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Summary
Contact:
John
Edwards
(203) 744-5905
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This page contains the
entire content of the PNA Blog Site
Diesel Production Control - Combination
of NMR and Simulated Distillation to Yield On-Line Carbon Number Distributions
Process NMR Associates has developed a
database of Simulated Distillation database on a large number of diesel fuels on
our Shimadzu 2010-GC with SimDis Software. The analysis is being used to develop
distillation prediction models for the process NMR systems as well as explore
new avenues of control information that can be derived by combining carbon
number distributions obtained from the GC data with the predictive capabilities
of online NMR.
For a PDF version of this application
article download this: Combination
of NMR and Simulated Distillation for Diesel Production Control
Simulated distillation allows carbon
number distributions to be calculated and in combination with chemistry observed
in the NMR analysis the effect of aromatics and olefins on the paraffin
distributios can be estimated. Online NMR predictions can be established that
yield real-time carbon number distributions for production control and sulfur
species monitoring.
Contact: Paul Giammatteo at paul@process-nmr.com
or +1 (203) 744-5905
Extensive
NMR Diesel Database Enhances NMR Model Performance for Unit Control and
Product Manufacturing
An extensive database (10
years) of diesel samples incorporating all refining processes
(distillation through product blending) enables development of robust,
wide ranging property predictions independent of crude sources and
refinery processing. Consistent attention to data integrity enables
expanding model ranges well beyond any typical single unit or process
operation. The following slides elucidate the consistency in spectra
whether obtained 10 years ago or last week, from within a refinery or on a
laboratory spectrometer.
For a PDF version of this
application article download this: NMR
for Diesel Production Control
If you are interested in discussing the
applicability of NMR to diesel production control do not hesitate to
contact us at (203) 744-5905 or at paul@process-nmr.com.
September
15, 2008
Here
is an example of a 1H NMR analysis of a 2007 Red Wine submitted for chemical
analysis by John W.
If
you are interested in wine analysis please contact us.
Over
the past 20 years we have obtained the solid-state NMR analysis of pretty
much every carbonaceous material that exists - including coal/oil shales/bitumen,
polymers/catalysts/fibers, cellulose/polysaccharides/foodstuffs/gels,
deposits/dried sewage/meteorites/soils/clays, etc. With the increased
attention to coal liquifaction and gasification technologies we have
developed an interest in creating an NMR database for coals. Coals were
obtained from the Penn
State Coal Sample Bank at
a very reasonable cost. We have performed CP-MAS, DD-MAS, Variable Contact
Time, and T1 inversion recovery experiments on all the samples. We are
currently developing regression relationships between the NMR data and the
physical and chemical testing data that is provided with the samples. At
some point we will write this up as a journal article. Here are some
snippets of data from the coal analysis along with a few results obtained on
the menagerie of samples we look at on any given day including some oil
shales, engine deposits, refinery coke, asphaltenes, and pipe tobacco.
Please
inquire if you are interested in the details of the above analyses.
September
13, 2008
Process
NMR Associates and Spin Resonance Ltd have recently completed the
construction a small 60 MHz (1.4T) 5mm TD-NMR system that can be utilized to
study T1 and T2 characteristics of novel contrast agents at typical MRI
frequencies. Here are a few pictures of the magnet. It is based on N42
neodymium-iron discs (120mm diameter x 30 mm deep).
February
28, 2008
NMR
Process Systems – Integrated Solution
Application
for Crude Unit and Downstream Processes:
Spectro-Molecular Control for Enhanced Diesel Recovery
NMR
Process Systems’ (NPS) on-line NMR based analytical and process control
strategy for enhanced diesel recovery at the crude distillation unit
maximizes clean diesel recovery by enabling closer cut point control in the
mid-section of the CDU.
Clean
Fuels regulations in both the European and American markets have had a
substantial impact on a refiner’s ability to maximize product draws at the
refinery front end. Extremely low sulfur requirements for gasoline and
diesel have resulted in refiners now being more constrained at the
hydrotreaters. Lack of reliable, focused, measurement and control of
critical CDU product draws has forced many refiners to significantly
undercut these draws in order to ensure minimum error in the final product
blends, especially with respect to total sulfur. Depending on a refinery’s
crude supply and CDU capacity, a conservative estimate of 300-500+ barrels
per day of loss diesel production is typical. With an average of $25-$35 per
barrel margin loss, the economic impact of these Clean Fuels Regulations are
substantial.
Integrating
proven NMR technology with a focused measurement and control strategy
enables crude unit operations to cut “chemically” closer to the
hydrotreater constraint limit. The strength of NMR is that it quantitatively
and accurately “observes” the chemistry of each refinery stream and
readily relates that chemistry to chemically dependent parameters such as
distillation, cetane, freeze points, etc. The NPS strategy is to cut and
control CDU diesel production as closely to the dibenzothiophene
distillation limit as possible. Figure 1 illustrates this strategy in terms
of both current and proposed NMR based measurements.
Figure
1: Overall NMR measurement and control outline highlighting
measurement/control strategies.
Let
NMR Process Systems deliver “Spectro-Molecular” Control to your refinery
so that you can achieve real economic and production benefits.
January
28, 2008
Just
came across an old presentation on gasoline analysis by NMR and chemometrics
with direct comparisons to Mid-IR and NIR. Presented at the Experimental NMR
Conference in March 1996….PDF (3
MB)
Conjugated
diolefins are responsible for fouling of many processes in a refinery. COSY
NMR analysis can determine the concentration of these species in many
processed petroleum product streams….see
PNA webs site.
October
29, 2007
Title:
Process Analytical Technology (PAT) Manager
Description:
Implement Process Analytical Technology (PAT)
throughout all the Global Quality Sites to identification of incoming
materials and monitor manufacturing processes.
Work directly with the sites and Schering Plough Research Institute to help
support / initiate the development, validation, and deployment of PAT at the
sites.
Review, evaluate, implement, and manage PAT activities.
Provide guidance / technical help to the sites to conduct evaluation and
purchase commercial PAT related analytical equipment (e.g. NIR / FT-NIR,
Raman / FT-Raman, IR / FT - IR etc.).
Maintain analytical instruments in the lab to comply with cGMP standards and
requirements.
Train and mentor laboratory staff on PAT to generate analytical data for
routine experiments.
Generate network and infrastructures with various sites of the corporation.
Take full ownership / responsibility and provide effective, meaningful,
result driven and pro-active leadership on all PAT projects.
Responsible to transfer knowledge / technology of PAT related projects and
activities to sites. Job is located in New Jersey.
Respectfully, Vincent
L. Graziano
Recruiting Manager
/ Global Staffing
Schering-Plough
Corporation
556 Morris Avenue,
S1-1
Summit, N.J. 07901
Ph: 908-473-2745
Fx: 908-473-2793
Ph: 908-298-5232
(Kenilworth)
Careers: Employment
Opportunities
email: vincent.graziano@spcorp.com
Press
Release -
NMR Process Systems - Swagelok
Technology Conference, Teaneck NJ - October
23, 2007
NMR
Process Systems, LLC Announces : NPS-IS© - NPS
– Integrated Solutions
NMR
Process Systems (NPS) announces a new era in advanced analyzer and process
control solutions for on-line and at-line process applications. NPS’s
Integrated Solutions (NPS-IS©) approach is designed to take
advanced on-line analysis to the next level in delivering real engineering
and economic benefit to the user.
NPS-IS©:
the first and original source for any and all on-line NMR applications
regardless of NMR vendor.
NPS-IS©:
the first to offer integrated advanced analytical solutions using multiple
technologies “in one box”.
NPS-IS©:
the first to offer a fully integrated Swagelok sampling solution for
improved sample switching and reliable measurement.
Too
many spectroscopic based on-line analyzer projects (FTIR, NIR, NMR) have
failed to meet expectations and/or objectives due to:
· Overselling
the measurement
· Underestimating
the sampling requirements
· Trying
to replace all traditional analyzers with one technique.
NMR
Process Systems is positioned to deliver the real benefits of advanced
analytical systems in petroleum, petrochemical, chemical, food and beverage
and pharmaceutical applications. Moving beyond the traditional
replacement analyzer philosophy, “NPS-IS©” integrating
analyzers and advanced controls to deliver real process improvement and
economic benefit. Such integration leverages the strength of any individual
spectroscopy, shortens per stream analysis time, and builds in internal
cross-checking to ensure accuracy.
For
more information contact Paul
Giammatteo Principal,
NMR Process Systems
87A
Sand Pit Rd, Danbury, CT 06810 U.S.A. Tel: (203) 744-5905
Press
Release -
NMR Process Systems - Gulf
Coast Conference, Galveston Island, Texas - October
17, 2007
NMR
Process Systems, LLC and Smith’s Detection Launch RefinIRTM -
The New Refinery Products Analyzer
In
a joint development effort NMR Process Systems and Smith’s Detection have
developed a range of petroleum analyzer products based on a mid-infrared
spectrometer which utilizes an attenuated total reflection (ATR) sample
interface. The ATR allows wipe and swipe sample introduction that is ideal
for heavy petroleum analysis. Chemometric approaches to chemical and
physical property prediction have been developed as well as analysis by
spectral database matching. The FTIR-ATR spectrometer is called the RefinIR
which can be utilized in the laboratory for rountine, multi-parameter
prediction of petroleum product properties or to aid in process
troubleshooting on unusual samples or solid foulants.
For
more information contact Paul
Giammatteo Principal,
NMR Process Systems
87A
Sand Pit Rd, Danbury, CT 06810 U.S.A. Tel: (203) 744-5905
In
a joint development effort Process NMR Associates and Resonance Systems Ltd
have developed a replacement NMR spectrometer for the Oxford QP-20 TD-NMR
analyzer. In many cases the excellent magnet and probe of the QP-20 continue
to work effectively long after the NMR spectrometer has died. The Spin
Track-20 spectrometer enables the user to completely replace the QP-20 NMR
system while retaining the use of the original magnet and probe
configuration. The product represents state-of-the-art digital NMR
technology allowing newly developed TD-NMR methodologies to be applied to
complex systems with all the advantages of a windows computer system
(replacing the paper cartridge of the original system). Customers who have
malfunctioning QP-20 NMR systems can obtain a modern digital NMR system
within 8 weeks of order and for less than $16,000. The modular design of the
Spin Track TD-NMR systems allows our engineers to develop replacement
systems for all benchtop NMR systems such as those marketed by Oxford
Instruments, Bruker Minispec, and Resonance Systems. Contact us if you have
a non-functioning system that might be a candidate for the Spin Track
upgrade.
For
more information contact John
Edwards Principal,
Process NMR Associates - Spin Track Division
87A Sand Pit Rd, Danbury, CT 06810 U.S.A. Tel: (203) 744-5905
October 5, 2007
Eastern Analytical Symposium
– November 12-15, 2007
Garden State Convention Center,
Somerset, New Jersey
Process NMR Technology
Sessions
Wednesday, November 14, 2007
Chair: John Edwards, Process NMR
Associates
Sponsored by Process NMR Associates
Process NMR Technology I:
High-Resolution Studies
9:00 “Introduction to NMR in
Process Control”
John Edwards, Process NMR Associates
9:25 “Standardizing and Stabilizing
NMR Calibration Transfer”
Miko DeLevy, Qualion NMR Analyzers
9:50 “More from the Barrel –
On-line NMR Increases Diesel Production
and Quality”
Paul Giammatteo, Process NMR Associates
10:15 Break
10:35 “Taking NMR into the Refining
Process: Best Practices and Benefits”
Marcus Trygstad, Invensys Process
Systems
11:00 “Get Your Head Out of the
Sand: Use of Reaction NMR to Better
Understand Reactions in Process
Development”
Andreas Kaerner, Eli Lilly
11:25 “Direct Prediction of
Gasoline Properties for Monitoring
Refinery Processes by H-1 NMR
Spectroscopy”
Veena Bansal, Indian Oil Company
Process NMR Technology II:
Time-Domain Studies
Chair: John Edwards, Process NMR
Associates
Sponsored by Process NMR Associates
2:00 “Recent Developments in
Time-domain NMR and Its Applications in
Polymer Industry”
Harry Xie, Bruker Optics
2:25 “Time-domain NMR: Uses and
Contributions to Process Control”
Vaughn Davis, Progression
2:50 “Recent Progress of NMR and
MRI in Petroleum Exploration”
YiQiao Song, Schlumberger-Doll
3:15 Break
3:35 “Applications of Time-domain
NMR to Laboratory and On-line Polymer
Analysis”
Maziar Sardashti,ConocoPhillips
4:00 “Challenges in On-line Water
Cut Monitoring of Heavy Oil Thermal
Operations Using Low Field NMR”
Sergey Kryuchkov, University of Calgary
4:25 “Benchtop Fluoride NMR: A
Rapid QC/QA Method”
Chris Borgia, Colgate-Palmolive
The
Mid-Hudson Section of the American
Chemical Society and Vassar College
Announce
“The
Wood-Based Biorefinery in a Petroleum
Depleted World”
Dr.
Arthur J. Stipanovic,
Professor
and Chair, Department of Chemistry
State
University of New York,
College of Environmental Science and
Forestry (SUNY-ESF)
Wednesday,
November 7th, 2007
Time:
7:00 pm
Location:
Mudd Chemistry Building, Third Floor
Refreshments
will be served at 6:30 pm
Vassar
College, Poughkeepsie, New York
Contact:
Dr Joseph Tanski (jotanski@vassar.edu,
845-437-7503)
Abstract:
The 21st century is
envisioned to become the “age of
biology” as renewable biomass
resources replace petroleum in energy
and industrial product applications.
Motivated by concerns over national
energy security, global CO2
reduction, a need for biodegradable
products, and enhanced rural economic
development, the engineering and
construction of “biorefineries” for
the manufacture of fuels, chemicals,
polymeric materials and power from
renewable resources is now a critical
national priority. The context and
intent of a biorefinery must be much
more than simply replacing crude oil
with renewable raw materials. A
successful biorefinery must: 1)
efficiently separate its raw material
source into individual components, and,
2) be able to convert these components
into marketplace products. The
biorefinery must mirror the efficiency
of today’s modern petrochemical
refinery in using all components of its
raw material source for the production
of chemicals, fuels, and power.
Woody
“lignocellulosic” biomass is a
complex, composite material consisting
of three polymers in close association:
hemicellulose, cellulose, and lignin
plus small amounts of low molecular
weight extractives and inorganics. In
this presentation, a group of
synergistic biomass feedstock and
“biorefining” technologies under
development at SUNY-ESF, in
collaboration with many industrial and
academic partners, will be discussed
including: short-rotation fast growing
willow production, biodelignification,
hemicellulose extraction, polymer
conversion to fermentable sugars,
biodegradable thermoplastics and
hemicellulose-based composites.
See
the Stipanovic Website at SUNY_ESF for
further details…..http://www.esf.edu/chemistry/faculty/stipanov.htm
Bio:
Dr. Arthur J. Stipanovic is currently
Professor and Chair of the Department of
Chemistry at the SUNY College of
Environmental Science and Forestry (SUNY-ESF)
in Syracuse , NY , and also serves as
Director, Analytical and Technical
Services. His research interests include
biodegradable polymers from renewable
resources, high-throughput analytical
techniques for determining the
composition of woody biomass and new
processes for the wood-based biorefinery.
Dr. Stipanovic received both his B.S.
and Ph.D. degrees from SUNY-ESF in
polymer chemistry and much of his career
was spent at the Texaco R&D labs in
Beacon, NY, in new technology and
lubricants research. He is a past
Councilor and Executive Board member of
the Mid-Hudson ACS section and, more
recently, has served as Chair of the
Syracuse section.
Directions:
Vassar College is located off Raymond
Avenue in Poughkeepsie , NY. Refer to
the following link for driving
directions and campus map: http://www.vassar.edu/directions/.
Enter the
Main Entrance of the campus on Raymond
Avenue and
go right towards the Mudd
Chemistry Building. The Security Guard
at the Main Entrance will direct you to
parking.
June 12, 2007
NMR
analysis of Jasmine Absolute.
For
more information on NMR of Essential
Oils visit the PNA website.
May 15, 2007
Fish
Oils - Flaxseed Oils
NMR is extensively utilized to
analyze fish oils and edible oils high
in omega-3 fatty acids.
Examples of 1H and 13C
data and analysis are provided below:
13C NMR Analysis of Fish
Oil Supplement
13C NMR of Flaxseed Oil
Supplement
May 14, 2007
Brief
Overview of Wine Analysis by 1H
and 13C NMR
Wine
analysis by 1H or 13C
NMR can be used to follow acid content
during maturation. Lactic, succininc and
acetic acid can be followed readily by
both techniques and presence of sugar,
glycerol, and methanol can be observed.
Chemometric
approaches are starting bear fruit with
respect to quantitative analysis:
1H and
13C NMR NMR is typically
obtained using deuterated NMR solvents
to lock the field during acquisition. In
some cases the use of these solvents is
problematic as it prevents observation
of solublized phases present in the
sample. As an example we show here the
NMR data obtained on a biodiesel
production process. One of the major
issues with the FAME product is the
presence of glycerol in the product. NMR
analysis is usually performed by
dissolving the FAME in CDCl3
in which glycerol is completely
insoluble. Thus NMR analysis performed
in this way does not allow analysis of
residual glycerol content. However, if
the FAME is run neat this issue does not
arise.
Another
analysis of enormous interest from the
process control standpoint is the
analysis of the glycerol/methanol phase.
This phase contains considerable free
fatty acids as well as the glycerol by
product and excess methanol from the
transesterification process. The three
components are readily observed by 1H
and 13C NMR, and 23Na
can be used to observe NaOH content in
the phase. Finally the shift and shape
of the observed OH resonance can yield
information on the pH of the glycerol
phase. Typically this analysis is done
in DMSO-d6
Below are some
examples of NMR obtained without a
deuterated solvent:
Difference in aliphatic carbon
distribution between FAME phase and Free
Fatty Acids (FFA)
found in the glycerol - methanol
phase.
1H NMR of aliphatic component found
in the FAME phase as well as the FFA in
the glycerol phase.
May 10, 2007
I am posting this on behalf of Damien
Jeannerat.
PhD
Position Available Starting in September
2007
April 16, 2007
The
19.5 MHz Spintrack NMR analyzer was
utilized to study a FAME biodiesel
production reaction. The samples
analyzed were:
1)
Used vegetable oil
2)
Partially transesterified biodiesel
product (bad biodiesel)
3)
High yield FAME biodiesel product
4)
Glycerin by-product from the process
CPMG
T2 decays were generated and then that
data was processed with a inverse
laplace transformation to produce T2
distribution profiles.
NMR
Experiment explanation is given below:
The
CPMG data obtained on the four samples
is shown below:
The
T2 distribution profiles obtained by
inverse Laplace transformation of the
CPMG data are shown below:
Plainly
TD-NMR can play a role in monitoring the
biodiesel production process.
The
19.5 MHz Spintrack NMR analyzer was
utilized to study a large series of
vacuum gas oils and FCC feeds for
which PNA also has laboratory test data.
The
analysis was performed on a SpinTrack
19.5 MHz TD-NMR spectrometer - CPMG
T2 decays were generated and then that
data was processed with a inverse
laplace transformation to produce T2
distribution profiles. These T2
distribution profiles are currently
being correlated to physical and
chemical property data.
NMR
Experiment explanation is given below:
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