Monograph

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

Water, Reagent
(Distilled Water, Deionized Water)
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 Water, Reagent provides, in addition to common physical constants, a general description including
typical appearance, applications, change in state (approximate), density, and pKa. The monograph also details the
following specifications and corresponding tests for verifying that a substance meets ACS Reagent Grade specifications
including: Specific Conductance, Silicate, Heavy Metals, Substances Reducing Permanganate, Chloride, Nitrate,
Phosphate, Sulfate, Ultraviolet Spectrophotometry, and Liquid Chromatography Suitability.

H2O Formula Wt 18.015 CAS No. 7732-18-5

Note: The specifications for water are for freshly dispensed material and not intended for bottled or stored product.

GENERAL DESCRIPTION
Typical appearance . . . . . . . . . . . . . . . . . . . clear, colorless liquid
Applications . . . . . . . . . . . . . . . . . . . . . . . . solvent; diluent
Change in state (approximate) . . . . . . . . . . . . boiling point, 100 °C
Density . . . . . . . . . . . . . . . . . . . . . . . . . . . 0.99
pKa . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15.7

SPECIFICATIONS
General Use
Maximum Allowable
Specific conductance at 25 °C . . . . . . . . . . . 2.0 × 10–6 ohm–1 cm–1
Silicate (as SiO2) . . . . . . . . . . . . . . . . . . . . 0.01 ppm
Heavy metals (as Pb) . . . . . . . . . . . . . . . . . 0.01 ppm

DOI:10.1021/acsreagents.4421
© 2017 American Chemical Society A ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals Monograph

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

Substances reducing permanganate . . . . . . . . Passes test

Chloride (Cl) . . . . . . . . . . . . . . . . . . . . . . 0.4 ppm
Nitrate (NO4) . . . . . . . . . . . . . . . . . . . . . . 0.4 ppm
Phosphate (PO4) . . . . . . . . . . . . . . . . . . . . 1.0 ppm
Sulfate (SO4) . . . . . . . . . . . . . . . . . . . . . . 1.0 ppm

Specific Use
Ultraviolet Spectrophotometry
Wavelength (nm) Absorbance (AU)
300 . . . . . . . . . . . . . . . . . . . . . . . . . . . . 0.005
254 . . . . . . . . . . . . . . . . . . . . . . . . . . . . 0.005
210 . . . . . . . . . . . . . . . . . . . . . . . . . . . . 0.010
200 . . . . . . . . . . . . . . . . . . . . . . . . . . . . 0.010
Liquid Chromatography Suitability
Absorbance . . . . . . . . . . . . . . . . . . . . . . . Passes test
Gradient elution . . . . . . . . . . . . . . . . . . . . Passes test

TESTS
Specific Conductance
Fill a conductance cell that has been properly standardized. Take precautions to prevent the water from absorbing carbon
dioxide, ammonia, hydrogen chloride, or any other gases commonly present in a laboratory. Immerse in a constant-
temperature bath at 25 °C, equilibrate, and measure the resistance with a suitable conductance bridge. The calculated
specific conductance should not exceed 2.0 × 10–6 ohm–1 cm–1.

Silicate
Evaporate 1500 mL to 80 mL in a platinum dish on a hot plate (~100 °C) (in portions, if necessary). Add 10 mL of silica-free
ammonium hydroxide (described below), cool, and add 5 mL of a 10% ammonium molybdate reagent solution. Adjust the pH
to between 1.7 and 1.9 (using a pH meter) with hydrochloric acid or silica-free ammonium hydroxide. Heat the solution just
to boiling, cool to room temperature, and dilute with water to 90 mL. Transfer the solution to a separatory funnel, add 10
mL of hydrochloric acid and 35 mL of ethyl ether, and shake vigorously for a few minutes. Allow the two layers to separate,
draw off the aqueous layer into another separatory funnel, and add 10 mL of hydrochloric acid and 50 mL of butyl alcohol.
Shake vigorously, allow to separate, draw off the aqueous phase, and discard. Wash the butyl alcohol phase three times
with 20 mL of dilute hydrochloric acid (1:99), discarding the aqueous solution each time. Add 0.5 mL of freshly prepared 2%
stannous chloride reagent solution to the butyl alcohol. Any blue color should not exceed that produced by 0.015 mg of
silica ion (SiO2) (use the silicate solution in ammonium hydroxide, described below) when treated exactly like the sample.
Because the blue color fades on standing, compare immediately after the reduction with stannous chloride. Treatment
again with stannous chloride will restore a fading blue color to its original intensity.

For the Determination of Silicate

A m m o n i u m H y d r o x i d e , S i l i c a - F r e e . Aqueous ammonia in contact with glass, even momentarily, will dissolve

sufficient silica to make the reagent useless for this test. Because ammonium hydroxide is ordinarily supplied in glass
containers by commercial sources, silica-free ammonium hydroxide must be prepared in the laboratory. The most
convenient method is the saturation of water with ammonia gas from a cylinder of compressed anhydrous ammonia.
Plastic tubing and bottles (for example, polyethylene) must be used throughout.

DOI:10.1021/acsreagents.4421
© 2017 American Chemical Society B ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals Monograph

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

S i l i c a t e S o l u t i o n i n A m m o n i u m H y d r o x i d e . (0.01 mg of SiO2 in 1 mL). To prepare a stock solution of silica, dissolve

0.946 g of assayed sodium silicate in 9 mL of silica-free ammonium hydroxide, and dilute to 100 mL (99.7 g at 25 °C)
with water. Dilute 5.0 mL of this solution plus 5 mL of silica-free ammonium hydroxide to 1 L (997.1 g at 25 °C) with
water. If volumetric polyolefin ware is unavailable, dilute the silica solution by weight.

Heavy Metals
[Part 2: Colorimetry and Turbidimetry; Heavy Metals (as Lead); Procedure for Heavy Metals, Method 1]. Add 10 mg of sodium
chloride and 1 mL of 1 N hydrochloric acid to 2 L of sample, and evaporate to dryness on a hot plate (~100 °C). Dissolve the
residue in about 20 mL of water, and dilute with water to 25 mL. For the control, evaporate 1 mL of 1 N hydrochloric acid to
dryness on a hot plate (~100 °C), cool, add 0.02 mg of lead ion (Pb), and dilute with water to 25 mL.

Substances Reducing Permanganate

To 500 mL, add 1 mL of sulfuric acid and 0.30 mL of 0.01 N potassium permanganate, and allow to stand for 1 h at room
temperature. The pink color should not be entirely discharged.

Chloride, Nitrate, Phosphate, and Sulfate

To each of three 100 mL beakers, add 2.0 mg of sodium carbonate. To two beakers, add 50 mL of the sample. To one of these
beakers (the standard), add 0.02 mg each of chloride and nitrate ions and 0.05 mg each of phosphate and sulfate ions. To
the third beaker (blank), add 20 mL of 0.06 micromho cm–1 (resistivity 17 megohm cm) water. Evaporate each beaker on a
steam bath or low-temperature hot plate to about 20 mL. Cool. Dilute to 25 mL. Analyze 100 µL aliquots by ion
chromatography, and measure the various peaks. The differences between the sample and the blank should not be greater
than the corresponding differences between the standard and the sample.

Ultraviolet Spectrophotometry
Use the procedure in [Part 2: Chromatography; Recommended Procedures; LC Suitability; Procedure for Absorbance] to
determine the absorbance.

Liquid Chromatography Suitability

Analyze the sample by using the general procedure in [Part 2: Chromatography; Recommended Procedures; Liquid
Chromatography; Solvent Suitability for Liquid Chromatography; Procedure for Liquid Chromatography]. Use the procedure
in [Part 2: Chromatography; Recommended Procedures; LC Suitability; Procedure for Absorbance] to determine the
absorbance.

DOI:10.1021/acsreagents.4421
© 2017 American Chemical Society C ACS Reagent Chemicals, Part 4