MM-302: X-ray Diffraction and Crystallographic Techniques

(Test-1: January/February 2009)

1- X-rays penetrate human body and matter because it is _____________ radiation.

a) electromagnetic radiation b) longer wavelength c) shorter wavelength d) invisible

2- X-rays are_____________ radiations then ultraviolet light.

a) higher energy b) lower energy c) lower frequency d) longer wave length

3- X-rays cannot penetrate_____________.

a) Lead b) wood c) steel d) Plastics

4- During radiography of human body a ___________ will appear as darkest regions

a) Crack b) Bone c) Muscle d) Skin

5- X-rays posses a wavelength ___________ to atomic lattices.

a) Comparable b) not comparable c) Very different
d) Large enough

6- The wavelength of x-rays is measured in ___________.

a) cm b) angstrom c) micron d) nanometer

7- X-rays can penetrate metals because of______________ radiation.

a) high energy b) longer wavelength c) shorter wavelength
d) low energy

8- The wavelength of X-rays is given by ______________ .

a) λ = C/V b) V = λ C c) C = λ V d) none of there relations

9- X-rays of 1Å to 3Å are in use, which has more penetration?

a) 3Å b) 1Å c) 1.5Å d) 4Å

10- ___________ wavelength X-rays used in medicals applications.

a) Shorter b) longer c) Medians d) none of these

11- If an electron from L shell fills the vacancy in K shell it emit ________ radiation.
a) Kα b) Lα c) Kβ d) none of these

12- A crack will appear as _________ in radiography.

a) white b) black c) grey d) point

13- In X-ray tube _________ is used as source of electrons.

a) anode b) cathode c) grid d) lead

14- White radiation Consists of __________ wavelength light.

a) Single b) Two c) Three d) multiple
15- The energy of X-rays depend upon the __________ .
a) acceleration voltage b) heater current c) anode current
d) heater voltage

16- The characteristic X-rays have __________ wavelength than white radiation.
a) Smaller b) Longer c) Multiply d) no radiation its

17- The λswl depend upon __________ .

a) heater current b) anode current c) anode voltage
d) heater voltage

18- The intensity of the X-rays depend on ________ of materials.

a) atomic weight b) atomic number c) volume electron
d) number of nutron

19- The wavelength of X-rays depend upon ________________.

a) anode materials b) cathodes materials c) applied anode voltage
d) atomic number

20- The mass absorbance coefficient of X-rays depend upon ____________.

a) atomic weight b) atomic number c) volume electron
d) number of nutron

21- If an electron from M shall fills the hole in K shall the radiantion is called____________.
a) Kα3 b) Kβ1 c) Mα3 d) Mβ

22- The emission of characteristic X-rays depend upon a critical applied ___________ of each material.
a) anode voltage b) anode current c) heated voltage
d) heated current

23- The total intensity (I) of the continuous spectrum as given by _________________.
a) I=AiZVm b) I=Ai/ZVm c) I= ZVm/Ai d) I= AiZ/Vm

24- To get maximum intensity a __________ element should be used as target.

a) high atomic number b) low atomic number
c) high atomic weight d) low atomic weight

25- Bremsstahlung consist __________ wavelength of radiation.

a) single b) Two c) Triple d) multiple

26- Energy of Kα radiation is __________ than Kβ radiation.

a) lower b) higher

27- The wavelength Kβ radiation is___________ to Kα radiation.

a) smaller b) longer c) equal d) Comparable
28- The mass absorption coefficient _____________with density of Material.
a) decreases b) increases c) not affected

29- ___________ radiation used for X-ray florescence to determine chemical composition.
a) Kα b) Kβ c) Lα d) none of these

30- The heater of x-ray tube is made of ______________.

a) tungsten b) nickel c) stainless steel d) nichrome

Q- Draw schematic of an X-ray tube and label the essential parts.

Q- Write down at least 10 applications of X-ray diffraction.

Q- What are the essential requirements of an anode material for X-ray tubes?
 MM-302: X-ray Diffraction and Crystallographic Techniques
(Test-2 March 2009)

1. An x-ray radiation of_________ wavelength is most dangerous.

a) 1.5Å b) 20Å c) 100Å d) 1Å

2. _________ radiation is most dangerous.

a) Bremstrahlung x-rays b) α-particles c) γ-particles d) 1Å x-rays

3. Diffraction with divergent slit is ____________.

a) very good b) possible c) not possible d) excellent

4. A_________ is more suitable for diffraction.

a) pen laser b) halogen lamp c) tungsten bulb d) Florescent tube light

5. A collimated beam is ___________ for diffraction.

a) essential b) not necessary

6. X-rays are higher energy radiations than visible light. If you could see the x-rays in the same
way you can see visible light would it appear brighter than light?
a) true b) no c) may be d) surely

7. A diffracted beam may be defined as a beam composed of a large number of scattered rays
mutually reinforcing one other.
a) true b) not true

8. By atoms arranged randomly in space, the scattering of light occurs in __________ directions
a) all b) some c) very few d) none of the

9. By atoms arranged randomly in space, the scattered light is ______.

a) weak b) strong c) mixed d) very strong

10. If the_________are added during scattering, the scattered light gives weak illumination.
a) intensities b) amplitudes c) frequencies d) wavelengths

11. If the_________are added during scattering, the scattered light gives strong illumination.
a) intensities b) amplitudes c) frequencies d) wavelengths

12. The diffracted beam from a crystal is built up of rays scattered by all the atoms of the crystal
which lie ________ of the incident beam.
a) in the path b) out of path as well c) in any plane d) in the crystal

13. The diffraction of monochromatic x-rays takes place only at those particular angles of incidence which
satisfy the Bragg law while the reflection of visible light takes place at any angle of incidence.
a) true b) not true c) may be

14. The reflection of visible light takes place from atoms of_______ layers.
a) surface b) all c) few d) deep

15. The reflection of visible light by a good mirror is almost 100 percent efficient.
a) true b) may be c) not true
16. The intensity of a diffracted x-ray beam is extremely small compared to that of the incident beam.
a) true b) may be c) not true

17. Diffraction is a scattering phenomenon in which a _______ number of atoms cooperate than reflection.
a) larger b) smaller c) few

18. The diffracted beam from a crystal is built up of rays scattered by ________ of the crystal
which lie in the path of the incident beam.
a) all the atoms b) some of the atoms c) any atom d) very few atoms

19. By using x-rays of known wavelength λ and measuring θ, we can determine the spacing d of
various planes in a crystal, called x-ray diffraction.
a) true b) may be c) not true

20. The d-spacing of various plane provides information about the structure of the crystal.
a) true b) may be c) not true

21. If we use a crystal with planes of known spacing d, measure θ,, and thus determine the
wavelength λ of the radiation used: this is called x-ray spectroscopy.
a) true b) may be c) not true

22. The first diffraction used was _________ method.

a) Debye-Scherrer b) Laue c) Roentgen d) Cullity

23. White radiations are used in __________ diffraction method.

a) Debye-Scherrer b) Laue c) Roentgen d) Cullity

24. The Bragg angle theta is fixed in __________ diffraction method.

a) Debye-Scherrer b) Laue c) Roentgen d) diffractometer

25. λ is variable in ______________ diffraction method.

a) Debye-Scherrer ) Laue c) Roentgen d) diffractometer

26. ___________ method is the most commonly used for large single crystals.
a) Debye-Scherrer b) Laue c) Roentgen d) diffractometer

27. ___________ method is potentially more health hazardous than other methods.
a) Debye-Scherrer b) Laue c) Roentgen d) diffractometer

28. ____________ method is commonly used for the determination of unknown crystal structure.
a) Rotating-crystal b) Debye-Scherrer c) Laue d) diffractometer

29. Deby-Scherrer diffraction method _________ be used for single crystal.

a) can b) cannot c) occasionally d) perhaps

30. _____________ method is most suited method for determination of lattice parameters.
a) Debye-Scherrer b) Laue c) Roentgen d) diffractometer
Answers of descriptive questions: (Test-2 March 2009)

Q-1: Bragg's law is used in XRD to relate repetitive structural size to the diffraction pattern.
-Give Bragg's Law.
-Sketch a diffractometer showing x-ray source, collimation, slits system, sample, detector and the scattering
angle to explain the parameters in Bragg's Law.

[Answer: Bragg’s Law nλ = 2dsinθ

Bragg's law requires monochromatic light in

order to fix λ, a collimated beam in order to
fix the angle, and coherent radiation to have
coherent interference between the waves.
The coherence length must be larger than the
size observed, i.e. d.]

Q-2: Using the example of a halogen lamp and a

pen laser, explain what a collimated beam of
electromagnetic radiation is. Why is collimation
important to Bragg's Law?

[Answer: Collimated means that the

component beams all travel in the same
direction. A halogen lamp has divergent
beams meaning that the beams emit in
directions that serve to spread out the light.
Collimation is important to Bragg's Law
since the angle can only be measured with precision if
the beam is well collimated. Diffraction with a divergent beam is not possible.

Halogen Bulb Laser Pen

Q-3: X-rays are electromagnetic radiation of higher energy compared to visible light. If you could
see X-rays in the same way you can see light would they appear brighter than light? Explain.

[Answer: Energy, E = hν, reflects the capacity of a photon of the radiation to do work. Since the
interaction of radiation with matter involves collisions of photons with atoms and molecules and
transfer of this energy, the energy decides what the radiation can physically do. The brightness
or flux is the number of photons per area per time. The energy does not have to do with the
brightness.]

Q-4: Light is a form of electromagnetic radiation. Visible light differs from a laser in several ways
from visible light from a light bulb.
-List 4 ways that laser light differs from light from a light bulb.
-How do these differences allow laser light to travel long distances?

[Answer:
a)
o Laser light is usually plane polarized, monochromatic, collimated and coherent.
o Light from a light bulb is unpolarized, polychromatic, uncollimated and incoherrent.
b)
o Polarization and monochromicity don't really effect the distance traveled.
o Collimation ensures that the light doesn't dissipate by divergence and coherency ensures that the light
doesn't decay due to
interference with itself.]
X-ray Methods-Whiston
SAQ 2.2a/47: What happens when a monochromatic x-ray beam is incident odthe following?
(i) A stationary single crystal.
(ii) A rotating crystal
(iii) A crystalline powder.
(iv) Powdered glass.

SAQ 2.4a/64: List (i) the advantages an disadvantages of the flat film method.----ÆP-338-339
SAQ 2.5a/70: List ways in which the powder diffractometer method differs from the Debye-Scherrer method.

Questions

Distinguish between the roentgen and sievert.

Q- Write down at least 10 applications of X-rays

Q- What are the essential requirements of an anode material for X-ray tube.
 MM-302: X-ray Diffraction and Crystallographic Techniques
(Test-3 March 2009)-X-ray Safety and Precautions

1- REM (Röentgen-Equivalent-Man) is the absorbed dose in ‘RADs’ equivalent absorption

corrected for the living tissue.
a) true b) false

2- The x-ray of one rem is equal to one rad.

a) true b) false

3- One sievert is equal to _____________ rem.

a) 1 b) 100 c) 1000 d) 10

4- X-ray exposure doses are commonly expressed as R/hr (röentgen per hour) or m R/hr
(milliröentgen per hour )
a) True b) False

5- Normal background radiation levels are in the order of 0.01-0.1 mR/hr.

a) True b) False

6- which of the following is the most serious?

a) A dose of 3.37 Sv delivered to the elbow in one second.
b) A constant dose of 1.07x10-7 Sv per second for one year to the whole body

7- X-rays _______ kill human tissue.

a) can b) cannot 3) never 4) some times

8- ___________ exposure to x-ray is most dangerous

a) localized b) long time c) short time d) full body

9- RAD (Röentger-Absorbed-Dose) “rad” is the amount of radiation that will deposit

__________ Jules of energy in a kilogram (or 100 ergs / gm) of material.
a) 0.01 b) 0.1 c) 1.0 d) 10

10- One gray (Gy) is equal to ___________ rad.

a) 100 b) 1 c) 1000 d) 0.1

11- X-ray produces___________ changes in biological tissue

a) chemical b) physical c) deep d) shallow

12- Exposure to x-ray _______ cause graying of hair.

a) can b) cannot c) impossible d) perhaps

13- Dosimeters can _________ operator from x-ray exposure.

a) protect b) monitor c) reduced d)avoid
14- X-ray diffractometer are equipped with___________ glass to stop leakage of x-rays
during operation.
a) tinted b) tempered c) leaded d) annealed

15- Soft x-rays are ____________ absorbed in biological tissue.

a) easily b) difficult c) less d) equally

16- Primary beam in analytical x-ray systems are generally well collimated with a beam
diameters less than _____ centimeter
a) 1 b) 10 c) 20 d) 100

17- A short time exposure about 0.1 second of primary beam in an analytical system can
cause __________ injury.
a) no b) harmless c)permanent d) temporary

18- Potential exposure to the primary beam is generally not a major concern in analytical
system.
a) true b) false c) partially true d) absolute false

19- In medical applications __________ x-rays are used.

a) soft b) hard c) medium d) hardest

20- Soft X-rays are ___________ to Shield.

a) difficult b) easy c) impossible d) not required

21- In analytical methods ___________ x-ray are used

a) soft b) hard c) medium strength d) very soft

22- X-rays used in medical applications are __________than x-rays use in analytical method.
a) more dangerous b) less harmful c) equally dangerous
d) more patient friendly

23- X-rays penetrate human body and matter because it is _____________ radiation.
a) electromagnetic radiation b) longer wavelength c) shorter wavelength d) invisible

24- During x-ray diffraction primary beam is ________ dangerous than diffracted beam.
a) not so b) very c) equally d) not

25- X-rays _______deform biological cells.

a) can b) cannot c) should not d) truly not

26- TLD badges can_________ operator from x-ray exposure.

a) protect b) monitor c) reduced d)avoid
Q-1: Which of the following is the most serious and why? Whiston P42/333

c) A does of 3.37 Sv delivered to the elbow in one second.

d) A constant exposure of 1.07x10-7 Sv per second for one year to the whole
body
Q-2: Write down at least 3 short-term effects and 3 long-term effects of x-ray exposure.

Q-3: Distinguish between the röentgen, gray and sievert ___________ P 41/332/whiston

Q-4: If you are an incharge of XRD lab, what safety measures you suggests? Describe at least
10 safety measures.
 MM-302: X-ray Diffraction and Crystallographic Techniques
(Test-4 May 2009)-Chemical Analysis by XRF

1- Measurement of wavelength or energy of characteristic x-rays enables us

_________analysis.
a) qualitative b) quantitative c) semi-quantitative d) semi-qualitative

2- Measurement of wavelength or energy of how many characteristic x-rays of any type

enables us _________analysis.
a) qualitative b) quantitative c) semi-quantitative d) semi-qualitative

3- X-ray dispersion methods are used for__________ analysis of materials.

a) structural b) chemical c) fractional d) in-depth

4- XRD provides information about structure and chemistry of the sample.

a) True b) False

5- In XRD we use known ______ measure___________and calculate _______ spacing

of materials.
a) λ, θ, d b) λ, d, θ c) θ, λ, d d) θ, d, λ

6- In spectroscopy we use known ______ measure___________and calculate _______

spacing of materials.
a) λ, θ, d b) d, θ, λ c) θ, λ, d d) θ, d, λ

7- Fluorescence involves __________ of primary x-rays.

a) absorbance b) transmission c) scattering

8- In WDS___________ of characteristic x-rays is measured.

a) Wavelength b) energy c) both wavelength and energy d) only counts

9- In EDS___________ of characteristic x-rays is measured.

a) wavelength b) energy c) both wavelength and energy d) only counts

10- Flat-Crystal WDS spectrometer consist of ____________.

a) Divergent and Convergent slits b) collimators
c) both slits and collimators d) convergent slits only

11- Curved-Crystal WDS spectrometer consist of ____________ .

a) Divergent and Convergent slits b) collimators
c) both slits and collimators d) convergent slits only

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12- The EDS spectrometer consists of __________.
a) Divergent and Convergent slits b) collimators
c) both slits and collimators d) none of these

13- The focusing distance D in WDS spectrometer __________ with θ.

a) decreases b) increases c) does not change d)initially decreases

14- We have to use different crystals in WDS spectrometer to keep the focusing distance
within limits.
a) True b) False

15- For measurement of hi-Z elements crystal of ___________ d spacing shall be used.
a) smaller b) larger c) any d) equal

16- For measurement of lo-Z elements crystal of ___________ d spacing can be used.
a) smaller b) larger c) any d) equal

17- The resolution of WDS spectrometer is _______ than EDS.

a) Poorer b) better

18- The intensity of _________ characteristic x-ray is highest.

a) Kα b) Kβ c) Lα d) Lβ

19- The maximum wavelength that a crystal can reflect is equal to its 2d spacing.
a) True b) False

20- The Crystals with smaller 2d spacing can reflect __________ wavelength x-rays.
a) shorter b) longer c)both shorter and longer d) medium

21- The Crystals with larger 2d spacing can reflect __________ wavelength x-rays.
a) shorter b) longer c) both shorter and longer d) medium

22- In Flat-Crystal spectrometer the analysing crystal is mounted on a turntable.

a) True b) False

23- For qualitative analysis the analysing crystal is ___________during analysis .

a) rotated b) stationary

24- For quantitative analysis the analysing crystal is ___________during analysis.

a) rotated b) stationary

25- The recorded intensity is _____________ to the element’s concentration.

a) related b) not related

26- The energy resolution of WDS spectrometer is _______ than EDS.

a) Poorer b) better

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27- The wavelength resolution of EDS spectrometer is _______ .
a) Poorer b) better
28- EDS spectrometers are ______________ than WDS.
a) Faster b) Slower

29- The peak resolution of EDS is __________ than WDS.

a) Poorer b) better

30- The ED-spectrometer are ___________ for determining elements of longer wavelength.
a) suitable b) not suitable c)

31- The XRF technique is applicable to a wide concentration range___________. %

a) fractional ppm to 100 b) 1 to 10 c) ppb to 100 d) fractional ppm to 10

32- The XRFA can analyse __________concentrations.

a) 1μgm dm-3 b) 1 ngm g-1 c) 0.0001% d) 1 ngm g-2

33- WDS can analyse ___________ elements than EDS.

a) more b)less c) equal number of d) in some cases less number

34- XRF is basically a techniques which can determine_____________ in the sample.

a) elements b) compounds c) both elements and compound d) molecules

35- XRF is based on that __________ can excite by external energy, emit characteristic
x-ray photon.
a) atom b) molecule c) both atom and molecule c) ions

Page No. 3 of 5
 MM-302: X-ray Diffraction and Crystallographic Techniques
(Test-4 May 2009)-Chemical Analysis by XRF

Q-1: What x-ray method/s will be used for analysis of:

a) Corrosion product b) Austenite and Martensite Phases in Steel c) Analysis
of Cr and Ni in stainless steel
d) Analysis of Boron in boroided steel.

Justify your selection in few lines.

Q-2: Draw schematic diagram of Flat-Crystal and Curved-Crystal WDS

spectrometer. Elaborate difference between the two.

Q-3: What are the differences between X-ray powder diffractometer and a WD
spectrometer?

Q-4: Describe the four types of basic spectrometers. What type of spectrometer
will you select for following application and Why?
a) Materials Characterisation Lab of MMD
Manual Type-To demonstrate students various
functions of the spectrometer by analysing a variety
of material samples+ it is a cheaper option-which is of
prime importance in the University.
b) Pak Land Cement Factory
Simultaneous Spectrometer ideally suited to online
analysis for production control-routine analysis.
c) Pak Suzuki Semi-Automatic-A Large number of diverse samples.
d) People’s Steel Mills
Automatic-sequential- Routine analysis of large
number of samples - producing more than 300
different grade of steels!

Q-5: List the advantages and disadvantages of qualitative XRF analysis.

Advantages
You probably thought of most of the following:
__
A large range of elements can be detectedÆ Most commercial
instruments can detect elements heavier than fluorine, though
some very modern instruments can detect elements from beryl-
lium upwards in the Periodic Table.

Page No. 4 of 5
 __
The technique is applicable to a wide concentration range: frac-
tional ppm to 100%.
__
Samples can be bulk solids, powders, slurries and liquids.
__
Both large and small samples can be handled.
__
The technique is generally non destructive.
__
The method is applicable to 'difficult' samples such as slags,
which cannot be analysed by techniques which require the sam-
ple to be in solution.
__
Automatic instruments can deal with large numbers of samples
and can be left running overnight.
__
The actual analysis is rapid (by an experienced analyst
anyway!)
__
Running costs are relatively low.

Disadvantages
I expect you included all or most of the following:
__
Not applicable to very light elements, so not always useful for
organic samples.
__
Not generally applicable to gaseous samples.
__
X-ray penetration is small so specimen preparation may be nec-
essary to ensure that the surface is representative of the sample
as a whole.
__
Certain organic and biological samples may become chemically
changed.
__
High initial capital cost.
__
The machines are complicated and require trained personnel to
operate them.
__
Sample preparation may destroy the shape of the sample e.g., a
metal casting.

Q-6: Describe the limitations of EDS and WDS techniques.

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