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Separation Methods III

Total questions: 86

Worksheet time: 57mins

Name
Class
Date
1.

What does this represent? σ2E

(a)  

2.

Which of these represents the total observed peak variance?

a)

σ2tot

b)

σ2E

c)

σ2C

d)

σ2inj

e)

σ2Tu

3.

Which of these represents the sum of the variance that occurs in the column?

a)

σ2tot

b)

σ2E

c)

σ2C

d)

σ2inj

e)

σ2Tu

4.

Which of these represents the variance from things outside the column?

a)

σ2Det

b)

σ2E

c)

σ2C

d)

σ2Inj

e)

σ2Tu

5.

Which of these represents variance from tubing and fittings?

a)

σ2Det

b)

σ2E

c)

σ2C

d)

σ2Inj

e)

σ2Tu

6.

Which of these represents variance due to the injector or injector process?

a)

σ2Det

b)

σ2E

c)

σ2C

d)

σ2Inj

e)

σ2Tu

7.

Which of these represents variance due to the detector?

a)

σ2Det

b)

σ2E

c)

σ2C

d)

σ2Inj

e)

σ2Tu

8.

What type of injectors should a UHPLC system have?

(a)  

9.

What type of tubing should a UHPLC system have?

(a)  

10.

What type of detector cells should a UHPLC system have?

(a)  

11.

Peaks are Gaussian to an acceptable or unacceptable degree

a)

True

b)

False

12.

What is the equation for peak asymmetry factor (AF)?

(a)  

13.

What does this equation represent?

(a)  

14.

What type of abnormal peak shape is shown here?

(a)  

15.

What type of abnormal peak shape is shown here?

(a)  

16.

Langmuir Isotherm results in

a)

peak fronting

b)

peak tailing

c)

concave

d)

convex

e)

ideal

17.

Linear Isotherm results in

a)

peak fronting

b)

peak tailing

c)

concave

d)

convex

e)

ideal

18.

Anti-Langmuir Isotherm results in

a)

peak fronting

b)

peak tailing

c)

concave

d)

convex

e)

ideal

19.

What type of LC focuses on resolution and quantitation?

a)

Analytical

b)

Preparative

20.

What type of LC focuses on purification and throughput?

a)

Analytical

b)

Preparative

21.

What type of LC operates in the non-linear isotherm region?

a)

Analytical

b)

Preparative

22.

What type of LC operates in the linear isotherm region (dilute samples)?

a)

Analytical

b)

Preparative

23.

Which type of isotherm is often seen in silica columns?

a)

Linear

b)

Langmuir

c)

Anti-Langmuir

24.

Which type of isotherm is often seen in reversed-phase columns?

a)

Linear

b)

Langmuir

c)

Anti-Langmuir

25.

Which type of isotherm must be cut off early?

a)

Linear

b)

Langmuir

c)

Anti-Langmuir

26.

Which type of isotherm has greater solute-solute than solute-sp binding??

a)

Linear

b)

Langmuir

c)

Anti-Langmuir

27.

Which type of isotherm can separate more cleanly from early-eluting impurities?

a)

Linear

b)

Langmuir

c)

Anti-Langmuir

28.

Which type of isotherm is caused by finite binding sites?

a)

Linear

b)

Langmuir

c)

Anti-Langmuir

29.

Which type of isotherm has a purity vs yield trade-off?

a)

Linear

b)

Langmuir

c)

Anti-Langmuir

30.

Which type of isotherm can improve both purity and yield?

a)

Linear

b)

Langmuir

c)

Anti-Langmuir

31.

Exponential peak tailing reduces with loading of less sample

a)

True

b)

False

32.

Are secondary silanol interactions a chemical or physical cause?

a)

Chemical

b)

Physical

33.

Are trace metal contamination a chemical or physical cause?

a)

Chemical

b)

Physical

34.

Is column bed deformation a chemical or physical cause?

a)

Chemical

b)

Physical

35.

Is a blocked inlet frit a chemical or physical cause?

a)

Chemical

b)

Physical

36.

Which of these describes secondary silanol interactions?

a)

most common in RP-HPLC

b)

impurities in silica create active sites

c)

a fraction of analyte is held longer

d)

voids at inlet disrupt flow

e)

particulates distort flow into bed

37.

Which of these describes trace metal contamination?

a)

most common in RP-HPLC

b)

impurities in silica create active sites

c)

a fraction of analyte is held longer

d)

voids at inlet disrupt flow

e)

particulates distort flow into bed

38.

Which of these describes column bed deformation?

a)

most common in RP-HPLC

b)

impurities in silica create active sites

c)

a fraction of analyte is held longer

d)

voids at inlet disrupt flow

e)

particulates distort flow into bed

39.

Which of these describes a blocked inlet frit?

a)

most common in RP-HPLC

b)

impurities in silica create active sites

c)

a fraction of analyte is held longer

d)

voids at inlet disrupt flow

e)

particulates distort flow into bed

40.

Which of these fixes secondary silanol effects?

a)

lower mobile-phase pH

b)

high purity columns

c)

guard columns and in-line filters

d)

use buffers

e)

reverse-flush

41.

Which of these fixes a blocked inlet frit?

a)

lower mobile-phase pH

b)

high purity columns

c)

guard columns and in-line filters

d)

use buffers

e)

reverse-flush

42.

Which of these fixes trace metal contamination?

a)

lower mobile-phase pH

b)

high purity columns

c)

replace column

d)

use buffers

e)

reverse-flush

43.

Which of these fixes column bed deformation?

a)

lower mobile-phase pH

b)

high purity columns

c)

replace column

d)

use buffers

e)

reverse-flush

44.

How do you diagnose mass overload?

a)

dilute 10X and re-inject; check improved shape

b)

reduce sample concentration

c)

change detector wavelength

d)

reduce injection volume

e)

increase resolution

45.

How do you fix a mass overload?

a)

dilute 10X and re-inject; check improved shape

b)

reduce sample concentration

c)

change detector wavelength

d)

reduce injection volume

e)

increase resolution

46.

How do you diagnose a co-eluting impurity?

a)

dilute 10X and re-inject; check improved shape

b)

reduce sample concentration

c)

change detector wavelength

d)

reduce injection volume

e)

increase resolution

47.

How do you fix a co-eluting impurity?

a)

dilute 10X and re-inject; check improved shape

b)

reduce sample concentration

c)

change detector wavelength

d)

low-volume cell

e)

increase resolution

48.

How do you fix extra-column volume?

a)

dilute 10X and re-inject; check improved shape

b)

reduce sample concentration

c)

change detector wavelength

d)

low-volume cell

e)

increase resolution

49.

Which of these are examples of column hardware?

a)

porous particles

b)

tubing

c)

mobile phase

d)

frits

50.

Which of these are examples of packing support?

a)

porous particles

b)

tubing

c)

mobile phase

d)

frits

51.

What is the chemical formula of silica?

(a)  

52.

Which of these pore regimes is diffusive?

a)

micropores

b)

mesopores

c)

macropores

53.

Which of these pore regimes is convective?

a)

micropores

b)

mesopores

c)

macropores

54.

Which of these pore regimes is used for most separations?

a)

micropores

b)

mesopores

c)

macropores

55.

Which of these pore regimes lowers C-term?

a)

micropores

b)

mesopores

c)

macropores

56.

Which of these pore regimes is best for proteins/biopolymers?

a)

micropores

b)

mesopores

c)

macropores

57.

Which method of silica synthesis contains mostly mesopores?

a)

tetraalkoxysilane hydrolysis

b)

sol-gel method

c)

spray-dry particles from fumed silica

d)

microencapsulation and polymer induced colloid aggregation

58.

Which method of silica synthesis uses organosiloxane oligomers as a variation method?

a)

tetraalkoxysilane hydrolysis

b)

sol-gel method

c)

spray-dry particles from fumed silica

d)

microencapsulation and polymer induced colloid aggregation

59.

Which of these describes silanols?

a)

weak acids

b)

high pKa than alcohols

c)

similar to carboxilic acids

d)

less stable SiO than CO

e)

primary cause of peak fronting

60.

Which silanol type has two OH groups on the same Si atom?

a)

Free/Isolated

b)

Geminal

c)

Associated

d)

Activated

61.

Which silanol type is the most acidic?

a)

Free/Isolated

b)

Geminal

c)

Associated

d)

Activated

62.

Which silanol type has neighboring silanols linked by hydrogen bonds?

a)

Free/Isolated

b)

Geminal

c)

Associated

d)

Activated

63.

Which silanol type is the primary cause of peak tailing for basic compounds?

a)

Free/Isolated

b)

Geminal

c)

Associated

d)

Activated

64.

Which microenvironment effect on silanol ionization does this describe?

(a)  

65.

Which microenvironment effect on silanol ionization does this describe?

(a)  

66.

Which of these is a silica structure?

a)

b)

c)

d)

67.

Which of these is a first generation hybrid silica structure?

a)

b)

c)

d)

68.

Which of these is a second generation hybrid silica structure?

a)

b)

c)

d)

69.

Which of these is a hydride silica structure?

a)

b)

c)

d)

70.

Which supporting material has no micropores?

a)

controlled porosity glass

b)

metal oxides

c)

porous graphite

71.

Which supporting material is more hydrolytically stable at extreme pH and high temperature?

a)

controlled porosity glass

b)

metal oxides

c)

porous graphite

72.

Which supporting material has high chemical and thermal stability?

a)

controlled porosity glass

b)

metal oxides

c)

porous graphite

73.

Which supporting material has many dead-end pores?

a)

controlled porosity glass

b)

metal oxides

c)

porous graphite

74.

Which supporting material has high retentivity?

a)

controlled porosity glass

b)

metal oxides

c)

porous graphite

75.

Which polymer based packing material has permanent pores?

a)

Soft-gel

b)

Rigid resin beads

c)

Perfusion beads

76.

Which polymer based packing material has temporary pores?

a)

Soft-gel

b)

Rigid resin beads

c)

Perfusion beads

77.

Which polymer based packing material is made from macroporous polymer?

a)

Soft-gel

b)

Rigid resin beads

c)

Perfusion beads

78.

Which of these describes silica type A?

a)

old processes

b)

new processes

c)

metal impurities

d)

from water glass solution and acids

e)

highly pure colloidal silica

79.

Which of these describes silica type B?

a)

old processes

b)

new processes

c)

silica is acid-washed after synthesis

d)

irreversible adsorption of analyses like proteins

e)

highly pure colloidal silica

80.

Which of these describes silica type C?

a)

old processes

b)

new processes

c)

metal impurities

d)

irreversible adsorption of analyses like proteins

e)

chemical surface heterogeneity

81.

Which silica type is most common?



(a)  

82.

Which of these pore regimes is NOT useful for LC?

a)

micropores

b)

mesopores

c)

macropores

83.

What pH range is the stability window for standard silica?

(a)  

84.

What happens at LOW pH?

a)

risk of bonded phase hydrolysis (cleavage)

b)

risk of silica support dissolving

c)

risk of swelling

d)

risk of increased band broadening

85.

What tradeoff is common with increased stability?

a)

risk of bonded phase hydrolysis (cleavage)

b)

risk of silica support dissolving

c)

risk of pore swelling

d)

risk of increased band broadening

86.

What happens at HIGH pH?

a)

risk of bonded phase hydrolysis (cleavage)

b)

risk of silica support dissolving

c)

risk of swelling

d)

risk of increased band broadening

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