Welcome to
the U. Maine Chemistry Department's
Instrument Status Page
David LaBrecque, Room 146 Aubert Hall, Tel. 581-1195
Exploring the
"Inner Space" of atoms and molecules requires sophisticated, state of
the art, instrumentation and software. I repair, enhance and when necessary,
design and build analytical components and instrumentation. I also offer many
instrument workshops and participate in research projects. I am also a Graduate
Faculty Instructor offering a course in Practical Computer Interfacing in the
Laboratory in alternate years. Click News, Where to find me, Department's
Instruments and Job
Priorities for more information on these topics.
This web page
provides information on the Department's Instruments and on Innovative Projects
that I am working on. It also includes
information on instrument training and instrument use costs for outside users.
It is intended as a dynamic resource for faculty, staff, students and
off-campus teachers and researchers. I am solely responsible for its content.
PhysicsGuy.Org is my homepage listing more of
the innovative projects I’ve worked on over the years.
Various
software I’ve developed is listed here and can be downloaded for free by
clicking on the links below. Send questions to DavidLaB@Maine.edu
Click
here to access Chemistry Department Faculty Staff Pictures.
Click here
to access Chemistry Department Student pictures.
1-20-07
A
lot has taken place since the last update. Listed here are some of the research
and teaching projects I’ve worked on.
The
XL 200 NMR is now the Gemini 200 NMR thanks to the donation of a Gemini
console. Although we tried to “upgrade” the Gemini 300 NMR with a Unity
console, the newer console had serious problems, so we are still using the
Gemini 300. Both NMRs are working well.
NMR
services and consulting are available to researchers in the area. I give 3
levels of NMR workshops that train users how to perform experiments ranging
from basic hydrogen to heavier nuclei. Variable temperature and decoupling experiments
are also covered. NMR maintenance is another workshop I offer. For more
advanced users or for users who need consulting services on advanced
applications, Dr. Karl Bishop is an NMR application expert who can assist all
types of users through all stages of their experiments from data collection to
analysis. Dr. Bishop also teaches an NMR course. Click here to access
NMR website for more information.
NMR
scheduling will be going on-line soon using the First Class Scheduling Tool.
Only trained users will have access to the scheduling tool. See me for
training.
Data
files can be downloaded from the Gemini NMR by using a program I’ve written
called NMR2PC. Once the data files are on a PC they can be analyzed using an
NMR data analysis program like NUTS. See Acorn.com for a free trial download.
Contact DavidLaB@Maine.edu for a copy
of this program.
Part
of Level 2 NMR training includes an NMR
shimming exercise where a user tries to get the magnetic field as homogenous or
uniform as possible by monitoring the deuterium signal and adjusting current
values in a set of shim coils. Shimwork.exe is a simple DOS program designed to
let the user see what is happening to the magnetic field and the shape of their
data peaks as they adjust the shim values. Click here to
download Shimwork.exe.
I
offered a course entitled Practical Computer Interfacing in the Lab which was
well received. I’m looking forward to teaching this course in alternate years.
We
just connected a BioRad IR microscope to a Bomem FTIR spectrometer. The system
is working and should be a valuable asset to Prof. Tripp’s research in LASST.
We’re still tweaking the alignment and hope to have it performing to factory
specs within a few weeks.
Prof.
Solouki is breaking world records on mass spectrometer resolution. We’ve
created a cryofocusser which is a thin sample tube submersed in a liquid
nitrogen bath. Sample is collected and concentrated in the sample tube over
time. A short high current pulse of electricity across the sample tube rapidly
heats the tube to high temperatures resulting in a flash of concentrated sample
which is injected into the ICR mass spectrometer.
MIST,
Mass Identification Smart Tool, was developed for Prof. Solouki’s research. A
molecular mass is entered into the program and the program outputs the possible
chemical fragments that could make up the mass. Users can control the database
that is searched. MIST is currently being enhanced by incorporating
visualization code that utilizes the human ability to see patterns in data.
This allows heavier molecules, such as DNA fragments to be searched. Click here to
download the current version of MIST.
QED
is a tool that uses Richard Feynman’s basic description of Quantum Electrodynamics
to create diffraction patterns from slits and gratings. Click here to download
the QED tool.
The
Gaussian Fit Tool is an interactive plotting tool used to fit multiple Guassian
curves to fluorescence data. Users manipulate multiple Gaussian curve
parameters in real time to create the best fit to the data. Autofit algorithms
sometimes crash or do not produce reliable results. The Gaussian Fit Tool
enables users to explore “Gaussian Space” in real time taking advantage of our
human ability to visualize patterns in data. Energy transfer can be explored as
models can be made up of both positive
peaks and negative peaks. Click here to
dowload the Gaussian Fit Tool.
Another
item in the works is a large screen monitor that will display faculty, staff
and students, and the research projects that take place in the chemistry
department. The monitor will be in the Chemistry Lobby in Aubert Hall where it
can be utilized by students and visitors to the department as an informational
source. The Chemistry web browser that is utilized with the monitor, can also
be downloaded and utilized on any PC. You will be able to click here to
download the Chemistry Department Browser when it is available.
If
you are interested in an interesting perspective on teaching, do a Google search on: “Physics of
Learning”. Usually the first item
listed is my Physics of Learning web page. This describes how teachers can use
a physics analogy to optimize learning in the classroom. The analogy also
provides some insight into Artificial Intelligence. Click here to go
directly to the Physics of Learning Page.
ICN,
InterChemNet, is a networked instrumentation model intitiated by Prof. Francois
Amar and Prof. Mitchell Bruce. By utilizing networked instrumentation for data
collection and any available networked computer for data analysis, a few
instruments can serve a large population of students at a low cost. The
Chemistry Department is helping other schools adopt the model by lending out
instruments and software. ICN software also comes with a large assortment
of reference and simulation tools that
can be modified to suit teachers needs. I’ve written the user and instrument
interface for the ICN program. Other ICN developers have developed the network
interface and teacher database tools. Click
here to access the ICN website.
Contact
me for details on instruments or instrument workshop training:
DavidLaB@Maine.edu
Here is a partial
listing of the instruments available in the Chemistry Dept. Click on an
instrument for more details. There are more instruments in the department not
covered here. Please see me if you need specific information on them.
Atomic Absorption, Balances, Computers, Cyclic Voltammetry, Fluorescence Spectrophotometer, FT-IR (Fourier Transform - Infra-Red), ICN (Instrument Network), GC's, LC's, 200 NMR, 300 NMR, Lifetime Instrument, Mass Spec. (GC-MS), Raman Spectrometer, UV-VIS, 316 Lecture Hall
Some instruments
(NMR, UV-Vis, FT-IR) are available to non-department or off-campus
individuals on a cost per hour basis. Training is also available. Modern
instruments such as UV-Vis and FT-IR are simple to use. Contact me for more
information.
Contact me
regarding research, design and repair of scientific instrumentation.
Routine Items:
Instrument training/testing, meetings, colloquiums, less than 30 minute
repairs, updating this web page ... are not listed.
By repairing
instruments in-house, engineering new components for old instruments and
creating state-of-the-art modern instruments utilizing low-cost computers, I've
been able to save the department over $100,000 over the past few years. Many
current projects make the future look bright and exciting: Inter-Chem-Net is an
ambitious project directed by Prof. M. Bruce that networks instruments with
computers and thus reduces costs and improves student/teacher communication. A
revolutionary cyclotron mass spectrometer which can identify large molecules
has been implemented by Prof. Solouki. Under Prof. Patterson's direction we not
only have a state-of-the-art Raman and Luminescence Lifetime instruments but
more enhancements are planned. Prof. Tripp and I will be upgrading our
micro-probe FT-IR. Aubert Hall has had extensive renovations over the past few
years. As always, thanks to the faculty for letting me work on such intriguing
and rewarding projects.
Room 438. We have
two lamps, lead and iron, appropriated from another AA and rewired for this AA.
(A new AA would cost 10 to 20 thousand.) This instrument is used primarily for
course work. Please inform me if you need to use this instrument and allow
potentially 7 days for me to properly align and adjust this instrument.
Room 438. Undergraduate
students tend to leave the balances on after use, causing the lamps to burn out
prematurely. Unfortunately the lamps in these balances are unique and expensive
($10-$20 each.) I have installed a timer that can be set up to 60 minutes.
Users have to turn a dial to get additional time.
The department has many Windows and Linux based PC's located in various parts of the building. We have a large selection of state of the art chemistry software, both canned and developed in-house. Part of my responsibilities include software and hardware development. Return to Home Page.
Fluorescence Spectrophotometer
This (PTI)
instrument is in room 372-B. Sample holders have been and can be designed if
needed. Also see: Lifetime Spectrophotometer. Training is required for these
instruments.
FT-IR (Fourier Transform - Infra-Red)
The FT-IR in room
362 is functioning well. See Prof. Jensen for permission to use this instrument
as it is heavily used in Organic Chemistry.
Four Midac FT-IRs
are used for general chemistry lab, advanced courses and research with our
networked instrument-computer approach. See ICN.
ICN (Instrument Network)
Imagine being
able to quickly and easily look at and analyze instrument data on your PC. The
data you’ve just collected, a graduate students or one set out of a large
library of data files. Imagine incorporating this data in a lecture by
displaying it with a video projector in room 316. Imagine being able to access
a large variety of chemistry software from any PC in the building and again
being able to utilize that software on the video projector in room 316. Imagine
giving quizzes, tests, exercises on-line to students and automatically and
quickly analyzing student input no matter how large the class. That technology
is here now thanks to the ICN development team.
Dividends: Add
four new UV-Vis and four new FT-IR to the department’s instrument list at no
extra cost to the department. These instruments are also available for research
use. Wow! Also with my expertise in software development I’ve been able to save
this project more than $20,000 in development costs.
Although the
backbone is in place, we are just beginning to shape this powerful tool for use
in education. To optimize this powerful tool, we need the input of all faculty,
staff and grad. students to help us address the large range of pedagogical
issues. For example: what types of chemistry software should we include, should
we rewrite the software we already have to meet our needs or should we utilize
public domain software or perhaps purchase software site licenses. How should
networked chemistry software be incorporated into lectures or student homework,
quizzes and tests?
Last semester
students performed lab course evaluations on-line. Data was analyzed and
summarized almost immediately. The process was a complete success and will be a
permanent addition to our General Chemistry Lab course. Another advantage with
this approach is that the evaluation questions can be quickly and easily
created/edited by anyone who knows how to use a word processor.
GC's
2 GC's are
operating well. An older type is in room 462-A has been replaced with a newer
Varian version and a newer HP type is in room 438. The one in 462-A has a new
HP integrator with many new advanced features.
LC's
The HP 1090 LC is
operating well and is located in room 438. It has a new source (~$500), new
flow cell (~$500), new pump valve ($200) and new processor board ($700). This
high maintenance instrument is working well but has been costly to use and
prone to failure. Training is required.
The XL 200 NMR is
now the Gemini 200 NMR. This instrument
is not networked so you should save your data on a floppy disk.
This instrument located
in the NMR facility, room 362, is more available than the 300, so please check
it out if you can’t get time on the 300. Outside users are encouraged to use
this NMR. See Outside User Policy below for details.
NMR Checkout
Information
All users must be
checked out before they can use the NMR. Users can be checked out by either
Prof. Jensen or by me. Prof. Jensen checks out student in his Organic Chemistry
Courses. Users who have not taken these courses or have not completed the
checkout in these courses, must be checked out by me. I have 3 levels of
checkouts. The first is the simplest and involves doing only proton experiments
with deuterated chloroform as a solvent. The second level involves doing carbon
experiments, decoupling and alternate solvents. The third level involves other
nuclei, variable temperature and use of the 200 NMR.
Each of the
levels requires a checkout process that typically takes 4 weeks. I present to
the potential user the NMR in a 1 hour meeting. The user is given a worksheet
which they typically complete and hand in to me in two weeks. If the worksheet
is completed correctly, the user can use the NMR weekdays, 8-4, only when there
is another experienced NMR user around. After this 2 week training period the
user meets with me again for a final hands-on checkout.
Anyone who uses
an NMR without being checked out will be denied access to the department’s
instruments for a period of time.
Individuals who are not U. M. Chemistry Department faculty,
staff or students may use the Chemistry Department’s NMRs under the following
conditions:
The NMR computer
cluster in room 362 consists of a SUN workstation and 4 PC’s. Prof. Jensen has
installed a good variety of useful chemistry software on the PC’s.
The 300 NMR is
operating well. The floppy drive has been disconnected. Save your data on DSK9
and you can use the NMR2PC program to download it to a PC where you can analyze
it using a program like NUTs. See me
for more information. The VT has been disconnected but it can be reconnected
when needed with one weeks notice. (A long term (months) drift in Z3 is being
monitored.)
The 300 NMR has
had three major problems since I’ve arrived. Each problem would have cost the
department around $10,000 if a Varian field engineer had been called in. The
NMR had a problem with a misaligned probe, a burnt out transmitter coil and a
serious vacuum leak which would have caused an expensive quench if it had not
been caught in time. Along with other relatively insignificant problems, we’ve
spent about $700 in parts over the last two years.
The PC’s have
been networked to the Sun workstation so that we can download NMR files to the
PC’s. Special software is available ("Nuts") for analyzing NMR data
on PCs.
Check the
following if you are having problems:
1. Use RTP(...)
as indicated on card above monitor.
2. Use RTS(CDCL3)
for shim files.
3. Adjust only
Z0, Z1 fine, Z2 fine. Adjust Z4 sparingly.
There is an Outside User
Policy for this instrument.
The Lifetime
Instrument is actually made of several powerful components that I’ve restored.
The department now has:
A Nitrogen 10
nanosecond, 337 nm, pulse laser. A newer 266 nm pulsed laser is also used.
A dye laser
attachment that can produce several ranges of laser wavelengths in the UV and
Vis.
A 1 meter
monochromator that will be computer controlled.
A very sensitive,
wide range, detector coupled to a state-of-the-art digital oscilloscope.
The ability to
measure Fluorescence lifetimes down to 10 nanoseconds.
Replacement costs
for this instrument is probably $20000 to $50,000
We’ve spent about
$700.
Wow!
Mass Spec. (GC-MS)
Mass Spec. is operational.
- The Mass Spec.
now has a new, easier to use and more powerful PC based windows system.
- See David L. if
you want to use it. We might have to change columns before you can use it.
- User must be
trained by me before they can use the Mass Spec.
- Everyone must
submit an Auto-tune report to the Mass Spec. log book located near the
instrument every time they use the instrument.
This high
maintenance instrument currently has low use due to renovation issues. If you
need to use it for research quality work please see me before using it. I’ll
run a complete diagnostic and get it back to factory specs. for you.
The computer
monitor failed recently and was replaced. Ion source filaments (~$500) and
columns (~$500 ea.) have been replaced. This instrument works well when it is
used correctly and can fail miserably when it is used improperly. Use minimal
amount of sample. Some users have literally injected nothing into the
Mass-Spec. and have observed useful data. Just the presence of the needle
inserted into the septum after it was inserted in the sample was enough.
Outside Users
GC-MS Policy
Individuals who are not U. M. Chemistry Department faculty,
staff or students may use the Chemistry Department’s GC-MS under the following
conditions:
1/14/99: Mass
Spec. in 438 is operational. Controller replaced and air leak repaired.
Abundance on 502 peak slightly low but will improve over time with pumping.
Approximately $5k - $8k was saved. (Faulty controller is now in NMR turbo pump.
Waiting on manual for repair. $25 repair bill for new transformer.)
The Raman
Spectrometer in room 370 is working well except for the Argon laser which is
currently being refurbished. This PC controlled instrument can be used with
liquids and solids at variable temperatures. A rebuilt laser was purchased
($5000) and failed two months after the purchase. After I repaired it (saving
$1000) it has worked well since. A computerized Raman is a $20000 - $50000
instrument.
- 4 UV-VIS’s
(fast diode array) are part of the ICN project and are available to students
and professors for their research. 4-6 Ocean Optics UV-Vis are also available.
- A new (Beckman,
scanning monochromator type) UV-VIS is set up in room 131. Lamps have been
replaced at least twice on this instrument.
The AV department
has installed a projector system with good sound capability. They are
responsible for maintaining this system so forward questions to them. Many of
the faculty as well as myself can
handle questions about operating the system. A VGA connector and an audio
connector are located on the far side of the first lecture bench as you viewed
from the North door to 316. Instructions are located on or in the lecture
bench.
A PC has been
installed in the cabinet. It contains Microsoft Office, First Class and ICN.
Please feel free to install any software you need. See me if have questions.
- Since I work on
various instruments and projects at various locations I could be anywhere in
the building.
- That's why I
carry a cordless phone. I am usually a phone call away. 581-1195
- My hours are
posted on my door. Arrive 7:00 to 8:30. Lunch usually around 1. Leave 3 to 5.
- Room 146 is my
office. Room 148 is my computer, electronics and physics lab. Check there if I
am not in my office. Room 124 will also be used for "organized"
storage. You might try there if you need a part.
Priorities (using
1999 data)
|
Category |
Priority |
Demand |
Money Saved |
Parts |
My Time |
|
NMRs |
1 |
Very High |
$35000 |
$750 |
20% |
|
Other Instruments |
2 |
Moderate |
$15000 |
$2000 |
20% |
|
Special Projects |
3 |
Moderate |
$25,000 |
$7500 |
25% |
|
Instrument Network |
4 |
High |
$20000 |
See below. |
25% |
|
Misc. |
5 |
Low |
$2000 |
$100 |
10% |
Each column and row are described below. See specific instrument
for more information.
Category
The work I do can be divided into 5 major categories.
Priority
With input from faculty, staff and grad. students these
categories can be prioritized.
Demand
Very High: Daily use for 30 or more weeks per year.
High: Daily use for approximately 15 weeks per year.
Moderate: Daily use for approximately 5 weeks per year.
Low: Minimal use and/or instrument is easily replaced.
Money Saved
These are rough estimates of cost of repairs and/or the
purchase of new equipment if I simply used outside sources for repair and new
equipment. (These costs were last calculated Spring of 1998.)
Parts
These are rough estimates of the actual money spent on
repairs and new equipment. (As of Spring 1998)
NMRs
About 20% of my time is spent on the NMRs. The 300 NMR has
had 3 major problems and I estimate I've saved the department approximately
$30,000 in just these repair costs alone over the last two years.
Other Instruments
These instruments: FTIR, GC-MS, UV-Vis, GC, AA, HPLC, IR,
Balances, are repaired as needed. Please let me know in advance if you intend
to use any of these instruments and I'll run checks on them and make sure they
are up to factory specs. An issue here is whether to have a routine maintenance
schedule on instruments that have only moderate use. Unless I hear otherwise
I'll continue to maintain these instruments on an as-needed basis. Thanks to
grad. students for letting me know A.S.A.P. when their is a problem with an
instrument.
Special Projects
These projects: Raman, Lifetime, Cyclic Voltammetry, AA,
HPLC, open up new areas of research by providing researchers with
state-of-the-art instrumentation. Please let me know if you have a special
project in mind.
Instrument Network
The ICN project brought 4 new FT-IRs and 4 new UV-Vis
instruments to the department. A program was written to control these
instruments and to provide access to the departments computer network.
ICN is not only a powerful instrumentation network where
students can download real data files for analysis on PCs it is also an
excellent source of software tutorials, exercises and references. Most of the
cost of ICN has been for computers and software. Four of these PC's and a laser
printer are available for graduate student use. An issue here is the legitimate
copying of copyrighted software on these computers. For example, until we
purchase site licenses we can not legitimately provide Word and Excel on these
computers. Now that the backbone is in place, we are addressing pedagogical
issues. Our goal is to duplicate the advantages of small labs in large labs by
using networked computers and instrumentation. We are attempting to customize
labs for students by implementing multi-path, mastery based labs. Now is the
time for faculty, staff and grad. students to help shape and optimize this
powerful tool for use in education.
Miscellaneous
This includes hot air blowers, ovens, PC's and any
easy-to-repair, easily replaced items. The money that has been saved when I do
this work is low because either the item is inexpensive or there are low-cost
repair services available. Although I enjoy repairing these items, I have to be
conscious of whether this is the most cost effective and efficient use of my
time. Thus these items, unless you indicate otherwise, have low priority.
Miscellaneous also includes attending special lectures, seminars, colloquiums
and workshops.
9-01-03
200 NMR has an acquisition computer memory access error which is proving difficult to solve. The acquisition computer has been sent to Varian for repair, but this 20 year old instrument could have other problems which may further delay its repair. The 300 NMR is working well.
One of the four Midac FTIR spectrometers has a bad laser. A new laser will be ordered. The other 3 FTIRs are working well.
The Raman, PTI fluorescence spectrometer, Beckman UV-Vis, SPF500 fluorescence spectrometer have been moved and should be working.
The microprobe (microscope) from the BioRad FTIR will be moved onto the Nicolet FTIR as soon as a data acquisition code has been completed. The code must be written in assembly language to eliminate timing errors resulting from the VB data acquisition code.
4-08-03
All instruments
are running well. The GC-MS in 438 suffered some problems with the flood but is
now running well after one power supply capacitor and 2 transistors were
replaced. The GC-MS was also recently cleaned. EM Voltage = 2400. The XL200 NMR
(1987) is still running after all these years but 5.25” disks and drives are
getting scarce. I am working on networking the 200 into the Interchemnet
network so data files will be much more accessible and backup data files can be
easily made. The same networking approach will be added to the 300. Students
will be able to access and display their data from anywhere on campus or the
world for that matter. Electronic driving and interfacing circuits have been
developed for cold trapping techniques that will probably break mass
spectrometer world sensitivity records. The 266 nm nano-laser and the Argon
laser were sent out for repair and are now working well.
8-06-02
All instruments
are running well. A 2 Watt Argon laser used for the Raman is being refurbished
and is due back in 3 weeks.
Non-symmetrical
acoustic vibrations were used on this laser in an attempt to bend an internal
filament back into position. Although the attempt was not successful, this work
may lead to an ion filtering technique that could be used with low-cost
sensors. Work was also done on the design of solid-state diode pumped lasers
which could be used in place of the failed Argon laser. Again this effort may
prove useful as we research strongly fluorescent materials for their potential
lasing properties. The Nicolet FTIR along with the replacement PC will be moved
to LASST. Custom designed software was designed to control the instrument and
port spectra to Grams software for analysis. The GC in Organic was replaced
with a newer GC.
4-26-02
300 NMR
Tin plated circuit board
in RF amp had oxidized connections which caused intermittent no signal problems
on proton channel. Cleaning the connections eliminated the problem. The problem
was especially difficult to isolate since the problem occurred at random and
the problem would disappear when test probes were connected.
New red light above air
valve tells user if decoupler is on. Users should not turn off air if light is
on. Use RTP(STDPAR.HCDCL3) SU to turn off decoupler.
Now users can download
their 300 NMR data files directly to their PCs with a new program I wrote
called NMR2PC. The new program is
available on several computers in the cluster. Free copies are available on
request. Users can analyze their data
with Nuts software. They can also back up their data on PC floppies or burn
their data on CDs. This replaces the older 5.25” floppies. This will also
reduce demand for analysis time on the 300 and reduce 300 NMR printer use.
“NEW” NICOLET FTIR
The dedicated computer
failed on this instrument making the 10 year old FTIR useless. I designed a PC
interface and PC software to replace the failed computer saving Prof. Tripp $20000+ FTIR. An extra benefit
to this project was like taking an in-depth course in FTIR design.
Projects I am
currently working on:
Networking the XL200
(similar to NMR2PC for 300). 2 replacement fans are also needed in the 200 NMR.
A simplified QED
simulation approach to analyzing optics and optical surfaces using Feynman
description.
PC controlled BioRad FTIR.
The fogged beamsplitter in this FTIR makes this a low-priority project.
Computer Modeling /
Gaussian 1.6GHz 640MB Ram computer. (This PC’s faulty RAM was repaired.)
Ventilation issues for NMR
rooms.
Analysis of a wealth of
ICN timing data collected several years.
300 NMR
After improving the
ventilation in the NMR no more freeze-ups have occurred.
The freeze-ups occurred
about once per week at random.
This problem was traced to
faulty connections in the RF amplifier.
Old Projects :
ICN upgrade (Done 4/26/02)
PC controlled Nicolet FTIR
(Done 5/1/02)
PC controlled BioRad FTIR
MIST: Mass Identification
Smart Tool program (Done 4/26/02)
NMR compressor repair
(Done)
Computer Modeling /
Gaussian 1.6GHz 640MB Ram computer
NMR Training Workshop in
early January (Done)
Ventilation issues for NMR
rooms
Possible Upcoming
Projects:
Supercomputer made of
Networked PCs.
A Beowolf cluster is being
constructed out of 8 Athlon Computers. PI: Prof. R. Fort
Students must complete
a checkout procedure before they can use
most instruments
in the department.
Typical checkout
procedures take about 1 week.
They involve 2 or more
training sessions with me and successfully completing a worksheet.
I use a mastery-based
approach so the actual time and work depend on the student.
Here is what is available:
300 NMR Checkout Level 1:
Proton experiments with deuterated chloroform
300 NMR Checkout Level 2:
Carbon experiments, Decoupling, Other Deuterated Solvents.
300 NMR Checkout Level 3:
Probe tuning for heavier nuclei, Variable Temperature Experiments
200 NMR Checkout for
Beginners
200 NMR Checkout for
Advanced users
NMR maintenance: LN and
LHE fills, Advanced Shimming Techniques, Failure Analysis.
All users should log in
and report how they are using the NMR.
This makes repairs easier
and quicker. Students should never use a transmitter power
that is too high for the
solvent they are using. Specifically TPWR=51 is too high for Acetone.
Use RTP(STDPAR.HCCDCL3) SU for chloroform and for Acetone, use
RTP(STDPAR.HACETN)
Contact me if you get AD
overflows or bizarre spectra.
Other Checkouts
are also available:
GC-MS Checkout
AA Checkout
HPLC Checkout
BioRad FTIR and
Microprobe Checkout
Luminescence PTI Checkout
Lifetime Luminescence
Checkout
Raman Checkout
Advanced ICN
computer/instrument applications with UV-Vis and FTIRs.
****************************************************************************************************
11-28-01: Good News: The
300 NMR has been repaired and is ready for use.
The RF amplifier failed
probably due to power spikes/variations.
It was sent out for repair
and arrived back here this morning.
The repair cost was only
$200, but next day shipping and insurance costs were $300.
Note RF amplifier failed
again briefly on 11-27-01 but now seems ok as of 11-28-01.
9/07/01: An
Acetone parameter file has been created for the 300 NMR. RTP(DSK8.CACETN) See me if you need to use solvents besides
Chloroform, Methylene Chloride, Water or Acetone.
9/07/01 Margy has
a new computer and printer. Her old printer will be used for the graduate
office cluster. Her old computer will be used with the digital camera system
mentioned earlier.
9/07/01: ICN now
uses an abbreviated lookup table. The ICN program and the instrument program
should now start faster.
8/27/01: Due to
renovations this page has not been updated recently. A lot has happened in 8
months. All instruments including the NMRS and ICR have been moved successfully
and are operating well. Only the BioRad FTIR and 1 of 4 Midac FTIRs are not
operating and are undergoing repairs.
8/27/01: The
department has a new FTIR thanks to Prof. Jensen. Contact Prof. Jensen for
details. Contact me about using the Midac FTIRs.
8/27/01: A new
high resolution, high sensitivity black and white camera combined with a
digital video capture card gives us a state of the art digital microscope and
spectroscopic detector. We can make movies and high resolution (theoretically
1200X1600) snapshots. The tool will be useful for research, preparing
presentations and enhancing grant proposals and published papers.
8/27/01:
Renovation Plans: The East Wing will be closed for the summer and early fall as
construction crews remove asbestos. Last minute minor changes are still being
made to the plans. Soon they will go out to bid and hopefully construction will
begin soon after that process.
12/20/00: All instruments are functioning except for one FTIR in the Gen.
Chem. instrument room. A new laser is on order. Only one of the 3 FTIR's will
be left on over break. The others will be turned off and bagged to extend the
lifetime of the lasers in them. The 300 NMR had an overheating problem that
resulted in spectral errors. Cleaning the air filters resolved the issue.
9/29/00: All instruments are functioning. Mass Spec. turbo pump has been
replaced. Integrator printer for GC in 438 has been repaired. New pump safety
valves have been installed on ICR.
9/29/00: New ICNLite data analysis browser page is available.
6/26/00: NMRs are functioning well.
6/23/00: Good News: The 300 NMR problem has been isolated and it should
be operational for Monday and possibly for this weekend. The proton transmitter
shifted in frequency by 2 kHz. I'm still investigating the cause. Changing TO,
the transmitter offset frequency to a large negative number on the parameter
page is a quick fix. I'm investigating a better fix. Most users will not be
aware of the changes except that the NMR is now working.
6/20/00: 300 NMR can be used for Carbon and heavier nuclei experiments.
The decoupler is also working. It will not work for proton spectra. Recent
tests suggest either probe capacitors are suspect or the proton preamp is bad.
6/19/00: 300 NMR is down possibly until July 1. It may be used for processing.
Proton/decoupler coil is probably burnt out due to users leaving decoupler.
Remember to always type in RTP(STDPAR.HCDCL3) followed by Enter Key, then SU
followed by Enter key.
5/25/00: Current
projects: Magnetic field PMT gating, low temperature (1.4K) cryostat, ActiveX
ICN means ICN can be used cross platform with standard browsers like Netscape
and Explorer, Summer Clean up in preparation for building renovations,
Preparations for NMR quenching and recharging.
5/25/00: Midac
FT-IR ICN stand-alone program is near completion. We'll be burning CDs with the
ICN program on it. This will allow new Midac FT-IR users access to free
software for using their FT-Irs.
5/25/00: A
low-level security feature was added to the graduate student computers in the
computer cluster. Now all users must enter their name when they turn on the
computer. Misuse of the computer or failing to turn off the computer at the end
of the day are automatically reported to the network specialist who in turn
will notify by email those responsible for the misuse.
5/24/00: A new
optics system for exposing samples to UV light was installed on the PTI. The
system allows for both UV exposure and spectral studies on solid samples.
5/22/00:
Polarizer mounts were installed on the PTI Cuvette holder. A wedge type
polarizer allows excitation wavelengths into the UV range. The
emission/detection side uses a standard plastic polarizer since we are not
interested in the UV range of emissions on the current samples. Both polarizers
can be rotated 90 degrees for polarization studies.
5/17/00: All
instruments are working well.
5/16/00: GC-MS in
438 was cleaned and turned back on. One filament was replaced. This instrument
is working well.
5/15/00: BioRad
laser replaced. System tuned. Microprobe functioning. Note the optics in this
instrument are somewhat fogged and are too expensive to replace at this time.
Users should use Midac FT-IR's. See me for instructions on optimizing the
performance of these FT-IR's.
5/3/00: BioRad
FT-IR laser needs replacement. This instrument will be down until a new laser
arrives next week. ($350)
5/1/00: 300 NMR
spinner was cleaned. Don't forget to turn off air at night.
4/1/00: 200 NMR
was producing erratic spikes in spectra. Power supply capacitors were replaced.
($100) The NMR is tuned for Flourine instead of proton and on the broadband
tuned to Phosphorus instead of Carbon. Let me or Scott Larkin know if you need
to use this NMR.
12/7/99: The GC
Integrator in 438 is being repaired. The integrator output is poor. A new print
mechanism costs $290. I am exploring other lower cost solutions.
11/29/99: Don't
forget there is free stuff in the basement of Aubert Hall between rooms 124 and
126.
11/29/99: A new
vacuum gauge has been installed with the turbo pump.
11/29/99: I've
designed a new computer controlled temperature controller for temperatures
ranging from liquid nitrogen 78K to 473K (200C). The controller will be used
with Prof. Solouki's Breath Analysis project and with Prof. Pattersons
spectroscopy studies. This will relieve the wear and tear on the Heli-tran
which is capable of achieving liquid Helium temperatures.
11/22/99: About 5
new computers will be installed in the cluster over Christmas vacation. The ICN
web page server will also be replaced.
11/22/99: The new
NMR/FTIR air compressor is working well. To lengthen its lifetime we will be
shutting off the air to the NMRs at night. We will leave the BioRad FTIR air on
but at a lower pressure. A new air chiller to remove water from the air will be
connected sometimes in December. Downtime should be minimal.
11/15/99: Since
the 200 NMR has had minimal use as a general purpose instrument, we are now
using it for dedicated research purposes. The 200 NMR observe channel will now
remain tuned for phosphorus instead of carbon. Also the proton/decoupler
channel will be left tuned to flourine. Also where possible the 200 will be
used for variable temperature experiments. This should minimize the wear and
tear on the 300 probe thus keeping it for teaching and research where higher quality
results are needed.
10/28/99: Y2K
issues. November is a good time to check your computer for Y2K problems. I
suggest everyone back up their computer before Y2K strikes. Also beware of free
software or anything that might subject your computer to a Y2K virus. Microsoft
has a good web site to learn about Y2K and how it might affect your computer: http://www.microsoft.com/y2k Check it out early in the morning when the site is
less busy.
10/28/99: A new
YAG laser with frequency doubling crystals was set up today. The laser outputs
4.6 mw average power with .5 nanosecond pulses at 266 nm. This is a significant
improvement over the old Nitrogen laser system which produced many unwanted
plasma lines and generated electrical noise that often overwhelmed our signal
detection circuits. We are already measuring lifetimes with the new system.
10/27/99: Both
NMRs and the FTIR will be shut down Tuesday, November 2 through Wednesday noon
while the compressor is being replaced and a new chiller is installed. The
chiller should reduce significantly the amount of water that gets to the
instruments through compressed air.
10/26/99: Two new
modes have been added to the ICN program bringing the total number to 5. The
software can operate in stand-alone, floppy (new), small intranet (new),
intranet, and internet modes. The 2 new modes were developed when we realized
that most high schools could not easily implement the intranet mode. We also
did not want to use our server in internet mode to service high schools. The
small intranet mode requires only a group of Windows 95 PC's linked by a
network hub. For schools that don't have a reliable functioning network system
we now have floppy mode. Students save their spectrometer data on a floppy and
carry the floppy over to a PC where they can analyze it using ICN. The whole 5
MB ICN program is now available for downloading from the ICN site:
http://icn.umeche.maine.edu/Icn/
10/25/99: Free
Stuff: I will be placing old equipment and parts between rooms 124 and 126 in
the basement. These are items that have been determined to have no value to
anyone in the department and to be not worth selling. These items include: dot
matrix printers, chart recorders, old Apple computers ... Please take whatever
you like because these items will be thrown away in the coming months. I will
be placing more items in the hall in the next few months.
10/18/99: NMR
situation has been resolved due to vacuum pump-down and LHe refill. Note safety
vent valve on LHe dewars should be left open during storage and transportation.
A closed valve results in over-pressured, turbulent LHe where quantities are
difficult to measure with a flutter tube.
10/14/99: NMR
warning: The He flow rate on both NMRs is fluctuating from 18 to offscale.
Barometric pressure has been falling over the past 24 hours and is now 29.27
and falling. A number of other factors are combining to make this an uncertain
situation: The NMR's should have been filled on Wednesday but the shipment has
been delayed due to a mixup by the vendor. The 300 NMR is due for a vacuum
pump-down. This will be done on Friday. Unrelated power outages have occurred
last night and today which makes a pump-down today risky.
9/28/99:
Instrument compressor has a cracked cyclinder head. A new one is being ordered.
NMRs and DigiLab FTIR will be down probably for 1 day, possibly October 12. The
old compressor is running but complete failure is possible. The old 15HP
compressor is much larger than required by our current needs. It was designed
to handle both Chemical Engineering and our instrument needs. With Chem. E.
gone a 5 HP compressor (17.1 CFM) will more than meet our needs. (4.4 CFM) For
$1600, we will get a new compressor plus a badly needed air dryer.
9/27/99: A new
intranet web server has been set up for General Chemistry. Students can
download and print labs from any PC in the building. You must log on to the
Interchemnet domain with an account name of public and password: public. Use
your browser to link to http:\icn. An internet version for both PC and Mac is
under development.
9/27/99: New
molecular modelling windows software is on order for Prof. Pattersons group.
The software includes Gaussian 98W and Chem 3D.
9/27/99: Two HP
workstations have been set up in room 114. The workstations are intended to
serve students in Prof. Rasaiah's Quantum Mechanics course, but others may want
to take advantage of these stations.
9/27/99: New
Inter-Chem-Net functionality allows users to save data directly on a floppy
disk and analyse that data using the ICN program. Users should place a floppy
in the disk drive and type in FLOPPY when running the instrument control
program. To analyse the data type in A: in the login box in the ICN spectral
analysis program. Users can work with floppy data files and their server data
files at the same time. This functionality is intended for researchers only.
(General Chemistry students will not receive credit for data files labelled
floppy.)
9/16/99: In
anticipation of power outages tonight and tomorrow due to the storm the
following instruments will be turned off this afternoon: 300NMR, 200NMR,
GC-Mass Spec., FT-ICR turbo pumps, all computers.
9/16/99: The ICN
program is being tested on 600 students this week. The new version has internet
and browser capability. Students create accounts and complete HTML type
questionaires using the browser. Also being tested this week is ASAPs Navigator
project.
9/16/99: The
GC-MS is due for hard drive maintenance. Files will be moved from the GC-MS to
a computer in the cluster.
9/8/99: New GC-MS
Outside User policy is posted below. See Mass Spec. (GC-MS)
9/8/99: New ICN
program is available in computer cluster. This has internet and distance
learning capabilities.
9/7/99:
Mechanical balances have been calibrated. I've aligned one and installed new
bulbs on several.
8/20/99: I'm on
vacation next week. 8/23 through 8/27. All instruments are currently working
well. Contact Quansheng Song for Inter-Chem-Net technical issues.
8/20/99: I am
planning 300 NMR maintenance on September 2 - 3. This includes a vacuum pump
down and reshimming.
8/20/99: ICN
program was upgraded to VB6 this summer. The program now has better Internet
(Web page) and database capabilities along with Chemistry software tools and
UV-Vis, FT-IR data gathering/analysis capabilities. The program will be
utilized in General Chemistry lab sections this Fall.
8/19/99: New UV
(266 nm) $8000 laser ordered. Laser uses 50 mw diode laser, Q switching and
frequency quadrupling to generate high energy (~3 microJoule) sub nanosecond
pulses at 10 kHz pulse rate. The pulse signal out option coupled with our
digital storage oscilloscope will expand our flourescence lifetime measuring
capabilities. Raman scattering and kinetic studies will also be possible.
8/18/99: Spinner
and probe on 300 NMR has been cleaned to correct erratic spinner problems.
8/17/99: Spinner
on 300 NMR malfunctions occasionally. Try reinjecting sample. Make sure sample
height is correct. Spin sample slightly before injecting. Spinner and probe
will be cleaned tomorrow.
8/13/99: UV
irradiating instrument repaired.
8/12/99: FT-ICR
installation complete.
8/11/99: 300 NMR
spinner assembly cleaned.
8/5/99:
Preparations for FT-ICR installation.
8/6/99: New
Thermocouple in PTI installed.
7/9/99: Trigger
signal input on PTI instrument repaired. (New quad nand chip on PC I/O board.)
7/9/99: Recurring
intermittent problems with Raman quantum photometer power up. Problem
disappears when I attempt to isolate it.
7/8/99: Helitran
thermocouple junction repaired again.
7/7/99: 300 NMR
pump-down all day. He flow rate had risen to 20 on 7/6/99 which means an
increase risk of a $10k quench. Flow rate now less than 2.
6/29/99: All
instruments are working well.
6/28/99: Mass
Spec head pressure increased to 20. EM Voltage is 2000.
6/28/99: TTL
signal input to PTI is faulty. This will have no effect on most users. Fault
appears to be on I/O card in PC. I'm waiting for a 4 hour stretch of downtime
on this heavily used instrument.
6/28/99: Power
supply replaced on Midac FTIR. Manufacturer admitted the original power supply
was underdesigned. New 6 amp power supply replaced the old 4.3 amp type. Cost
$250.
6/25/99: Some
students have been trained for phosphorus, D2O and other solvents on the 300
NMR. Please inform me if you find the 300 NMR not in its default status.
6/24/99: SciNet
returned to primary server after ICNServer errors occurred when it was the
primary.
6/23/99: Melting
point heating apparatus repaired.
6/4/99: Network
printers in cluster and instrument room are now controlled by ICNServer and are
called Wuhan and Minos respectively.
6/4/99: Mass
Spec. is working well. Problems resolved: Someone had closed the fine
adjustment valve for PFTBA. New HE gas tank installed. Head pressure was
reduced to 10. New column needed to be baked. Vacuum is now excellent. Autotune
EM voltage is 2400, a little high but acceptable.
6/3/99: Helitran
Temp controller was tested for LN leaks. No leaks found. Suggest cautious use
of heating bring sample to room temperature reducing wattage near RT.
6/3/99: Injection
of gas into a vacuum now possible with turbo pump with addition of new valve.
6/2/99: Parameter
and shim files added to NMR for deuterated THF
6/2/99: Mass
Spec. roughing pump installed. This 230 volt pump was rewired to 120 volts to
work with the Mass Spec. Vacuum pressure slightly high but steady.
6/1/99:
Thermocouple junction on heli-tran temp controller is pressure sensitive if not
made correctly. Junction should be totally sealed in solder. Indalloy solder
recommended.
5/27/99: Mass
Spec. roughing pump has failed. A replacement from an older mass spec. will be
used as a replacement. Expect some down-time as parts may have to be ordered.
5/26/99:
Heli-Tran temperature controller thermo-couple has failed. Replacement is $600.
We are working on making our own Thermocouple junctions. Should be operational
in a few days.
5/26/99: The 200
NMR low power decoupler setting is not working properly. High power works. Most
decoupler users should use the 300 until more is known about this problem.
5/25/99: Old ICN
server has been upgraded to NT 4.0. Internet (modem) version is available on
Inter-Chem-Net Web page.
5/24/99: Network
printer problems in computer cluster have been resolved.
5/19/99: 300 NMR
is now functioning well. Signal to Noise is close to specs. You should see
significant improvement in your NMR spectra, comparable to when the NMR was
new. Further paramenter adjustments and shimming which I will be doing in the
next week or so may improve spectra further.
5/18/99:
Quinsheng Song, a computer science graduate student, will be assisting me with
Inter-Chem-Net / General Chemistry issues this summer. Song has already set up
the network printer on our new server and is currently busy performing
maintenance on our computer cluster.
5/17/99: A field
shape test on the 300 NMR revealed that our reduced signal to noise ratio was
due to the probe being slightly out of position and a significant shim problem.
NMR S/N is now about 80% of specifications and should be close to specs after a
final shimming process and parameter adjustment. Note the proton pre-amp was
checked with a signal generator and two 30 dB attenuators. (One is a low power
attenuator that I designed and built.) The proton preamp gain which is a
function of frequency meets specifications.
5/12/99: Computer
cluster printer is now working. Old server restart fixed the problem. NT 4.0
and new printer drivers will be installed on the old server this summer. This
should eliminate this problem.
5/12/99: After
probe tuning, PW90 and shimming 300 NMR Proton signal to noise is (35) 39% of
specs (90). Decoupler test suggests probe proton coil is ok. (Decoupler coil is
shared with proton coil.) This indicates the problem is either with the preamp
or receiver. A signal generator has been ordered to diagnose and repair if
needed the preamp. A noise test algorithm suggests the receiver channel B is
faulty but the test is not conclusive. Estimated repair costs and down-time
with the new generator should be minimal. The observe channel and carbon are
ok.
5/11/99: Mass
Spec. air leak was discovered to be in the roughing pump. Keeping the oil level
high eliminates the leak. A pump from an old mass spec. (or other source) will
be used as a replacement when the pump fails completely.
5/11/99: 200 NMR
spinning problem corrected by lowering air pressure and readjusting spin rate.
Reason for regulator air pressure increase that caused problem is not known.
5/4/99: 300 NMR
Proton signal to noise ratio is down to 30% of specifications. Carbon and
heavier nuclei S/N are ok. Problem has been traced to either proton pre-amp or
proton probe circuit. Varian contacted for procedure for further isolating
problem. Potential repair cost $800 - $2000 with 5 - 10 day downtime.
5/3/99: Air leak
on Mass Spec. repaired. 502 peak at 3.5%.
5/3/99: Lamp on
PTI Fluorescence Instrument has gone bad. New one on rush order.
4/28/99: Version
3 of ICN program available on cluster.
4/27/99: NMR shim
mapping study will be performed in the coming weeks. Although time consuming,
this project should result in enhanced resolution and peak shapes.
4/26/99: Biorad
FTIR disk full problems. Note extra IR files will be erased Friday. Save your
data on floppy.
4/22/99: 200 NMR Outside User charges result in about $1000 in revenue for Chem. dep