Reagent blank corrections

A reagent blank corrects the measured signal for signals due to reagents other than the sample that are used in an analysis. The most common reagent blank is prepared by omitting the sample. When a simple reagent blank does not compensate for all constant sources of determinate error, other types of blanks, such as the total Youden blank, can be used. 

A reagent blank corrects the measured signal for signals dyi reagents other than the sample that are used in he... 

Carry out the method exactly as described in Section F, paragraphs 2-9 inclusive, using redistilled water in place of the sample. The reagent blank corrected for cell-to-cell blank should not exceed 0.100. If the blank exceeds this amount either the molybdate reagent or the iso-butanol is suspect. The reagent blank should be determined for each batch of samples measured. 

A propagation of uncertainty also helps in deciding how to improve the uncertainty in an analysis. In Example 4.7, for instance, we calculated the concentration of an analyte, obtaining a value of 126 ppm with an absolute uncertainty of 2 ppm and a relative uncertainty of 1.6%. How might we improve the analysis so that the absolute uncertainty is only 1 ppm (a relative uncertainty of 0.8%) Looking back on the calculation, we find that the relative uncertainty is determined by the relative uncertainty in the measured signal (corrected for the reagent blank)... 

In a single-point standardization, we assume that the reagent blank (the first row in Table 5.1) corrects for all constant sources of determinate error. If this is not the case, then the value of k determined by a singlepoint standardization will have a determinate error. 

In discussing ways to standardize a method, we assumed that an appropriate reagent blank had been used to correct S eas for signals originating from sources other than the analyte. At that time we did not ask an important question— What constitutes an appropriate reagent blank Surprisingly, the answer is not intuitively obvious. 

The following data were obtained for a set of external phosphate standards. All absorbances have been corrected for a reagent blank. 

Running a blank determination. This consists in carrying out a separate determination, the sample being omitted, under exactly the same experimental conditions as are employed in the actual analysis of the sample. The object is to find out the effect of the impurities introduced through the reagents and vessels, or to determine the excess of standard solution necessary to establish the end-point under the conditions met with in the titration of the unknown sample. A large blank correction is undesirable, because the exact value then becomes uncertain and the precision of the analysis is reduced. 

Carbon was estimated by a variation of the Van Slyke method.(2) A 30-100 mg sample was heated for 30 minutes with 0.5 g K2Cr207, lg KIOj, 10 mL 20% fuming H2S01( and 5 mL HjPO in a closed flask swept by a purified N2 stream. The N2 stream carried the evolved C02 to an absorption solution of 0.5M Na0H-0.3M N H. After the wet combustion, the absorbed C02 was released from an aliquot of the NaOH solution with lactic acid in a manometric apparatus. Corrections were applied for the vapor pressure of water and for reagent blank. 

The parathion was removed from the surface of the fruit with benzene (redistilled) in an end-over-end type tumbling machine at a speed of 72 revolutions per minute. All samples were washed in this manner for a period of 0.5 hour. Reagent blanks and unsprayed fruit blanks were run with all samples. All results, as reported, have been corrected for reagent and fruit blanks. 

Of the methods available for potentiometrically estimating the amount of iodine bound by amylose, the differential method of Gilbert and Marriott36 is by far the most satisfactory for accurate work as it eliminates corrections for reagent blanks. In this method, the amylose solution and control solution form two half-cells connected by a salt-bridge, and the... 

Spengler and Jumar [90] used a spectrophotometric method and thin layer chromatography to determine carbamate and urea herbicide residues in sediments. The sample is extracted with acetone, the extract is evaporated in vacuo at 40°C and the residue is hydrolysed with sulphuric acid. The solution is made alkaline with 15% aqueous sodium hydroxide and the liberated aniline (or substituted aniline) is steam distilled and collected in hydrochloric acid. The amine is diazotized and coupled with thymol, the solution is cleaned up on a column of MN 2100 cellulose power and the azo-dye is determined spectrophotometrically at 440nm (465nm for the dye derived from 3-chloro- or 3.4-dichloroaniline) with correction for the extinction of a reagent blank. 

Further lowering of the blank correction occurs when nonisotopic carriers in chemical procedures are used to replace inert carriers of the element of interest when it is difficult to obtain the inert carrier in a contamination-free condition. Obviously, only clean glassware should be used, reagents should not be reused, and the laboratory should be kept in an immaculate condition. Separations that have high chemical yields and high radiochemical purity reduce the blanks. 

There may be contribution from CIOH. This can be estimated from the reagent blank. d For variable isotopes of lead. e Isobaric elemental correction for ruthenium. f Krypton might be present as an impurity in some argon supplies. 

Solvent/Reagent Blank. A solvent blank checks solvents and reagents that are used during sample preparation and analysis. Sometimes, a blank correction or zero setting is done based on the reagent measurement. For example, in atomic or molecular spectroscopy, the solvents and reagents used in sample preparation are used to provide the zero setting. 

Inductively Coupled Plasma. Analyses by ICP were performed on the same dissolutions used for the AA analyses for Cd and Pb. The solutions were diluted as necessary and were then nebulized and introduced into the plasma. Line spectra were collected with a multichannel analyzer and corrections were made for reagent blanks and background shifts. For all analyses, NBS Standard Reference Material 1632 was used for instrument calibration. 

The absorbance produced by the solution from the Sample Preparation, after correction for a reagent blank, is not greater than that produced by a solution from the Standard Preparation, treated in the same manner in the above procedure as the Sample Preparation, beginning with Add 1.0 mL of 0.1 N ceric sulfate.. .. ... 

Make several reagent blank determinations, using only the chromium trioxide solution in the above procedure. The ratio of the sodium hydroxide titration (Vb) to the sodium thiosulfate titration (7b), corrected for variation in normalities, will give the acidity-to-oxidizing ratio, V b/Kb = K, for the chromium trioxide carried over in the distillation. The factor K should be constant for all determinations. 

Calculation, Procedure 2 Calculate the corrected absorbances Ar for each Sample Preparation (absorbance Phytase Reference Solution minus corresponding absorbance blank) and for each Potassium Dihydrogen Phosphate Solution, Ap (absorbance Potassium Dihydrogen Phosphate Solution minus average absorbance reagent blank). Calculate C, the phosphate concentration of each Potassium Dihydrogen Phosphate Solution ... 

Three or four aliquots of the sample solution are transferred to volumetric flasks and known, different amounts of a standard solution of the analyte element are added to each of these except one. The solutions in the flasks are then made up to volume. These solutions plus a reagent blank are then run in the electrothermal atomizer. Each reading should have the blank subtracted before plotting. The sample result is then itself blank-corrected. 

Film and reagent blank determinations were always made and used to correct the data appropriately. The assay was linear throughout the range encountered here. 

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