Monograph pubs.acs.org/doi/book/10.1021/acsreagents
Sulfuric 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
ABSTRACT This monograph for Sulfuric 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, Nitrate, Mercury, Selenium, and Trace Metals.
H2SO4
Formula Wt 98.07
CAS No. 7664-93-9
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 . . . . . . . . . Density . . . . . . . . . . . . . . . . pKa . . . . . . . . . . . . . . . . . .
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clear, colorless liquid digestion for trace analysis boiling point, 290 °C miscible; generates heat 1.84 ~ –3
SPECIFICATIONS Assay . . . . . . . . . . . . . . . . . . . . . . . . . . . . 85–98% H2SO4 Maximum Allowable Chloride (Cl) . . . . . . . . . . . . . . . . . . . . . . . 0.2 ppm Nitrate (NO3) . . . . . . . . . . . . . . . . . . . . . . . 0.5 ppm Mercury (Hg) . . . . . . . . . . . . . . . . . . . . . . . 1 ppb Selenium (Se) . . . . . . . . . . . . . . . . . . . . . . . 100 ppb
© 2017 American Chemical Society
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DOI:10.1021/acsreagents.4389 ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals
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pubs.acs.org/doi/book/10.1021/acsreagents
Aluminum (Al) . . 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 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 ppb
TESTS Assay (By acid–base titrimetry). Tare a small, glass-stoppered flask, add about 1 mL of the sample, and weigh accurately. Cautiously add 30 mL of water, cool, 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 0.04904 g of H2SO4.
Chloride [Part 2: Colorimetry and Turbidimetry; Chloride].
Nitrate [Part 2: Colorimetry and Turbidimetry; Nitrate; Procedure for Nitrate, Method 1 (Brucine Sulfate)].
Mercury (By CVAAS, [Part 2: Trace and Ultratrace Elemental Analysis; Mercury Determination by CVAAS]). Cool each of three 100 mL volumetric flasks containing about 35 mL of water in an ice-water bath for 15 min, and then slowly and cautiously add 10.0 g
© 2017 American Chemical Society
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DOI:10.1021/acsreagents.4389 ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
of sample to each. To the second and third flasks, add mercury ion (Hg) standards of 10 ng (1.0 ppb) and 20 ng (2.0 ppb), respectively. Add 5 mL of nitric acid to all, and dilute to the mark with water. Mix. Zero the instrument with a blank, and determine the mercury content using a suitable mercury analyzer system. Cool to room temperature (1.0 mL of 0.01 µ/mL Hg = 10 ng).
Selenium (By HGAAS, [Part 2: Trace and Ultratrace Elemental Analysis; Selenium Determination by HGAAS; Analysis; Procedure for Selenium Determination by HGAAS]). To a set of three 100 mL volumetric flasks, transfer 10.0 g (5.4 mL) of sample. To two flasks, add selenium ion (Se) standards of 1.0 µg (100 ppb) and 2.0 µg (200 ppb), respectively. Dilute each to 100 mL with (1:1) hydrochloric acid. Mix. Prepare fresh working standard before use.
Trace Metals 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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DOI:10.1021/acsreagents.4389 ACS Reagent Chemicals, Part 4
