Measuring the Titration of Nicotine in Liquids

Liquids are being produced for use in e-cigarettes, and these liquids contain nicotine. Similar to pharmaceutical bases, these can be titrated with perchloric acid in glacial acetic acid. The three key components of the liquids are glycerine, glycols and water. A pH electrode is suggested to be used for this application and has a filling solution of LiCl in ethanol or in glacial acetic acid.

Measuring the Titration of Nicotine in Liquids

Image Credit: YSI

The European pharmacopeia describes nicotine as a titration with 0.1 mol/l perchloric acid, and the sample is dissolved in 30 ml glacial acetic acid. It is often better to use increased amounts of glacial acetic acid due to the water content of these liquids and the result is calculated in mg/ml of nicotine.

Instruments

Measuring the Titration of Nicotine in Liquids

Image Credit: YSI

Table 1. Source: YSI

   
Titrator TL 7000 or higher
Electrode N 6480 Eth (electrolyte L 5034) or N 6480 eis or N 61 eis (electrolyte L 5014 for both options)
Cable L1A
Stirrer Magnetic stirrer TM 235 or similar
Titration tip Long version TZ 1643 required
Lab accessories Glass beaker 100 or 150 mL
Magnetic stirrer bar 30 mm

 

Reagents

Table 2. Source: YSI

   
1 Perchloric acid in glacial acetic acid 0.1 mol/l
2 Glacial acetic acid
3 Electrolyte L 5034 (LiCl/ethanol) or L 5014 (LiCl/glacial acetic acid)
All reagents should be in analytical grade or better.

 

Procedure of Titration

Reagents:

The titer determination of the HClO4 solution is performed as explained in the application report “Titer determination of Perchloric acid in glacial acetic acid.”

Electrode Cleaning and Storage:

For cleaning the electrode, Ethanol or Iso propyl alcohol is used, and the same electrolyte solution used in the electrode L 5034 (N6480 eth) or L 5014 (N 6480 eis/N 61 eis) should be used for storage.

Preparation of the Sample:

To prepare the sample, it is positioned in a beaker and filled up to 30 - 60 ml with glacial acetic acid, and then titrated with HClO4 0.1 mol/l. For each titration, the nicotine measurement should be 20 – 60 mg.

The density of the perchloric acid in glacial acetic acid is largely temperature-dependent. Recommendations suggest measuring and reporting the temperature at which the titration was performed.

The temperature at the titer determination and the temperature at the sample titration should be identical. If the temperature differs, the volume can be amended according to the European pharmacopeia:

EQcorr = EQ1*(1+(T1-T2 )*0.0011

Table 3. Source: YSI

   
EQ1 Consumption of titrant at first equivalence point
EQcorr Corrected volume of titrant
T1 Temperature at titer determination
T2 Temperature at sample titration

 

Titration Parameter

Sample Titration:

Measuring the Titration of Nicotine in Liquids

Image Credit: YSI

Table 4. Source: YSI

   
Default method: –––
Method type: Automatic titration
Modus: Dynamic
Measured value: mV
Measuring speed / drift: User defined
Initial waiting time: 0 s
Dynamic: Average
Damping: Average
Pretitration: Off
End value: Off
EQ: On (1)
Max. titration volume: 20 mL
Dosing speed: 100%

 

Table 5. Source: YSI

   
Minimum holding time: 4 s
Maximum holding time: 20 s
Measuring time: 3 s
Drift: 10 mV / min

 

Table 6. Source: YSI

   
Max step size: 1.0 mL
Slope max mL: 10
Min. step size: 0.02 mL
Slope min. mL: 120
Titration direction: Increase
Delay time: 0 s

 

Table 7. Source: YSI

   
Slope value: 300

 

Table 8. Source: YSI

   
Filling speed: 30

 

Calculation:

ImageForArticle_18982_15814825254975150.png

Table 9. Source: YSI

     
B 0 Blank value
EQ1   Consumption of titrant at first equivalence point
T WA Actual concentration of the titrant
M 162,23 Molecular mass of nicotine
V man Volume of the sample
F1 1 Conversion factor
F2 2 Conversion factor

 

This information has been sourced, reviewed and adapted from materials provided by YSI.

For more information on this source, please visit YSI.

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