Acids primary standard

Step 1 It shows the solution of benzoic acid (primary standard) in DMF,... 

Standard substances in clinical chemistry include primary standards, which can be obtained sufficiently pure to be used for the preparation of solutions by weighing or by reference to other definable physical characteristics (e.g., constant-boiling hydrochloric acid). Primary standard chemicals are available for acid-base reactions, precipitation reactions, oxidation-reduction reactions, etc. (V3), and are used in these various categories of analytical determination to validate the preparation of solutions of other chemical substances which cannot be obtained in a form suitable to meet the criteria demanded for a primary standard. Following their calibration in terms of a primary standard, these other chemieals can act as secondary standards. 

Table 11.27 Primary Standards for Aqueous Acid-Base Titrations Table 11.28 Titrimetric (Volumetric) Factors...

H0CH3)3CNHH3 121.137 Tris(hydroxymethyl)aminomethane is available commercially as a primary standard. Dry at 100-103°C (<110°C). In titrations with a strong acid the equivalence point is at about pH 4.5-5. Equivalent weight is the formula weight. [J. H. Eossum, P. C. Markunas, and J. A. Riddick, Anal. Chem., 23 491 (1951).]... 

Alkaline arsenite, O.IA As(lll) to As(V). Dissolve 4.9460 g of primary standard grade AsjOj in 40 mL of 30% NaOH solution. Dilute with 200 mL of water. Acidify the solution with 6N HCl to the acid color of methyl red indicator. Add to this solution 40 g of NaHC03 and dilute to 1 L. 

Selecting and Standardizing a Titrant Most common acid-base titrants are not readily available as primary standards and must be standardized before they can be used in a quantitative analysis. Standardization is accomplished by titrating a known amount of an appropriate acidic or basic primary standard. 

The majority of titrations involving basic analytes, whether conducted in aqueous or nonaqueous solvents, use HCl, HCIO4, or H2SO4 as the titrant. Solutions of these titrants are usually prepared by diluting a commercially available concentrated stock solution and are stable for extended periods of time. Since the concentrations of concentrated acids are known only approximately,the titrant s concentration is determined by standardizing against one of the primary standard weak bases listed in Table 9.7. 

Selected Primary Standards for the Standardization of Strong Acid and Strong Base Titrants... 

Primary Standard Standardization of Acidic Titrants Titration Reaction Comment... 

Solutions of Na2S203 are prepared from the pentahydrate and must be standardized before use. Standardization is accomplished by dissolving a carefully weighed portion of the primary standard KIO3 in an acidic solution containing an excess of KI. When acidified, the reaction between 103 and K... 

Thompson, R. Q. Identification of Weak Acids and Bases by Titration with Primary Standards, /. Chem. Educ. 1988, 65, 179-180. 

Standard 1/10 N nitrite is used to titrate a solution prepared by dissolving 10—100 mg of sulfamic acid and about 6 mL of (1 + 1) H2SO4 in 300 mL of distilled water at 40—50°C. At the end point, the colorless external potassium iodide starch-paste indicator changes to blue. A 1-mL solution of 1/ION NaN02 is equivalent to 9.709 mg of sulfamic acid. The 1/10 N nitrite titrant solution is standardized using primary standard-grade sulfamic acid. For sulfamate assay determination, the same procedure is used as for sulfamic acid. 

The malonaldehyde thus formed can be estimated quantitatively by the thiobarbituric acid method (58, 59). As a control of the method s reliability, we used, as primary standard, 1, 3, 3-tri-ethoxypropene (46, 47) purified by gas-liquid chromatography (56) and hydrolyzed to malonaldehyde at room temperature with IN sulfuric acid. The molar... 

In this connection it must be pointed out that standard samples which have been analysed by a number of skilled analysts are commercially available. These include certain primary standards (sodium oxalate, potassium hydrogenphthalate, arsenic(III) oxide, and benzoic acid) and ores, ceramic materials, irons, steels, steel-making alloys, and non-ferrous alloys. 

Note on the gravimetric standardisation of hydrochloric acid. The gravimetric standardisation of hydrochloric acid by precipitation as silver chloride is a convenient and accurate method, which has the additional advantage of being independent of the purity of any primary standard (compare Section 10.38). Measure out from a burette 30-40mL of the, say, 0.1M hydrochloric acid which is to be standardised. Dilute to 150 mL, precipitate (but omit the addition of nitric acid), and weigh the silver chloride. From the weight of the precipitate, calculate the chloride concentration of the solution, and thence the concentration of the hydrochloric acid. 

A limited number of pure substances are available from NIST, primarily clini-cally-relevant compounds such as cholesterol, urea, uric acid, creatinine, glucose, cortisol, tripalmitin, and bilirubin (NIST SRM website). These compounds are certified for purity (greater than 99 %) and are used as primary calibrants in definitive methods for these clinical analytes (see below). Several additional pure substances are available for specific applications such as microchemistry, i.e. elemental composition (acetanilide, anisic acid, cystine nicotinic acid, o-bromobenzoic acid, p-fluoro-benzoic acid, m-chlorobenzoic acid), polarimetric standards (sucrose and dextrose), acidimetric standard (benzoic acid and boric acid). Only three pure substance NIST RMs are available for environmental contaminants, namely the chlorinated pesticides, lindane, 4,4 -DDT, and 4,4 -DDE. 

Step 2 Weigh out an appropriate amount of an acidic material, suitable for use as a primary standard, such as potassium hydrogen phthalate (KHP). 

Typically, acid soils are titrated with a sodium or calcium hydroxide [NaOH or Ca(OH)2] solution and basic soils with hydrochloric acid (HC1), and pH changes are most commonly followed using a pH meter. Carbonates in basic soils release C02 during treatment with HC1, thus making the titration more difficult. For this reason, carbonates are often determined by other methods. It is important to keep in mind that basic solutions react with carbon dioxide in air and form insoluble carbonates. This means that either the basic titrant is standardized each day before use or the solution is protected from exposure to carbon dioxide in air. Specific descriptions of titrant preparation, primary standards, and the use of indicators and pH meters in titrations can be found in Harris [1] and in Skoog et al. [2],... 

In a standardization experiment, 0.4920 g of primary standard sodium carbonate (Na2C03) was exactly neutralized by 19.04 mL of hydrochloric acid solution. What is the molarity of the HC1 solution Refer to Equation (4.7) for the reaction involved. 

Primary standard tris-(hydroxymethyl)amino methane, also known as THAM or TRIS (FW = 121.14 g/mol), is used to standardize a hydrochloric acid solution. If 0.4922 g of THAM is used and 23.45 mL of HC1 is needed, what is the normality of HC1 ... 

Suppose a sulfuric acid solution, rather than the hydrochloric acid solution in question 22, is standardized with primary standard THAM. Does the calculation change in any way Explain. 

For standardizing a base solution, primary standard grade potassium biphthalate is a popular choice. Also called potassium hydrogen phthalate, potassium acid phthalate, or simply KHP, it is the salt representing partially neutralized phthalic acid and is a monoprotic weak acid. The true formula is KHC8H404. Figure 5.8 shows the chemical structure of phthalic acid and KHP. The reaction with a base is as follows ... 

For standardizing acid solutions, primary standard tris-(hydroxymethyl)amino methane, THAM (also referred to as TRIS), can be used. Its formula is... 

Primary standard sodium carbonate may also be used to standardize acid solutions. Sodium carbonate also possesses all the qualities of a good primary standard, like KHP and THAM. When titrating sodium carbonate, carbonic acid, H2C03, is one of the products and must be decomposed with heat to push the equilibria below to completion to the right ... 

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