Document Number: PROC-SHE-OP-014640

Document Title: NaOH,A/NaOH,B - Sodium Hydroxide Titrations 455-094

Document Version: 6.0
Effective Date: 27 Jul 2015 11:42:23 GMT -06:00
Current Status: Effective

Release Approval Panel:

Signed By : Macedo, Felipe (fmacedo)
Decision : Approved
Decision Date : 11 May 2012 10:09:03 GMT -06:00
Role : SHE_Approver
Purpose : 3 year review of NaOH titration SOP
Meaning Of Signature : I have reviewed and approved this document.

Signed By : Gutierrez Abecia, Unai (ugutierr)

Decision : Approved
Decision Date : 08 Jul 2012 09:58:08 GMT -06:00
Role : SHE_Author
Purpose : 3 year review of NaOH titration SOP
Meaning Of Signature : I have reviewed and approved this document.

       
  
      
     
 


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Quality Control
Sheboygan

NaOH,A/NaOH,B - Sodium Hydroxide Titrations

PURPOSE: The purpose of this Standard Operating Procedure is to provide a general

procedure for sodium hydroxide titrations.

SCOPE: This SOP applies to all sodium hydroxide titrations.

MATERIALS/EQUIPMENT:

1. 0.1N or 0.5N Sodium Hydroxide Solution in water, standardized

2. Methanol, HPLC, (270474 or equivalent)

3. DI water

4. Autotitrator

5. Combination glass electrode

6. Hydrochloric acid in water, standardized

REFERENCES:

1. PROC- SHE- OP- 016096: Sodium Hydroxide Standardization Solutions (SOP 455-
065)

2. Aldrich Procedure: “Titrimetric Analysis of Organic Acids and Bases”, dated May 1990.

3. Aldrich Procedure: “Titrimetric Determination of Acid Chlorides”, dated February 1990.

TABLE OF CONTENTS:
I. Sodium Hydroxide Titration......................................................................................... 1
II. Sodium Hydroxide, Back Titration............................................................................... 2

I. Sodium Hydroxide Titration

A. PROCEDURE

1. Analytically add the appropriate amount of sample to a beaker equipped with a stir
bar.

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. , : ( ) ' ; < = - > # # ; ? @ % A : ' B C D # # ; E F . , : ( ) " K ) ' - 7 6 Q K = L 6 7 9 S - O T - O 6 U Q P Q R 2 6 9 - 6 6 1 0 * V W " 5 * R W U X

Quality Control
Sheboygan
2. Dissolve and dilute the sample to ca. 60 mL with DI water and/or methanol as
appropriate.

NOTE: Certain products, i.e. carboxylic acids, may be insoluble in water. Dissolve
these samples in ca. 30 mL of methanol and dilute to ca. 60 mL with DI water.
Some samples may require methanol only.

NOTE: Dissolving of some samples may require heating on a hot plate.

NOTE: If samples must be warmed on a hot plate, cool to room temperature

before titrating.

3. Titrate with standardized sodium hydroxide (NaOH) using the combination glass
electrode.

4. Record the equivalence point in mL of titrant.

5. Calculate the purity as follows:

% purity = (V NaOH) (N NaOH) (Equivalent Weight of sample) (100)

(mg sample)
OR

Molarity = (V NaOH) (N NaOH)

(mL sample)

6. Dispose of waste into the drain unless indicated otherwise.

II. Sodium Hydroxide, Back Titration

A. PROCEDURE

1. Analytically add the appropriate amount of sample to a beaker equipped with a stir
bar.

2. Dissolve and dilute the sample to ca. 60 mL with DI water.

3. Add an excess of standardized hydrochloric acid (HCl) to the sample.

NOTE: Refer to instructions on the QC computer system or in the product file for
the normality and amount of HCl to add to the sample. Sufficient excess HCl is
added to consume ca. 10 mLs of sodium hydroxide.

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. , : ( ) ' ; < = - > # # ; ? @ % A : ' B C D # # ; E F . , : ( ) " K ) ' - 7 6 Q K = L 6 7 9 S - O T - O 6 U Q P Q R 2 6 9 - 6 6 1 0 * V W " 5 * R W U X

Quality Control
Sheboygan
4. Record the amount and the normality of the HCl added to the sample.

5. Titrate the sample with standardized sodium hydroxide (NaOH) using the
combination glass electrode.

6. Record the equivalence point in mL of titrant.

7. Calculate the purity as appropriate:

% purity = [(V HCl) (N HCl) - (V NaOH) (N NaOH)] (Eq. Wt. sample) (100)
(mg sample)

OR
Molarity = (V HCl) (N HCl) - (V NaOH) (N NaOH)
(mL sample)

8. Dispose of waste into the drain unless indicated otherwise.

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