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〈181〉 Identification-Organic Nitrogenous Bases

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101 views1 page

〈181〉 Identification-Organic Nitrogenous Bases

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Hamid
Copyright
© © All Rights Reserved
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Printed on: Wed Feb 08 2023, 11:06:51 PM(EST) Status: Currently Official on 09-Feb-2023 DocId: GUID-A87EB337-8482-42D5-A171-128444F8F6A5_1_en-US

Printed by: Dang Van Vu Official Date: Official Prior to 2013 Document Type: GENERAL CHAPTER @2023 USPC
Do Not Distribute DOI Ref: 7hu5g DOI: https://doi.org/10.31003/USPNF_M98930_01_01
1

á181ñ IDENTIFICATION—ORGANIC NITROGENOUS BASES


INTRODUCTION
The purpose of this test is the identification of tertiary amine compounds. This spectroscopic test has a limited degree of
specificity and, therefore, the conformance with all additional identification tests listed in a particular monograph is necessary
to ensure the identity of the specimen under examination.
ASSAY
• PROCEDURE
Standard solution: In a separator dissolve 50 mg of the corresponding USP Reference Standard in 25 mL of 0.01 N
hydrochloric acid.
Sample solution: Depending upon the nature of the sample, dissolve 50 mg of the bulk substance under test in 25 mL of
0.01 N hydrochloric acid, or shake a quantity of powdered tablets or the contents of capsules, equivalent to 50 mg of the
substance, with 25 mL of 0.01 N hydrochloric acid for 10 min. Transfer the liquid to a separator, filtering if necessary, and
washing the filter and the residue with several small portions of water.
Instrumental conditions
(See Mid-Infrared Spectroscopy á854ñ.)
Mode: IR
Wavelength range: 7–15 µm (1430 cm−1 to 650 cm−1)
Cell: 1-mm
Blank: Carbon disulfide
Analysis

al
Samples: Standard solution and Sample solution
Treat each solution as follows: Add 2 mL of 1 N sodium hydroxide and 4 mL of carbon disulfide, and shake for 2 min.
Centrifuge if necessary to clarify the lower phase, and pass it through a dry filter, collecting the filtrate in a small flask
provided with a glass stopper. Determine the absorption spectra of the filtered Standard solution and Sample solution
without delay. ci
Acceptance criteria: The spectrum of the Sample solution must show all of the significant absorption bands present in the
spectrum of the Standard solution.
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