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At least 19 records

Determination of Biogenic Content by 14 C in fuels using Liquid Scintillation Analysis Laboratory Analytical Procedure (Laboratory Analytical Procedure)

This procedure covers the determination of the percent 14 C in biogenic gasoline, jet fuel, and diesel range hydrocarbons prepared from distillation of hydrotreated pyrolysis oils and blended with fossil derived hydrocarbons (e.g. fossil diesel, gasoline, jet, or toluene). Either an internal 14C standard or a color quench curve is used to correct for potential signal quenching effects. Recent publications provide some background of direct LSC methods used for determination of biogenic fuel content.

02 PETROLEUM↗

Microbial ecology laboratory procedures manual NASA/MSFC

An essential part of the efficient operation of any microbiology laboratory involved in sample analysis is a standard procedures manual. The purpose of this manual is to provide concise and well defined instructions on routine technical procedures involving sample analysis and methods for monitoring and maintaining quality control within the laboratory. Of equal importance is the safe operation of the laboratory. This manual outlines detailed procedures to be followed in the microbial ecology laboratory to assure safety, analytical control, and validity of results.

Huff, Timothy L.↗

The Genesis Non-flight Implant Sample Archive

Introduction: For the past 20 years the Genesis science community has been analyzing solar wind captured in sample collectors now curated at Johnson Space Center (JSC). Non-flown flight like collector materials (non-flight) considered reference material was always allocated by the JSC Genesis team for testing experimental procedures. However, to expedite Genesis science, distribution of non-flown reference materials were also provided by, D. S. Burnett (Genesis PI, Caltech) and A. J. G. Jurewicz (ASU) who were funded to aid all Genesis PIs by providing engineering test materials archived at Caltech pre-flight as well as ion implants into these materials [1]. Implanted materials (non-flight reference, flight-like semiconductor materials, and NIST SRM glass) received from the Caltech collection during a pilot project are being used to develop an accession procedure for the purpose of making these materials available to researchers in the future. These implant samples are important because they can be utilized as measurement standards [2]. This is a work in progress and this work reports progress in documentation and imaging. The pilot program received 63 implanted reference materials with known implanted ions. Genesis Non-Flight Database: The existing non-flight material database was modified to allow for the description of implant sessions and to allow correlation of the implant information to individual specimens. An implant session has three main components: a known ion, a known dose (ion/cm2), and a known energy (keV). Procedure: Laboratory Procedure. Upon receiving non-flight analytical standards (independently calibrated implants), or implant samples (nominally calibrated implants), they will be imaged in their current containers to capture any information written before being brought into the Genesis Sample Laboratory. Documentation is provided by the donor and used for correlating the data between the implant sessions and implant samples. This information is not verified by Genesis Curation. The microscope used to image samples in the laboratory has an automated stage with a stainless-steel plate to hold samples and a camera that utilizes the software Surveyor to take photomosaic images of the implant samples. The camera attached to the microscope is a QICAM High Performance IEEE 1394 FireWire Digital CCD Camera. This setup, shown in Fig. 1, allows for photomosaics of small-scale samples with a 10x objective or 25x objective. Examples of images taken with this microscope setup are shown in Fig.2 and Fig. 3. After imaging, samples get stored in a clean fluoroware container or polypropylene vial depending on sample size for long term storage. Database Procedure. The Genesis Non-Flight Database currently allows for the addition of implant sessions. The required fields for adding an implant session are the implant session ion, the implant session dose, and the implant session energy. There are also fields for the date and vendor of the sessions as well as a field for if the session was calibrated or not. Once an implant session has been inserted into the database, additional documentation from the session can be attached. The database will automatically assign an Implant Session Number. After inserting an implant session, the implanted samples can be inserted. The fields required for an implant sample are the material of the sample and the size of the sample. The Generic name for the implant sample with be automatically generated by the database once it has been inserted. Implant sample numbers begin with 3X to distinguish from flown Genesis sample numbers. There are also fields for processors to add the location (room, cabinet, tray) and container type (fluoroware, polypropylene vial). Once an implant session and an associated sample(s) have been inserted into the database the sample can be then tied to all associated implant sessions. An implant sample can be tied to multiple implant sessions. Future work: For curation, future work consists of creating an online catalogue for implant samples as well as updating the database with more samples as we receive them. For the scientific community these implant samples have many potential uses. For Genesis research, they are directly applicable for testing and, in some cases, as analytical standards. For non-Genesis research, implants (especially calibrated implants) could be used for calibrating other, unique planetary materials [1].

C D Calva↗

Determination of Total, Organic, and Inorganic Carbon and Total Nitrogen in Biological Cultures and Liquid Fraction Process Samples: Laboratory Analytical Procedure (LAP)

This Laboratory Analytical Procedure (LAP) describes the quantitative determination of total organic carbon, inorganic carbon in whole suspended biological samples and in the cell-free supernatant, by combustion and CO 2 detection with a non-dispersive infrared (NDIR) detector. This allows for distinct reporting of soluble and insoluble organic and inorganic carbon. In addition, this procedure covers the quantitative determination of soluble nitrogen in the cell-free supernatant.

09 BIOMASS FUELS↗

Accelerated Aging of Fast Pyrolysis Bio-Oil Using Carbonyl Titration: Laboratory Analytical Procedure (LAP)

This laboratory analytical procedure covers the accelerated aging of fast pyrolysis bio-oils. Bio-oils undergo reactions that result in physical and chemical changes over time. These changes typically result in an increase in molecular weight, decrease in some functional groups such as carbonyls, and an increase in viscosity; additionally, the aging process often leads to phase separation. Studies have shown that accelerated aging of bio-oils using this method closely mimics room temperature aging for long periods of time (over 3 years). This procedure has been developed for the accelerated aging of fast pyrolysis bio-oils only. Fast pyrolysis bio-oils are more reactive than other bio-oils (e.g., catalytic fast pyrolysis) and undergo aging much more rapidly. Therefore, this procedure should only be used for fast pyrolysis bio-oil samples.

09 BIOMASS FUELS↗

Identification and Quantification of Photosynthetic Pigments in Algae (Laboratory Analytical Procedure (LAP))

The Laboratory Analytical Procedure (LAP) outlined here describes a method to quantitatively extract phytopigments from microalgae biomass, as well as to identify and quantify individual pigments based on separation and detection with a High-Performance Liquid Chromatography (HPLC) system coupled to a Diode Array Detector (DAD). Pigments were extracted with greater than 95 % extraction efficiency. Chromatographic conditions allowed for isomeric resolution between pigments and identification based on UV/Vis spectra and comparison to analytical standards.

09 BIOMASS FUELS↗

Procedures For Microbial-Ecology Laboratory

Microbial Ecology Laboratory Procedures Manual provides concise and well-defined instructions on routine technical procedures to be followed in microbiological laboratory to ensure safety, analytical control, and validity of results.

Huff, Timothy L.↗

Determination of Phenolic Groups in Bio-Oils Using Revised Folin-Ciocalteu Methods: Single Cuvette and Plate Reader. Laboratory Analytical Procedure (LAP), Issue Date: May 12, 2022

Phenol components are ubiquitous in wood-derived bio-oils and biocrudes. Their reaction with other functional groups (e.g., aldehydes) may contribute to the formation of carbonaceous species and the expected thermal instability of pyrolysis oils. During hydrotreating, phenols can be recalcitrant species, requiring higher reaction temperatures than other oxygen-containing functional groups. Phenols are also present in upgraded products and have been shown to lead to catalyst deactivation during hydrotreating. They also are the first oxygenated functional group to re-appear in the upgraded product, signaling catalyst deactivation. This procedure covers the determination of phenolic compounds in fast pyrolysis oils. This Laboratory Analytical Procedure (LAP) includes two methods, the first allowing for shorter analysis time at increased reaction temperature, while the second employs a longer analysis time but at room temperature. Additionally, the use of both a single cuvette and of a plate reader are also presented.

09 BIOMASS FUELS↗

Corrosivity Screening of Pyrolysis Bio-Oils by Short-Term Alloy Exposures. Laboratory Analytical Procedure (LAP), Issue Date: May 12, 2022

Bio-oils contain organic acids and oxygenated compounds that can lead to corrosion issues during bio-oil processing and storage. This Laboratory Analytical Procedure (LAP) allows for rapid screening of a bio-oil's corrosivity without the need for complex equipment and long-term exposures. A robust and repeatable method for assessing the corrosivity of bio-oils is necessary in order to remove materials degradation as an obstacle to research, upgrading, use and storage of bio-oils. This LAP involves the incubation of a representative alloy, 410 stainless steel (410 SS), specimen in bio-oil over a period of 48 hours at 50 degrees C in a sealed container. The corrosive species in the bio-oil react with and deplete alloy elements such as iron (Fe) and/or chromium (Cr) from the specimen into the bio-oil solution. The depletion of Fe and Cr from the specimen results in a significant mass loss that can be recorded. The mass loss is directly correlated to the corrosivity of a bio-oil. Examples of bio-oils in scope include the ones produced by fast pyrolysis and catalytic fast pyrolysis, as well as liquids produced from hydrothermal liquefaction.

09 BIOMASS FUELS↗

Elemental Analysis of Bio-Oils by Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES). Laboratory Analytical Procedure (LAP), Issue Date: May 13, 2022

Concentrations of inorganic elements is a key quality metric for bio-oils as certain elements impact upgrading processes and product quality. Unless reduced or removed during production and processing, alkali and alkaline metals native to lignocellulosic biomass can carry over into bio-oils contributing to ash content and degraded catalyst performance during upgrading to hydrocarbon fuels or chemical products. Non-metallic elements such as sulfur and phosphorus can also negatively impact upgrading catalysts and product quality. Inductively coupled plasma optical emission spectroscopy (ICP-OES) can be used to measure inorganic elements of interest in bio-oils. This procedure covers the preparation and analysis of fast pyrolysis (FP) and catalytic fast pyrolysis (CFP) bio-oils. The concentrations of these elements can indicate potential bio-oil quality from the perspective of deoxygenation processes. The implications of elemental composition will depend on process parameters such as upgrading catalyst sensitivities. This Laboratory Analytical Procedure (LAP) covers two methods for quantification of inorganic elements by ICP-OES: Procedure A uses microwave assisted digestion with concentrated nitric acid, and Procedure B is an organic ICP-OES method utilizing a diglyme solvent.

09 BIOMASS FUELS↗

Determination of Carbon Functional Groups in Pyrolysis Bio-Oils using 13 C NMR: Laboratory Analytical Procedure (LAP)

Pyrolysis is a process that can be used to convert biomass to solid, liquid and gaseous products for use as renewable chemicals and fuels. The liquid fraction, known as “bio-oil” is complex and challenging to characterize, particularly by means of GC/MS, GPC, LC and FT-IR. NMR is capable of analyzing whole bio-oil samples and can provide quantitative results to characterize different functional groups or types of carbon present in bio-oil. This Laboratory Analytical Procedure (LAP) quantifies different carbon functional groups in whole bio-oil samples. This information can be used for comparisons between different pyrolysis experimental conditions or different upgrading processes and catalysts, and also allow for comparisons between bio-oils produced at different facilities.

09 BIOMASS FUELS↗

Determination of Carbon, Hydrogen, Nitrogen, and Oxygen in Bio-Oils: Laboratory Analytical Procedure (LAP)

The determination of total carbon, hydrogen, and nitrogen in bio-oils is important as these values can be used to track the carbon balance of production processes as well as calculate total oxygen content by difference. Oxygen content of bio-oils is a key metric for production and upgrading strategies as these are typically aimed at reducing oxygen. Oxygenates in bio-oils contribute to poor hydrocarbon miscibility, high acidity, high viscosity, and poor stability. Upgrading of bio-oils via deoxygenation produces hydrocarbons which can be used to generate feedstocks for renewable fuels and chemicals. In this Laboratory Analytical Procedure (LAP), combustion-based ultimate analysis is used to determine the weight percent (wt%) of C, H, and N in bio-oils and upgraded products. Ultimate analysis uses high temperatures and a pure oxygen environment to completely combust organic samples to carbon dioxide (CO 2 ), water (H 2 O), and nitrogen oxides (NO x ). In this procedure the amount of C and H in the sample are quantified by measuring resultant CO 2 and H 2 O with Fourier-transform infrared spectroscopy (FTIR). For N, NO x is reduced to nitrogen (N 2 ) which is measured with a thermal conductivity detector (TCD), providing total N content.

09 BIOMASS FUELS↗

Determination of Water Content in Bio-Oils by Volumetric Karl Fischer Titration: Laboratory Analytical Procedure (LAP)

The water content of bio-oils is a key metric for several reasons. Water is typically the most concentrated single component of fast pyrolysis oils, though this will be much lower in catalytic fast pyrolysis and upgraded products. Reduced water content is preferable in bio-oil as water can contribute to phase separation, corrosivity, and instability. Additionally, lower water is beneficial for physical properties such as energy density. The percentage of water can also be used to correct the calculation for organic oxygen when determining total oxygen content of bio-oils via combustion-based ultimate analysis. The procedure described here is specifically written for the analysis of bio-oils, and is based on ASTM E203, Standard Test Method for Water Using Volumetric Karl Fischer Titration. This standard test method is specified for measuring the mass % water in pyrolysis liquid biofuels in ASTM D7544, Standard Specification for Pyrolysis Liquid Biofuel. Although the standard method is prescribed for the analysis of pyrolysis liquids for use in industrial and commercial burners, the method is not specifically written for this product. The method described with this Laboratory Analytical Procedure (LAP) provides specific guidance for the analysis of bio-oils. Both organic and aqueous phases can be measured with this technique.

09 BIOMASS FUELS↗

A Corrected Score Function Framework for Modelling Circadian Gene Expression

Many biological processes display oscillatory behaviour based on an approximately 24 h internal timing system specific to each individual. One process of particular interest is gene expression, for which several circadian transcriptomic studies have identified associations between gene expression during a 24 h period and an individual's health. A challenge with analysing data from these studies is that each individual's internal timing system is offset relative to the 24 h day-night cycle, where day–night cycle time is recorded for each collected sample. Laboratory procedures can accurately determine each individual's offset and determine the internal time of sample collection. However, these laboratory procedures are labour-intensive and expensive. Here, in this paper, we propose a corrected score function framework to obtain a regression model of gene expression given internal time when the offset of each individual is too burdensome to determine. A feature of this framework is that it does not require the probability distribution generating offsets to be symmetric with a mean of zero. Simulation studies validate the use of this corrected score function framework for cosinor regression, which is prevalent in circadian transcriptomic studies. Illustrations with data from three circadian transcriptomic studies further demonstrate that the proposed framework consistently mitigates bias relative to using a score function that does not account for this offset.

59 BASIC BIOLOGICAL SCIENCES↗

Determination of Cellulosic Glucan Content in Starch Containing Feedstocks (Laboratory Analytical Procedure)

Carbohydrates make up a major portion of biomass samples. These carbohydrates are polysaccharides constructed primarily of glucose, xylose, arabinose, galactose, and mannose monomeric subunits. One such polysaccharide is starch, which is present in certain types of biomass. Starch will contribute to the overall glucose measurement when it breaks into the glucose subunit. Starch is often a more readily accessible source of glucose than structurally bound glucose polymers. Due to the different chemical nature of the glucan species, it is often advantageous to determine the amount of cellulosic glucose separately from the starch glucan.

09 BIOMASS FUELS↗