J.D. McCullough X-ray Facility

Welcome to UCLA’s J.D. McCullough X-ray Facility

1416 Molecular Sciences Building

About

James Douglas McCullough was born in Oskaloosa, Iowa on May 17, 1905 and grew up in Seattle. After graduating from Seattle’s Lincoln High School in 1923, he went to work for the Standard Oil Company of California, first as a junior clerk and then in a service station in Los Angeles, a job that he used to help support himself while earning his A.B. degree in chemistry at UCLA. Upon graduation in February 1932 he was regarded, in the words of Professor W.C. Morgan, the first chairman of the Department of Chemistry, as “possibly the most outstanding man we have had in Department of Chemistry since we started giving instruction”. He was appointed to the UCLA teaching staff at once, first with a six-months’ temporary position and then with a series of one –year appointments as Associate (essentially a high-level teaching assistant) while he was earning his Ph.D. in physical chemistry at the California Institute of Technology under the guidance of A.O. Beckman and Linus Pauling. After receiving his Ph.D. in 1936, Dr. McCullough joined the UCLA faculty on a full time basis and remained at UCLA throughout his career. He retired in 1971 after 39 years of service, remaining active in research for another half dozen years, although his move to Orange County made coming into the laboratory less convenient.Professor McCullough established the first X-ray laboratory at UCLA in 1936, in the basement of the “old chemistry building” (now Haines Hall). He started with an old powder camera (which he converted into a camera for taking single-crystal rotation photographs), borrowed from Caltech, and a specially ordered cold-cathode gas-ion x-ray tube (see picture below). A decade later he received a grant to buy our first Weissenberg camera. From those modest beginnings grew the well equipped laboratory that you see around you today.

This photograph was taken about 1938 by a student (Nichols) in Professor McCullough’s Chemistry Class. The gas-ion X-ray generator tube is in the left and center foreground. The anode or target (interchangeable Cu or Mo) is to the left and is water cooled at ground potential. The cold Cathode is to the right and is air cooled at high potential. At the extreme right we have the high capacity vacuum pump which maintains a pressure in the 103 to 102 mm range. The desired operating pressure was maintained by admitting air through an adjustable slow leak made of coiled up, flattened silver tube. The pressure was not measured as such, but was adjusted to optimum X-ray emission. The rebuilt powder camera, now as oscillation camera, is in the left rear. Unfortunately, it does not show up very well, being obscured by the X-ray tube. The vertical black cylinder encloses the film and the oscillating single crystal. It also holds the beam collimator and the beam stop.

Services

Single-Crystal XRD:

  • Full service single-crystal X-ray diffraction (Mo or Cu Kα radiation)
  • Single-crystal X-ray data collection
  • Single-crystal X-ray unit cell determination
  • Absolute configuration determination (not possible in all cases)
  • Variable temperature studies (100K – 300K)

Powder XRD:

  • Powder X-ray data collection
  • Powder X-ray phase analysis

Note: Powder XRD services are limited to 5 samples. If you have more, we will be happy to train you to run your own samples. 

All of the above services have nominal fee. Please consult with Tyler Kerr for charges.

Training

Single-Crystal XRD:

Training in single-crystal X-ray diffraction is available to all who meet the following criteria:

  • Interest in learning to collect, refine, and/or publish SC-XRD data

  • Has (or expects to have) many single crystal samples

We offer training that will cater to your needs. If a user desires a full-service XRD dataset and report, if the user is completely independent, or anywhere in between, we are happy to work with you.

Powder XRD:

Standard PXRD training is available to all who need it. Please see the Access & Training tab for more information.

Sample Submission

For users inside UCLA, please contact Tyler Kerr directly.

For users outside of UCLA desiring single-crystal analysis, submit your sample and a fully completed sample submission form (copies are also available in the lab) to:

Dr. Tyler Kerr

1412 Molecular Science Building
Dept. of Chemistry & Biochemistry
University of California, Los Angeles
Los Angeles, CA 90095-1569

Your sample will be analyzed on a first come first serve basis. Normal turn around time is 2-3 days. For powder samples no sample submission form is required. Outside users should mail properly sealed samples to:

Instrumentation

Panalytical X’Pert Pro X-ray Powder Diffractometer

  • Installed in 2004
  • Bragg-Brentano and Parallel Beam Optics
  • Incident and Diffracted Beam Mirrors
  • Computer Controlled Slits
  • X’celerator RTMS Scanning Detector
  • Sealed Proportional Detector
  • High Temperature Stage up to 1000°C

Bruker DUO ApexII CCD Single-Crystal X-ray Diffractometer

  • Installed in 2013
  • Quazar multilayer Microfocus Cu
  • Triumph Monochromator Mo-X-ray source
  • Low temperature device (100K – 300K)
  • APEX2 software suite

Bruker D8 Discover Powder X-ray Diffractometer

  • Installed in 2006
  • Push Plug Gobel Mirror
  • 9-Position Sample Stage
  • Vantac Detector for Fast Simultaneous Recording
  • Rotary Absorber

Zeiss Stereo Discover V12 Microscope

General Training for the X-ray Facility

The following must be completed in order to be trained on the MIC powder X-ray diffractometers:

  1. Users within UCLA must have a Chemistry & Biochemistry Department recharge account. If you do not have one, one can be requested by filling out and submitting this form to the recharge@chem.ucla.edu.
  2. Users from outside UCLA must create an online ID here to continue to the following step.
  3. All users must complete the following training modules within Worksafe:
    • Laboratory Safety Fundamental Concepts (LSFC) Training
    • Radiation Safety for Users of Radiation Producing Machines

Powder X-ray Diffractometer Training

After completing both LSFC and Radiation Safety Training sessions, please contact Hootan Roshandel for training on the powder diffractometer.

Scheduling and Instrument Reservations

Powder XRD: Users within UCLA must be logged in to the VPN and may access the reservation website. Users outside of UCLA, please contact Tyler Kerr to reserve time up to four weeks in advance.

Single-Crystal XRD: Use of UCLA’s single crystal X-ray diffractometer is governed through a queue. The diffractometer waits for no one. To be added to the queue and to receive an estimated time, please contact Tyler Kerr

Instrument Rates

For information regarding our instrument rates, please contact Tyler Kerr directly.

X-ray structure. 
L. M. A. Saleh, R. M. Dziedzic, S. I. Khan, A. M. Spokoyny, Chem. Eur. J. 2016, 22, 8466.  http://onlinelibrary.wiley.com/doi/10.1002/chem.201601292/full

Instrument Rates

Single Crystal Structural Determination

  • UCLA User: $500 each
  • External Nonprofit: TBD
  • External Commercial: TBD

Single Crystal Data Collection

  • UCLA User: $50/hour (Day Rate), $25/hour (Night and Weekend Rate)
  • External Nonprofit: TBD
  • External Commercial: TBD

Powder Diffraction Data Collection

  • UCLA User: $50/hour (Day Rate), $25/hour (Night and Weekend Rate)
  • External Nonprofit: TBD
  • External Commercial: TBD

**Consultation is $100/hour

Reservations

All reservations for powder X-ray diffractometers are made through our online reservation website. If your sample is unstable and you need to arrange for special circumstances, please contact Tyler Kerr.

You must log onto each instrument through the LinRL computer in the X-Ray lab. For directions on using the LinRL, please click here.

How to make a reservation

Web–based X-Ray Reservations

  1. You must be at UCLA or using a UCLA VPN to connect to the web-based reservations. (See 6. below for information on obtaining a UCLA VPN.)
  2. Firefox is the recommended browser. Internet Explorer will work but will require a “refresh” after making or canceling a reservation.
  3. To use the web-based reservation system, you will need to know at least the first three characters of your username as it was entered in the LinRL system.
    • This is not usually the same as a login name you may have on any instrument. Usually this is your surname. Be sure to note what it is at the time you are first given access to LinRL.
    • It is not case-sensitive, i.e. you may enter it in the “Your Name:” box without concern for capitalization.
  4. The four digit code you use to log on is the “Access Code” for the web-based reservation. It is also not
  5. Web address: http://xrayrl1.chem.ucla.edu/web_res.php
    • Notice that the instruments currently in use will be listed at the bottom.
    • On the upper left, select the Instrument you want to reserve.
    • Select the day. This will highlight in green all the days for which reservations are allowed, even if they may be currently filled. This will also bring up the “Your Name:” and “Access Code:” boxes. Fill them in and select “Login”.
    • You may need to again select the day for which you want to make or cancel a reservation. This will display all 24 hours, in 10 minute blocks. You can navigate to other days by just selecting the day. You can change to a different instrument by selecting the instrument, then selecting the day even if it is the same day you had selected for the previous instrument.
    • Once you are displaying the schedule for the appropriate instrument and date, select a “Starting:” time and the “Until:” time. Select “Reservation” or “Cancellation”. Then click “Submit”. A window will pop up for you to confirm or cancel the submission. If you had chosen “Cancellation” an extra pop-up will remind you to be sure to read the next pop-up so you don’t inadvertently cancel the wrong thing.
    • When you are through, select “Log Out”.
  6. How to obtain a UCLA VPN.
    To obtain a Bruin OnLine (BOL) VPN, go to the following link and follow the directions: http://www.bol.ucla.edu/services/vpn/.