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. Go to the RAD center at 35th and Washington Way. 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 lecture on neutron activation analysis of zeolites (NAA).
2. Return to GBAD and continue the ion exchange procedure on page 8 through point 6. Be sure to use the AgNO3 bottle marked "zeolite".
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 Sleight'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. The research associate in Dr. Sleight's lab 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 (p. 12). 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 C. Analytically weigh 0.25 g hydrated 5A zeolite into a tared 2/5 dram polyvial provided by the instructor. Wear gloves when handling the vials. First heat seal the inner 2/5 dram vial, slide it into a larger outer vial and heat seal the outer vial. This will help prevent contamination in the advent that the sample vial breaks after activation. 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 work.
2. Promptly appear at the Radiation Center at 1:00 with your sample on your assigned day. Sign in and obtain a radiation badge from the Receptionist.
3. With an instructor and the Radiation Center representative, proceed to the counting room (B100) 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 the laboratory notebook and record the experimental parameters.
5. When leaving the Rabbit Room, survey yourself with the automatic frisker and if clean, return to the counting room, B100. Notify the instructor if you are contaminated. Count the sample and standard in Rm. B100. Be sure you have saved your pulse height spectrum for the sample and standard rock. Get a hardcopy of all the major peaks and peak areas.
STUDENT DIRECTIONS FOR EXPERIMENT 1 ZEOLITES PART D 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 a small sample of the hydrated 5A zeolite.
2. Check with the instructor for directions on operating the instrument.
STUDENT DIRECTIONS FOR EXPERIMENT 1 ZEOLITES PART E SORPTION
Before coming to class: study lab write-up pages 24 - 28 and 31-32 .
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. (see p. 8) 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 and measure the height of the empty bucket in air using the cathetometer next to your vacuum line.
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 McBain Balance apparatus on the vacuum line in GBAD 314 and cover with the glass tube slowly evacuate the Balance. (If your powder bumps out of the bucket, start over again with a new portion).
5. Determine your spring constant (in cm/g) and check this with the instructor.
6. Record the time, pressure, and spring position (weight) every 5 minutes upon admitting successive 5 to 10 torr increments of N2 gas from the gas bulb. Remeasure the pressure after each 5 minute delay. Continue additions until a constant weight is reached. See p. 28.
7. Shut down the vacuum line, remove your bucket, clean up.