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PubMed2005

137Cs measurement uncertainties and detection limits for airborne gamma spectrometry (AGS) data analysed using a spectral windows method.

The uncertainties associated with airborne gamma spectrometry (AGS) measurements analysed using a spectral windows method, and associated detection limits, have been investigated. For individual short measurements over buried 137Cs activity detection limits of 10 kBq m(-2) are achieved. These detection limits are reduced for superficial activity and longer integration times. For superficial activity, detection limits below 1 kBq m(-2) are achievable. A comparison is made with the detection limits for other data processing methods.

Journal Article↗

PubMed2002

Synthesis of electron energy loss spectra for the quantification of detection limits.

We describe a method for predicting detection limits of minority elements in electron energy loss spectroscopy (EELS), and its implementation as a software package that gives quantitative predictions for user-specified materials and experimental conditions. The method is based on modeling entire energy loss spectra, including shot noise as well as instrumental noise, and taking into account all the relevant experimental parameters. We describe the steps involved in modeling the entire spectrum, from the zero loss up to inner shell edges, and pay particular attention to the contributions to the pre-edge background. The predicted spectra are used to evaluate the signal-to-noise ratios (SNRs) for inner shell edges from user-specified minority elements. The software also predicts the minimum detectable mass (MDM) and minimum mass fraction (MMF). It can be used to ascertain whether an element present at a particular concentration should be detectable for given experimental conditions, and also to quickly and quantitatively explore ways of optimizing the experimental conditions for a particular EELS analytical task. We demonstrate the usefulness of the software by confirming the recent empirical observation of single atom detection using EELS of phosphorus in thin carbon films, and show the effect on the SNR of varying the acquisition parameters. The case of delta-doped semiconductors is also considered as an important example from materials science where low detection limits and high spatial resolution are essential, and the feasibility of such characterization using EELS is assessed.

Calcium↗

PubMedDate not supplied

The use of method detection limits in environmental measurements.

Environmental measurements often produce values below the method detection limit (MDL). Because low or zero values may be used in determining compliance with regulatory limits, in determining emission factors (typical concentrations emitted by a given type of source), or in modeling efforts, there is considerable interest in methods for determining detection limits and in procedures for using MDLs in summary statistics. Selection of methods for determining detection limits and treatment of MDL data should depend on the end-use of the data. The MDL should be determined in the environmental matrix that contains the analyte of interest. Treatment of missing values (values below the MDL) should be specified before the initiation of a measurement effort. When calculating a mean value for a source or area, one approach is to set the missing values at the MDL. This approach is appropriate when there are significant risks associated with incorrectly assuming a low level of a toxic compound; this method of summarizing data introduces a positive bias. Missing values may be assumed to equal zero if there is not a high risk of overlooking a hazard; this method produces a negative bias. However, if enough measurement data are available and the distribution of these data can be established then look-up tables can be used to estimate missing values, using statistically based estimates, without introducing high or low biases in a calculated mean.

Environmental Monitoring↗

PubMed2003

Rotating disk potentiometry for inner solution optimization of low-detection-limit ion-selective electrodes.

The extent of optimization of the lower detection limit of ion-selective electrodes (ISEs) can be assessed with an elegant new method. At the detection limit (i.e., in the absence of primary ions in the sample), one can observe a reproducible change in the membrane potential upon alteration of the aqueous diffusion layer thickness. This stir effect is predicted to depend on the composition of the inner solution, which is known to influence the lower detection limit of the potentiometric sensor dramatically. For an optimized electrode, the stir effect is calculated to be exactly one-half the value of the case when substantial coextraction occurs at the inner membrane side. In contrast, there is no stir effect when substantial ion exchange occurs at the inner membrane side. Consequently, this experimental method can be used to determine how well the inner filling solution has been optimized. A rotating disk electrode was used in this study because it provides adequate control of the aqueous diffusion layer thickness. Various ion-selective membranes with a variety of inner solutions that gave different calculated concentrations of the complex at the inner membrane side were studied to evaluate this principle. They contained the well-examined silver ionophore O,O' '-bis[2-(methylthio)ethyl]-tert-butylcalix[4]arene, the potassium ionophore valinomycin, or the iodide carrier [9]mercuracarborand-3. Stir effects were determined in different background solutions and compared to theoretical expectations. Correlations were good, and the results encourage the use of such stir-effect measurements to optimize ISE compositions for real-world applications. The technique was also found to be useful in estimating the level of primary ion impurities in the sample. For an iodide-selective electrode measured in phosphoric acid, for example, apparent iodide impurity levels were calculated as 5 x 10(-10) M.

Ion-Selective Electrodes↗

PubMed1978

Experimental optimization of the detection limit of one-step solid-phase radioimmunoassay.

The minimal detection limit and the conditions of maximal sensitivity of a one-step solid-phase inhibition radioimmunoassay for human immunoglobulin A have been determined by application of statistical methods of experimental optimization. The choice of the optimal combination of qualitative variables, such as the origin of the antibody and the nature of the solid phase, was made by the study of a covariable under non-optimal conditions of the quantitative variables, such as the amount of antibody. The covariable was the avidity of the antibody, which is expected to have a large influence on the sensitivity. Only the difference in avidity between two immunosorbents with cellulose or Sepharose as solid-phase material proved to be statistically significant, and further study was done with cellulose. The experimental optimization of the sensitivity as a function of five quantitative variables yielded a reduction of the detection limit by a factor 5.6 (from 23.5 to 4.2 ng IgA). The variables determining the amount of insolubilized antibody in the assay had the largest influence on the value of the detection limit. The conditions of optimal sensitivity did agree with the predictions by a physical model of radioimmunoassay. The results are discussed in relation to the assay parameters such as the amount and the avidity of the insolubilized antibody and the initial percentage of binding, and in relation with theoretical optimization of the sensitivity.

Animals↗

PubMed2006

Estimation of microbial growth using population measurements subject to a detection limit.

In this paper we develop a maximum likelihood estimation procedure for determining the mean and variance in microbial population size from microbial population measurements subject to a detection limit. Existing estimation methods generally set non-detectable measurements equal to the detection limit and are highly biased. Because changes in the mean and variance in the microbial population size are typical in industrial processes we also outline statistical tests for detecting such changes when measurements are subject to a detection limit, which is critical for process control. In an industrial process there may also potentially be variability in the microbial growth rate due to variation in the microbial strain, environment, and food characteristics. Accordingly, we also present a maximum likelihood procedure for estimating microbial growth model parameters and their variance components from microbial population measurements subject to a detection limit. Such information can be used to generate the mean and variance through time of the microbial population size, which is vital for the application of predictive microbiological models to risk assessment and food product shelf-life estimation.

Bacteria↗

PubMed1994

Evaluation of the detection limits of PCR for identification of Mycoplasma pneumoniae in clinical samples.

The detection limits of the polymerase chain reaction (PCR) for Mycoplasma pneumoniae were determined using specimens from persons known to have had M. pneumoniae pneumonia. Four primers were selected from the known sequence of the P1 gene. The primer pair (P1-178 and P1-809) which generates a 631 fragment gave the lowest detection limit. Nineteen of 21 throat swabs, which contained between 0.06 and 2 colony-forming units (CFU) per microlitre, from culture positive patients, were positive by PCR. The fact that M. pneumoniae grows in broth culture in spherules causes problems for determining the number of CFU detected in PCR. Filtering broth cultures through a 0.6 micron polycarbonate filter increased the number of CFUs two-to-ten-fold compared to unfiltered cultures. The lysis method needed to assay throat swabs differed from that necessary for broth cultures in that proteinase K treatment for 18 h increased the detection limit 10- to 100-fold when compared to NaOH digestion.

Base Sequence↗

PubMed1999

[A gas chromatographic method to decrease the detection limit of trace benzene in CS2 extract].

A method to decrease the detection limit of trace benzene in CS2 extract from coastal water by gas chromatography has been studied. A direct injection port (Shimadzu WBI-17) and a 2 m x 2 mm i.d. column packed with Chromosorb W(AW-DMCS) coated with 10% SE-30 was used. It is simpler and has low detection limit, small sample amount and high repeatability. The experiment showed that the trace water in the organic phase and the too small purge flow of the direct injection port could cause serious tailing of CS2 peak. There was an optimum value of the purge flow (purge flow/total flow = 5%). The minimum detectable limit of benzene was 4 micrograms/L. The repeatability (RSD) was better than 6% and the average recovery was 96.7%.

Benzene↗

PubMed2002

Statistical calculation of detection limits for DNA adducts using the 32P-postlabeling assay with a standard addition procedure.

The 32P-postlabeling assay is widely used for the analysis of DNA adducts. Some adducts can be detected with very high sensitivity but quantification can be unreliable, particularly if it is based only on comparison with unmodified nucleotides (relative adduct labeling, RAL values). Furthermore, guidelines to calculate detection limits for adduct concentrations are lacking. This is particularly important for human biomonitoring studies of environmental exposures, where a low adduct level can remain undetected. Reports of null results of toxicity studies should always include a limit of detection, indicating the effect magnitude that would have produced, with a given probability of false negative (type II error), a statistically significant increase (type I error). Here, we report on a procedure based on t-statistics to calculate two types of detection limits, the "critical level (CL)" and the "detection level (DL)". The first is the size of the difference between exposed and controls required to achieve statistical significance. The second is the size of the difference that will be detected with a chosen probability of a false negative. For the degrees of freedom (d.f.) to be used for the t-values, a general formula is given so that different standard deviations and group sizes of control and exposed groups can be handled. A sample calculation of the whole procedure is shown, using the null data for the formation of a particular adduct in lung DNA of styrene-treated mice, analyzed by 32P-postlabeling. The procedure takes into account: (i) TLC-specific background radioactivity; (ii) variability within the control and exposed groups; and (iii) confidence limits for the factor to convert 32P-radioactivity to amounts of adduct. The latter step incorporates the variance of the differences between the samples and replicates spiked with adduct standard. A statement such as follows is the result: the concentration of the alpha-isomer adduct of styrene 7,8-oxide at the O(6)-position of guanine in mouse lung DNA would have to be at least 12 adducts per 10(8) nucleotides to be detected in the given experiment on a 5% level (type I error), with a probability of 5% to miss an existing effect (type II error).

Animals↗

PubMed1984

Femtogram detection limits for biogenic amines using microbore HPLC with electrochemical detection.

Detection limits for biogenic amines, serotonin (5-HT), 5-hydroxyindoleacetic acid, 5-hydroxytryptophan, norepinephrine, epinephrine, dopamine and 3,4-dihydroxyphenylacetic acid (DOPAC), of 50-200 fg are reported. This was accomplished using microbore HPLC with electrochemical detection. Reproducibility at the 1-5 pg level of 1.6-8.1% was obtained. The utility of this approach is demonstrated for analysis of brain tissues of 1 microgram or less.

3,4-Dihydroxyphenylacetic Acid↗

PubMed1995

Decision and detection limits for linear homoscedastic assays.

This paper focuses on the effect of estimating the calibration parameters on the decision and detection limits for linear homoscedastic assays. Assay decision and detection limits are defined. For linear homoscedastic assays expressions for these limits are derived when the calibration parameters are known and unknown. These expressions, together with others previously reported in the literature, are used to calculate limits for a particular example of a cyclic AMP assay. The various methods of computing decision and detection limits are compared in a simulation study. The results demonstrate the importance of taking into consideration the variation in the estimators of the calibration parameters.

Chemistry, Clinical↗

PubMed2004

Precision and detection limit of quality test for amorphous drug in powder X-ray diffractometry.

This report puts forward a method of powder X-ray diffractometry to estimate the precision and detection limit of the crystalline component in an amorphous drug. Cefditoren pivoxil (CP) was employed as a model drug. The major error source of the measurement at low crystal contents is shown to be the random noise in a diffraction pattern (halo pattern) of the amorphous material. For the analysis of the noise, the obstructive halo pattern should be eliminated from the observed pattern. The subtraction of the observed halo pattern from another one derived from the same material, extracts the random noise alone, although the noise is amplified by square root 2 times. The noise in the powder X-ray diffractometry was identified as the white noise. On the basis of the stochastic properties of the extracted noise and signal parameters (peak area) of CP, the relative standard deviations (R.S.D.) of the area measurements of the crystalline diffraction peaks were estimated over a wide range of crystal contents without repeated experiments. The detection limit was determined such that the crystal content at detection limit produced 30% R.S.D. of the measurements. The R.S.D. and detection limit obtained from FUMI theory were in good agreement with the results from the repeated measurements.

Anti-Bacterial Agents↗

PubMed1982

Detection limits for protein after electrophoresis on cellulose acetate.

The detection limits for protein, when stained with nigrosine after electrophoresis on cellulose acetate, was studied and shown to be: albumin, 3-0 ng; transferrin, 0.8 ng; and Bence-Jones protein, 0.8 ng. This was less than one-hundredth of the previously reported levels. Immunofixation, although useful for identification, did not lower the detection limit for Bence-Jones protein.

Bence Jones Protein↗

PubMedDate not supplied

Limitations on the uses of multimedia exposure measurements for multipathway exposure assessment--Part I: Handling observations below detection limits.

Multimedia data from two probability-based exposure studies were investigated in terms of how censoring of nondetects affected estimation of population parameters and associations. Appropriate methods for handling censored below-detection-limit(BDL)values in this context were unclear since sampling weights were involved and since bivariate associations/measures were of interest. Both simple substitution(e.g., using 1/2 or 2/3 of the detection limit(DL)for BDL values)and truncation-based strategies were investigated by creating some artificial DLs and comparing resultant estimates with the original studies'uncensored results. The substitution methods generally outperformed the truncation methods, with the(2/3)DL substitution generally performing best.

Child↗

PubMed1989

Solid-phase electrochemical enzyme immunoassay with attomole detection limit by flow injection analysis.

A sandwich electrochemical enzyme immunoassay with flow injection analysis for the model antigen mouse IgG has been developed with alkaline phosphatase as the enzyme label. The enzyme substrate, 4-aminophenyl phosphate and its enzymatic reaction product, 4-aminophenol have been studied by cyclic and hydrodynamic voltammetry. The determination of 4-aminophenol by flow injection analysis with electrochemical detection (FIAEC) has a linear range of 5.0 x 10(-8) to 1.0 x 10(-5) M, a detection limit of 2.4 x 10(-8) M, and a sample throughput of 72 samples/h. The detection limit is set by a background capacitance response, which depends on the ionic strength difference between the sample and the mobile phase. The sandwich immunoassay has been characterized with respect to substrate concentration for the enzymatic reaction, detection limit, dynamic range and sources of error. Mouse IgG can be determined with a detection limit of 0.81 pg ml-1 by a 30-min substrate incubation time and a six orders of magnitude linear dynamic range.

Aminophenols↗

PubMed1987

Use of environmental TLD data at a nuclear power station to estimate detection limits for radiation exposure due to station operation.

The environmental radiation monitoring network maintained by the Georgia Department of Natural Resources at the Hatch Nuclear Plant, Baxley, GA, was used to determine the variability in measured background exposures in order to estimate the detection limits for radiation due to station operation. Data were obtained from LiF thermoluminescent dosimeters (TLDs) exposed in sets of four at 46 locations for 16 consecutive quarters from 1982 to 1985. The average exposure for 695 values was 11.8 microC kg-1 y-1 (mR/quarter). At individual locations, the averages of quarterly exposures ranged from 9.3 to 14.3 microC kg-1 y-1 and had standard deviations from 0.8 to 2.2 microC kg-1 y-1 with a typical standard deviation of 1.5 microC kg-1 y-1. The standard deviation due to reading the TLDs and subtracting the transit plus storage exposure, estimated as 0.4 microC kg-1 y-1, contributed only a small fraction of the uncertainty of the mean background; the greater contribution is from temporal fluctuations. There is a spatial pattern of higher background along the Altamaha River but no distinct seasonal pattern. The observation that exposure values at most locations rose and fell in unison suggested a calculational model that adjusts the average exposure level at a location by an increment determined each quarter at control locations. This model reduced the standard deviation for a predicted quarterly background exposure to 0.9 microC kg-1 y-1, with a range of 0.5 to 1.3 microC kg-1 y-1. If the standard deviation of the net value is multiplied by an error probability constant of 3.3 (type I and II errors not greater than 5%), the detection limits range from 2 to 5 microC kg-1 y-1 at the individual locations, with an average of 3 microC kg-1 y-1. This approach or two similar ones described earlier are recommended for improving the detection limit where needed. The standard deviation, and hence the detection limit, can be further reduced by selecting a subset of indicator and control locations with more closely matched background exposure fluctuations. This was demonstrated with five indicator and five control locations, but further study is needed to determine selection guides.

Cesium Radioisotopes↗

PubMed2003

Comparison of detectability limits for elemental mapping by EF-TEM and STEM-XEDS.

The analytical sensitivity in terms of the signal-to-noise ratio (SNR) was investigated for elemental mapping by a transmission electron microscope equipped with an energy filter (EF-TEM) and a scanning transmission electron microscope with an X-ray energy dispersive spectrometer (STEM-XEDS). To compare the detectability limits of the elemental maps by the two techniques, homogeneous Cu-0.98+/-0.34 wt% Mn and Cu-4.93+/-0.49 wt% Mn thin specimens were used. Elemental maps can be considered as either an image or a spectrum. Therefore, the detectability limits of the elemental maps were characterized by the spectral SNR. To evaluate the detectability limits of the elemental maps with statistical confidence limits such as 1 sigma, 2 sigma and 3 sigma, the SNR values were reviewed from the statistical point of view. In STEM-XEDS mapping, the spectral SNR values improve as the specimen thickness increases since the signal intensity increases. Conversely, the spectral SNR in EF-TEM mapping is maximized at a certain thickness and then reduces as the thickness increases. To compare the two mapping techniques with regard to the analytical sensitivity, a method to estimate the minimum mass fraction (MMF) from measured signal and background intensities was developed. In this experimental approach, the MMF value can be evaluated by selecting the appropriate SNR value corresponding to the statistical confidence limits. In comparing the estimated MMF values from the two mapping approaches, EF-TEM mapping can be more sensitive than STEM-XEDS mapping up to specimen thicknesses <20-30 nm in the 1 sigma confidence limit and < approximately 50 nm in the 3 sigma limits. However, as the specimen thickness increases, the XEDS maps provide better detectability limits in the Cu-Mn dilute alloy specimens.

Journal Article↗

PubMed2002

A radiographic study of the detection limits of bone-cement remnants in total joint arthroplasty.

Management of an infected hip prosthesis typically requires that all associated cement be removed. In the absence of gross mantle loosening, the surgeon frequently resorts to intraoperative radiographs to assess the completeness of removal. For this reason, we undertook a study to determine limits of detection of retained cement by routine radiography. Polymethyl methacrylate bone-cement beads (Simplex-P; Stryker-Howmedica-Osteonics, Allendale, NJ) were fashioned into graduated sizes and placed within cadaver medullary canals using 2 different methods. Standard radiographic images were obtained. Individually and independently, we viewed these images and proposed the limit of resolution to be 2.4 to 3.2 mm. It is difficult to remove all cement based on radiographs alone. These results suggest a need to use techniques that permit visualization of the canal to ensure adequate cement removal.

Arthroplasty, Replacement, Hip↗