USGS Science⌕ Search

SEARCH · USGS Science

Results for “Techniques and Methods”

Search indexed USGS publications on groundwater, aquifers, geologic maps, mineral resources and earthquakes. Explore source records by subject and place.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 451 records · Page 25Linked to original sources

Estimating suspended sediment concentrations in turbid coastal waters of the Santa Barbara Channel with SeaWiFS

A technique is presented for estimating suspended sediment concentrations of turbid coastal waters with remotely sensed multi-spectral data. The method improves upon many standard techniques, since it incorporates analyses of multiple wavelength bands (four for Sea-viewing Wide Field of view Sensor (SeaWiFS)) and a nonlinear calibration, which produce highly accurate results (expected errors are approximately ±10%). Further, potential errors produced by erroneous atmospheric calibration in excessively turbid waters and influences of dissolved organic materials, chlorophyll pigments and atmospheric aerosols are limited by a dark pixel subtraction and removal of the violet to blue wavelength bands. Results are presented for the Santa Barbara Channel, California where suspended sediment concentrations ranged from 0–200+ mg l −1 (±20 mg l −1 ) immediately after large river runoff events. The largest plumes were observed 10–30 km off the coast and occurred immediately following large El Niño winter floods.

California↗

Combining split-beam and dual-frequency identification sonars to estimate abundance of anadromous fishes in the Roanoke River, North Carolina

Riverine hydroacoustic techniques are an effective method for evaluating abundance of upstream migrating anadromous fishes. To use these methods in the Roanoke River, North Carolina, at a wide site with uneven bottom topography, we used a combination of split-beam sonar and dual-frequency identification sonar (DIDSON) deployments. We aimed a split-beam sonar horizontally to monitor midchannel and near-bottom zones continuously over the 3-month spring monitoring periods in 2010 and 2011. The DIDSON was rotated between seven cross-channel locations (using a vertical aim) and nearshore regions (using horizontal aims). Vertical deployment addressed blind spots in split-beam coverage along the bottom and provided reliable information about the cross-channel and vertical distributions of upstream migrants. Using a Bayesian framework, we modeled sonar counts within four cross-channel strata and apportioned counts by species using species proportions from boat electrofishing and gill netting. Modeled estimates (95% credible intervals [CIs]) of total upstream migrants in 2010 and 2011 were 2.5 million (95% CI, 2.4–2.6 million) and 3.6 million (95% CI, 3.4–3.9 million), respectively. Results indicated that upstream migrants are extremely shore- and bottom-oriented, suggesting nearshore DIDSON monitoring improved the accuracy and precision of our estimates. This monitoring protocol and model may be widely applicable to river systems regardless of their cross-sectional width or profile.

North American Journal of Fisheries Management↗

The ecological limits of hydrologic alteration (ELOHA): A new framework for developing regional environmental flow standards

The flow regime is a primary determinant of the structure and function of aquatic and riparian ecosystems for streams and rivers. Hydrologic alteration has impaired riverine ecosystems on a global scale, and the pace and intensity of human development greatly exceeds the ability of scientists to assess the effects on a river-by-river basis. Current scientific understanding of hydrologic controls on riverine ecosystems and experience gained from individual river studies support development of environmental flow standards at the regional scale. 2. This paper presents a consensus view from a group of international scientists on a new framework for assessing environmental flow needs for many streams and rivers simultaneously to foster development and implementation of environmental flow standards at the regional scale. This framework, the ecological limits of hydrologic alteration (ELOHA), is a synthesis of a number of existing hydrologic techniques and environmental flow methods that are currently being used to various degrees and that can support comprehensive regional flow management. The flexible approach allows scientists, water-resource managers and stakeholders to analyse and synthesise available scientific information into ecologically based and socially acceptable goals and standards for management of environmental flows. 3. The ELOHA framework includes the synthesis of existing hydrologic and ecological databases from many rivers within a user-defined region to develop scientifically defensible and empirically testable relationships between flow alteration and ecological responses. These relationships serve as the basis for the societally driven process of developing regional flow standards. This is to be achieved by first using hydrologic modelling to build a 'hydrologic foundation' of baseline and current hydrographs for stream and river segments throughout the region. Second, using a set of ecologically relevant flow variables, river segments within the region are classified into a few distinctive flow regime types that are expected to have different ecological characteristics. These river types can be further subclassified according to important geomorphic features that define hydraulic habitat features. Third, the deviation of current-condition flows from baseline-condition flow is determined. Fourth, flow alteration-ecological response relationships are developed for each river type, based on a combination of existing hydroecological literature, expert knowledge and field studies across gradients of hydrologic alteration. 4. Scientific uncertainty will exist in the flow alteration-ecological response relationships, in part because of the confounding of hydrologic alteration with other important environmental determinants of river ecosystem condition (e.g. temperature). Application of the ELOHA framework should therefore occur in a consensus context where stakeholders and decision-makers explicitly evaluate acceptable risk as a balance between the perceived value of the ecological goals, the economic costs involved and the scientific uncertainties in functional relationships between ecological responses and flow alteration. 5. The ELOHA framework also should proceed in an adaptive management context, where collection of monitoring data or targeted field sampling data allows for testing of the proposed flow alteration-ecological response relationships. This empirical validation process allows for a fine-tuning of environmental flow management targets. The ELOHA framework can be used both to guide basic research in hydroecology and to further implementation of more comprehensive environmental flow management of freshwater sustainability on a global scale. ?? 2009 Blackwell Publishing Ltd.

Freshwater Biology↗

Movements of yellow perch marked in southern Green Bay, Lake Michigan, in 1950

To obtain information on the post-spawning movements of yellow perch that spawn in southern Green Bay, Lake Michigan, 4,172 fish caught in drop nets were marked by tagging with monel-metal strap tags attached to the right operculum and 24,799 were marked by clipping off the second or membranous dorsal fin. Marking was done during the period from May 3 to 17, 1950, at six main stations, all located in the southern end of Green Bay. The average length of the tagged perch was 7.3 inches and all fell within the range 5.5–14.4 inches. Most (90.9 percent) of the fish were below the minimum legal length of 8.0 inches. The follow-up procedure consisted of informing commercial and sports fishermen of the program and enlisting their cooperation in watching for marked fish; accounts of the investigation were released through newspapers and descriptive posters were distributed. The personnel connected with the investigation examined catches frequently. The large majority (101 or 79.5 percent) of the 127 tagged perch recaptured in the experimental nets during the marking operations were retaken at the tagging station at which they were released. Of the 108 tagged perch captured by commercial fishermen and anglers following the opening of the season on May 20, 96 were taken by drop nets, 6 by gill nets, and 6 by hook and line. The mean lengths for the three groups were 7.7, 7.1, and 9.25 inches, respectively. All recoveries were made in the Wisconsin waters of Green Bay. Most of the “open-season” recoveries (86 fish; 79.6 percent) were made during the period May 20-May 31. Recaptures during subsequent months were: June–14; July–7; August–none; September–1. Of the 86 perch recaptured May 20–31, 70 were retaken inside and 16 outside the tagging area. The majority (14 of 22) of those recovered after May 31 were retaken outside the tagging area. The average length of the 20 tagged yellow perch recaptured by drop nets (data restricted to fish from a single type of net to avoid bias from gear selectivity) outside the tagging area (8.42 inches) was 0.96 inch greater than the mean length (7.46 inches) of the 76 fish retaken inside the area. This statistically highly significant difference lends support to the belief of commercial fishermen that the larger of the yellow perch that spawn in southern Green Bay move out soon after spawning. The percentage of recapture of tagged perch increased sharply with increase in the size of the fish. Not one of 169 tagged fish less than 6.5 inches long was recovered. The rates of recapture at greater lengths were: 6.5 to 8.9 inches–2.5 percent; 9.0 to 9.9 inches–11.4 percent; 10.0 to 14.4 inches–16.7 percent. Among the several factors suggested in explanation of this relationship, the most important appear to be the lesser ability of the smaller fish to survive the rigors of handling and tagging, greater loss of tags from the smaller fish, and the greater likelihood of overlooking the smaller of the tagged fish in the sorting of the catch. The factors just mentioned and the lack of knowledge of the efficiency of measures taken to obtain records of recoveries preclude the 2.6-percent return of all tagged fish from being accepted as an approximation of the rate of recapture. Neither should the 6.6-percent return of tagged fish of legal size (8 inches and longer) be taken as an estimate of the rate of exploitation. Although 465 fin-clipped perch were recovered in the experimental nets during the marking operations, only 68 of 24,799 fish so marked were recovered after the fishing season opened. All but one of these 68 were retaken near the point of marking. The difficulty of detecting a perch with a missing membranous dorsal is believed to be a major cause of the poor returns from fin-clipped fish. These investigations have demonstrated that for studying migration of yellow perch, tagging is superior to fin-clipping as a method of marking. The technique of the tagging, however, needs to be improved, and better means must be found to trace tagged fish of small size. Furthermore certain small regions in the bay not at present open to commercial fishing must be explored in order to obtain more comprehensive information as to migration.

Transactions of the American Fisheries Society↗

Estimating survival rates with time series of standing age‐structure data

It has long been recognized that age‐structure data contain useful information for assessing the status and dynamics of wildlife populations. For example, age‐specific survival rates can be estimated with just a single sample from the age distribution of a stable, stationary population. For a population that is not stable, age‐specific survival rates can be estimated using techniques such as inverse methods that combine time series of age‐structure data with other demographic data. However, estimation of survival rates using these methods typically requires numerical optimization, a relatively long time series of data, and smoothing or other constraints to provide useful estimates. We developed general models for possibly unstable populations that combine time series of age‐structure data with other demographic data to provide explicit maximum likelihood estimators of age‐specific survival rates with as few as two years of data. As an example, we applied these methods to estimate survival rates for female bison ( Bison bison ) in Yellowstone National Park, USA. This approach provides a simple tool for monitoring survival rates based on age‐structure data.

Ecology↗

Management of predator populations with antifertility agents

The search for methods, other than lethal techniques, for controlling predatory animals causing economic losses to the livestock industry prompted investigation of antifertility agents to suppress reproduction. Diethylstilbestrol was selected for initial trials because of its demonstrated antifertility effect on rabbits, mink ( Mustela vison ), dogs, and cattle. In penned tests with stilbestrol, pregnancy was terminated in six coyotes ( C anis latrans ) fed a single 100-mg oral dose dissolved in tallow. A subsequent field trial was conducted in New Mexico on 20 townships, March 5-15, 1963. Five thousand (100 mg stilbestrol in ½ ounce of tallow) drop baits were placed wherever coyote sign was found. After a delay of 3 weeks to allow the drug to take effect, a collection of female tracts from the treated area and a reference area 25 miles away was made to measure and compare reproductive success. Of the 20 females in reproductive condition recovered from the treated area, only 4 had viable embryos, while reproduction was blocked in 16 specimens by failure of implantation or resorption of embryos. All of the 13 females in reproductive condition from the reference area would have produced pups as evidenced by viable embryos. Future tests are scheduled to determine effects on other species and to confirm results on coyotes under a variety of field conditions.

Journal of Wildlife Management↗

The 3D Elevation Program and energy for the Nation

High-resolution light detection and ranging (lidar) data are used in energy infrastructure siting, design, permitting, construction, and monitoring to promote public safety through the reduction of risks. For example, lidar data are used to identify safe locations for energy infrastructure by analyzing terrain parameters and identifying and evaluating geologic hazards (for example, landslide and fault locations) and their potential public safety effects on the location or design of infrastructure. Increasingly, engineering companies and regulatory agencies are using lidar and other remote sensing techniques as an efficient method to collect accurate, comprehensive data while reducing risks to field personnel. The U.S. Geological Survey (USGS) 3D Elevation Program (3DEP) is collecting lidar data nationwide (interferometric synthetic aperture radar [IfSAR] data in Alaska) to support a wide range of applications, including projects related to energy infrastructure construction and safety. Renewable energy resources, resource mining, and oil and gas resources were identified by the National Enhanced Elevation Assessment as business uses requiring three-dimensional (3D) elevation data. Elevation data are critical in assessing potential sites for energy infrastructure, such as pipelines, refineries and other facilities, to mitigate risks from natural hazards. For example, the Federal Energy Regulatory Commission (FERC), an independent agency that regulates the interstate transmission of electricity, natural gas, and oil, uses enhanced elevation data to conduct National Environmental Policy Act (NEPA) compliance assessments. The acquisition of high-resolution lidar data by the USGS 3DEP initiative helps the FERC and NEPA permit applicants by providing accurate and consistent data for hazards analysis. The use of these data accelerates the application and review process and avoids the much higher costs of acquiring elevation data along proposed energy facility locations and pipeline corridors.

Fact Sheet↗

Preliminary report on the geology of the continental borderland of Southern California

Appraisal of the mineral resource potential and assessment of environmental problems of any specific area require an understanding of the regional geology. The geology of t he coastal zone and offshore islands from Point Conception to the Mexican boundary serves as a frame of reference from which rock units and structures can be extrapolated into submerged parts of the borderland (sheet 1). Such extrapolations should be used with caution, for the tectonic evolution and depositional history of parts of the borderland may not have paralleled those of the mainland. On shore, rocks and structures c an be observed directly with supplemental aid from deep drill holes; but in areas covered by deep water, only indirect techniques such as geophysical methods and shallow coring provide information from which geologic intepretations can be made.

California↗

Modeling the Spatial and Temporal Variation of Monthly and Seasonal Precipitation on the Nevada Test Site and Vicinity, 1960-2006

The Nevada Test Site (NTS), located in the climatic transition zone between the Mojave and Great Basin Deserts, has a network of precipitation gages that is unusually dense for this region. This network measures monthly and seasonal variation in a landscape with diverse topography. Precipitation data from 125 climate stations on or near the NTS were used to spatially interpolate precipitation for each month during the period of 1960 through 2006 at high spatial resolution (30 m). The data were collected at climate stations using manual and/or automated techniques. The spatial interpolation method, applied to monthly accumulations of precipitation, is based on a distance-weighted multivariate regression between the amount of precipitation and the station location and elevation. This report summarizes the temporal and spatial characteristics of the available precipitation records for the period 1960 to 2006, examines the temporal and spatial variability of precipitation during the period of record, and discusses some extremes in seasonal precipitation on the NTS.

Open-File Report↗

Methodology and technical input for the 2025 U.S. List of Critical Minerals—Assessing the potential effects of mineral commodity supply chain disruptions on the U.S. economy

The Secretary of the Interior, acting through the Director of the U.S. Geological Survey, is tasked by section 7002 (“Mineral Security”) of title VII (“Critical Minerals”) of the Energy Act of 2020 (Public Law 116–260, December 27, 2020, 116th Congress) with reviewing and revising the methodology used to evaluate mineral commodity supply risk and the U.S. List of Critical Minerals (LCM) no less than every 3 years. Following two previous LCM assessments, this analysis represents the latest technical input for evaluating each mineral commodity’s supply risk and determining their recommended status on the LCM. We evaluated mineral commodity supply risk using two criteria: (1) an economic effects assessment that quantified the potential effects of various trade disruption scenarios on the U.S. economy, and (2) an examination of whether the mineral commodity’s U.S. supply chain relied on a sole domestic producer that represented a single point of failure. For the first criterion, postdisruption equilibrium quantities and prices for each mineral commodity were calculated based on their price elasticities of supply and demand and the availability of excess production capacity for each yearlong foreign trade disruption scenario. Subsequently, a nonlinear optimization routine was used with detailed economic input-output tables to estimate the potential economic effects on the U.S. economy of over 1,200 scenarios for 84 mineral commodities. After accounting for the probability of each scenario’s occurrence, the overall results are presented in terms of changes in U.S. gross domestic product (GDP) by individual industry and the economy overall. The results, which ranged from a net decrease in U.S. GDP of nearly $4.5 billion to a net increase of $33 million, largely reflect U.S. import dependency and world production concentration. Using the Jenks natural breaks optimization method, a statistical classification technique, we categorized the mineral commodities into several classes based on this overall risk quantification. Mineral commodities with annualized probability-weighted net decreases in U.S. GDP greater than $2 million were recommended for inclusion on the LCM. If a mineral commodity did not meet the threshold for inclusion on the LCM under the first criterion, its domestic supply chain was examined under the second criterion, which recommended a mineral commodity for inclusion on the LCM if there was only a single domestic producer. Ultimately, the two criteria resulted in the recommendation of the addition of six mineral commodities (in descending risk order, potash, silicon, copper, silver, rhenium, and lead) to and the removal of two mineral commodities (arsenic and tellurium) from the LCM. By using an economic effects assessment, the results of this analysis provide a prioritization that can also be compared directly against other risk analyses and the cost of various risk mitigation strategies.

Open-File Report↗

Computational considerations for collecting and using data in the equidistant cylindrical map projection and the bounds of sampling geographic data at progressively higher resolution

The Equidistant Cylindrical Map projection is popular with digital modelers and others for storing and processing worldwide data sets because of the simple association of latitude and longitude to cell values or pixels in the resulting grid. This projection does not accurately display area, and the diminished geographic area represented by cells at high latitudes is not often carefully considered. A simple mathematical analysis quantifies the discrepancy in area sampled by cells at different latitudes. The presence of this discrepancy indicates that the use of this projection can induce bias in data sets when both sampling and reporting data. It is demonstrated that as the resolution requirements of input data for models increase, the necessity of providing data to accurately describe smaller cells, particularly at high latitude, will be a challenge.

Techniques and Methods↗

Determination of the δ 34 S of sulfate in water; RSIL lab code 1951

The purpose of the Reston Stable Isotope Laboratory (RSIL) lab code 1951 is to determine the δ( 34 S/ 32 S), abbreviated as δ 34 S, of dissolved sulfate. Dissolved sulfate is collected in the field and precipitated with BaCl 2 at pH 3 to 4 as BaSO 4 in the laboratory. However, the dissolved organic sulfur (DOS) is oxidized to SO 2 , and the carbonate is acidified to CO 2 . Both are degassed from the water sample before the sulfate is precipitated. The precipitated BaSO 4 is filtered and dried before introduction into an elemental analyzer (EA) Carlo Erba NC 2500. The EA is used to convert sulfur in a BaSO 4 solid sample into SO 2 gas, and the EA is connected to a continuous flow isotope-ratio mass spectrometer (CF-IRMS), which determines the differences in the isotope-amount ratios of stable sulfur isotopes ( 34 S/ 32 S) of the product SO 2 gas. The combustion is quantitative; no isotopic fractionation is involved. Samples are placed in a tin capsule and loaded into the Costech Zero Blank Autosampler of the EA. Under computer control, samples are dropped into a heated tube reaction tube that combines the oxidation and reduction reactions. The combustion takes place in a helium atmosphere containing an excess of oxygen gas at the oxidation zone at the top of the reaction tube. Combustion products are transported by a helium carrier through the reduction zone at the bottom of the reaction tube to remove excess oxygen and through a separate drying tube to remove any water. The gas-phase products, mainly CO 2 , N 2 , and SO 2 , are separated by a gas chromatograph. The gas is then introduced into the isotope-ratio mass spectrometer (IRMS) through a Finnigan MAT (now Thermo Scientific) ConFlo II interface, which also is used to inject SO 2 reference gas and helium for sample dilution. The IRMS is a Thermo Scientific Delta V Plus CF-IRMS. It has a universal triple collector with two wide cups and a narrow cup in the middle. It is capable of measuring mass/charge ( m/z ) 64 and 66 simultaneously. The ion beams from SO 2 are as follows: m/z 64 = SO 2 = 32 S 16 O 16 O; m/z 66 = SO 2 = 34 S 16 O 16 O primarily.

Techniques and Methods↗

Determination of the δ 15 N of total nitrogen in solids; RSIL lab code 2893

The purpose of the Reston Stable Isotope Laboratory (RSIL) lab code 2893 is to determine the δ( 15 N/ 14 N), abbreviated as δ 15 N , of total nitrogen in solid samples. A Carlo Erba NC 2500 elemental analyzer (EA) is used to convert total nitrogen in a solid sample into N 2 gas. The EA is connected to a continuous flow isotope-ratio mass spectrometer (CF-IRMS), which determines relative difference in the isotope-amount ratios of stable nitrogen isotopes ( 15 N/ 14 N)of the product N 2 gas. The combustion is quantitative; no isotopic fractionation is involved. Samples are placed in a tin capsule and loaded into the Costech Zero Blank Autosampler of the EA. Under computer control, samples are dropped into a heated reaction tube that contains an oxidant, where the combustion takes place in a helium atmosphere containing an excess of oxygen gas. Combustion products are transported by a helium carrier through a reduction tube to remove excess oxygen and convert all nitrous oxides into N 2 and through a drying tube to remove water. The gas-phase products, mainly CO 2 and N 2 , are separated by a gas chromatograph. The gas is then introduced into the isotope-ratio mass spectrometer (IRMS) through a Finnigan MAT (now Thermo Scientific) ConFlo II interface, which also is used to inject N 2 reference gas and helium for sample dilution. The IRMS is a Thermo Scientific Delta V Plus CF-IRMS. It has a universal triple collector, two wide cups with a narrow cup in the middle, capable of measuring mass/charge ( m/z ) 28, 29, 30, simultaneously. The ion beams from N 2 are as follows: m/z 28 = N 2 = 14 N 14 N; m/z 29 = N 2 = 14 N 15 N primarily; m/z 30 = NO = 14 N 16 O primarily, which is a sign of contamination or incomplete reduction.

Techniques and Methods↗

Determination of the delta(15N/14N)of Ammonium (NH4+) in Water: RSIL Lab Code 2898

The purpose of the technique described by Reston Stable Isotope Laboratory (RSIL) lab code 2898 is to determine the N isotopic composition, delta(15N/14N), abbreviated as d15N, of ammonium (NH4+) in water (freshwater and saline water). The procedure involves converting dissolved NH4+ into NH3 gas by raising the pH of the sample to above 9 with MgO and subsequently trapping the gas quantitatively as (NH4)2SO4 on a glass fiber (GF) filter. The GF filter is saturated with NaHSO4 and pressure sealed between two gas-permeable polypropylene filters. The GF filter 'sandwich' floats on the surface of the water sample in a closed bottle. NH3 diffuses from the water through the polypropylene filter and reacts with NaHSO4, forming (NH4)2SO4 on the GF filter. The GF filter containing (NH4)2SO4 is dried and then combusted with a Carlo Erba NC 2500 elemental analyzer (EA), which is used to convert total nitrogen in a solid sample into N2 gas. The EA is connected to a continuous-flow isotope-ratio mass spectrometer (CF-IRMS), which determines the relative difference in ratios of the amounts of the stable isotopes of nitrogen (15N and 14N) of the product N2 gas and a reference N2 gas. The filters containing the samples are compressed in tin capsules and loaded into a Costech Zero-Blank Autosampler on the EA. Under computer control, samples then are dropped into a heated reaction tube that contains an oxidant, where combustion takes place in a He atmosphere containing an excess of O2 gas. To remove S-O gases produced from the NaHSO4, a plug of Ag-coated Cu wool is inserted at the bottom of the reaction tube. Combustion products are transported by a He carrier through a reduction furnace to remove excess O2, toconvert all nitrogen oxides to N2, and to remove any remaining S-O gases. The gases then pass through a drying tube to remove water. The gas-phase products, mainly N2 and a small amount of background CO2, are separated by a gas chromatograph (GC). The gas is then introduced into the IRMS through a Finnigan ConFlo II interface. The ConFlo II interface is used to introduce not only sample into the IRMS but also N2 reference gas and He for sample dilution. The flash combustion is quantitative, so no isotopic fractionation is involved. The IRMS is a Finnigan Delta V CF-IRMS with 10 cups and is capable of detecting ion beams with mass/charge (m/z) 28, 29, 30. The ion beams from N2 are as follows: m/z 28 = 14N14N, m/z 29 = 14N15N, and m/z 30 = 15N15N. The ion beam with m/z 30 also represents 14N16O, which may indicate contamination or incomplete reduction.

Techniques and Methods↗

Determination of the δ 15 N of nitrate in water; RSIL lab code 2899

The purpose of the Reston Stable Isotope Laboratory (RSIL) lab code 2899 is to determine the δ 15 N of nitrate (NO 3 - ) in water. The δ 15 N of the dissolved NO 3 - is analyzed by conversion of the NO 3 - to nitrous oxide (N 2 O), which serves as the analyte for mass spectrometry. A culture of denitrifying bacteria is used in the enzymatic conversion of the NO 3 - to N 2 O, which follows the pathway shown in equation 1: NO 3 - → NO 2 - → NO → 1/2 N 2 O (1) Because the bacteria Pseudomonas aureofaciens lack N 2 O reductive activity, the reaction stops at N 2 O, unlike the typical denitrification reaction that goes to N 2 . After several hours, the conversion is complete, and the N 2 O is extracted from the vial, separated from volatile organic vapor and water vapor by an automated -65 °C isopropanol-slush trap, a Nafion drier, a CO 2 and water removal unit (Costech #021020 carbon dioxide absorbent with Mg(ClO 4 ) 2 ), and trapped in a small-volume trap immersed in liquid nitrogen with a modified Finnigan MAT (now Thermo Scientific) GasBench 2 introduction system. After the N 2 O is released, it is further purified by gas chromatography before introduction to the isotope-ratio mass spectrometer (IRMS). The IRMS is a Thermo Scientific Delta V Plus continuous flow IRMS (CF-IRMS). It has a universal triple collector, consisting of two wide cups with a narrow cup in the middle; it is capable of simultaneously measuring mass/charge ( m/z ) of the N 2 O molecule 44, 45, and 46. The ion beams from these m/z values are as follows: m/z = 44 = N 2 O = 14 N 14 N 16 O; m/z = 45 = N 2 O = 14 N 15 N 16 O or 14 N 14 N 17 O; m/z = 46 = N 2 O = 14 N 14 N 18 O. The 17 O contributions to the m/z 44 and m/z 45 ion beams are accounted for before δ 15 N values are reported.

Techniques and Methods↗

Determination of the δ 15 N and δ 18 O of nitrate in water; RSIL lab code 2900

The purpose of the Reston Stable Isotope Laboratory (RSIL) lab code 2900 is to determine the δ 15 N and δ 18 O of nitrate (NO 3 - ) in water. The δ 15 N and δ 18 O of the dissolved NO 3 - are analyzed by converting the NO 3 - to nitrous oxide (N 2 O), which serves as the analyte for mass spectrometry. A culture of denitrifying bacteria is used in the enzymatic conversion of the NO 3 - to N 2 O, which follows the pathway shown in equation 1: NO 3 - → NO 2 - → NO → 1/2 N 2 O (1) Because the bacteria Pseudomonas aureofaciens lack N 2 O reductive activity, the reaction stops at N 2 O, unlike the typical denitrification reaction that goes to N 2 . After several hours, the conversion is complete, and the N 2 O is extracted from the vial, separated from volatile organic vapor and water vapor by an automated -65 °C isopropanol-slush trap, a Nafion drier, a CO 2 and water removal unit (Costech #021020 carbon dioxide absorbent with Mg(ClO 4 ) 2 ), and trapped in a small-volume trap immersed in liquid nitrogen with a modified Finnigan MAT (now Thermo Scientific) GasBench 2 introduction system. After the N 2 O is released, it is further purified by gas chromatography before introduction to the isotope-ratio mass spectrometer (IRMS). The IRMS is a Thermo Scientific Delta V Plus continuous flow IRMS (CF-IRMS). It has a universal triple collector, consisting of two wide cups with a narrow cup in the middle; it is capable of simultaneously measuring mass/charge ( m/z ) of the N 2 O molecule 44, 45, and 46. The ion beams from these m/z values are as follows: m/z = 44 = N 2 O = 14 N 14 N 16 O; m/z = 45 = N 2 O = 14 N 15 N 16 O or 14 N 14 N 17 O; m/z = 46 = N 2 O = 14 N 14 N 18 O. The 17 O contributions to the m/z 44 and m/z 45 ion beams are accounted for before δ 15 N values are reported.

Techniques and Methods↗

Determination of the δ 34 S of Total Sulfur in Solids: RSIL Lab Code 1800

The purpose of Reston Stable Isotope Laboratory Lab (RSIL) Code 1800 is to determine the δ( 34 S/ 32 S), abbreviated as δ 34 S, of total sulfur in a solid sample. A Carlo Erba NC 2500 elemental analyzer (EA) is used to convert total sulfur in a solid sample into SO 2 gas. The EA is connected to a continuous flow isotope-ratio mass spectrometer (CF-IRMS), which determines the relative difference in stable sulfur isotope-amount ratio ( 34 S/ 32 S) of the product SO 2 gas. The combustion is quantitative; no isotopic fractionation is involved. Samples are placed in tin capsules and loaded into a Costech Zero-Blank Autosampler on the EA. Under computer control, samples are dropped into a heated tube reaction tube that combines both the oxidation and the reduction reactions. The combustion takes place in a He atmosphere that contains an excess of oxygen gas at the oxidation zone at the top of the reaction tube. Combustion products are transported by a He carrier through the reduction zone at the bottom of the reaction tube to remove excess oxygen and through a separate drying tube to remove any water. The gas-phase products, mainly CO 2 , N 2 , and SO 2 , are separated by a gas chromatograph (GC). The gas is then introduced into the isotope-ratio mass spectrometer (IRMS) through a Thermo-Finnigan ConFlo II interface, which also is used to inject SO 2 reference gas and He for sample dilution. The IRMS is a Thermo-Finnigan DeltaPlus CF-IRMS. It has a universal triple collector with two wide cups and a narrow cup in the middle. It is capable of measuring mass/charge ( m/z ) 64 and 66 simultaneously. The ion beams from SO 2 are as follows: m/z 64 = SO 2 = 32 S 16 O 16 O; and m/z 66 = SO 2 = 34 S 16 O 16 O primarily.

Techniques and Methods↗

Determination of the δ 15 N and δ 13 C of total nitrogen and carbon in solids; RSIL lab code 1832

The purpose of the Reston Stable Isotope Laboratory (RSIL) lab code 1832 is to determine the δ( 15 N/ 14 N), abbreviated as δ 15 N, and the δ( 13 C/ 12 C), abbreviated as δ 13 C, of total nitrogen and carbon in a solid sample. A Carlo Erba NC 2500 elemental analyzer (EA) is used to convert total nitrogen and carbon in a solid sample into N 2 and CO 2 gas. The EA is connected to a continuous flow isotope-ratio mass spectrometer (CF-IRMS), which determines the relative difference in stable nitrogen isotope-amount ratio ( 15 N/ 14 N) of the product N 2 gas and the relative difference in stable carbon isotope-amount ratio ( 13 C/ 12 C) of the product CO 2 gas. The combustion is quantitative; no isotopic fractionation is involved. Samples are placed in tin capsules and loaded into a Costech Zero Blank Autosampler on the EA. Under computer control, samples then are dropped into a heated reaction tube that contains an oxidant, where combustion takes place in a helium atmosphere containing an excess of oxygen gas. Combustion products are transported by a helium carrier through a reduction furnace to remove excess oxygen and to convert all nitrous oxides into N 2 and through a drying tube to remove water. The gas-phase products, mainly CO 2 and N 2 , are separated by a gas chromatograph. The gas is then introduced into the IRMS through a Finnigan MAT (now Thermo Scientific) ConFlo II interface. The Finnigan MAT ConFlo II interface is used for introducing not only sample into the IRMS but also N 2 and CO 2 reference gases and helium for sample dilution. The flash combustion is quantitative; no isotopic fractionation is involved. The IRMS is a Thermo Scientific Delta V CF-IRMS. It has a universal triple collector, two wide cups with a narrow cup in the middle; it is capable of measuring mass/charge ( m/z ) 28, 29, 30 or with a magnet current change 44, 45, 46, simultaneously. The ion beams from these m/z values are as follows: m/z 28 = N 2 = 14 N/ 14 N; m/z 29 = N 2 = 14 N/ 15 N primarily; m/z 30 = NO = 14 N/ 16 O primarily, which is a sign of contamination or incomplete reduction; m/z 44 = CO 2 = 12 C 16 O 16 O; m/z 45 = CO 2 = 13 C 16 O 16 O primarily; and m/z 46 = CO 2 = 12 C 16 O 18 O primarily.

Techniques and Methods↗