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NAME the PARTS ICP-MS Place your answers below: 1. 2. 3. 4. 5. 6. 7. 8.

Instrumental Analysis Exam

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Page 1: Instrumental Analysis Exam

NAME the PARTS

ICP-MS

Place your answers below:

1.

2.

3.

4.

5.

6.

7.

8.

Page 2: Instrumental Analysis Exam

ICP-MS (sample introduction section) Fill in the boxes for your answers

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+

+

+ +

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23456

1. ?

Items 2-6

7834

Physical states

of analyte

Analyte transformations

ICP-MS (plasma torch)

1

3

2

56

4

Page 3: Instrumental Analysis Exam

Place your answers below:

1.

2.

3.

4.

5.

6.

SEM (electron detectors)- fill in the boxes for your answers

Page 4: Instrumental Analysis Exam

Multiple choices (encircle the letter):

1) The analytical zone of the plasma usually has a temperature of:

a) 5000 – 6000 K

b) 600 – 7000 K

c) 7000 – 8000 K

d) none of the above

2) The ICP-MS sample introduction, what fraction of the sample reaches the

plasma for ionization?

a) 1-2%

b) 0.01-0.02

c) 10-20%

d) 0.1-0.2

3) In ICP-MS, the sampling cone has an orifice diameter of:

a)0.05-0.06 mm

b) 0.5-0.6 mm

c) 800 -1200 microns

d) 0.8-1.2 cm

ENUMERATION ICP-MS

1) Two main components of sample introduction system .

① _____________________

② ______________________

2) Two functions of spray chamber

① __________________________

② __________________________

3) Aside from ICP, there are other types of plasma sources, what are these? List full

words (not acronyms).

Page 5: Instrumental Analysis Exam

① ____________________________________

② ____________________________________

4) List the three criteria of a good ion focusing system.

① ____________________________________

② ____________________________________

③ ____________________________________

5) The chances of undesirable species entering the mass spectrometer are reduced by:

① ____________________________________

② ____________________________________

③ ____________________________________

THERMAL ANALYSIS

6) List the three main types of thermal analysis (no acronyms) and briefly describe

each (2 sentences maximum for each type).

① ____________________________________

② ____________________________________

③ ____________________________________

7) Two input parameters needed during thermal analysis?

① ____________________________________

Page 6: Instrumental Analysis Exam

② ____________________________________

8) Enumerate 5 parameters that can be measured using DSC.

① ____________________________________

② ____________________________________

③ ___________________________________

④ ___________________________________

⑤ ___________________________________

9) Enumerate 5 parameters that can be measured using TGA.

① ____________________________________

② ____________________________________

③ ___________________________________

④ ___________________________________

⑤ ___________________________________

SEM 10) List the three main components of SEM and describe the functions of each (limit your

answers to two sentences for each component).

① ____________________________________

② ____________________________________

③ ___________________________________

Page 7: Instrumental Analysis Exam

11) Enumerate 5 parameters that can be measured using SEM.

① ____________________________________

② ____________________________________

③ ____________________________________

④ ____________________________________

⑤ ____________________________________

True or false. Write T for true and F for false at the end of the sentence.

1) Plasma can generate both positive and negative ions.

2) Between the two Plasma sources, MIP is more prone to matrix effects than DIP.

3) Among the three plasma sources, DIP dominates both ICP and MIP.

4) Skimmer cone has smaller orifice diameter than sampling cone.

5) The impact of a secondary discharge at the interface region cannot be over-

estimated with respect to its effect on the kinetic energy of the ions being sampled.

The energy spread on the ions entering the mass spectrometer must be as high as

possible to ensure that they can be focused efficiently by the ion optics and mass

separation device.

6) The generation of positively charged ion beam is the first stage in the charge

separation process.

7) The compositional integrity of the ion beam after it exits the extraction lens is still

maintained if the heavier ions dominates the center of the beam followed by mid-

sized elements followed by lighter masses at the outermost region.

8) Cylindrical ion lens can produce lower background levels and long-term stability as

compared to multi-component lens system.

9) Analytical sensitivity is also improved when the resolution of the quadrupole is

increased.

10) Abundance sensitivities of quadrupole mass analyzers are generally worse for the

adjacent heavier mass than for the adjacent lower mass.

Page 8: Instrumental Analysis Exam

11) Poor abundance sensitivity of quadrupole can lead to lower detection limit of an

analyte interfered with doubly charge ions.

Concise answers 1) What is the main difference between ICP-EOS and ICP-MS? (1 line answer only!)

2) In ICP-MS, you became familiar with another state of matter. What is it?

3) Explain the mechanism of image formation in SEM (limit your answer to 4 sentences).

4) Differentiate the difference between the two DSC results shown below. Limit your

answers to 3 sentences.

(B) (A

)

Page 9: Instrumental Analysis Exam

5) Based on your understanding of TGA, interpret the TG curves shown below.

1)

2)

3)

4)

5)

6)

7)

Page 10: Instrumental Analysis Exam

FILL in the blanks

ICP-MS

1) The mechanism of liquid sample introduction into the analytical plasma can

considered as two separate ways: _____________ and ______________ (in order). The

sample is normally pumped using _________________ into the ________________, where

the liquid sample is broken up into a fine ____________.

2) The most common design of nebulizer in ICP-MS system is

____________________________.

3) ________________nebulizer design situates the argon gas at right angle with the tip of

a capillary tube while in ________________ nebulizer, the argon gas is along the same

line with the sample.

4) Double pass and Cyclonic type are typical designs of a ___________________.

5) Cyclonic type is operation via __________________ force where droplets are

discriminated to their size by means of a vortex.

6) An ICP plasma discharge is made of argon atoms,____________ and ___________.

7) For plasma generation and electromagnetic field is produced by______________

oscillation at the end of the torch.

8) Inside the plasma torch, there are various heating zones. Coming out from the sample

injector, the sample enters the ____________ zone and then continues to the

_____________zone before it finally becomes ionized in the _________________zone.

9) Both cones are usually made of ________________ but other materials have been used

such as _______________.

Page 11: Instrumental Analysis Exam

10) The undesirable secondary discharge causes several problems like increase in

doubly charged interfering ions, shorter lifetime of the cones, formation of ions

generated from the sampler cone, etc. This problem in instrumentation is usually

solved by______________________________________________.

11) When the ions emerge from the plasma, they will have different kinetic energies

based on their _____________________.

Thermal analysis

12) In thermal analyzer, temperature conditions can be controlled by ___________

depending on your analytical method while ____________ is a component of the

instrument which provides the necessary temperature environment needed.

MATCHING TYPE. Write the letter at left side of each number

1) Heart of the ICP-MS a)quadrupole

2) Achilles heel of ICP-MS b) ceramic

3) mass analyzer material c) mass analyzer

4) Most crucial part of ICP-MS d) time-of-flight

5) most common mass analyzer e) Sample introduction

system

6) resolving power f) stainless steel

7) abundance sensitivity g) molybdenum

8) similar to the photomultiplier tube used in

ICP-EOS.

h) electron gun

9) low ion count rates i) Width of a peak at 10%

height

10) most common detector in ICP-MS j) Channeltron

11) measure heat into or out of a sample k) Faraday cup

12 measures the heat of a sample relative to a

reference sample

l) electron multiplier

13) source of monochromatic electrons m) differential calorimeter

n) calorimeter

o) mass analyzer

performance criteria

Page 12: Instrumental Analysis Exam

ACRONYMS (BONUS):

1) ICP-MS –

2) SEM -

3) TGA –

4) DIP-