STUDENT DIRECTIONS FOR EXPERIMENT 1 ZEOLITES: PART A SYNTHESIS OF 4A AND ION EXCHANGE TO 5A.
FIRST PERIOD
1. Read (study, learn) pages 1 - 8 of the lab write-up.
2. Listen to the "Zeolite Molecular Sieves" audio-cassette tape and study the accompanying booklet.
3. Filter and wash the 4A that has been curing since last term (p 7-8). Complete the calcium exchange to obtain Zeolite type "5A" procedure on page 8.
SECOND PERIOD
1. Meet at GBAD 309 at 1 pm and continue the ion exchange procedure on page 8 through point 6. Be sure to use the AgNO3 bottle marked "zeolite" to test for excess chloride ion from the rinse.
2. Promptly at 2:30 go to the OSU Radiation Center at 35th and Washington Way (you need to be there promptly at 2:45 or you will not be allowed to continue). Meet at the front desk. Sign in if required. Tell the Receptionist that you are with CH 462 for the tour and safety orientation. You will also have a lecture by Dr. Leah Minc an expert on instrumental neutron activation analysis (INAA).
3. Look over the Zeolite Booklet #2 available in GBAD 311.
STUDENT DIRECTIONS FOR EXPERIMENT 1 PART B X-RAY DIFFRACTION
1. In advance, read the lab write-up pp. 9 - 14, 29 and SGN 6 th ed. Experiment 45, pp 472-487.
2. In class, listen to the X-ray Diffraction audio-cassette tape and read the accompanying booklet. (You may repeat this activity if desirable when it comes time to do the calculations).
3. The instructor will give you directions on how much sample is needed and how to fill the sample holder. Do this and then proceed with the instructor, to Professor Subrumanian's laboratory in Gilbert Hall where the experiment will be performed.
4. Carry out the exposure (p. 11).You will not be exposed to any Xradiation. One of your TA's will load the samples in the diffractometer and operate it. You are only to observe this operation.
5. Find a PC and print out your data file. Also import your data file into a spreadsheet and work on the analysis during class.
STUDENT DIRECTIONS FOR EXPERIMENT 1 ZEOLITES PART C NEUTRON ACTIVATION ANALYSIS
Before class carefully study pages 13 - 20 and
29-30 of the lab write-up.
1. Prepare your zeolite 5A hydrated sample for NAA analysis. This must be done in advance of the day your group is assigned to go to the Radiation Center for part D. Analytically weigh 0.25XX g hydrated 5A zeolite into a tared 2/5 dram polyvial provided by the instructor. Wear gloves when handling the vials. Label the vial with your group number using a sharpie and store the sealed vial in a zip lock bag and bring it with you to the Radiation Center when you are scheduled to do the activation and counting work. When you are at the RCenter, this vial will be heat sealed and it will be put into a larger outer vial and that vial will also be heat sealed. This will help prevent contamination in the advent that the sample vial breaks after activation.
2. Promptly appear at the Radiation Center at 1:00 with your sample on your assigned day. Sign in at the front desk and obtain a radiation dosimeter from the Receptionist.
3. With an instructor and the Radiation Center representative, proceed to the counting room for an explanation of the counting equipment and directions on operation of the counting software on the PC. You will use sealed sources to calibrate the detector for your assigned counting system (e.g., 137Cs or 60Co). Look up the gamma ray energies for these before going to the Rad Center.
4. Go with the instructor or another qualified user to the Pneumatic transfer room (Rabbit room) to irradiate your zeolite sample and one standard rock sample. One person in each group should bring a laboratory notebook and record the experimental parameters while in the Rabbit room.
5. When leaving the Rabbit Room, survey yourself with the automatic frisker and if clean, return to the counting room. Notify the instructor if you are contaminated. Count the sample and standard at your station. Be sure you have saved your pulse height spectrum for the sample and standard rock and saved the region of interest report for both the sample and the standard at your station. Get a hardcopy of all the major peaks and peak areas if the printer is working otherwise, save a copy of the report in Word so that you can print it back in the GBAD lab.
STUDENT DIRECTIONS FOR EXPERIMENT 1 ZEOLITES PART C THERMOGRAVIMETRIC ANALYSIS
Before coming to class: study lab write-up pages 21-23 and 30.
1. The TGA is next to the DSC in GBAD 314. You will need only about 20 mg of the hydrated 5A zeolite.
2. Check with the instructor for directions on operating the instrument and using the software to analyze the data.
STUDENT DIRECTIONS FOR EXPERIMENT 1 ZEOLITES PART E SORPTION
Before coming to class: study lab write-up pages 20 - 27.
1. Listen to the audio-cassette tape "Sorption of Nitrogen by Zeolites" and read the accompanying booklet.
2. The instructor will show you the vacuum set-up and the apparatus in room 314. Heat 2 g of the zeolite in a muffle furnace for at least 2 hours (or overnight) at 400 °C before the experiment is to begin (do this the day before if possible).
3. Preweigh the foil bucket to ± 0.1 mg.
4. Quickly transfer the anhydrous solid to the preweighed bucket and reweigh to ± 0.1 mg using the same analytical balance as in step 3. Quickly hang the bucket in the modified McBain Balance apparatus on the vacuum line in GBAD 314 and cover with the glass outer tube and slowly evacuate the Balance. (If your powder bumps out of the bucket, start over again with a new portion).
5. Calibrate the mass balance following the directions in the lab manual.
6. Read the directions in the lab manual. Start the program and collect data after small admittance of N2 gas from the gas bulb over time and collect the mass of the bucket, zeolite and nitrogen. Continue additions until a constant weight is reached.
7. Shut down the vacuum line, remove your bucket, and clean up.