TITLE: Acidity for Reaction Titration Samples by Autotitration

1. Purpose and Scope

Describe the procedure for the determination of Acidity as %MAA in Reaction Titration (Combo
Kettle) Intermediate Monomer samples by automatic titration. The instrument typically detects two
equivalence points and reports MSA (Methanesulfonic Acid) and MAA (Methacrylic Acid)
separately. Total acidity is calculated as MAA.

2. Reference Documents
None

3. Abbreviations and/or Definitions

MAA – Methacrlic Acid
MSA – Methanesulfonic Acid
NaOH – Sodium Hydroxide
IPA – Isopropyl Alcohol or 2-Propanol
EP – Titration Endpoint
798MPT Titrino – Instrument used for the titration
4. Requirements
NOTE: Observe the following guidelines:
► Error 42 means that the printer is out of paper.
► The automatic titrator determines %MSA and %MAA separately. After test completion the
display shows 3 separate results: %MSA, %MAA and Total Acid (calculated as MAA). Some
samples may have little or no MAA present. If only MSA is detected, and MAA and
Total Acid are reported as “missing EP”, report %MSA as the total acid in the sample.
See Example on PAGE 5 and step 8.10 of this procedure.
►There are two different buret trays, each has a different concentration of titrant. Choose the tray
with 0.1N NaOH for this procedure.
► Insure that there are no bubbles in the titration hoses before starting analysis. Remove bubbles
by pressing the DOS button while tapping the hose with a finger.
► Fill the pH electrode with 2M Lithium chloride in ethanol solution.
► Rinse the electrode thoroughly with deionized water before each use.
► Mix the sample well before taking an aliquot for testing.
► Store the pH electrode in DI water between measurements.

)
3 enter
4.1 Recall Methods by pressing user meth followed by the key on the
798 MPT Titrino Keyboard.

Right
4.2 Select method arrow , then enter on the keyboard.
key press
REACT-TR

Using the

4.3 Clean the electrodes by rinsing thoroughly with deionized water.

4.4 Place the electrodes in the electrode holder on the 728 Ti Stand.

4.5 Place a rinse vessel on the 728 Ti Stand, and press “DOS” button to clear any air bubbles in the
lines. Press the RED “FILL/STOP” button to refill the buret.

4.6 Add  80 mL of iso-propyl alcohol (IPA) to a 100 mL plastic beaker with a magnetic stir bar and
place the beaker on the 728 Ti Stirrer stand.

4.7 Draw  5 ml of the well mixed sample into a disposable pipet. Place the pipet in a plastic beaker on
the balance pan, then press the tare bar (“TARE”) on the balance.

4.8 Transfer the sample to the beaker on the 728 Ti Stand. Return the pipet to the plastic beaker on
the balance pan. Then lower the electrodes into the alcohol/sample solution and start the stirrer
by pressing the GREEN “Start” Button.

4.9 After the balance stabilizes press the “PRINT” key on the balance. This automatically enters the
weight into the titroprocessor and starts the titration.

4.10 Upon completion of the titration, the lower display of the Titrino will show the % MSA, %MAA
and % Total Acid.
Example of typical results displayed:
MSA 0.63
MAA 0.76
Tot Acid 1.33
Some samples may have little or no MAA present. If only MSA is detected, and MAA and
Total Acid are reported as “missing EP” repeat the titration. If the 2nd titration still
detects MSA only, report %MSA as the total acid in the sample. See Example on PAGE 5
of this procedure.
Example of results displayed when only MSA is detected:
MSA 0.84
MAA missing EP
Tot Acid missing EP

4.11 After the titration is completed, remove the sample beaker from the titrator, hold a rinse vessel in
place and wash with DI water.

4.12 Remove the rinse vessel from the titrator, and store the pH electrode DI water.
Sample Type Sample Size Sample Weight Reagent Method Name
Reaction Titration 5ml 4.0 – 4.5 grams 0.1N NaOH “REACT-TR”
Raffinate-Heavy 2ml 1.5 – 2.5 grams 0.1N NaOH “0.1NNaOH”
Strippings 1ml 0.5 – 1.0 grams 1.0N NaOH “1.0NNaOH”
Extractor-Light 1ml 0.5 – 1.0 grams 1.0N NaOH “1.0NNaOH”

Calculations:
MSA, wt. % = EP1*CO5*CO1/C00
MAA, wt. % = (EP2-EP1)*C05*C02/C00
Total Acid (as % MAA) = EP2*C05*C02/C00
Where:
EP1 = Volume in mLs of titrant to Endpoint #1
EP2 = Volume in mLs of titrant to Endpoint #2
C01 = 9.611 (Formula weight of MSA /10)
C02 = 8.609 (Formula weight of MAA/10)
C05 = 0.1 (Normality of NaOH titrant)
C00 = Sample weight in grams