

A、贮液器

B、输液泵

C、检测器

D、温控装置

17. 高效液相色谱、原子吸收分析用标准溶液的配制一般使用()水

A.国标规定的一级、二级去离子水B.国标规定的三级水

C.不含有机物的蒸馏水D.无铅(无重金属)水

18. 高效液相色谱仪与普通紫外-可见分光光度计完全不同的部件是()

A、流通池

B、光源

C、分光系统

D、检测系统

19. 下列哪种是高效液相色谱仪的通用检测器

A、紫外检测器

B、荧光检测器

C、安培检测器

D、蒸发光散射检测器

20. 高效液相色谱仪中高压输液系统不包括

A、贮液器

B、高压输液泵

C、过滤器

D、梯度洗脱装置

E、进样器

二、判断题:

1. 液相色谱分析时,增大流动相流速有利于提高柱效能。

2. 高效液相色谱流动相过滤效果不好,可引起色谱柱堵塞。

3. 高效液相色谱分析的应用范围比气相色谱分析的大。

4. 反相键合相色谱柱长期不用时必须保证柱内充满甲醇流动相。

5. 高效液相色谱分析中,使用示差折光检测器时,可以进行梯度洗脱。

6. 在液相色谱法中,提高柱效最有效的途径是减小填料粒度。

7. 在液相色谱中,范第姆特方程中的涡流扩散项对柱效的影响可以忽略。

8. 由于高效液相色谱流动相系统的压力非常高,因此只能采取阀进样。

9. 高效液相色谱仪的色谱柱可以不用恒温箱,一般可在室温下操作。

10. 高效液相色谱中,色谱柱前面的预置柱会降低柱效。

11. 液相色谱中,化学键合固定相的分离机理是典型的液-液分配过程。

12. 高效液相色谱分析中,固定相极性大于流动相极性称为正相色谱法。

13. 高效液相色谱分析不能分析沸点高,热稳定性差,相对分子量大于400的有

机物。

14. 在液相色谱法中,约70-80%的分析任务是由反相键合相色谱法来完成的。

15. 在高效液相色谱仪使用过程中,所有溶剂在使用前必须脱气。

16. 填充好的色谱柱在安装到仪器上时是没有前后方向差异的。

17. 保护柱是在安装在进样环与分析柱之间的,对分析柱起保护作用,内装有与

分析柱不同固定相。

18. 检测器、泵和色谱柱是组成高效液相色谱仪的三大关键部件。

19. 紫外-可见光检测器是利用某些溶质在受紫外光激发后,能发射可见光的性

质来进行检测的。

20. 应用光电二极管阵列检测器可以获得具有三维空间的立体色谱光谱图。

三、简答题

1. 为什么作为高效液相色谱仪的流动相在使用前必须过滤、脱气?

2. 高效液相色谱有哪几种定量方法,其中哪种是比较精确的定量方法,并简述之。

参考答案

一、选择题

1.D

2.C

3.B

4.C

5.A

6.D

7.A

8.C

9.C 10.B 11.A 12.D 13.B 14.B 15.D 16.B 17.A 18. A 19. D 20. E

二、判断题

1.×

2.√

3.√

4.√

5.×

6.√

7.×

8.×

9.√ 10.√ 11.× 12.√ 13.× 14.√ 15.√ 16.× 17.× 18.√ 19.× 20.√

三、简答题

1. 高效液相色谱仪所用溶剂在放入贮液罐之前必须经过0.45μm滤膜过滤,除去

溶剂中的机械杂质,以防输液管道或进样阀产生阻塞现象。所有溶剂在上机使用前必须脱气;因为色谱住是带压力操作的,检测器是在常压下工作。若流动相中所含有的空气不除去,则流动相通过柱子时其中的气泡受到压力而压缩,流出柱子进入检测器时因常压而将气泡释放出来,造成检测器噪声增大,使基线不稳,仪器不能正常工作,这在梯度洗脱时尤其突出。

2. 高效液相色谱的定量方法与气相色谱定量方法类似,主要有归一化法、外标

法和内标法。其中内标法是比较精确的定量方法。它是将已知量的内标物加到已知量的试样中,在进行色谱测定后,待测组分峰面积和内标物峰面积之比等于待测组分的质量与内标物质量之比,求出待测组分的质量,进而求出待测组分的含量。

思考题与练习题

1.高效液相色谱是如何实现高效、快速、灵敏的?

解:

气相色谱理论和技术上的成就为液相色谱的发展创造条件,从它的高效、高速和高灵敏度得到启发,采用5-10μm微粒固定相以提高柱效,采用高压泵加快液体流动相的流速;设计高灵敏度、死体积小的紫外、荧光等检测器,提高检测灵敏度,克服经典液相色谱的缺点,从而达到高效、快速、灵敏。

2.简述液相色谱中引起色谱峰扩展的主要因素,如何减少谱带扩张,提高柱效?

解:

液相色谱中引起色谱峰扩展的主要因素为涡流扩散、流动相传质、停留流动相传质及柱外效应。

在液相色谱中要减少谱带扩张,提高柱效,要减少填料颗粒直径,减小填料孔穴深度,提高装填的均匀性,采用低黏度溶剂作流动相,流速尽可能低,同时要尽可能采用死体积较小的进样器、检测器、接头和传输管线等。

3.色谱柱A柱长为15cm,载体粒度为5μm。另一B柱长为30cm,载体粒度为10μm。两

柱的柱效相等吗?

解:

∵l=L/dp

∴lA=15/0.0005=30000

lB= 30/0.0010=30000

A柱的折合柱长为30000,B柱的折合柱长也为30000,表明组分在两根柱内从柱入口到出口都经过30000个载体颗粒,两柱的柱效相等。

4.流动相为什么要脱气?常用的脱气方法有拿几种?

解:

流动相中溶解气体存在以下几个方面的害处

(1)气泡进入检测器,引起光吸收或电信号的变化,基线突然跳动,干扰检测;

(2)溶解在溶剂中的气体进入色谱柱时,可能与流动相或固定相发生化学反应;

(3)溶解气体还会引起某些样品的氧化降解,对分离和分析结果带来误差。因此,使用前必须进行脱气处理。

常用的脱气法有以下几种:

(1)加热脱气法;

(2)抽吸脱气法

(3)吹氦脱气法;

(4)超声波振荡脱气法。

5.在液相色谱中。常用作固定相,又可用作键合相基体的物质是

A. 分子筛

B. 硅胶

C. 氧化铝

D. 活性炭

解:

B 硅胶

要形成化学键合固定相,所用的基质材料应有某种化学反应活性,在四种固体固定相中只有硅胶含有硅醇基,是能进行键合的活性官能团。

6.在150×Φ2mm硅胶柱流动相为己烷/甲醇(150:2),紫外检测器色谱条件下分离丙烯

酰胺,判断以下组分的出峰次序,为什么?

A. B.

解:

在给定的色谱条件下,组分B先出峰,组分A后出峰。以硅胶为固定相,己烷/甲醇(150:2)为流动相,该体系为正相色谱,样品的极性A>B,在正相色谱体系极性小的组分先出峰,极性大的组分后出峰,所以出峰次序为B先出,A后出。

7.在硅胶柱上,用甲苯为流动相,某组分的保留时间为30min,如果改用四氯化碳或乙醚

为流动相,试指出选用哪中溶剂能减少该组分的保留时间?为什么?

解:

该体系为正向色谱体系。在该体系中流动相的极性增大保留值减少。流动相甲苯、四氯化碳及乙醚的溶剂强度参数分别是0.29、0.18、0.38,因此选用溶剂强度参数大于甲苯的乙醚,可缩短该化合物的保留时间。

8.为什么体积排阻色谱中任何组分的分配系数必须符合0≤K≤1?如果K>1说明什么问

题?

解:

因为组分的分配系数为K=Cs/Cm,Cs与Cm分别为组分在固定相和流动相中的浓度,当分子直径大于孔径时,此时Cm=0,∴K=0.当分子直径小于固定相孔径时,组分向空隙内流动相扩散,达到平衡时,一半组分在空隙内,一半组分在空隙外,此时K=1.0,若分子直径介于以上两种极限情况之间,K一定介于0与1之间,可见体积排阻色谱中,任何祖父呢的分配系数为0≤K≤1,如果K>1说明此时的分离方式已不是纯粹的体积排阻色谱,其分离过程受到其他作用力(如吸附)的支配.

9.为了测定邻氨基苯酚中微量杂质苯胺,现有下列固定相:硅胶,ODS键合相,流动相有:水-

甲醇,异丙醚-己烷,应选用哪种固定相,流动相?为什么?

解:

邻氨基苯酚中微量杂质苯胺测定,为了良好分离,应让苯胺先出峰,由于苯胺的极性小于邻氨基苯酚,因此应采用正相色谱法,选用硅胶为固定相,异丙醚-己烷为流动相.

10.在ODS键合相固定相,甲醇-水为流动相时试判断四种苯并二氮杂苯的出现峰顺序.为什

么?

1. 2.

3. 4.

解:

色谱条件为反相键合相色谱体系,在反相色谱体系中极性大的组分k 小,首先出峰,按四

种苯并二氮杂苯的结构,出峰顺序为4-3-2-1.

自测题

1. 在GC 和LC 中, 影响柱选择性的不同的因素是

A.

固定相的种类;

B. 柱温;

C

.流动相的种类; D .分配比。

2. 在液相色谱中, 范氏方程中的哪一项对柱效能的影响可以忽略不计

?

A .涡流扩散项;

B .分子扩散项;

C

.固定相传质阻力项;

D .流动相中的传质阻力。

3. 在液相色谱中, 某组分的保留值大小实际反映了哪些部分的分子间作用力?

A .组分与流动相;

B .组分与固定相;

C .组分与流动相和固定相;

D .组分与组分。

4. 在液-固色谱法中, 以硅胶为固定相, 对以下四组分, 最后流出色谱柱的组分可能是

A.苯酚;

B. 苯胺; C

.邻羟基苯胺; D .对羟基苯胺。

5. 在液-固色谱法中, 以硅胶为固定相, 对以下四组分, 最后流出色谱柱的组分可能是

A.

苯酚;

B. 苯胺;

C .邻

羟基苯胺; D .对羟基苯胺。

6. 用液相色谱法分离长链饱和烷烃的混合物, 应采用下述哪一种检测器

? A

.紫外吸收检测器;

B .示差折光检测器;

C

.荧光检测器;

D .电化学检测器。

7. 液-液色谱法中的反相液相色谱法,其固定相、流动相和分离化合物的性质分别为:

A .非极性、极性和非极性;

B

.极性、非极性和非极性;

C .极性、非极性和极性;

D .非极性、极性和离子化合物。

8. 若在一个 1m 长的色谱柱上测得两组分的分离度为 0.68,若要使它们完全分离, 则柱长 (m) 至少应为:

A.0.5;

B.

2; C

.5; D

.9。 9.

在液相色谱中,梯度洗脱最宜于分离:

A .几何异构体;

B .沸点相近,官能团相同的试样;

C .沸点相差大的试样;

D .分配比变化范围宽的试样。

10. 液-液色谱法中的反相液相色谱法,其固定相、流动相和分离化合物的性质分别为:

A. 非极性、极性和非极性;

B. 极性、非极性和非极

性;

C. 极性、非极性和极性;

D. 非极性、极性和离子化合

物。

正确答案:

1:(C)、2:(B)、3:(C)、4:(D)、5:(D )

6:(B)、7:(A)、8:(C)、9:(D)、10:(A ) !

云南省中考英语单项选择真题汇编(带答案)

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