Aromatic Hydrocarbon | Karl Fischer titrator AQ-300/MOICO-A19 - JM Science
HIRANUMA APPLICATION DATA Karl Fischer Titrator Data No. KF3 Jun.6. 2017
Water contents Aromatic Hydrocarbon

1. Abstract

 Water content of Aromatic hydrocarbons are determined by Karl Fischer coulometric titrator. In coulometric titration, iodine of Karl Fischer reagent is generated by electrolysis and generated iodine quantitatively reacts with water. Reaction formula is described below.

 H₂O + I₂ + SO₂ + 3RN + CH₃OH → 2RN・HI + RN・HSO₄CH₃

 2RN・HI → I₂ + 2RN + 2H⁺ + 2e⁻

 Aromatic hydrocarbons do not interfere the Karl Fischer reaction and direct injection method could apply. Anode solution is selected from General-use or Oil in accordance with sample solubility. General-use anode solution contains methanol as solvent. When the sample has low solubility in methanol, the use of anode solution for oil is appropriate. When fritless cell is used, cathode solution is not necessary.

2. Apparatus and Reagents

(1) Apparatus    
    Titrator : HIRANUMA Karl Fischer Coulometric titrator AQ-series or MOICO-A19
    Electrolytic cell : Standard Cell
Fritless Cell
(2) Reagents    
    Anode solution : Hydranal coulomat AG (for general use, nonhalogenated)
    Cathode solution : Hydranal coulomat CG

3. Procedure

(1) Fill 100 mL of anode solution and one ampoule of cathode solution into the electrolytic cell as shown in Fig.3.1.
(2) Start blanking to attain stable background.
(3) Wash the syringe with sample.
(4) Draw the sample into syringe and then weigh the syringe.
(5) Inject sample from rubber septum of electrolytic cell as shown in Fig.3.2.
(6) Start titration. Measurement parameter is shown in Table 4.1.
(7) Weigh the syringe again and then set the difference of weight to sample size.

Fig.3.1. Preparation of the reagents.



Fig.3.2. Injection of sample.

4. Parameters and results

Table 4.1. Parameters

Condition File    
Cal Mode 0:Sample weight(net)  
  X-(H₂O-BLANK)/SIZE  
Interval Time 20 sec
Current SLOW  
S-Timer 0 min
Blank Value 0 ug
Unit Mode AUTO  
Auto Interval 0 g
Minimum Count 5 ug
Back Ground ON  
Sample Size Input Every Time  
Cell Type Standard/Fritless  

 

Table 4.2. Results of water content measurement in aromatic hydrocarbons

Sample Apparatus Cell Reagent Sample
Size (g)
Water
(μg)
Water
Content
Toluene AQ Standard AG 1.7520 94.3 53.8 ppm
      CG 1.7483 93.3 53.4
        1.7348 92.7 53.4
             
    Fritless AG 1.7549 91.4 52.1 ppm
        1.7398 92.1 52.9
        1.7356 91.9 53.0
Xylene AQ Standard AG 1.77164 110.5 62.4 ppm
      CG 1.62378 94.3 58.1
        1.65876 99.9 60.2
             
    Fritless AG 1.62232 93.2 57.4 ppm
        1.51125 88.0 58.2
        1.77412 104.5 58.9

5. Note

(1) Use dried syringe and syringe vial in Fig.5.1, for preventive of contamination by atmospheric water
(2) Put appropriate anode solution in use according to the solubility of the sample. For example, Hydranal Coulomat AG-H and Oil are suitable for oils.
Note : these reagents does not correspond to Fritless cell.


Fig.5.1. Draw the sample from syringe vial.

Hiranuma aquacounter aq-300 coulometric karl fischer titratorHiranuma aquacounter coulometric karl fischer titrator moico-a19Water contents

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