Sample preparation blanks

Sample Analysis Inject the Sample Preparation in duplicate, and record the integrated absorbance. If the instrument response exceeds that of the calibration curve, dilute with 5% nitric acid to bring the sample s response into the working range, and note the dilution factor (DF). A11 sample analyses should be blank corrected using a sample preparation blank. 

Standard Curve Inject each calibration standard in triplicate. Normal instrument linearity extends to 25 ng/mL. If nonlinear calibration capability is not available, limit the working calibration curve to <25 ng/mL. Use the calibration algorithms provided in the instrument software. Recheck calibration periodically (<15 samples) by running a 25- or 50-ng/ mL calibration standard interspersed with samples. If recheck differs from calibration by >10%, recalibrate the instrument. The instrumental detection limit (DL) and quantitation limit (QL), in picograms, may be based on 7 to 10 replicates of the Sample Preparation Blank and calculated as follows ... 

Blank samples are used to determine if any contamination has occurred during sample handling. Prepare two blanks for the first 1 to 20 samples. For sets containing greater than 20 samples, prepare blanks as 10% of the samples. Handle blank samples in the same manner as air samples with one exception Do not draw any air through the blank samples. Open the blank cassette in the place where the sample cassettes are mounted on the employee. Hold it open for about 30 seconds. Close and seal the cassette appropriately. Store blanks for shipment with the sample cassettes. 

The methods I- 4 of sample preparation are classics. As a mle they give a high value of blank and some of them take a lot of time. Microwave sample preparation is perspective, more convenient and much more faster procedure than classical mineralization. There are some problems with the combination Cendall-Kolthoff s kinetic method and microwave sample preparation which discussed. The experimental data of different complex organic matrix are demonstrated (food products on fat, peptides, hydrocarbone matrix, urine etc). 

Third, the bulk of the items in Table 1 address method performance. These requirements must be satisfied on a substrate-by-substrate basis to address substrate-specific interferences. As discussed above, interferences are best dealt with by application of conventional sample preparation techniques use of blank substrate to account for background interferences is not permitted. The analyst must establish a limit of detection (LOD), the lowest standard concentration that yields a signal that can be differentiated from background, and an LOQ (the reader is referred to Brady for a discussion of different techniques used to determine the LOD for immunoassays). For example, analysis of a variety of corn fractions requires the generation of LOD and LOQ data for each fraction. Procedural recoveries must accompany each analytical set and be based on fresh fortification of substrate prior to extraction. Recovery samples serve to confirm that the extraction and cleanup procedures were conducted correctly for all samples in each set of analyses. Carrying control substrate through the analytical procedure is good practice if practicable. 

Blank which arises from contamination IUPAC [1995], Currie [1999] from the reagents, sampling procedure, or sample preparation steps which correspond to the very analyte being sought . 

Spectrophotometric determination with 4-hexylresorcinol and a fluorometric method with m-aminophenol are the most commonly used procedures for the determination of acrolein. However, gas chromatography and high-performance liquid chromatography procedures are also used (USEPA 1980 Kissel etal. 1981 Nishikawa and Hayakawa 1986). Acrolein concentrations in rainwater between 4 and 200 pg/L can be measured rapidly (less than 80 min) without interference from related compounds the method involves acrolein bromination and analysis by gas chromatography with electron capture detection (Nishikawa and Hayakawa 1986). Kissel etal. (1981) emphasize that water samples from potential acrolein treatment systems require the use of water from that system in preparing blanks, controls, and standards and that acrolein measurements should be made at the anticipated use concentrations. 

Method Performance. A blank sample, prepared using the same procedure as for the samples, was included with every five samples. PCB 28 and y-HCH were the only compounds detected in the blanks. Detection limits, calculated as mean blank +3 SD, were typically 2.3-13.3 pg/pF = 0.02-0.12 ng/g soil. Results were not blank corrected. Replicate analysis (the same soil sample extracted three times) was done for several samples. The relative standard deviation (RSD) for replicate analysis was always less than 20% (n = 3). Analytical recoveries were monitored with the aid of two recovery standards mirex for FI and 5-HCH for F2. The mean recovery for mirex was 100 ... 

In general, most procedures are like the ones described above. For the modified method, an alternative DMB reagent is used and ten parts of this reagent are added to one part of Tris buffer to yield a reagent with a pH of 8.7-8.8. The reagent - Tris mixture is not stable and has to be prepared just prior to analysis. First, 20 pi of urine (sample) or water (blank) is added to the cuvettes or microtiter plates. The volume of standards, samples, and blanks are adjusted to 50 pi with demineralized water. Then, 275 pi of DMB-Tris reagent is added to each cuvette/well. Either all samples... 

Analytical methods for monitoring the compounds were developed or modified to permit the quantification of all 23 compounds of interest. As noted earlier, the compounds were initially studied in small-scale extractions by groups. This approach assured minimal interferences in the analyses conducted during the initial supercritical fluid carbon dioxide extractions. Table II summarizes the data on the recovery of organics from aqueous samples containing the compounds of interest at concentration levels listed in Table I when the sample preparation techniques and analytical methods described were used. For each experimental run, blank and spiked aqueous samples were carried through the sample prepration and analytical finish steps to ensure accurate and reproducible results. Analyses of sodium, calcium, and lead content were also conducted on selected samples by using standard atomic ab-... 

A method blank is a sample containing all components except analyte, and it is taken through all steps of the analytical procedure. We subtract the response of the method blank from the response of a real sample prior to calculating the quantity of analyte in the sample. A reagent blank is similar to a method blank, but it has not been subjected to all sample preparation procedures. The method blank is a more complete estimate of the blank contribution to the analytical response. 

As a summary of observations on sample preparation of all types, some generalizations can be reiterated. Whenever possible, blank samples spiked with standards should be employed and recovery studies should include assays of each extract, to monitor possible drug-substrate interaction. One technique effective in this regard, is to examine the aqueous phase by TLC after all the "free" drug has been extracted. Standard calibration curves should be compared to similar plots in the presence of sample matrix constituents whenever possible. GC should never be employed as the sole criterion in any analytical evaluation. 

Providing that care has been taken in the disc preparation the final disc should be slightly opaque due to the presence of the sample (the blank disc should be transparent). Should the disc show a number of white spots, it is probable that the mixture has been unevenly ground. If the disc shows a tendency to flake, then excessive grinding of the powder is indicated. If after being removed from the die the disc becomes cloudy this is indicative of the uptake of water to avoid this difficulty it is necessary to ensure that the die is evacuated for a sufficiently long period and that the removal of the disc from the die is carried out under a radiant heater. 

One alternative is to compare the results of the method with results from an established reference method. This approach assumes that the uncertainty of the reference method is known. Second, accuracy can be assessed by analyzing a sample with known concentrations (e.g., a certified reference material) and comparing the measured value with the true value as supplied with the material. If such certified reference material is not available, a blank sample matrix of interest can be spiked with a known concentration by weight or volume. After extraction of the analyte from the matrix and injection into the analytical instrument, its recovery can be determined by comparing the response of the extract with the response of the reference material dissolved in a pure solvent. Because this accuracy assessment measures the effectiveness of sample preparation, care should be taken to mimic the actual sample preparation as closely as possible. 

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