CHE 515 XRD Lab Schedule (Fall 2010)

This semester I will be teaching more experimental than I used to do. Each student will go through a set of experiments designed to teach him/her the practical aspects of XRD. A total of 8 labs will be performed. Your lab assistant Erdem will be available to help you with your runs. Please turn in your reports to Erdem on the due dates. He will be grading your reports. Please see him for details about report format. 

Lab No

Lab Name

Date to Perform the Lab

Report Due Date

 

Introduction of the machine and safety regulations reminder

5 October, 2010 Tue 13:30

No report

1

Sample X-Ray Run

12 October, 2010 Tue 13:30

No report

2

Use of X-Pert Software for Phase Identification-1

26 October, 2010 Tue 13:30

9 November 2010

3

Use of X-Pert Software for Phase Identification-2

9 November, 2010 Tue 13:30

23 November 2010

4

Lattice Parameter Measurement of Silicon

23 November, 2010 Tue 13:30

7 December 2010

5

Use of X-Pert Software for Phase Identification-3

7 December, 2010 Tue 13:30

21 December 2010

6

Internal Standard Method

21 December, 2010 Tue 13:30

4 January 2011

7

Determination of Firing Temperature of Ceramic Ware

4 January, 2011 Tue 13:30

18 January 2011

Lab phone number: 750-6231

XRD Machine Authorized Operators: Duygu Oguz, Mine Bahceci, Gokhan Erdogan  and Evrim Yakut

 

CHE 515 Lab 2,3

Use of X-Pert Software for Phase Identification

Date Done: See above list

Report Due Back: See above list

Download Lab Info 

 

In this lab you will be provided unknown materials containing single and multiple phases and you will be asked to

(1)     learn to prepare samples for XRD analysis, 

(2)     analyze an unknown sample for its crystal structure,

(3)     use search match software to identify the unknown phases,

(4)     report your results in a proper format including the literature survey on the characteristics and applications of the material. Please prepare individual reports, not group reports.

 

 

CHE 515 Lab 4

Lattice Parameter Measurement of Silicon

Date Done: 23 November, 2010

Report Due Back: 7 December, 2010

 

In this lab you will do the following:

  1. Read Page 354-358 and 360-363 from Cullity
  2. Determine the crystal structure of silicon from Cullity (Use appendices)
  3. Calculate the expected peaks and their 2q positions on 2q versus intensity chart for CuKa radiation (lCuKa=1.5406 Angstrom). Make a list of all the expected peaks up to 120 degrees.
  4. Based on item 2 determine the best angular range (2q start - 2q end) to run the machine. For lattice parameter measurements also consider the information on page 355 when you decide on the angular range. 
  5. Obtain the difractogram of the polycrystalline silicon sample for the angular range determined in item 3.
  6. Precisely determine the peak positions (2q) using the software. 
  7. Calculate the lattice parameter of silicon using the peak positions found in item 6.
  8. Plot sin2q to the horizontal and the lattice parameters on the vertical axis and do a least squares fit to the data. Least squares method is explained in the textbook. You are required to learn that method and implement it in doing the lab report.
  9. The intercept will give you the best estimate of the lattice parameter of silicon. That is the estimate of the a value at 2q=90 degrees.
  10. Write a lab report and turn it in before December 8th.
  11. Your report should contain introduction, all steps of calculations and the measurement conditions in a proper format.

 

CHE 515 Lab 5

Use of X-Pert Software for Phase Identification

Date Done: 7 December, 2010

Report Due Back: 21 December, 2010

 

 In this lab you will find an unknown crystalline material that you are interested to identify (may be a rock in the street, pebble from the beach, or the corrosion product in your kettle) and you will be asked to  

(1)     prepare a representative sample for XRD analysis, 

(2)     analyze the unknown sample for its crystal structure,

(3)     use search match software to identify the unknown phases,

(4)     report your results in a proper format including the literature survey on the characteristics and applications of the material.  

                                              

 

CHE 515 Lab 6

Internal Standard Method    

Date Done: 21 December, 2010

Report Due Back: 4 January, 2011

 

 

Sample Code

Weight Percent Quartz

Weight Percent Calcite

Weight Percent Fluorite

Total Weight 

1

20

60

20

100

2

30

50

20

100

3

40

40

20

100

4

50

30

20

100

Unknown

*

*

20

100

 

Based on the above table and the XRD Charts you have measured, plot ICalcite/IFluorite versus weight fraction of calcite and do a least squares fit to the data. Look up the percentage of unknown from this calibration curve. Again use both peak height and peak area for your work and comment on the results. Your least squares fit may not be the best fit in the world but still use it and calculate the results.    

  1. Read page 407-420 (especially 415-417) from Cullity about The Internal Standard Method and follow the recipe given in the book. 
  2. Based on the information in the book determine the best angular range for a quartz-calcite-fluorite mixture.
  3. Obtain the diffractogram for the sample with unknown calcite concentration.
  4. Identify each peak for quartz, calcite and fluorite. 
  5. Determine (1) the area and (2) height of the largest peak for each constituent. Also calculate the area and height ratio for calcite and fluorite peaks.
  6. Plot the calibration curve for samples 1 to 4 (See Table above). Plot weight percent calcite against largest peak height and area ratio (IC/IFluorite).  
  7. Do a linear least squares fit to the data and determine the percentage of unknown material in the host material. Remember you will be doing two separate plots: (1) for peak height and (2) for peak area. 
  8. Determine whether area or height gives best results.  Comment on the results. 
  9. Write a lab report, comment on the results and turn it in before January 5th.
  10. Your report should contain introduction about the internal standard method, least squares method, all steps of calculations and the measurement conditions.

 

CHE 515 Lab 7

Determination of the Phase Changes on Heating (<1200oC) a Commercial Clay

Date Done: 4 January, 2011

Report Due Back: 18 January, 2011

  1. Do a literature survey to determine the phase changes on heating a commercial clay sample that contains possibly kaolinite, quartz and maybe some accessory phases (Canakkale Seramik Product). Remember that Kaolinite, for example, is an aluminosilicate hydrate which loses its chemically bound water at around 500oC. This loss of water results in the collapse of the crystal structure that produces an amorpous phase known as Metakaolin.  Further heating results in the formation of other new phases. You are expected to find out which phase transition sequence takes place upon heating the clay samples. You should report the temperature ranges in which the above mentioned phases are stable. 
  2. You will be given clay samples that were heated at 400, 600, and 1200oC for 60 minutes. 
  3. Obtain the diffractograms for the four samples (including the unheated sample) that were heated at 400, 600, and 1200°C for 60 minutes from 4-70 degrees. 
  4. Do phase identification and search match to identify the constituents.
  5. Overlap all peaks on one chart, comment on the disappearing or appearing peaks based on the information in the literature.
  6. Write a lab report, comment on the results and turn it in before January 19th.
  7. Your report should contain the literature survey, all steps of calculations and the measurement conditions in a proper lab report format.

 

 

This page last updated Sept 30th, 2010 by S.Akkurt.