Monograph pubs.acs.org/doi/book/10.1021/acsreagents
Nitric 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 Nitric Acid, Ultratrace provides, in addition to common physical constants, a general description including typical appearance, applications, change in state (approximate), aqueous solubility, density, 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.
HNO3
Formula Wt 63.01
CAS No. 7697-37-2
Suitable for use in ultratrace elemental analysis. Note: This material may darken during storage as a result of photochemical reactions. 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 . . . . . . . . . Density . . . . . . . . . . . . . . . . pKa . . . . . . . . . . . . . . . . . .
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clear, colorless liquid; fuming in moist air with a characteristic odor analysis for trace metal content boiling point, 83 °C miscible 1.50 –2.3
SPECIFICATIONS Assay . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65–70% HNO3 Maximum Allowable Chloride (Cl) . . . . . . . . . . . . . . . . . . . . . . . 0.5 ppm Sulfate (SO4) . . . . . . . . . . . . . . . . . . . . . . . 1 ppm Mercury (Hg) . . . . . . . . . . . . . . . . . . . . . . . 1 ppb Aluminum (Al) . . . . . . . . . . . . . . . . . . . . . . 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.4244 ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals
Monograph
Downloaded by CORNELL UNIV on June 12, 2017 | http://pubs.acs.org Publication Date (Web): February 28, 2017 | doi: 10.1021/acsreagents.4244
pubs.acs.org/doi/book/10.1021/acsreagents
Barium (Ba) . . . . 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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1 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 ppb
TESTS Assay (By acid–base titrimetry). Tare a small, glass-stoppered flask containing about 15 mL of water. Quickly pipette about 2 mL of the sample under the surface, stopper, and weigh accurately. Dilute with about 40 mL of water, add 0.15 mL of methyl orange indicator solution, and titrate with 1 N sodium hydroxide volumetric solution. One milliliter of 1 N sodium hydroxide corresponds to 0.06301 g of HNO3.
Chloride See test as for nitric acid, [Part 4: Nitric Acid].
Sulfate [Part 2: Colorimetry and Turbidimetry; Sulfate; Procedure for Sulfate, Method 3]. Use a 50 g sample.
Mercury (By CVAAS, [Part 2: Trace and Ultratrace Elemental Analysis; Mercury Determination by CVAAS]). To each 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
© 2017 American Chemical Society
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ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.4244 ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
(Hg) standards of 10 ng (0.5 ppb) and 20 ng (1.0 ppb), respectively. 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 the 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.4244 ACS Reagent Chemicals, Part 4
