The determination of lead in 13 USGS standard rocks

P. J. Aruscavage; E.Y. Campbell

doi:10.1016/0039-9140(79)80018-1

Home/Archive/USGS

USGS · 70010344

The determination of lead in 13 USGS standard rocks

P. J. Aruscavage·E.Y. Campbell

View original source ↗Export metadata ↓

Abstract

Lead was determined in 13 U.S. Geological Survey standard rocks by graphite furnace atomization and atomic-absorption spectrometry after extraction of lead with diethylammonium diethyldithiocarbamic acid. An analysis of variance of the results obtained from a random sampling of three different bottles of each standard rock showed no heterogeneity among bottles, at the F0.95 level, for a 100-mg sample-size. The relative error of the method, based on the standard deviation of the mean within bottles, was generally less than 10%.

Explore related subjects

Talanta Article

Keep this discovery

Explore connections, maps & timelines

BibTeX RIS

P. J. Aruscavage, E.Y. Campbell. 1979. The determination of lead in 13 USGS standard rocks. https://doi.org/10.1016/0039-9140(79)80018-1

Cite the original work for its findings. Save a collection to share your selection of sources.

KEEP EXPLORING

Related USGS reports

USGS2025

Geographic determination of Pinus ponderosa using DART TOFMS, ICP-MS, and LIBS handheld analyzer

Due to legal requirements on international imports, it is important for law enforcement and regulatory agencies to identify the geographical provenance of timber. Current methods for geographic identification utilize data generated by direct analysis in real time time-of-flight mass spectrometry (DART TOFMS), genetics, and isotope-ratio mass spectrometry (IRMS), but identification methods based on genetics and IRMS data require months to years to create usable databases. This study used machine learning algorithms to compare the results of DART TOFMS, inductively coupled plasma mass spectrometry (ICP-MS), and a handheld laser-induced breakdown spectroscopy (LIBS) analyzer for use in geographic identification of five populations of Pinus ponderosa spaced between 14 to 72 km apart. The results of the study showed comparable performances from machine learning algorithms applied to the ICP-MS and LIBS data with accuracy and kappa values over 90% while the DART TOFMS had an accuracy of 76% and a kappa value of 70%. This study demonstrated that data from the LIBS handheld analyzer is a viable and intriguing alternative to ICP-MS and DART TOFMS analyses in generating training databases and further indicates that trace elemental analysis via ICP-MS is a promising method for generating databases used to identify the origin of timber.

California, Oregon↗

USGS2021

Comparison of detection limits estimated using single- and multi-concentration spike-based and blank-based procedures

Spike- and blank-based procedures were applied to estimate the detection limits (DLs) for example analytes from inorganic and organic methods for water samples to compare with the U.S. Environmental Protection Agency's (EPA) Method Detection Limit (MDL) procedures (revisions 1.11 and 2.0). The multi-concentration spike-based procedures ASTM Within-laboratory Critical Level (DQCALC) and EPA's Lowest Concentration Minimum Reporting Level were compared in one application, with DQCALC further applied to many methods. The blank-based DLs, MDL b99 (99th percentile) or MDL bY (= mean blank concentration + s × t ), estimated using large numbers (>100) of blank samples often provide DLs that better approach or achieve the desired ≤1% false positive risk level compared to spike-based DLs. For primarily organic methods that do not provide many uncensored blank results, spike-based DQCALC or MDL rev. 2.0 are needed to simulate the blank distribution and estimate the DL. DQCALC is especially useful for estimating DLs for multi-analyte methods having very different analyte response characteristics. Time series plots of DLs estimated using different procedures reveal that DLs are dependent on the applied procedure, should not be expected to be static over time, and seem best viewed as falling over a range versus being a single value. Use of both blank- and spike-based DL procedures help inform this DL range. Data reporting conventions that censor data at a threshold and report “less than” that threshold concentration as the reporting level have unknown and potentially high false negative risk. The U.S. Geological Survey National Water Quality Laboratory's Laboratory Reporting Level (LRL) convention (applied primarily to organic methods) attempts to simultaneously minimize both the false positive and false negative risk when <LRL is reported and data between DL and the higher LRL are allowed to be reported.

Talanta↗

USGS2019

Measurement of nutrients in saline and hypersaline waters by discrete analyzer colorimetry without matrix matched calibration standards

Automated, colorimetric analysis of nutrients in samples with high and variable salinity can be time consuming due to the need to matrix match calibration and reference solution matrices with those of samples—particularly when using flow-based analyzers that are prone to detector artifacts caused by optical inhomogeneities, “schlieren”, that form at interfaces between samples and deionized water carrier or wash solutions. Such detector artifacts do not occur in discrete analyzers. Here we report spike recoveries when nitrite, nitrite plus nitrate, ammonia, orthophosphate, and silica were determined in estuarine waters, seawater, and hypersaline surface water samples without calibrator matrix matching using an automated discrete analyzer set up with standard colorimetric methods. Salinities of these samples varied from 0 to 22 percent (%). Spike recoveries and precision were excellent for nitrite and nitrite plus nitrate analyses in samples with salinities up to 15%, for ammonia in samples with salinities up to about 1.7%, and for orthophosphate in samples with salinities up to about 3.5%. Orthophosphate spike recoveries were high biased in hypersaline matrices (salinity >3.5%), likely due to an unidentified sample matrix interference. After applying linear correction factors to account for chemistry-related salt effects, spike recoveries were acceptable for ammonia analyses in samples with salinities in the range of 1.7 to 3.5%, and for silica analyses in samples with salinities in the range of 0 to 3.5%.

Talanta↗