Standardized Solutions

The equivalent is the molar mass of the species containing one atom of cerium in its structure. They are prepared 

The reaction is slow, but it is accelerated when osmium tetraoxide is present in the reaction vessel. It is a catalyst for the reaction. Oxide AS2O3 is dissolved in a sodium hydroxide solution, and the solution is acidified by the addition of sulfuric acid. Then some drops of an osmium tetraoxide solution are added and the solution under study is titrated with a ceric sulfate solution  

20 Oxidizations with Permanganate, Dichromate, and Ceric Ions... 

The titration is achieved in hydrochloric acid with an excess of potassium iodide  

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Several variations of the chemical method are in use. In the one described below, a freshly prepared Fehling s solution is standardised by titrating it directly against a standard solution of pure anhydrous glucose when the end-point is reached, I. e., when the cupric salt in the Fehling s solution is completely reduced to cuprous oxide, the supernatant solution becomes completely decolorised. Some difficulty is often experienced at first in determining the end-point of the reaction, but with practice accurate results can be obtained. The titrations should be performed in daylight whenever possible, unless a Special indicator is used (see under Methylene-blue, p. 463). 

Table 8.33 Standard Solutions for Calibrating Conductivity Vessels 8.160...

Table 11.30 lists standard solutions for precipitation titrations and Table 11.31 lists specific reagents as indicators, adsorption indicators, and protective colloids for precipitation titrations. 

The list given below includes the substances that are most used and most useful for the standardization of solutions for precipitation titrations. Primary standard solutions are denoted by the letter (P) in Column 1. 

From J. A. Dean and T. C. Rains, Standard Solutions for Flame Spectrometry, in Flame Emission and Atomic Absorption Spectrometry, J. A. Dean and T. C. Rains (Eds.), Vol. 2, Chap. 13, Marcel Dekker, New York, 1971. 

Bismuth standard solution (quantitative color test for Bi) dissolve 1 g of bismuth in a mixture of 3 mL of concentrated HNO3 and 2.8 mL of H2O and make up to 100 mL with glycerol. Also dissolve 5 g of KI in 5 mL of water and make up to 100 mL with glycerol. The two solutions are used together in the colorimetric estimation of Bi. 

A standard solution of Mn + was prepared by dissolving 0.250 g of Mn in 10 ml of concentrated HNO3 (measured with a graduated cylinder). The resulting solution was quantitatively transferred to a 100-mL volumetric flask and diluted to volume with distilled water. A 10-mL aliquot of the solution was pipeted into a 500-mL volumetric flask and diluted to volume, (a) Express the concentration of Mn in parts per million, and estimate uncertainty by a propagation of uncertainty calculation, (b) Would the uncertainty in the solution s concentration be improved... 

A standard solution containing a known amount of analyte, prepared separately from samples containing the analyte. 

A standardization in which aliquots of a standard solution are added to the sample. 

Illustration showing the method of standard additions in which separate aliquots of sample are diluted to the same final volume. One aliquot of sample is spiked with a known volume of a standard solution of analyte before diluting to the final volume. 

Three replicate determinations of the signal for a standard solution of an analyte at a concentration of 10.0 ppm give values of 0.163, 0.157, and 0.161 (arbitrary units), respectively. The signal for a method blank was found to be 0.002. Calculate the concentration of analyte in a sample that gives a signal of 0.118. 

II. 5 (arbitrary units). A second 50-mL aliquot of the sample, which is spiked with 1.00-mL of a 10.0-ppm standard solution of the analyte, gives a signal of 23.1. What is the concentration of analyte in the original sample ... 

Following the separation outlined in Example 7.10, an analysis is to be carried out for the concentration of Cu in an industrial plating bath. The concentration ratio of Cu to Zn in the plating bath is 7 1. Analysis of standard solutions containing only Cu or Zn give the following standardization equations... 

Inorganic Analysis Acid-base titrimetry is a standard method for the quantitative analysis of many inorganic acids and bases. Standard solutions of NaOH can be used in the analysis of inorganic acids such as H3PO4 or H3ASO4, whereas standard solutions of HCl can be used for the analysis of inorganic bases such as Na2C03. 

CO2 is determined by titrating with a standard solution of NaOH to the phenolphthalein end point, or to a pH of 8.3, with results reported as milligrams CO2 per liter. This analysis is essentially the same as that for the determination of total acidity, and can only be applied to water samples that do not contain any strong acid acidity. 

The purity of a pharmaceutical preparation of sulfanilamide, C6H4N2O2S, can be determined by oxidizing the sulfur to SO2 and bubbling the SO2 through H2O2 to produce H2SO4. The acid is then titrated with a standard solution of NaOH to the bromothymol blue end point, where both of sulfuric acid s acidic protons have been neutralized. Calculate the purity of the preparation, given that a 0.5136-g sample required 48.13 mL of 0.1251 M NaOH. 

Procedure. Select a volume of sample requiring less than 15 mL of titrant to keep the analysis time under 5 min and, if necessary, dilute the sample to 50 mL with distilled water. Adjust the pH by adding 1-2 mL of a pH 10 buffer containing a small amount of Mg +-EDTA. Add 1-2 drops of indicator, and titrate with a standard solution of EDTA until the red-to-blue end point is reached. 

Selection and Standardization of Titrants EDTA is a versatile titrant that can be used for the analysis of virtually all metal ions. Although EDTA is the most commonly employed titrant for complexation titrations involving metal ions, it cannot be used for the direct analysis of anions or neutral ligands. In the latter case, standard solutions of Ag+ or Hg + are used as the titrant. 

Cyanide is determined at concentrations greater than 1 ppm by making the sample alkaline with NaOH and titrating with a standard solution of AgN03, forming the soluble Ag(CN)2 complex. The end point is determined using p-dimethylaminobenzalrhodamine as a visual indicator, with the solution turning from yellow to a salmon color in the presence of excess Ag+. 

Another reducing titrant is ferrous ammonium sulfate, Fe(NH4)2(S04)2 6H2O, in which iron is present in the +2 oxidation state. Solutions of Fe + are normally very susceptible to air oxidation, but when prepared in 0.5 M 1T2S04 the solution may remain stable for as long as a month. Periodic restandardization with K2Cr20y is advisable. The titrant can be used in either a direct titration in which the Fe + is oxidized to Fe +, or an excess of the solution can be added and the quantity of Fe + produced determined by a back titration using a standard solution of Ce + or... 

Experiments are described for determining GO2 in carbonated beverages, NaHG03 in Alka-Seltzer tablets, and the molecular weight of GO2. Garbon dioxide is collected in NaOH and the concentrations of G03 are determined by titrating with a standard solution of HGl to the phenolphthalein and methyl orange end points. 

A quantitative analysis for NH3 in several household cleaning products is carried out by titrating with a standard solution of HGl. The titration s progress is followed thermometrically by monitoring the temperature of the titration mixture as a function of the volume of added titrant. Household cleaning products may contain other basic components, such as sodium citrate or sodium carbonate, that will also be titrated by HGl. By comparing titration curves for prepared samples of NH3 to titration curves for the samples, it is possible to determine that portion of the thermometric titration curve due to the neutralization of NH3. 

Solutions containing both Le + and AF+ can be selectively analyzed for Le + by buffering to a pH of 2 and titrating with EDTA. The pH of the solution is then raised to 5 and an excess of EDTA added, resulting in the formation of the AF+-EDTA complex. The excess EDTA is back titrated using a standard solution of Le +, providing an indirect analysis for AF+. 

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