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

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.

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.

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 RefinIR^TM - 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

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

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

• Registration form

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

• Lodging Options

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.

• Maps and Directions

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

Tentative Program

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 21^st 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.

NMR analysis of Jasmine Absolute.

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

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

Brief Overview of Wine Analysis by ¹H and ¹³C NMR

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.

I am posting this on behalf of Damien Jeannerat.

PhD Position Available Starting in September 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:

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.

pdf version

Below are examples of ¹³C NMR data obtained on biodiesel (FAME) and the vegetable oil precursor that it was made from by transesterification process involving microwave activation of the reaction between triglycerides and methanol in the presence of a caustic catalyst. Process NMR Associates is developing correlations between ¹³C NMR data and biodiesel properties stipulated in ASTM 6751.

Today one often finds hydrocarbon mixtures described by the detailed carbon type analysis that is possible from ¹³C NMR.