Monograph pubs.acs.org/doi/book/10.1021/acsreagents
Acetic Acid, Ultratrace Part 4, Monographs for Reagent Chemicals: General Descriptions, Specifications, and Tests eISBN: 9780841230460 Tom Tyner Chair, ACS Committee on Analytical Reagents James Francis Secretary, ACS Committee on Analytical Reagents
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ABSTRACT This monograph for Acetic Acid, Ultratrace provides, in addition to common physical constants, a general description including typical appearance, applications, change in state (approximate), aqueous solubility, and pKa. The monograph also details the following specifications and corresponding tests for verifying that a substance meets ACS Reagent Grade specifications including: Assay, Chloride, Sulfate, Mercury, and Trace Metals.
CH3COOH
Formula Wt 60.05
CAS No. 64-19-7
Suitable for use in ultratrace elemental analysis. Note: Reagent must be packaged in a preleached Teflon bottle and used in a clean laboratory environment to maintain purity.
GENERAL DESCRIPTION Typical appearance . . . . . . . . Applications . . . . . . . . . . . . . Change in state (approximate) . Aqueous solubility . . . . . . . . . pKa . . . . . . . . . . . . . . . . . .
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clear liquid with a sharp odor trace metal analysis boiling point, 118 °C; freezing point, 16 °C miscible with water 4.8
SPECIFICATIONS Assay . . . . . . . . . . . . . . . . . . . . . . . . . . . . ≥90% CH3COOH Maximum Allowable Chloride (Cl) . . . . . . . . . . . . . . . . . . . . . . . 1 ppm Sulfate (SO4) . . . . . . . . . . . . . . . . . . . . . . . 1 ppm Mercury (Hg) . . . . . . . . . . . . . . . . . . . . . . . 1 ppb Aluminum (Al) . . . . . . . . . . . . . . . . . . . . . . 1 ppb Barium (Ba) . . . . . . . . . . . . . . . . . . . . . . . . 1 ppb
© 2017 American Chemical Society
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ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.4003 ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals
Monograph
Downloaded by CORNELL UNIV on June 7, 2017 | http://pubs.acs.org Publication Date (Web): February 28, 2017 | doi: 10.1021/acsreagents.4003
pubs.acs.org/doi/book/10.1021/acsreagents
Boron (B) . . . . . Cadmium (Cd) . . Calcium (Ca) . . . Chromium (Cr) . . Cobalt (Co) . . . . Copper (Cu) . . . . Iron (Fe) . . . . . . Lead (Pb) . . . . . Lithium (Li) . . . . Magnesium (Mg) . Manganese (Mn) . Molybdenum (Mo) Potassium (K) . . . Silicon (Si) . . . . . Sodium (Na) . . . . Strontium (Sr) . . Tin (Sn). . . . . . . Titanium (Ti) . . . Vanadium (V) . . . Zinc (Zn) . . . . . . Zirconium (Zr) . .
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5 1 1 1 1 1 5 1 1 1 1 1 1 5 5 1 1 1 1 1 1
ppb ppb ppb ppb ppb ppb ppb ppb ppb ppb ppb ppb ppb ppb ppb ppb ppb ppb ppb ppb ppb
TESTS Assay (By acid–base titrimetry). The assay of acetic acid used for ultratrace metal analysis may vary, depending on the method of purification. Tare a glass-stoppered flask containing about 30 mL of water. Quickly add about 3 mL of the sample, stopper, and weigh accurately. Dilute to about 50 mL, add 0.15 mL of methyl orange indicator solution, and titrate with 1 N sodium hydroxide. One milliliter of 1 N sodium hydroxide corresponds to 0.06005 g of acetic acid.
Chloride [Part 2: Colorimetry and Turbidimetry; Chloride]. Dissolve 10.0 g in 10 mL of water.
Sulfate To 48 mL (50 g) of sample, add 2 mL of 1% sodium carbonate solution, and evaporate to dryness on a hot plate (~100 °C). Dissolve the residue in 1.0 mL of 10% hydrochloric acid and 15 mL of water. Dilute to 25 mL with water. For the control, take 0.05 mg of sulfate ion (SO4) in 20 mL of water, add 1.0 mL of 10% hydrochloric acid, and dilute to 25 mL. To sample and control solutions, add 1 mL of 12% barium chloride solution. Compare after 10 min. Sample turbidity should not exceed that of the control solution.
© 2017 American Chemical Society
B
ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.4003 ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
Mercury (By CVAAS, [Part 2: Trace and Ultratrace Elemental Analysis; Mercury Determination by CVAAS]). To a set of three 100 mL volumetric flasks containing about 35 mL of water, add 20.0 g of sample. To the second and third flasks, add mercury ion (Hg) standards of 10 ng (0.5 ppb) and 20 ng (1.0 ppb), respectively. Add 5 mL of nitric acid to all three flasks, and dilute to the mark with water. Mix. Zero the instrument with the blank, and determine the mercury content using a suitable mercury analyzer system (1.0 mL of 0.01 μg/mL Hg = 10 ng).
Trace Metals
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Determine aluminum, barium, boron, cadmium, calcium, chromium, cobalt, copper, iron, lead, lithium, magnesium, manganese, molybdenum, potassium, silicon, sodium, strontium, tin, titanium, vanadium, zinc, and zirconium by the ICP–OES Preconcentration method described in [Part 2: Trace and Ultratrace Elemental Analysis; Inductively Coupled Plasma−Optical Emission Spectroscopy (ICP–OES); Preconcentration of Ultratrace-Grade Reagents for Analysis by ICP–OES].
© 2017 American Chemical Society
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ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.4003 ACS Reagent Chemicals, Part 4
