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Monograph

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

Phenol
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

A u t h o r i t a t i v e V e r s i o n : This version is current as of 01 Jun 2016.

ABSTRACT
Publication Date (Web): February 28, 2017 | doi: 10.1021/acsreagents.4263.20160601

This monograph for Phenol 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
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details the following specifications and corresponding tests for verifying that a substance meets ACS Reagent Grade
specifications including: Assay, Freezing Point, Clarity of Solution, Residue after Evaporation, and Water.

OH

C6H5OH Formula Wt 94.11 CAS No. 108-95-2

SUPPLEMENTS & UPDATES

Published Authoritative Expired Type Summary Other Versions


28 Feb 2017 01 Jun 2016 Original First on-line publication, based on 11th ed.

Note: Phenol that conforms to this specification may contain a stabilizer. If a stabilizer is present, its presence should
be stated on the label.

GENERAL DESCRIPTION

Typical appearance . . . . . . . . . . . . . . . . . . . colorless hygroscopic solid; may become pink on exposure to air
Applications . . . . . . . . . . . . . . . . . . . . . . . . pH indicator

DOI:10.1021/acsreagents.4263.20160601
© 2017 American Chemical Society A ACS Reagent Chemicals, Part 4

ACS Reagent Chemicals


ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
ACS Reagent Chemicals Monograph

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

Change in state (approximate) . . . . . . . . . . . . when free from water and cresol, it congeals at 41 °C and melts at 43 °C;
boiling point, 182 °C
Aqueous solubility . . . . . . . . . . . . . . . . . . . . 8.2 g in 100 mL at 15 °C; very soluble in hot water
Density . . . . . . . . . . . . . . . . . . . . . . . . . . . 1.07
pKa . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9.9

SPECIFICATIONS

Assay . . . . . . . . . . . . . . . . . . . . . . . . . . . . ≥99.0% C6H5OH


Freezing point . . . . . . . . . . . . . . . . . . . . . . Not below 40.5 °C (dry basis)
Clarity of solution . . . . . . . . . . . . . . . . . . . . Passes test
Publication Date (Web): February 28, 2017 | doi: 10.1021/acsreagents.4263.20160601

Maximum Allowable
Residue after evaporation . . . . . . . . . . . . . . . 0.05%
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Water (H2O) . . . . . . . . . . . . . . . . . . . . . . . . 0.5%

TESTS
Assay
(By iodometry after bromination of hydroxyl groups). Weigh accurately about 1.5 g, and dissolve in sufficient water to make
exactly 1 L. Transfer 25 mL into a 500 mL glass-stoppered iodine flask, add 30 mL of 0.1 N bromine solution and 5 mL of
hydrochloric acid, and immediately stopper the flask. Shake frequently during 30 min, and allow to stand for 15 min. Then
quickly add 10 mL of 10% potassium iodide reagent solution, being careful that no bromine escapes, and stopper
immediately. Shake, add 1 mL of chloroform, and titrate the liberated iodine (which represents the excess of bromine) with
0.1 N sodium thiosulfate volumetric solution, using 3 mL of starch indicator solution. One milliliter of 0.1 N bromine
corresponds to 0.001569 g of C6H5OH.
[(mL × NBr2) (mL × N Na 2S2O3)] × 1.569
% C6H5OH =
Sample wt (g)/ 40

Freezing Point
Dry the sample by adding 15 g of molecular sieve zeolite having 4A-size pores to 100 g of molten sample in a 400 mL conical
flask. (The zeolite may be in the form of a powder or of cylindrical granules about 3 mm in diameter.) Stopper the flask
loosely, and maintain the mixture at 55–60 °C for 20 min with frequent stirring. Quickly transfer a portion of the dried
sample to a jacketed test tube, filling the tube to a depth of 8 cm. Insert a suitable thermometer, graduated in 0.1 °C units,
and stir until the temperature falls to 10 °C above the expected freezing point. Immerse the tube in a water bath that is
adjusted to about 4 °C below the expected freezing point and clamp in a vertical position. Insert a ring-type stirrer around
the thermometer that is clamped to place the bottom of the bulb about 0.5 cm above the bottom of the test tube. Stir the
sample continuously until crystallization occurs and the temperature does not change more than 0.05 °C in 2 min or, if
supercooling occurs, the temperature rises rapidly to maximum accompanied by rapid crystallization. Record the constant
temperature or the maximum temperature as the freezing point.

Clarity of Solution
Dissolve 5.0 g in 100 mL of water. The solution should be free of turbidity and insoluble residue.

DOI:10.1021/acsreagents.4263.20160601
© 2017 American Chemical Society B ACS Reagent Chemicals, Part 4

ACS Reagent Chemicals


ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
ACS Reagent Chemicals Monograph

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

Residue after Evaporation


[Part 2: Gravimetric Methods; Residue after Evaporation]. Evaporate 10.0 g to dryness in a tared, preconditioned dish on a
hot plate (~100 °C), and dry the residue at 105 °C for 30 min.

Water
[Part 2: Titrimetric Methods; Water by the Karl Fischer Method; Volumetric Procedure; Volumetric Procedure for Samples
Using Karl Fischer Reagent, Method 1]. Use 25.0 g of molten sample.
Publication Date (Web): February 28, 2017 | doi: 10.1021/acsreagents.4263.20160601
Downloaded by RICE UNIV on May 29, 2018 | https://pubs.acs.org

DOI:10.1021/acsreagents.4263.20160601
© 2017 American Chemical Society C ACS Reagent Chemicals, Part 4

ACS Reagent Chemicals


ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.

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