Monograph pubs.acs.org/doi/book/10.1021/acsreagents
1-Methyl-2-pyrrolidone (N-Methyl Pyrrolidone)
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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 1-Methyl-2-pyrrolidone 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), Water, Free Amines, Chloride, and Ultraviolet Spectrophotometry.
C5H9NO
Formula Wt 99.13
CAS No. 872-50-4
Suitable for general use or in ultraviolet spectrophotometry. Product labeling shall designate the uses for which suitability is represented on the basis of meeting the relevant specifications and tests. The ultraviolet spectrophotometry specifications include all of the specifications for general use.
GENERAL DESCRIPTION Typical appearance . . . . . . . . Applications . . . . . . . . . . . . . Change in state (approximate) . Aqueous solubility . . . . . . . . . Density . . . . . . . . . . . . . . . .
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© 2017 American Chemical Society
clear liquid solvent boiling point, 202 °C miscible 1.03
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ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.4227 ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
SPECIFICATIONS General Use Assay . . . . . . . . . . . . . . . . . . . . . . . . . . . ≥99.0% C5H9NO Maximum Allowable Color (APHA) . . . . . . . . . . . . . . . . . . . . . . 50 Water (H2O) . . . . . . . . . . . . . . . . . . . . . . . 0.05% Free amines (as CH3NH2). . . . . . . . . . . . . . . 0.01% Chloride (Cl) . . . . . . . . . . . . . . . . . . . . . . 1 ppm
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Specific Use Ultraviolet Spectrophotometry Wavelength (nm) 400 . . . . . . . . . . . . . . . . . . . . . . . . . 350 . . . . . . . . . . . . . . . . . . . . . . . . . 300 . . . . . . . . . . . . . . . . . . . . . . . . . 285 . . . . . . . . . . . . . . . . . . . . . . . . . 275 . . . . . . . . . . . . . . . . . . . . . . . . . Headspace Analysis Assay by CG–HS [Part 2: Chromatography; Recommended Procedures; Extraction−Concentration; Procedure for Headspace Analysis Suitability]. . . . . . . .
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Absorbance (AU) . 0.01 . 0.01 . 0.05 . 0.15 . 1.00
. . . ≥99.9%
TESTS Assay Analyze the sample by gas chromatography by 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 the peaks, and calculate the 1-methyl-2-pyrrolidone content in area percent. Correct for water content.
Color (APHA) [Part 2: Measurement of Physical Properties; Color (APHA); Procedure for Color (APHA)].
Water [Part 2: Titrimetric Methods; Water by the Karl Fischer Method; Volumetric Procedure; Volumetric Procedure for Samples Using Karl Fischer Reagent, Method 1]. Use 24.3 mL (25 g) of the sample and a methanol-free system to prevent ketal formation with liberation of water.
© 2017 American Chemical Society
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ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.4227 ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
Free Amines Accurately weigh a 10.0 g sample in a tared, glass-stoppered flask. Add 100 mL of water and 0.1 mL of methyl red indicator solution. Titrate with standardized 0.01 N hydrochloric acid to the first permanent pink color. No more than 3.2 mL should be required. One milliliter of 0.01 N hydrochloric acid corresponds to 0.0003106 g of CH3NH2.
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Chloride Dilute 24.3 mL (25 g) of sample to the mark in a 100 mL volumetric flask with deionized water. Transfer 10.0 mL of sample solution to each of two 50 mL Nessler tubes and 30.0 mL to each of two additional Nessler tubes. Add 0.5 mL of chloride ion (Cl) standard solution to one tube containing 10 mL of sample solution (making a 0.5 ppm standard), and add 1.0 mL of chloride standard solution to the other tube, making a 1.0 ppm standard. Also add 0.5 mL of chloride standard to one tube containing 30 mL (making a spiked sample). Dilute all tubes to about 45 mL with deionized water, and mix. Add 1 mL of nitric acid and 1 mL of 0.1 N silver nitrate volumetric solution to each tube. Dilute to 50 mL, and mix thoroughly. After 10 min, observe the opalescence. Any opalescence in the sample must be no greater than that in the 0.5 ppm standard, and any opalescence in the spiked sample must be no greater than that in the 1 ppm standard.
Ultraviolet Spectrophotometry Use the procedure in [Part 2: Chromatography; Recommended Procedures; LC Suitability; Procedure for Absorbance] to determine the absorbance.
© 2017 American Chemical Society
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ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.4227 ACS Reagent Chemicals, Part 4
