Volumetric Solutions - ACS Reagent Chemicals (ACS Publications)

Preparation pubs.acs.org/doi/book/10.1021/acsreagents

Volumetric Solutions Part 3, Solutions and Mixtures Used in Tests eISBN: 9780841230460 Tom Tyner Chair, ACS Committee on Analytical Reagents James Francis Secretary, ACS Committee on Analytical Reagents

Downloaded by CORNELL UNIV on May 23, 2017 | http://pubs.acs.org Publication Date (Web): February 28, 2017 | doi: 10.1021/acsreagents.3003

ABSTRACT Throughout the monographs in this book, the term “volumetric solution” is used to designate a solution prepared and standardized as described in this section. Two background references that the analyst may find helpful are ASTM E20008(2008) and the section on Volumetric Solutions in United States Pharmacopeia (see the bibliographies on Analytical Chemistry [Part 6: List of Bibliographies; Analytical Chemistry], and on Physical Properties [Part 6: List of Bibliographies; Physical Properties]). Various textbooks on chemical analysis also deal with volumetric solutions and volumetric analysis on both a theoretical and a practical basis.

GENERAL INFORMATION The concentrations of volumetric solutions usually are expressed as N, normality (number of gram-equivalent weights in each liter of solution), although concentration sometimes is expressed as M, molarity (number of gram-molecular weights in each liter of solution). The accuracy of many analytical procedures is dependent on the manner in which such solutions are prepared, standardized, and stored. The directions that follow describe the preparation of these solutions and their standardization against primary standards or against already-standardized solutions. Alternatively, in cases where suitable primary standard chemicals are available, volumetric solutions may be prepared by dissolving accurately weighed portions of these substances to make an accurately known volume of solution. All volumetric solutions, of course, must be thoroughly mixed as part of their preparation. Stronger or weaker solutions than those described are prepared and standardized in the same general manner, using proportional amounts of reagents and standards. Lower strengths frequently may be prepared by accurately diluting a stronger solution. However, when necessary because of the accuracy requirements of the analysis being performed, volumetric solutions prepared in this manner should be standardized before use against a primary standard or by comparison with an appropriate volumetric solution of known strength. Certain reagents, such as arsenic trioxide, reductometric standard, are designated as standards in this book. Certified standards of a number of chemical compounds are available as standard reference materials (SRMs) from NIST. It is desirable to standardize a solution in such a way that the end point is observed at the same pH value (or oxidation–reduction potential) anticipated during subsequent use. For example, a sodium hydroxide solution found to be 0.1000 N when standardized against potassium hydrogen phthalate to phenolphthalein (pH 8.5) may behave like 0.1002 N when used for titrating a strong acid to methyl red (pH 5). Only a small part of this difference is due to the NaOH required to bring pure water from pH 5 to 8.5. In this case, the error can be avoided by titrating the strong acid to phenolphthalein (pH 8.5), the same indicator that was used in standardizing the sodium hydroxide.

© 2017 American Chemical Society

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ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.

DOI:10.1021/acsreagents.3003 ACS Reagent Chemicals, Part 3

ACS Reagent Chemicals

Preparation

pubs.acs.org/doi/book/10.1021/acsreagents

Storage Glass containers are suitable for the storage of most volumetric solutions. However, polyolefin containers are recommended for alkaline solutions. Volumetric solutions are stable for varying lengths of time, depending on their chemical nature and their concentration. Dilute solutions are likely to be less stable than those that are 0.1 N or stronger. If there is any doubt about the reliability of a solution, it should be restandardized at the time of use. Volumetric solutions should be stored appropriately to avoid environmental interaction that may adversely affect the stability of the assigned normality or molarity. Opaque containers and carbon dioxide or oxygen traps may be appropriate under certain conditions.


Temperature Considerations If possible, volumetric solutions should be prepared, standardized, and used at 25 °C. If a titration is carried out at a temperature different from that at which the solution was standardized, a temperature correction may be needed, depending on the accuracy requirement of the analysis being performed. If the temperature of use is higher than the temperature of standardization, the correction is to be subtracted from the standardization value; if the temperature of use is lower than the temperature of standardization, the correction is to be added. For guidance with respect to temperature corrections, consider that a 5 °C temperature change will alter the normalities of solutions approximately as follows: For aqueous solutions 0.1 N or less, by 1 part in 1000; 0.5 N, by 1.2 parts in 1000; and 1 N, by 1.4 parts in 1000. For nonaqueous solutions, based on the expansion coefficients of the solvents, by 5.4 parts in 1000 for glacial acetic acid; 5.5 parts in 1000 for dioxane; and 6.2 parts in 1000 for methanol. Errors caused by temperature differences, as well as by improper drainage of burettes or pipettes, can be avoided if measurements are made on a weight basis. With a sensitive direct-reading balance and the use of squeeze bottles, titrations by weight have become very practical and precise.

Correction Factors It is not necessary that volumetric solutions have the identical normalities (or molarities) indicated in this section or as specified in many of the standardization and assay calculations in this book. It is necessary, however, that the exact value be known because if it is different from the nominal value specified, a correction factor will have to be applied. Thus, if a calculation is based on an exactly 0.1 N volumetric solution and the solution actually used is 0.1008 N, its volume must be multiplied by a factor of 1.008 to obtain the corrected volume of 0.1 N solution to use in the calculation. Similarly, if the actual normality is 0.0984 N, the factor is 0.984.

Replication Because the results obtained by titrations depend on the reliability of the volumetric solutions used, it is imperative that the latter be standardized at least in triplicate with particular care and preferably by experienced analysts. Triplicate standardizations for solutions from 0.1 N to 1 N should agree at least to within 2 parts in 1000. Triplicates for 0.05 N solutions may differ by as much as 10 parts in 1000. If deviations are greater than indicated, the determinations should be repeated until the criteria are met.

SOLUTIONS Note: When “measure accurately” is specified in this section, the volumetric ware used shall conform to the tolerance accepted by NIST (see the bibliography on Measurement Techniques [Part 6: List of Bibliographies; Measurement Techniques]).

Acetic Acid, 1 N Add 61 g (58.1 mL) of glacial acetic acid to a 1 L volumetric flask, dilute to volume with water, and mix thoroughly. Standardize as follows: Measure accurately 40 mL of the solution into a 250 mL conical flask, add 0.10 mL of


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Preparation


phenolphthalein indicator solution, and titrate with freshly standardized 1 N sodium hydroxide volumetric solution to a permanent pink color.

Ammonium Thiocyanate, 0.1 N


Dissolve 7.61 g of ammonium thiocyanate in 100 mL of water. Transfer to a 1 L volumetric flask, dilute to volume with water, and mix thoroughly. Standardize as follows: Measure accurately 40 mL of freshly standardized 0.1 N silver nitrate volumetric solution into a 250 mL conical flask containing 50 mL of water. Add 2 mL of nitric acid and 2 mL of ferric ammonium sulfate indicator solution. While stirring, titrate with ammonium thiocyanate solution to the first appearance of a red-brown color.

Bromine, 0.1 N, Solution I (Prepared from bromine.) In a well-ventilated hood, pipette 2.6 mL of bromine into a 1 L glass-stoppered volumetric flask containing 25 g of potassium bromide and 5 mL of hydrochloric acid dissolved in 500 mL of water. Stopper and swirl until the bromine is dissolved, dilute to volume with water, and mix thoroughly. Standardize as follows: Measure accurately 40 mL of the solution into a 250 mL iodine flask containing 100 mL of water. Add 3 g of potassium iodide and titrate the liberated iodine with freshly standardized 0.1 N sodium thiosulfate volumetric solution. Add 3 mL of starch indicator solution near the end of the titration and continue to the absence of the blue starch–iodine complex.

Bromine, 0.1 N, Solution II (Prepared as a potassium bromate–potassium bromide mixture.) Transfer 2.8 g of potassium bromate plus 15 g of potassium bromide to a 1 L volumetric flask, dilute to volume with water, and mix thoroughly. Standardize as follows: Measure accurately 40 mL of the solution into a 250 mL iodine flask and dilute with 100 mL of water. Add 3 g of potassium iodide, stopper the flask, and swirl the contents carefully. Then add 3 mL of hydrochloric acid, stopper the flask again, swirl vigorously, and allow to stand in the dark for 5 min. Titrate the liberated iodine with freshly standardized 0.1 N sodium thiosulfate volumetric solution. Add 3 mL of starch indicator solution near the end of the titration and continue to the absence of the blue starch–iodine complex.

Ceric Ammonium Sulfate, 0.1 N Place 63.26 g of ceric ammonium sulfate dihydrate in a 1500 mL beaker and slowly add 30 mL of sulfuric acid. Stir to a smooth paste, and cautiously add water in portions of 20 mL or less, with stirring, until the salt is dissolved. Dilute, if necessary, to approximately 500 mL, and mix thoroughly by stirring. Allow to stand for at least 8 h. If a residue has formed


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Preparation


or the solution is turbid, filter through a fine-porosity sintered-glass filter (do not filter through paper or similar material). Transfer the filtrate to a 1 L volumetric flask, dilute to volume, and mix thoroughly. Standardize as follows: Titrate against freshly standardized 0.1 N ferrous sulfate solution described in [Part 3: Volumetric Solutions; Solutions; Ferrous Sulfate] using a Ferroin indicator, 0.025 M.


Cupric Sulfate, 0.1 M Weigh accurately 24.97 g of cupric sulfate pentahydrate. Dissolve in 500 mL of water and quantitatively transfer to a 1 L volumetric flask. Dilute to volume with water, and mix thoroughly. Standardize as follows: Using a 50 mL burette, measure 40.0 mL of the cupric sulfate solution into a 250 mL beaker. From a burette, add 45.0 mL of freshly standardized 0.1 M EDTA and 50 mL of methanol. Stir magnetically, and using a pH meter, adjust the pH of the solution to 5 with saturated aqueous ammonium acetate. Maintain the pH between 5.1 and 5.3 throughout the titration. Add 0.1 mL of PAN indicator solution, and continue to titrate with the 0.1 M copper sulfate volumetric solution to a permanent blue end point.

EDTA, 0.1 M Dissolve 37.22 g of Na2EDTA · 2H2O in 500 mL of water. Transfer quantitatively to a 1 L volumetric flask, dilute to volume with water, and mix thoroughly. Standardize as follows: Weigh accurately 0.40 g of calcium carbonate, chelometric standard (NIST SRM 915), previously dried at 210 °C for 4 h. Transfer to a 400 mL beaker, and add water. Cover the beaker with a watch glass, and introduce 4 mL of hydrochloric acid (1:1) from a pipette inserted between the lip of the beaker and the edge of the watch glass. Swirl the contents of the beaker to dissolve the calcium carbonate. Wash down the sides of the beaker and the watch glass with water, and dilute to 200 mL. While stirring, add from a 50 mL burette about 30 mL of the EDTA standard solution. Adjust the solution to pH 12–13 with 10% sodium hydroxide, and add 300 mg of hydroxy naphthol blue indicator mixture. Continue the titration with the EDTA volumetric standard solution to a blue end point.

Ferrous Ammonium Sulfate, 0.1 N Dissolve 39.21 g of ferrous ammonium sulfate hexahydrate in 200 mL of 25% sulfuric acid. Transfer quantitatively to a 1 L volumetric flask, dilute to volume with water, and mix thoroughly. On each day of use, standardize as follows: Measure accurately 40 mL of the solution into a 250 mL conical flask, add 0.1 mL of 1,10-phenanthroline reagent solution, and titrate with a freshly standardized 0.1 N ceric ammonium sulfate volumetric solution to the change from pink to pale blue.


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Preparation


Ferrous Sulfate, 0.1 N Dissolve 27.80 g of clear ferrous sulfate heptahydrate crystals in about 500 mL of water containing 50 mL of sulfuric acid. Transfer quantitatively to a 1 L volumetric flask, dilute to volume with water, and mix thoroughly. On each day of use, standardize as follows: Measure accurately 40 mL of the solution into a 250 mL conical flask, add 60 mL of water, and titrate with freshly standardized 0.1 N potassium permanganate to a pink end point. Perform a blank titration using only water.


Hydrochloric Acid, 1 N Add 85 mL of hydrochloric acid to 50 mL of water in a 1 L volumetric flask. Cool to room temperature, dilute to volume with water, and mix thoroughly. Standardize as follows: Weigh accurately about 2.2 g of sodium carbonate, alkalimetric standard (NIST SRM 351), that previously has been heated at 285 °C for 2 h. Dissolve in 100 mL of water, and add 0.1 mL of methyl red indicator solution. Add the acid slowly from a burette, with stirring, until the solution becomes faintly pink. Heat the solution to boiling, cool, and again titrate until the solution becomes faintly pink. Repeat this procedure until the faint color is no longer discharged on further boiling.

Iodine, 0.1 N Place approximately 40 g of potassium iodide and 10 mL of water in a large glass-stoppered weighing bottle. Mix the contents by swirling, allow to come to room temperature, and then weigh accurately. Add approximately 12.7 g of assayed iodine [Part 4: Iodine], previously weighed on a rough balance, and reweigh the stoppered bottle and contents to obtain the exact weight of the iodine added. Mix and transfer quantitatively to a 1 L amber volumetric flask. Dilute to volume with water, and mix thoroughly. Standardize as follows: Weigh accurately 0.21 g of arsenic trioxide reductometric standard (NIST SRM 83), previously dried for 12 h at 110 °C and cooled in a desiccator for 2 h, into a 250 mL iodine flask. Add 10 mL of 1.0 N sodium hydroxide, warm gently, and swirl to hasten dissolution, being certain that no particles of arsenic trioxide remain on the sides of the flask, and add 0.15 mL of phenolphthalein indicator solution. Neutralize with 6 M hydrochloric acid, and add 1 mL in excess of the acid. Add 75 mL of water and 2 g of sodium bicarbonate dissolved in 20 mL of water. Titrate with the iodine solution until within about 2 mL of the anticipated equivalence point. Then add 3 mL of starch indicator solution, and continue the titration to the first permanent blue color of the starch–iodine complex. Store in an opaque or amber glass bottle.

Lead Nitrate, 0.1 M Dissolve 33.12 g of lead nitrate in 300 mL of water. Transfer quantitatively to a 1 L volumetric flask, dilute to the mark with water, and mix thoroughly. Standardize as follows: Measure accurately 40 mL of the solution into a 400 mL beaker. Add 0.15 mL of acetic acid and 15 mL of a saturated aqueous solution of hexamethylenetetramine. Add a few milligrams of xylenol orange indicator mixture and titrate with freshly standardized 0.1 M EDTA volumetric solution to a yellow color.


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Preparation


Oxalic Acid, 0.1 N Dissolve 6.30 g of oxalic acid dihydrate in 200 mL of water in a 1 L volumetric flask, dilute to volume with water, and mix thoroughly. Standardize as follows: Measure accurately 40 mL of the solution in a 250 mL conical flask and add 50 mL of water and 7 mL of sulfuric acid. Add slowly, with stirring, 30 mL of freshly standardized 0.1 N potassium permanganate volumetric solution. Heat the solution to 70 °C, and continue the titration until the pink color persists for 30 s.


Perchloric Acid in Glacial Acetic Acid, 0.1 N

C a u t i o n : Perchloric acid in contact with some organic materials can form explosive mixtures. Use safety goggles and rubber gloves when preparing the solution. Rinse any glassware that has been in contact with perchloric acid before setting it aside.

Add slowly, with stirring, 8.5 mL of 70% perchloric acid to a mixture of 500 mL of glacial acetic acid and 21 mL of acetic anhydride. Cool, dilute to volume in a 1 L volumetric flask with glacial acetic acid, and mix thoroughly. Wait 30 min and determine the water content of the solution by titrating 30 g with Karl Fischer reagent [Part 3: Reagents, Buffers, and Indicators; Solutions and Mixtures; Karl Fischer Volumetric Reagent]. If the water content is greater than 0.05%, add a small amount of acetic anhydride, mix thoroughly, and again determine the water. Repeat until the water content is between 0.02% and 0.05%. In a similar manner, if the original water content is below 0.02%, add water to bring the water content into the 0.02–0.05% range. Allow the solution to stand for 24 h, and check the water content to be certain that it remains in this range. Standardize as follows: Weigh accurately about 0.7 g of potassium hydrogen phthalate, acidimetric standard (NIST SRM 84), previously lightly crushed and dried for 2 h at 120 °C. Dissolve in 50 mL of glacial acetic acid, add 0.1 mL of crystal violet indicator solution, and titrate with the perchloric acid solution until the violet color changes to blue-green. Perform a blank titration on 50 mL of glacial acetic acid in the same manner, and subtract the volume of perchloric acid solution consumed in the blank titration from that consumed in the first titration.

Potassium Bromate, 0.1 N Weigh accurately 2.78 g of potassium bromate, transfer to a 1 L volumetric flask, dilute to volume with water, and mix thoroughly. Standardize as follows: Measure accurately 40 mL of the solution into a 250 mL iodine flask, add 3 g of potassium iodide and 3 mL of hydrochloric acid, stopper the flask, and allow to stand in the dark for 5 min. Titrate the liberated iodine with a freshly standardized 0.1 N sodium thiosulfate volumetric solution. Add 3 mL of starch indicator solution near the end of the titration and continue to the absence of the blue starch–iodine complex.

Potassium Dichromate, 0.1 N Weigh accurately 4.90 g of potassium dichromate, previously dried for 2 h at 110 °C. Transfer to a 1 L volumetric flask, dilute to volume with water, and mix thoroughly. Standardize as follows: Measure accurately 40 mL of the solution into a


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Preparation


250 mL iodine flask, and add 100 mL of water, 3 g of potassium iodide, and 3 mL of hydrochloric acid. Stopper immediately, and allow to stand in the dark for 5 min. Titrate the liberated iodine with a freshly standardized 0.1 N sodium thiosulfate solution. Add 3 mL of a starch indicator solution near the end of the titration, and continue to the absence of the blue starch–iodine complex.


Potassium Hydroxide, Methanolic, 0.1 N Dissolve 6.8 g of potassium hydroxide in a minimum amount of water (about 5 mL) in a 1 L volumetric flask. Dilute to volume with methanol, and mix thoroughly. Allow to stand in a container protected from carbon dioxide for 24 h. Carefully decant the clear solution, leaving any residue behind, into a suitable container, mix well, and store protected from carbon dioxide. Standardize as follows: Weigh accurately about 0.85 g of potassium hydrogen phthalate, acidimetric standard (NIST SRM 84), previously lightly crushed and dried for 2 h at 120 °C. Dissolve in 100 mL of carbon dioxide-free water, add 0.15 mL of phenolphthalein indicator solution, and titrate with the methanolic potassium hydroxide solution to a permanent faint pink color.

Potassium Iodate, 0.05 M (0.3 N) Weigh exactly 10.70 g of potassium iodate, previously dried at 110 °C to constant weight, transfer to a 1 L volumetric flask, dilute to volume with water, and mix thoroughly. Standardize as follows: To 15.0 mL of solution in a 250 mL iodine flask, add 3 g of potassium iodide and 3 mL hydrochloric acid previously diluted with 10 mL of water. Stopper immediately, and allow to stand in the dark for 5 min. Then add 50 mL of cold water, and titrate the liberated iodine with freshly standardized 0.1 N sodium thiosulfate. Add 3 mL of starch indicator solution near the end of the titration, and continue to the absence of the blue starch–iodine complex.

Potassium Permanganate, 0.1 N Dissolve 3.3 g of potassium permanganate in 1 L of water in a 1500 mL conical flask, heat to boiling, and boil gently for 15 min. Allow to cool, stopper, and keep in the dark for 48 h. Then filter through a fine-porosity sintered-glass filter, and place in a glass-stoppered amber bottle. Standardize as follows: Weigh accurately about 0.26 g of sodium oxalate (NIST SRM 8040), previously dried for 2 h at 105 °C, transfer to a 500 mL conical flask containing 250 mL of water and 7 mL of sulfuric acid, and heat to 70 °C. Titrate immediately with the permanganate solution to a pink color that persists for 15 s. The temperature at the end of the titration should not be less than 60 °C. Perform a blank titration containing 250 mL of water and 7 mL of sulfuric acid in the same manner, and subtract the volume of the potassium permanganate consumed in the blank from the first titration. Store in an opaque or amber glass container.


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Preparation


Potassium Thiocyanate, 0.1 N


Weigh exactly 9.72 g of potassium thiocyanate, previously dried for 2 h at 110 °C, transfer to a 1 L volumetric flask, dilute to volume, and mix thoroughly. Standardize as follows: Measure accurately 40 mL of freshly standardized 0.1 N silver nitrate volumetric solution into a 250 mL conical flask, and add 100 mL of water, 1 mL of nitric acid, and 2 mL of ferric ammonium sulfate indicator solution. Titrate with the thiocyanate solution, with agitation, to a permanent light pink-brown color of the supernatant solution.

Silver Nitrate, 0.1 N Weigh exactly 16.99 g of silver nitrate, previously dried for 1 h at 100 °C, transfer to a 1 L amber volumetric flask, dilute to volume, and mix thoroughly. Standardize as follows: Weigh accurately about 0.33 g of potassium chloride (NIST SRM 999) ignited at 500 °C. Place in a 250 mL beaker, and dissolve in 100 mL of water. Add 2 mL of dichlorofluorescein indicator solution. With stirring, titrate with silver nitrate solution until the silver chloride flocculates and the mixture acquires a faint pink color. Store in an opaque container.

Sodium Acetate in Glacial Acetic Acid, 0.1 N Place 8.20 g of sodium acetate, anhydrous, previously dried to constant weight at 120 °C, in a 1 L volumetric flask. Add 500 mL of glacial acetic acid and 10 mL of acetic anhydride, and dissolve. Dilute to volume with glacial acetic acid, and mix thoroughly. Standardize as follows: Measure accurately 40 mL of freshly standardized perchloric acid in glacial acetic acid volumetric solution, and add 0.1 mL of crystal violet indicator solution. While stirring, titrate with the sodium acetate until the solution changes from an emerald green to a violet color.

Sodium Hydroxide, 1 N Dissolve 162 g of sodium hydroxide in 150 mL of carbon dioxide-free water, and cool the solution to room temperature. Prepare a 1 N solution by diluting 54.5 mL of the concentrated solution to 1 L with carbon dioxide-free water. Mix thoroughly, and store in a tight polyolefin container. Standardize as follows: Weigh accurately about 8.5 g of potassium hydrogen phthalate, acidimetric standard (NIST SRM 84), previously lightly crushed and dried for 2 h at 120 °C. Dissolve in 100 mL of carbon dioxide-free water, add 0.15 mL of phenolphthalein indicator solution, and titrate with the sodium hydroxide solution to a permanent faint pink color.


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Preparation


Sodium Methoxide in Methanol, 0.01 N


Dilute 20.0 mL of sodium methoxide in methanol, 0.5 M methanolic solution, with methanol to 1 L and mix thoroughly. Standardize as follows: Measure accurately 40 mL of 0.01 N sulfuric acid volumetric solution into a suitable container, add 0.10 mL of thymol blue indicator solution, and titrate with the sodium methoxide in methanol solution to a blue end point.

Sodium Nitrite, 0.1 N Weigh accurately 6.90 g of sodium nitrite. Dissolve in 100 mL of water in a 1 L volumetric flask, dilute to volume, and mix thoroughly. Standardize as follows: Add 5 mL of sulfuric acid to 200 ml of water, and while the solution is still warm, add 0.1 N potassium permanganate until a faint pink color persists for 2 min. Measure accurately 50 mL of freshly standardized 0.1 N potassium permanganate, transfer to the solution, and mix gently. Pipette, slowly and with constant agitation, 40 mL of the sodium nitrite solution, holding the tip of the pipette well below the surface of the liquid. Add 3 g of potassium iodide, and titrate the liberated iodine from the excess of potassium permanganate with 0.1 N sodium thiosulfate. Add 3 mL of starch indicator near the end point, and titrate to the absence of the blue starch–iodine complex. Perform a complete blank using all reagents except the 0.1 N sodium nitrite solution.

Sodium Thiosulfate, 0.1 N Dissolve 24.82 g of sodium thiosulfate pentahydrate and 200 mg of sodium carbonate, anhydrous, in 1 L of recently boiled and cooled water, and mix thoroughly. Allow to stand for 24 h, and standardize as follows: Weigh accurately about 0.21 g of NIST potassium dichromate, oxidimetric standard (NIST SRM 136), previously crushed and dried at 110 °C for 2 h. Dissolve in 100 mL of water in a glass-stoppered iodine flask. Swirl to dissolve the sample, remove the stopper, and quickly add 3 g of potassium iodide, 2 g of sodium bicarbonate, and 5 mL of hydrochloric acid. Insert the stopper, swirl slightly to release excess carbon dioxide, cover the stopper with water, and allow to stand in the dark for 10 min. Rinse the stopper and the inner walls of the flask with water and titrate the liberated iodine with the sodium thiosulfate until the solution becomes faintly yellow. Add 3 mL of starch indicator solution, and continue the titration to the disappearance of the blue starch–iodine complex. Restandardize the solution frequently.

Sulfuric Acid, 1 N Add slowly (use caution), with stirring, 30 mL of sulfuric acid to about 500 mL of water. Allow the mixture to cool to room temperature, dilute to 1 L, and mix thoroughly. Standardize against sodium carbonate, alkalimetric standard, as directed for hydrochloric acid, 1 N.


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Preparation


Zinc Chloride, 0.1 M Weigh accurately 6.54 g of zinc (13.63 g of ZnCl2), and dissolve in 80 mL of 10% hydrochloric acid. Warm if necessary to complete dissolution, cool, dilute with water to volume in a 1 L volumetric flask, and mix thoroughly. Standardize as follows: Pipette and transfer 40.0 ml of zinc chloride solution to a 400 mL beaker with sufficient hexamethylene tetramine to produce a purple-red color. Titrate with freshly standardized 0.1 M EDTA to a color change of purple-red to lemon yellow.


Zinc Sulfate, 0.1 M Weigh accurately 28.76 g of zinc sulfate heptahydrate, and dissolve in 500 mL of water in a 1 L volumetric flask. Dilute to the mark with water, and mix thoroughly. Standardize as follows: To 40.0 mL of freshly standardized 0.1 M EDTA volumetric solution, in a suitable beaker, add 10 mL of ammonium acetate–acetic acid buffer solution, 50 mL of ethyl alcohol, and 2 mL of dithizone indicator solution. Titrate with the zinc sulfate solution to a pink end point.


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Volumetric Solutions - ACS Reagent Chemicals (ACS Publications)

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