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2025

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Determination of hexamethylenetetramine content by fully automated potentiometric titration


1. Introduction

Urotropin, with the molecular formula C6H12N4, also known as hexamethylenetetrammonium, has a wide range of applications. In medicine, it is commonly used as a disinfectant and antiseptic, for the prevention and treatment of chronic or recurrent lower urinary tract infections, and for treating hyperhidrosis of the hands and feet and bromhidrosis. In the military, it is commonly used as military fuel. In industry, it is mainly used as a curing agent for resins and plastics, a catalyst and foaming agent for amino plastics, and an accelerator for rubber vulcanization. This method uses the Shanghai Jiahang JH-T6 fully automatic potentiometric titrator to determine the content of the active ingredient in this drug through perchloric acid titration to see if its content meets the requirements for mass production. This method has a simple experimental procedure, is time-efficient, and avoids subjective errors caused by manual endpoint determination, making it a good choice for detecting the content of this type of drug.

2. Instruments and Equipment

2.1 Instruments

JH-T6 fully automatic potentiometric titrator, composite non-aqueous pH electrode.

2.2 Reagents

Perchloric acid standard titration solution (0.1 mol/L), anhydrous methanol.

3 Experimental Methods

3.1 Experimental Procedure

Accurately weigh 0.1 g of the test sample (accurate to 0.0001 g), place it in a titration vessel, add 50 mL of anhydrous methanol, place the vessel on a titration stand, and turn on the stirrer to completely dissolve the sample. Titrate with the standardized 0.1 mol/L perchloric acid titrant until the potential breakthrough endpoint is reached, and record the volume consumed.

3.2 Parameter Settings

Titration mode: dynamic titration Minimum addition volume:

0.02mL

Electrode equilibration time:

4s

Pre-stirring time:

10s

Electrode equilibration potential:

1mv

Titration speed: standard
Minimum addition volume::

10mv

Working electrode:

pH composite electrode
Final volume:

20mL

Pre-titration addition volume:

0mL

Potential jump:

150

Pre-control mv value:

200

4. Results and Discussion

4.1 Experimental Results

Sample Name c (perchloric acid) (mol/L) Sample Amount (g) Titration Volume V1 (mL) Blank Volume V0 (mL) Content (%) Average Content (%)

RSD(%)

 

 

Urotropin

 

 

0.1018

0.12207

8.545

 

 

0.02

99.674

 

 

99.537

 

 

0.2493

0.10437

7.278

99.251

0.10788

7.555

99.68

Calculation formula:

Calculation formula:

4.2 Atlas

4.3 Conclusion

The determination of hexamethylenetetramine content using the JH-T6 fully automatic potentiometric titrator showed good repeatability, with all results falling within the standard range and RSD ≤ 0.5%. The T960 fully automatic potentiometric titrator fully meets the requirements for this sample determination.

References:

[1] 2020 Pharmacopoeia of the People's Republic of China [M]. Part II. Beijing: China Medical Science and Technology Press.

Keyword:

automated potentiometric titration