Process NMR Associates - http://process-nmr.com

October 31, 2008

1H NMR Analysis of Hard Apple Cider

Filed under: NMR — processn @ 4:18 pm

There have been quite a lot of NMR studies centered around apple cider (non-alcoholic) and apple cider vinegar. However a search of the literature turns up no reference for NMR analysis of hard apple cider. This effort was undertaken to analyse the alcohol content of the ciders and to determine the malic and acetic acid content. Ciders were produced by Dr Tim McMahon of Orange Community College, NY….for his own consumption.

Below are the NMR spectra obtained by regular 1H acquisition and with BINOM solvent suppression.

Data was obtained on our Varian 300 MHz spectrometer. Samples were prepared by degassing followed by addition of 1 drop of D2O as lock solvent.

Hard Cider #1 - NMR Analysis - Full Spectrum
Hard Cider #1 - Expansion NMR
Hard Cider #1 - Detailed Chemistry - 1H NMR
Hard Cider #2 - 1H NMR
Hard Cider #2 - Detailed Chemistry - 1H NMR

Micro-ESR Spectrometry of Crude Oils

Filed under: NMR — processn @ 3:36 pm

Process NMR Associates, LLC (Danbury CT) and Active Spectrum, Inc (San Carlos CA) are collaborating in the application of micro-ESR technology to petroleum applications. The initial work has focussed on crude oils but will soon be expanded to residues and cracker feedstocks.

Five samples of crude oil were tested by Micro-ESR spectrometry. The samples were:

1. Vasconia, Magdalena Basin, Columbia (V=39 ppm)
2. Merey, Eastern Venezuela Basin, Venezuela (V=303 ppm)
3. Oriente, Oriente Basin, Ecuador (V=65 ppm)
4. Qua Iboe, Agbada Formation, Niger Delta (V=2 ppm)
5. Basrah Light, Zubair Zone, Iraq (V=29 ppm)

The following spectra were observed:

Micro-ESR Spectra of Crude Oils

Figure 1: Micro-ESR Spectra of Crude Oil

The central peak is a combination of a persistent carbon-centered organic radical (g = 2.003) found in asphaltenes, and a vanadyl (VO2+) peak. The additional smaller peaks are associated with vanadyl only.

For producers, the technique could be used to rapidly measure asphaltene concentration on-line. The spin density of the organic radical is a function of the maturity of the oil and will of course vary between deposits. Notwithstanding, rapid electronic measurement of asphaltenes remains a topic of great interest. Similar techniques have also been used to assess the quality of coals. For refiners, vanadium is a contaminant that poisons the refinery catalyst. ESR has been used by refiners since 1962 to rapidly measure vanadium content in crude oil feedstocks both on-line and in laboratories. Active Spectrum Inc.’s Micro-ESR is shown below. It is 2.25″ in diameter by 2.5″ high. Power input is 12-30VDC, and the data interface is USB. The device is available as either an on-line sensor or as a benchtop unit.

Micro-ESR Probe/Magnet Assembly

Figure 2: Micro-ESR Sensor

Higher resolution ESR spectrum of Merey Crude Oil

Figure 3: Higher Homogeneity Spectrum of Merey Crude

Micro-ESR is complimentary to NMR in that it observes paramagnetic metals and organic radicals which are unobservable by NMR. The stable free radical signal is indicative and quantitative to the amount of asphaltenes in the crude oil sample and vanadium metal content is an important processing parameter for cracking processes as it is active in the passivation of catalysts. NMR on the other hand observed the detailed hydrocarbon chemistry of the sample and yields chemico-physical parameters such as aromaticity, paraffinicity, naphthenicity, distillation, density, PAH distribution. In combination these two technologies yield a detailed picture of the petroleum materials before and during the refining process.

Samples provided by John Edwards of Process NMR Associates, LLC. Micro-ESR analysis provided by James White of Active Spectrum, Inc,

Active Spectrum Inc Logo
Active Spectrum, Inc. 110 Glenn Way #15, San Carlos, CA 94070 650-610-0720 | 626-628-1970 f | activespectrum.com

Process NMR Associates, LLC Logo
Process NMR Associates, LLC. 87A Sand Pit Rd, Danbury, CT 06810 203-744-5905 | 203-743-9297 f | process-nmr.com

PDF Version of Application Note

For more information contact John Edwards (203) 744-5905

Residual Catalytic Cracking (RCC) - Feedstream Analysis by NMR

Filed under: NMR — processn @ 10:32 am

Current Technique for Feedstream Analysis:
Analysis Performed – Refractive Index, Distillation, Specific Gravity
Calculation Obtained – Watson K-Factor
Outcome: aromatic carbon number, aromatic hydrogen number, total hydrogen content
Proposition: Detailed hydrocarbon analysis for kinetic model development.

Our experience is that an improved and useful analysis can be obtained from NMR
analysis. There are several ways to approach the NMR analysis and the
chemometric approach to correlating NMR data to physico-chemical parameters of
use to process control.

RCC Feedstream Analysis by 1H and 13C NMR: Multivariate Prediction of Chemical and Physical Properties

Presented at the 236th ACS National Meeting, Philadelphia PA, August 17-21, 2008

John C. Edwards Ph.D.
Process NMR Associates LLC
87A Sand Pit Rd, Danbury, CT 06810

Jincheol Kim,
SK Energy Co., Ltd, SK Energy Technology Center,
140-1, Wonchon-dong, Yuseong-gu, Daejeon 305-712, Korea

Summary of Slides

1) 60 MHz process NMR data available from online NMR unit.

60 MHz Process NMR Data available from online NMR Unit

2) 300 MHz 1H NMR data available from standard NMR experiments on laboratory NMR system at Process NMR Associates

300 MHz 1H NMR Data - RCC Feeds

3) Expansions of 1H NMR data on RCC Feeds

Expansion of 300 MHz 1H NMR Data - RCC Feeds

4) Calculated 1H NMR Parameters Represented as an alternative “spectrum” for use in chemometric modeling and linear regression.

Calculated 1H NMR Parameters Represented as a

5) 13C NMR Data obtained on RCC Feeds

13C NMR Data  - RCC feeds

6) Expansions of 13C NMR Data

Expansions of 13C NMR Data - RCC Feeds

7) 13C NMR and Average Molecule Parameters Calculated from 13C Spectrum

13C NMR - Calculated Parameters

8) Calculated 13C NMR Parameters Represented as an alternative “spectrum” for use in chemometric modeling and linear regression.

13C NMR Parameters Represented as a

9) Correlations of Spectra and Calculated Parameters to Physico-Chemical properties of RCC Feeds

Correlations of Spectra and Calculated Parameters to Physico-Chemical Properties of RCC Feed

10) Correlation of Spectra and Calculated Parameters to Density

Correlation of Spectra and Calculated parameters with Density

11) Variable Selection for Linear Correlation of Calculated NMR Parameters to Physico-Chemical Properties of RCC Feeds.

Variable Selection for Linear Correlations

12) Correlation of Calculated 13C NMR Parameters (C-Type and Average Molecule) with both high resolution 1H and 13C NMR spectra. Models created can be utilized by personnel with no NMR experience to calculate NMR parameters directly from the spectrum without any prior knowledge of integrations or calculations to be performed.

Correlation of 1H and 13C NMR Spectra with Calculated 13C NMR Parameters

Summary
Chemical and Physical Properties of RCC Feedstreams can be determined
by 1H NMR (at 60 and 300 MHz) and by 13C NMR
H-Type and C-Type Parameters do not provide as good a correlation as is observed
by full spectrum regression. This is due to loss of resolved chemical shift information
when the spectrum is reduced to larger integral areas.
1H NMR can be combined with PLS regression modeling to provide detailed carbon
type analysis for RCC Feeds
Regression analysis of 13C NMR data can be utilized to fully automate the prediction
of 13C NMR type analysis : reducing the necessity for considerable knowledge and
analysis time on the part of the analyst.

For further Detail Contact John Edwards

September 23, 2008

Diesel Production Control - Combination of NMR and Simulated Distillation to Yield On-Line Carbon Number Distributions

Filed under: NMR, PAT, Process NMR — processn @ 6:58 am

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
NMR and SimDis - Diesels
SimDis of Diesels
Carbon Number Distribution by SimDis - Diesel
SimDis and NMR - Diesel #1
NMR and SimDis - Diesel #2
NMR and Simulated Distillation - Diesel #3
SimDis and NMR - Diesel #4
NMR and SimDis - Diesel #5
NMR and SimDis - Diesel #6
SimDis and NMR - Diesel #7
SimDis and NMR - Diesel #8

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 Tel: +1 (203) 744-5905

Process NMR Associates Website

Extensive NMR Diesel Database Enhances NMR Model Performance for Unit Control and Product Manufacturing

Filed under: NMR, PAT, Process NMR — processn @ 6:47 am

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.
NMR of Diesel
NMR - Aromatic Region of Diesels
NMR- Aliphatic Region of Diesel
Hydrotreated Diesels - NMR
Diesel Distillation Model - T50 (F) NMR
Diesel Distillation model - T50 (C) - NMR
Diesel Distillation Model - T90 (F) - NMR
Diesel Distillation Model - T90 (C) - NMR
Diesel Flash Model - NMR
Diesel Cloud Point Model - NMR
Diesel T50 Model Online Performance - NMR- 3 Weeks
Diesel Flash Point Model Online Performance - NMR - 3 Weeks
Diesel Cloud Point Model Online Performance - NMR - 3 Weeks
NMR - Diesel Production Control Scheme

If you are interested in finding out more about NMR and diesel production control contact Paul Giammatteo or phone him at +1 (203) 744-5905 - see the Process NMR Associates website for further information

September 15, 2008

Quantitative NMR Analysis of Wine - qNMR

Filed under: NMR — processn @ 7:52 am

Here is an example of a 1H NMR analysis of a 2007 Red Wine submitted for chemical analysis by John W.

1H NMR Spectrum - Quantitative Analysis of Wine

1H NMR of Wine - Detailed Component Breakdown

NMR Analysis - Quantitative Component Calculation

If you are interested in wine analysis please contact us.

Solid-State 13C NMR Analysis of Carbonaceous Materials

Filed under: Energy, NMR — processn @ 6:38 am

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.

Solid-State 13C NMR - Illinois #6 Coal

Solid-State 13C NMR - Hiawatha Coal

Solid-State 13C NMR - Coals: Rosebud and Dietz

Solid-State 13C NMR - Engine Deposits: CCD and IVD

Solid-State 13C NMR - Refinery Coke

Solid-State 13C NMR - Arab Medium Heavy Asphaltene

Solid-State 13C NMR - Pipe Tobacco

Please inquire if you are interested in the details of the above analyses.

September 13, 2008

60 MHz TD-NMR System

Filed under: NMR, TD-NMR — processn @ 9:42 pm

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).

60 MHz NMR Console - Hahn Echo

60 MHz NMR - CPMG

60 MHz NMR - T1 - 90-90 Experiment

60 MHZ NMR Magnet with 5 mm Probe

60 MHz TD-NMR Magnet

February 28, 2008

Process NMR Application: Spectro-Molecular Control for Enhanced Diesel Recovery

Filed under: Energy, NMR, Process NMR — processn @ 1:18 pm

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 refiners 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 hydro-treaters. 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 observesthe 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.

Enhanced Diesel Recovery

Let NMR Process Systems deliver Spectro-Molecular Control to your refinery so that you can achieve real economic and production benefits.

January 28, 2008

Process NMR Associates - Archives - Gasoline Analysis by NMR and Chemometrics - ENC 1996

Filed under: Chemistry, NIR, NMR, Process NMR — processn @ 8:55 pm

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 Analysis by COSY NMR

Filed under: Chemistry, NMR — processn @ 8:51 pm

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.

Conjugated Olefins by COSY NMR - 1D 1H NMR - Coker Naphtha

Conjugated Olefins by COSY NMR - COSY - Coker Naphtha Showing Conjugated Olefin Signals

Conjugated Olefins by COSY NMR - Hydrotreated Naphtha

Conjugated Olefins by COSY NMR - Hydrotreated Naphtha

October 29, 2007

Schering-Plough Corporation Seeks Process Analytical Technology Manager

Filed under: IR-ATR, NIR, NMR, PAT, Process NMR — processn @ 8:58 pm

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 

NPS - IS : A New Approach to Process Analytical

Filed under: Chemistry, Energy, IR-ATR, NIR, NMR, Process NMR, TD-NMR — processn @ 5:34 pm

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

The RefinIR - FTIR-ATR Petroleum Product Analyzer

Filed under: Chemistry, IR-ATR, Process NMR — processn @ 5:32 pm

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

Process NMR Associates Develops Oxford QP-20 Spectrometer Replacement

Filed under: NMR, Process NMR — processn @ 5:29 pm

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 7, 2007

PNA Presentation at 9th Upstate NY NMR Symposium

Filed under: NMR, Process NMR — processn @ 8:35 am

State University of New York
College of Environmental Science and Forestry (SUNY-ESF)
Syracuse, NY, 13210
Alumni Lounge– Marshall Hall
October 12, 2007

Co-Organizers

SUNY-ESF Syracuse University SUNY Upstate Medical University Bristol-Myers Squibb
Art Stipanovic Phil Borer Stewart Loh Doug Weaver
Dave Kiemle Stephan Wilkens  

Sponsors

  • SUNY-ESF
  • Syracuse University
  • Bruker Biospin
  • Bristol-Myers Squibb
  • Process NMR Associates LLC
  • Isotec
  • Cambridge Isotope Laboratories
  • Varian Inc.

The 9th annual Upstate NY NMR Symposium will be held at SUNY-ESF on Friday, October 12th featuring keynote speaker Professor Ruth E. Stark, Director Institute for Macromolecular Assemblies, CUNY. Others from around the region will also highlight their work in short presentations and posters.

  • Tentative oral presentation program
  • Poster session program (posted by 9/12)

There is no cost to attend this symposium due to the generosity of the sponsors listed above but pre-registration is required

Lodging arrangements have not been made for this symposium but a variety of options are available:

The conference will be held in the Alumni Lounge (a.k.a. Nifkin Lounge), Marshall Hall on the SUNY-ESF campus located adjacent to Syracuse University.

Parking has been arranged in the Irving Garage just a short walk from Marshall Hall (campus map).

Tentative Program

Time Place Speaker Title
8:00-9:10 AM Alumni Lounge
Marshall Hall
Check-In
Coffee + Bagels
Poster Setup
Posters on Display
9:15 Alumni Lounge Phil Borer
Syracuse University
Welcome
9:30 “ Thomas Szyperski
SUNY-Buffalo
Where do we stand on GFT projection NMR spectroscopy?
9:55 “ Yibing Wu
SUNY-Buffalo
GFT-NMR based high throughput structure determination exemplified for NESG targets NeT4 and SR500A
10:10 “ Arindam Ghosh
SUNY-Buffalo
NMR structure of NESG target MR32, a member of the family of Trm112p-like proteins
10:25 “ Bio-Break
10:35 “ David LeMaster Wadsworth Center - NYS Dept. of Health Electrostatic stabilization and general base catalysis in the active site of the human protein disulfide isomerasea domain monitored by hydrogen exchange
11:00 Joseph Hornack
RIT
The relaxivity of Gd-(DTPA-BMA) / Cu+2 mixtures and evidence for a Gd-(DTPA-BMA)-Cu complex.
11:25 Nelly Aranibar
Bristol-Myers Squibb
Metabolomics in Drug Discovery and development
11:50 “ Lunch
Poster Session
 
1:30 PM 140 Baker Lab Nikolaos Sgourakis
Rensselaer Polytechnic Institute
Pressure Effects on the Ensemble Dynamics of ubiquitin at the Picosecond-to-Nanosecond timescale investigated with isotropic reorientational eigenmode dynamics
1:55 Paul Giammatteo or John Edwards
Process NMR Associates, LLC
New Developments in Non-traditional NMR Applications
2:25 “ George Crull
Bristol-Myers Squibb
Extending Solid State NMR to Address Process Development Issues
2:50 “ Gwen Lubey
P+G Pharmaceuticals
Solid State NMR Characterization of Risedronate Hydrate Forms and Dehydrated Risedronate
3:15 “ - Break
3:30 Keynote Lecture Prof. Ruth Stark
CUNY
NMR Structural Studies of Protective Plant Biopolymers

October 5, 2007

Process NMR Sessions at Eastern Analytical Symposium - November 14

Filed under: NMR — processn @ 1:26 pm

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 Wood-Based Biorefinery in a Petroleum Depleted World

Filed under: Chemistry, Energy, IR-ATR, NIR, NMR, PAT, Process NMR, TD-NMR — processn @ 1:08 pm

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 - jasmine officinale - Egypt

Filed under: NMR — processn @ 12:51 pm

NMR analysis of Jasmine Absolute.

For more information on NMR of Essential Oils visit the PNA website.

May 15, 2007

Omega-3 Dietary Supplements - NMR Analysis

Filed under: Chemistry, NMR — processn @ 7:39 am

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

Wine Analysis by NMR

Filed under: Chemistry, NMR, Process NMR — processn @ 6:38 pm

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:

NMR Without Solvents - Biodiesel Production Process - FAME, Glycerol, FFA, and Methanol

Filed under: Chemistry, Energy, NMR, Process NMR — processn @ 6:36 pm

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

NMR PhD Position with Damien Jeannerat at Universite de Geneve

Filed under: NMR — processn @ 11:12 am

I am posting this on behalf of Damien Jeannerat.

PhD Position Available Starting in September 2007

April 16, 2007

Monitoring of a Biodiesel Transesterification Process with a TD-NMR Spectrometer

Filed under: Chemistry, Energy, NMR, Process NMR — processn @ 6:18 pm

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.

 

TD-NMR Analysis of Catalytic Cracker Feedstocks

Filed under: Chemistry, Energy, NMR, Process NMR — processn @ 6:16 pm


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:

 

 

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:

 

The correlation between T2 distribution and the metal content, viscosity, distillation range, density, asphaltene content are all being investigated at the current time.

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