Monograph

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

Xylenes
(Dimethylbenzenes)
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 Xylenes provides, in addition to common physical constants, a general description including typical
appearance, applications, change in state (approximate), aqueous solubility, and density. 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 Evaporation, Substances Darkened by Sulfuric Acid, Sulfur
Compounds, and Water.

C6H4(CH3)2 Formula Wt 106.17 CAS No. 1330-20-7

Note: This reagent is generally a mixture of the ortho, meta, and para isomers and may contain some ethylbenzene.

GENERAL DESCRIPTION
Typical appearance . . . . . . . . . . . . . . . . . . . clear liquid
Applications . . . . . . . . . . . . . . . . . . . . . . . . solvent
Change in state (approximate) . . . . . . . . . . . . boiling point, 140 °C
Aqueous solubility . . . . . . . . . . . . . . . . . . . . insoluble
Density . . . . . . . . . . . . . . . . . . . . . . . . . . . 0.87

DOI:10.1021/acsreagents.4423
© 2017 American Chemical Society A ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals Monograph

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

SPECIFICATIONS
Assay . . . . . . . . . . . . . . . . . . . . . . . . . . . . ≥98.5% xylene isomers plus ethylbenzene (ethylbenzene not to exceed
25%)
Maximum Allowable
Color (APHA) . . . . . . . . . . . . . . . . . . . . . . . 10
Residue after evaporation . . . . . . . . . . . . . . . 0.002%
Substances darkened by sulfuric acid . . . . . . . . Passes test
Sulfur compounds (as S) . . . . . . . . . . . . . . . . 0.003%
Water (H2O) . . . . . . . . . . . . . . . . . . . . . . . . 0.05%

TESTS
Assay
Analyze the sample by gas chromatography using the general parameters cited in [Part 2: Chromatography; Recommended
Procedures; Gas Chromatography]. The following specific conditions are also required.
Column . . . . . . . . . . . . . . . . . . . . . . . . . . Type I, methyl silicone

Measure the area under all peaks, and calculate the area percent of each peak. The total percent of xylenes is the sum of
the percents of ortho, meta, and para isomers and of ethylbenzene. Correct for water content.

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

Residue after Evaporation

[Part 2: Gravimetric Methods; Residue after Evaporation]. Evaporate 100 g (115 mL) to dryness in a tared, preconditioned
dish on a hot plate (~100 °C), and dry the residue at 105 °C for 30 min.

Substances Darkened by Sulfuric Acid

Shake 15 mL with 5 mL of sulfuric acid for 15–20 s, and allow to stand for 15 min. The xylene layer should be colorless, and
the color of the acid should not exceed that of a color standard composed of 1 volume of water and 3 volumes of a color
standard solution (described below).

For the Determination of Substances Darkened by Sulfuric Acid

C o l o r S t a n d a r d S o l u t i o n . In a 1 L volumetric flask, add 5 g of cobalt chloride hexahydrate, 40 g of ferric chloride

hexahydrate, and 20 mL of hydrochloric acid. Dilute to the mark with water.

Sulfur Compounds
Place 30 mL of approximately 0.5 N potassium hydroxide in methanol in a conical flask, add 6.0 mL of the sample, and boil
the mixture gently for 30 min under a reflux condenser, avoiding the use of a rubber stopper or connection. Detach the
condenser, dilute with 50 mL of water, and heat on a hot plate (~100 °C) until the xylenes and methanol have evaporated.
Add 50 mL of bromine water, and heat for 15 min longer. Transfer the solution to a beaker, neutralize with dilute
hydrochloric acid (1:3), add an excess of 1 mL of the acid, and concentrate to about 50 mL. Filter if necessary, heat the

DOI:10.1021/acsreagents.4423
© 2017 American Chemical Society B ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals Monograph

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

filtrate 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. Correct for the weight
obtained in a completed blank test.

Water
[Part 2: Titrimetric Methods; Water by the Karl Fischer Method; Coulometric Procedure; Coulometric Procedure for Samples
Using Karl Fischer Reagent, Method 2]. Use 100 µL (87 mg) of the sample.

DOI:10.1021/acsreagents.4423
© 2017 American Chemical Society C ACS Reagent Chemicals, Part 4