Monograph

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

Perchloric Acid
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 Perchloric Acid provides, in addition to common physical constants, a general description including
typical appearance, applications, and pKa. The monograph also details the following specifications and corresponding
tests for verifying that a substance meets ACS Reagent Grade specifications including: Assay, Color (APHA), Residue
after Ignition, Silicate, Phosphate, Chloride, Nitrogen Compounds, Sulfate, Heavy Metals, and Iron.

HClO4 Formula Wt 100.46 CAS No. 7601-90-3

Note: This specification applies to perchloric acid with nominal concentrations of 50%, 60%, or 70%.

GENERAL DESCRIPTION
Typical appearance . . . . . . . . . . . . . . . . . . . clear, colorless liquid
Applications . . . . . . . . . . . . . . . . . . . . . . . . solvent for metals and ores; standard acid; oxidizer; nonaqueous
titrimetry; wet ashing
pKa . . . . . . . . . . . . . . . . . . . . . . . . . . . . . < –10

SPECIFICATIONS
Assay . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48.0–50.0% HClO4; 60.0–62.0% HClO4; 69.0–72.0% HClO4
Maximum Allowable
Color (APHA) . . . . . . . . . . . . . . . . . . . . . . . 10
Residue after ignition. . . . . . . . . . . . . . . . . . 0.003%
Silicate and phosphate (as SiO2) . . . . . . . . . . . 5 ppm
Chloride (Cl) . . . . . . . . . . . . . . . . . . . . . . . 0.001%
Nitrogen compounds (as N) . . . . . . . . . . . . . . 0.001%
Sulfate (SO4) . . . . . . . . . . . . . . . . . . . . . . . 0.001%
Heavy metals (as Pb) . . . . . . . . . . . . . . . . . . 1 ppm
Iron (Fe) . . . . . . . . . . . . . . . . . . . . . . . . . . 1 ppm

DOI:10.1021/acsreagents.4257
© 2017 American Chemical Society A ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals Monograph

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

TESTS

Note: All tests are written for 70% concentration. The densities of the 60% acid (1.54 g/mL) and the 50% acid (1.40 g/
mL) are less than the density of the 70% reagent (1.67 g/mL), and proper allowance should be made for this when
measured volumes are taken for relevant tests.

Assay
(By alkalimetric titration). Weigh accurately about 3 mL in a suitable flask, and dilute with water to 60 mL. Add 0.15 mL of
phenolphthalein indicator solution, and titrate with 1 N sodium hydroxide volumetric solution. One milliliter of 1 N sodium
hydroxide corresponds to 0.1005 g of HClO4.

Color (APHA)
[Part 2: Measurement of Physical Properties; Color (APHA); Procedure for Color (APHA)].

Residue after Ignition

[Part 2: Gravimetric Methods; Residue after Ignition]. To 67 g (42 mL) in a tared, preconditioned dish, add 1 mL of nitric
acid, evaporate to dryness, and ignite at 600 ± 25 °C for 15 min.

Silicate and Phosphate

Dilute 2.0 g (1.2 mL) with 50 mL of water in a platinum dish, add 1.0 g of sodium carbonate, and digest on a hot plate (~100
°C) for 15–30 min. Cool, add 5 mL of a 10% ammonium molybdate reagent solution, acidify with hydrochloric acid to about
pH 4 (using indicator paper), and transfer to a beaker. Adjust the pH to 1.8 (using a pH meter) with dilute hydrochloric acid
(1:9). Dilute with water to 90 mL, heat just to boiling, and cool to room temperature. Add 10 mL of hydrochloric acid, and
dilute with water to 100 mL. Transfer to a separatory funnel, add 50 mL of 4-methyl-2-pentanone, shake vigorously, and
allow to separate. Draw off and discard the aqueous phase. Wash the ketone layer three times with 20 mL portions of dilute
hydrochloric acid (1:99), drawing off and discarding the aqueous layer each time. Add 10 mL of dilute hydrochloric acid
(1:99), to which has just been added 0.2 mL of a freshly prepared 2% stannous chloride reagent solution. Shake vigorously,
and allow to separate. Any blue color should not exceed that produced by 0.01 mg of silica and 1 g of sodium carbonate,
treated exactly like the sample.

Chloride
[Part 2: Colorimetry and Turbidimetry; Chloride]. Dilute 1 g (0.6 mL) with 25 mL of water.

Nitrogen Compounds
[Part 2: Colorimetry and Turbidimetry; Nitrogen Compounds: Test for Ammonia, Amines, and Nitrogen Compounds Reduced
by Aluminum]. Use 5 g (3.0 mL). For the standard, use 0.05 mg of nitrogen ion (N).

DOI:10.1021/acsreagents.4257
© 2017 American Chemical Society B ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals Monograph

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

Sulfate
Dilute 32.0 g (20 mL) with water to 160 mL, and neutralize with ammonium hydroxide, using litmus paper as an indicator.
Add 1 mL of hydrochloric acid, heat to boiling, add 5 mL of 12% barium chloride reagent solution, digest in a covered beaker
on a hot plate (~100 °C) for 2 h, and allow to stand for at least 8 h. If a precipitate is formed, filter, wash thoroughly, and
ignite. The weight of the precipitate should not be more than 0.0008 g greater than the weight obtained from a complete
blank test, including the evaporated residue from a volume of ammonium hydroxide equal to that used to neutralize the
sample.

†
For the Determination of Heavy Metals and Iron
S a m p l e S o l u t i o n A . To 40.0 g (25 mL), add 1 mL of nitric acid and 1 mL of 1% sodium carbonate reagent solution.
Evaporate to dryness on a hot plate in a well-ventilated hood, dissolve the residue in 2 mL of 1 N acetic acid, and
dilute with water to 40 mL (1 mL = 1.0 g).

Heavy Metals†
[Part 2: Colorimetry and Turbidimetry; Heavy Metals (as Lead); Procedure for Heavy Metals, Method 1]. Dilute 20 mL of
sample solution A (20 g sample) with water to 25 mL.

Iron†
[Part 2: Colorimetry and Turbidimetry; Iron; Procedure for Iron, Method 1 (Ammonium Thiocyanate)]. Use 10 mL of sample
solution A (10 g sample).

DOI:10.1021/acsreagents.4257
© 2017 American Chemical Society C ACS Reagent Chemicals, Part 4