John C Edwards

• Ph.D. Physical Chemistry
• Owner at Process NMR Associates

Benchtop high-resolution NMR systems are available at a number of field strengths and probe configurations. However beyond the obvious academic instruction market for these instruments very few applications have been demonstrated across all available platforms and thus proving the general applicability of benchtop NMR technology to industrial quali...

A brief description will be given of the analytical testing requirements at different stages in the growing, harvesting, processing, certification, and sale of hemp and marijuana products. A 1H qNMR method for quantitation of cannabinoids, terpenes and residual solvents in flower, mixed biomass, distillate and products such as tinctures, vapes, cre...

1H NMR applications to oregano authenticity, 31P NMR krill oil authenticity and fraud, coffee authenticity - robusta addition to arabica

Over the past few years a controversy has been raging over the analysis of non-traditional alcoholic beverages. Scientific shenanigans are being played out by an entire craft beverage industry sector concerning the accuracy, or perceived lack thereof, of traditional analytical approaches (density with NIR, GC, distillation) to quantify low alcohol...

In the scope of analytical method validation it is generally accepted, in the arena outside of NMR spectroscopy, that validation should include inter-laboratory comparison (ILC) studies or proficiency testing coordinated by a relevant third-party organization such as AOAC, AOCS, ASTM, ISO, USP, etc. Validated NMR methods that are in general use by...

The baijiu spirit is often the focus of fraudulent activity due to the widely varying prices of the products. In this work, Solid Phase Microextraction Gas Chromatography (SPME GCMS), Fourier Transform Infrared (FTIR) Spectroscopy and 1 H qNMR spectroscopy were evaluated as potential methods to authenticate baijiu samples. Data were collected for 3...

1H NMR Analysis of Biodiesel from the Front to the Back of the FAME Production Process and Blending with Diesel Fuel and Home Heating Oil

Coffee cherry is a rich source of caffeine and chlorogenic acids. In this study we investigate the structural analysis of caffeine-enriched whole coffee cherry extracts, CEWCCE by using ¹H and ¹³C NMR spectroscopy. The changes in ¹H chemical shift data in NMR spectra of CEWCCE compared to pure caffeine indicated the formation of complexes between c...

Through an integration of metagenomic and experimental approaches, our work reveals the diversity and nature of interactions among key taxa in kombucha microbiomes through the construction of synthetic microbial pairs. Manipulation of these microbes in kombucha has the potential to shape both the fermentation qualities of kombucha and the productio...

1H NMR of Beer, Cider, Kombucha, Wine, Hops, Juices, Sake, Vinegars, Near Beer, Hard Selter, Spirits, Liquor, Sherry, Port

The Chinese spirit baijiu is currently the world’s bestselling spirit, with more than ten billion liters sold in 2018. This is a figure that puts its sales higher than whiskey, vodka, gin, and tequila combined. The multitude of baijiu varieties available in the market differ in several ways ranging from aging to the traditional artisanship involved...

1H qNMR of Alcoholic Beverages

1H NMR of Beer

Industrial qNMR Using Low-Field Instrumentation

1H qNMR Fingerpriny Analysis of Cider

Invited Talk - qNMR and Benchtop Systems - Tokyo qNMR Summit 2018 - US Pharmacopoeia Session

Benchtop high-resolution NMR systems are available at a number of field strengths and probe configurations. However beyond the obvious academic instruction market for these instruments very few applications have been demonstrated across all available platforms and thus proving the general applicability of benchtop NMR technology to industrial quali...

Chemical analysis of the organic components in beer has applications to quality control, authenticity and improvements to the flavor characteristics and brewing process. This study aims to show the complementary nature of two instrumental techniques which, in combination, can identify and quantify a number of organic components in a beer sample. Nu...

1H nuclear magnetic resonance spectroscopy (NMR) has been used by chemists for 50 years as the ultimate tool for molecular structure elucidation. Another area where NMR spectroscopy excels is the quantitative analysis of complex mixtures where multiple individual molecular components produce NMR signals that can be identified and quantified to prod...

Chemical analysis of the organic components in beer has applications to quality control, authenticity and improvements to the flavor characteristics and brewing process. This study aims to show the complementary nature of two instrumental techniques which, in combination, can identify and quantify a number of organic components in a beer sample. Nu...

Different sugar borate esters (SBE) are found in fruits, vegetables, nuts and legumes and they are naturally absorbed by animal cells. Fructose and glucose borate esters are most common SBEs. In food they serve as soluble borate with potential health beneficial effects. The samples used for this study are magnesium and calcium sugar-borate complexe...

Fruitex-B® (FrxB) is a patented plant mineral complex that is marketed as a nutritional supplement with potential health benefits for conditions linked to inflammation such as bone, joint and cardiovascular conditions. The original product was a calcium fructoborate complex formed by the reaction of boric acid with fructose and calcium carbonate. R...

Over the last few years we have been developed a quantitative 1H NMR method for chemical fingerprinting in beer, cider, wine, kombucha, and spirits. As well as looking at hops, malts, worts, fermentations, sour ageing, apple and fruit juices. We can quantify ethanol (and methanol, isobutanol, isopentanol, 1-propanol, glycerol), organic acids (lacti...

The craft alcoholic beverage market has experienced dramatic growth over the past few years, and the Brewers Association estimates an 18% increase in sales volume of craft beer in 2014. Craft distilleries and cideries have also increased. Small fermentation beverage companies and home brew enthusiasts provide an increased demand for chemical analys...

Presentation on NMR Standard Methods ..... or lack therof

The purpose of this study is to evaluate how different binders react with polyphosphoric acid (PPA), and to contribute to a better understanding of this interaction. A number of bituminous binders were characterized before and after adding PPA, using rheological and chemical test methods, including FT-IR, uv-vis spectroscopy, NMR and gel permeation...

Bench-top Low field NMR Techniques for Detection of PDE-5 Inhibitors in Dietary Supplements

Nutritional Supplement and Diesel Fuel Application Development for Benchtop NMR Systems Operating at 42, 60, and 80 MHz – Equivalency with Supercon NMR

1H quantitative NMR (qNMR) has been utilized to assess the the small molecule and carbohydrate chemistry of a number of home-brewed and commercial alcoholic ciders. A quantitative chemistry distribution of the products of the various fermentations that occur in cider making. Malolactic fermentation as well as fermentation by saccharomyces and wild...

The adulteration of dietary supplements (or natural health products) with synthetic pharmaceuticals is an area of increasing concern, which presents substantial risk to public health. Widely available in retail and via the Internet, these products are often marketed as sexual enhancement, weight loss and/or bodybuilding supplements. Unlike prescrip...

Spontaneous biological acidification has long been a part of the German brewing tradition, and was historically used to optimize the pH of brewhouse mashes. By facilitating the growth of native barley flora, the production of lactic, acetic and succinic acids sours the mash, functioning in a similar way to the addition of food-grade acids, which ar...

For the past decade it has been well documented that many over-the-counter dietary supplement products that claim to enhance sexual performance are in fact adulterated with undeclared phosphodiesterase type 5 (PDE5) inhibitors1. Examples of these PDE5 inhibitors are sildenafil (Viagra) and Tadalafil (Cialis) and a large number of analog materials....

Aluminum (Al) is the third most abundant element and the most abundant element found in the Earth's crust. Elemin™ (FutureCeutical, Inc., Momence, IL, USA) is a multi inorganic element complex with more then 70 inorganic elements and minerals all of which are completely water soluble, including all the Al compounds. The objective of this study is t...

FruiteX-B®- calcium fructoborate (FrxB) plant mineral complex was investigated in this study. Although calcium fructoborate is naturally-occurring and found in commonly ingested fruits and vegetables, the commercially produced FrxB calcium fructoborate complex is formed by a proprietary reaction of boric acid with fructose and calcium carbonate. Li...

Fruitex-B® (FrxB) is a patented plant mineral complex that is marketed as a nutritional supplement with potential health benefits for conditions linked to inflammation such as bone, joint and cardiovascular conditions. The product is a calcium fructoborate complex formed by the reaction of boric acid with fructose and calcium carbonate. Liquid and...

An automated approach to complex mixture 1H qNMR was developed for the Mnova platform and small molecule quantitation was performed on a series of Aloe vera raw materials and Aloe vera containing products utilizing nicotinamide as the internal concentration standard. The analysis automatically generates a comprehensive report of the three active co...

Pursuing the goal to develop an express technique for the characterizing of forest ecology, this paper presents a description of the found dependence of nuclear magnetic resonance (NMR) relaxation times of water in soils on the pollution caused by vehicle exhausts. Test measurements were made in Mari El Republic of Russia where wildwood areas locat...

1H qNMR analysis of small molecules (esp. organic acids) in wild fermentation beers. PCA of beers styles.

1H NMR of a series of samples taken from different points in the manufacturing process of a fish oil nutritional supplement were obtained on a 300 MHz superconducting NMR system and a cryogen-free bench-top 60 MHz NMR system. The resulting spectra were utilized to develop single wide-range partial least-squares regression models of the EPA and DHA...

This 1 H Quantitative NMR (qNMR) method was developed and validated by Process NMR Associates (Danbury, CT) and a similar 1 H NMR approach has been subjected to independent validation by Spectral Service (Köln, Germany), Unigen Pharmaceuticals, Inc. (Lacey, WA), and the Department of Chemistry, Saint Martin's University (Lacey, WA) (Ref. 1, Jiao et...

Online NMR is routinely employed as a reaction monitoring tool in the process development area at Pfizer. Investigation of organic reaction processes by online NMR at 400 MHz provides detailed process understanding for development chemists. Here we outline the details of expansion of this reaction monitoring platform to include a 60 MHz NMR portabl...

The Yen?Mullins model, also known as the modified Yen model, specifies the predominant molecular and colloidal structure of asphaltenes in crude oils and laboratory solvents and consists of the following: The most probable asphaltene molecular weight is ?750 g/mol, with the island molecular architecture dominant. At sufficient concentration, asphal...

The molecular architecture of asphaltenes is still a matter of debate. Some literature reports provide evidence that the contrast of petroleum asphaltenes versus coal-derived asphaltenes is useful for understanding the governing principles of asphaltene identity. Coal-derived asphaltenes provide an excellent test for understanding the relationship...

Description This unique publication examines twelve spectroscopic techniques used in oil industry laboratories. Twenty-four chapters provide a detailed discussion of the fundamentals of the techniques and their application in the oil analysis field. This is the only book available that describes both theory and applicability. It also includes exten...

Direct Injection Spark Ignition (DISI) engine technology is becoming increasingly common in the South African and global vehicle pares. South Africa is in a unique position because a significant portion of all liquid fuels consumed are synthetically produced from coal and gas. These fuels are mainly supplied into the inland regions, particularly th...

ChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 100 leading journals. To access a ChemInform Abstract of an article which was published elsewhere, please select a “Full Text” option. The original article is trackable via the “References” option.

A large number of solid-state NMR and ESR experiments were explored as potential tools to study chemical structure, mobility, and pore volume of activated carbon. We used a model system where pecan shells were activated with phosphoric acid, and carbonized at 450 °C for 4 h with varying amounts of air flow. Through the use of different NMR experime...

The effect of phosphorus on the structure of NiMo/Al2O3 hydrotreating catalyst precursors has been investigated. Calcined and reduced P/Al2O3, PNi/Al2O3, P-Mo/Al2O3, and PNiMo/Al2O3 (where the wt% P = 0.0 to 10.0, wt% Mo = 8.0 to 12.0, and wt% Ni = 4.0) have been studied using FT-IR, XRD, and 31P and 27Al MAS NMR techniques. Phosphoric acid reacts...

The solid-state ⁹⁵Mo NMR of oxomolybdates and polyoxomolybdates adsorbed to γ-alumina was utilized to characterize the molybdenum species present at circa monolayer coverages of molybdenum. This represents the first attempt at using solid-state NMR to look directly at the molybdenum species on the surface of 'fresh' hydrodesulfurization cataly...

The integration of high resolution nuclear magnetic resonance (NMR) hardware with properly designed applications has played a key role in enhancing fuel production in refineries. Online NMR-based analytical and process control strategies enhance clean fuels production directly at the control display unit (CDU). NMR can maximize clean diesel recover...

Nuclear magnetic resonance spectroscopy (NMR) was first developed in 1946 by research groups at Stanford and M.I.T., in the USA. The radar technology developed during World War II made many of the electronic aspects of the NMR spectrometer possible. With the newly developed hardware physicists and chemists began to apply the technology to chemistry...

Clean Fuels regulations have a substantial impact on a refiner's ability to maximize product draws. Many refiners are significantly undercutting these draws ensure minimum error in downstream product blends. On-line Nuclear Magnetic Resonance (NMR) based analytical and process control strategies enhance clean fuels production directly at the CDU. A...

Nuclear Magnetic ResonanceLiquid-State NMRSolid-State NMREnvironmental Applications of NMRTechniques and Applications on the HorizonSummaryReferences

Mayo plots have been used to determine the rate constant ktr for chain transfer catalysis by (C5Ph5)Cr(CO)3• of the AIBN-initiated polymerization of MMA from 60 to 80 °C. The value of ktr decreases with temperature, implying that abstraction of H• from the chain-carrying radical by (C5Ph5)Cr(CO)3• does not occur in a single step and suggesting the...

BASF conducted a feasibility study to determine an appropriate equipment to handle its two steam crackers. A process magnetic resonance analyzer (MRA) was chosen due to its measurement linearity, fast-track project execution, and high availability. The feedstock analyzer system was successfully extended to both crackers, including naphtha recycle s...

Three classes of inorganic solid acid catalyst have been demonstrated to be effective for methyl tert-butyl ether (MTBE) syntheses from methanol/tert-butanol (TBA) feed mixtures using a continuous, plug-flow, reactor system. These catalysts include heteropoly acids, such as 12-tungstophosphoric acid and 12-molybdophosphoric acid, on Group III and I...

Nuclear magnetic resonance (NMR) technology is now being used for refinery process analysis and control. Online process NMR represents the breakthrough technology needed for refining as it is the first analyzer available for application throughout the entire refinery, from crude to products. The current and future installations and applications of...

The chemical and dynamic nature of the tungstophosphoric acid (TPA) species adsorbed on pressed, extruded, and powdered TiO2 support was studied by 31P and 1H solid-state NMR spectroscopy and diffuse reflectance FT-IR. From 31P NMR and FT-IR results the TPA appeared to be present in at least five forms on the titania surface: a bulk salt phase, two...

Inclusion complexes of polyisobutylene (PIB) with cyclodextrins (CDs) have been synthesized via molecular recognition. Our results show that the PIB structure and the CD cavity size are key factors in the formation of inclusion complexes. For example, mono- and diarm PIBs behave differently towards the formation of inclusion complexes with gamma-cy...

Sulfuric acid alkylation process control using online nuclear magnetic resonance (NMR) measurements is described. The method can be used to measure acid strength, acid/hydrocarbon emulsion quality, hydrocarbon/olefin ratios, and acid soluble oil content on the intact emulsion stream in the alkylation reaction zone. It is shown that using a process...

A soft coke-like substance often forms In the liquid product of visbreaking and hydrocracking processes for upgrading vacuum residue of heavy crude oil. This material usually limits the severity, or conversion of the process because it accumulates in downstream equipment. Although the amount of such material produced depends on the crude oil, it ha...

Non-template synthesized ferrierite/ZSM-35 has been successfully modified by removal of non-shape selective acid sites and lowering of the number of acid sites. Modified materials were extensively studied by XRD, FT-IR, NMR, XPS, ammonia TPD, and kinetic evaluations for skeletal isomerization ofn-butene to isobutylene. Removal of non-shape selectiv...

Several series of commercial alumina supported nickel-molybdenum and cobalt-molybdenum hydrotreating catalysts were exposed to differing degrees of reaction lengths and severities using a variety of naphtha and gas-oil feeds. Fresh and used catalysts were characterized by gas-oil desulfurization and denitrogenation activity, chemical analysis of de...

Semigelatinous interfacial films, which may influence the fluid mechanic and mass transfer properties of coal tar in porous media, have been observed to form in coal tar−water systems when coal tars are aged in water under quiescent conditions for a few days. Samples of the interfacial film were isolated after aging for a period of 1 year and compa...

Ferrierite/ZSM-35 is a shape selective zeolite catalyst for n-butene skeletal isomerization to isobutylene. Hydrothermal methods were used to synthesize well-crystallized ferrierite/ZSM-35 materials of different silicon to aluminum ratios and crystallinities in the presence of an organic template, pyrrolidine. Non-template-synthesized ferrierite wa...

Sodium ionic clusters have been prepared by chemical vapor deposition of sodium metal at 225{degree}C and 1 x 10{sup -4} Torr in NaX zeolites. A maximum loading of approximately 1.2 wt % sodium was vaporized onto dehydrated NaX zeolite. Ionic clusters prepared in this study have been determined to have the formula Na{sub 6}{sup 5+}. In this complex...

Studying the effect of secondary pores on the cracking activity of heavy gas oils we conclude that for Y zeolites having unit cell sizes in the range of 24.25 to 24.35 Å the cracking activity of heavy gas oil increases with increasing secondary porosity and secondary pore mode. We have been able to generate a range of total acid site densities, sec...

1H single pulse MAS and CPMG T2/CSA-filter NMR experiments have been performed in order to characterize the hydroxyl structure of γ-alumina, as well as fluoride- and phosphate-modified γ-alumina materials. We have shown that problems associated with the strong homonuclear dipole-dipole interactions between protons of neighboring OH groups can be ov...

Asphaltenes are a class of molecules that are defined by the conditions of their insolubility in a particular solvent, such as heptane. A better understanding of the molecular properties of this mixture of molecules is needed in order to understand the mechanisms of coke and sludge formation during refinery upgrading operations. In this work we dev...

The cross-polarization magic angle spinning (CPMAS) C-13 NMR spectra of N-15-enriched 2-phenethylamine as the ammonium salt and adsorbed on an aluminum-exchanged clay are compared with spectra for natural abundance 2-phenethylamine. An important gain in resolution is observed in the beta carbon chemical shift region of the C-13 CPMAS of the N-15-en...

Gas-oil hydrodesulfurization activity of Ni-Mo/Al2O3 catalysts was significantly improved when prepared with zirconium alkoxide, but lowered when prepared with Zr nitrate. IR of CO adsorption on reduced catalysts, and LRS and XPS of calcined catalysts show that the addition or zirconium does not effect the metal oxide structure. IR of pyridine adso...

[gamma]-alumina is used extensively as a catalyst support material. [sup 1]H single pulse MAS and CPMG T[sub 2]/CSA-filter NMR experiments have been performed in order to characterize the hydroxyl structure of [gamma]-alumina, as well as fluoride- and phosphate-modified [gamma]-alumina materials. The authors have shown that problems associated with...

A previously unobserved octahedral27Al MAS NMR resonance has been detected in rehydrated calcined Mo/Al2O3 hydrotreating catalyst precursors. This resonance is attributed to the presence of hydrated forms of aluminum molybdate such as [Al(OH)n (H2O)6-n ]n (MoO4) (n = 1 or 2). The cross-polarization relaxation parameters, obtained from variable cont...