Scribd
Upload
68 views5 pages

2023 UMA Template

Uploaded by

suhebtamboli
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as DOCX, PDF, TXT or read online on Scribd
68 views5 pages

2023 UMA Template

Uploaded by

suhebtamboli
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as DOCX, PDF, TXT or read online on Scribd
You are on page 1/ 5

Unilever R&D – Unilever Method of Analysis (UMA)

Version: DD-Mon-YYYY
UMA-#### UMA TITLE
Page 1 of 5

UMA-HPC Method of Analysis

UMA Number: UMA-####


Date of Issue: 21-11-2024
Old UMA Code: N/A
Status: Current
Method Owner: Home Care Analytical Mumbai
Source: Home Care Analytical Mumbai
Author: Suheb Tamboli, Home Care Analytical Mumbai
Approved By (Year): Sharavankumar Dhannure, Home Care Analytical Mumbai

Characterization of Primary Alcohol Sulphate: Carbon Chain


Distribution in PAS liquid and PAS Granule
Printed Copy = Uncontrolled Copy
The information contained in this document is proprietary to Unilever. No further distribution
is permitted without prior consent of Unilever.
1. Warning and Safety Precautions:
1.1. The main hazards of the materials involved are indicated below. Users should refer to supplier
safety information for further details. An assessment of the risk to employees, and safety
precautions required should be carried out locally before commencement of work. In some
countries there is a requirement to document this assessment.

2. Scope:
2.1. This method is applicable for the determination of relative chain length composition of raw
materials such as oils or waxes which are fatty acids or glycerides of fatty acids.

3. Normative References:
UOP Method 673-06

4. Definitions:
None
Unilever R&D – Unilever Method of Analysis (UMA)
Version: DD-Mon-YYYY
UMA-#### UMA TITLE
Page 2 of 5

5. Principle:

Primary Alcohol Sulphates is desulphonated/Acid hydrolysis using concentrated sulphuric acid. Fatty
alcohol is extracted and anlysed using GC-FID

6. Reactions:

R-SO3H + H2O R-OH + H2SO4

7. Reagents and Materials:


7.1. Sulphuric Acid 98% AR (H2SO4) CAS no: [7664-93-9]
7.2. N-Pentane AR CAS no: [109-66-0]
7.3. Glass GC 20ml vial with septa
7.4. GC vial 2ml
7.5. Sodium Hydroxide pellets (NaOH) CAS no: [1310-73-2]
7.6. De-mineralised water
7.7. Anti-bumping granule

Warning: Corrosive reagents, avoid inhalation and contact with skin and eyes. For preparation
never add water to sulphuric acid, but add sulphuric acid to water.

7.8. 25 ml dilute Sulphuric Acid (4M)


Dilute the 9.8g of Conc.Sulphuric acid to 25ml of De-mineralised water

7.9. 25 ml 15% Sodium Hydroxide Solution


Dissolve 3.25g of NaOH pellets in 25ml of De-mineralised water

8. GC-FID conditions:

8.1 Gas Chromatograph : Any standard make with Flame Ionisation Detector

8.2 Chromatographic column: HP-1 Methyl Siloxane (50 m x 200 µm x 0.33 µm) or equivalent

8.3 Oven Programme


Unilever R&D – Unilever Method of Analysis (UMA)
Version: DD-Mon-YYYY
UMA-#### UMA TITLE
Page 3 of 5

From ºC To ºC ºC/Min Hold Min


Initial 140 140 ---- 0 Min
Ramp 1 140 170 1 5 Min
Ramp 2 170 250 10 5 Min

Total run time : 48 min


Injector temperature : 250 ºC
Detector temperature : 240 ºC
Flow rate : 19.3
Injection Volume : 2 μl
Split ratio : 20:1
Total flow mL/min :19.3
Hydrogen flow mL/min :50
Air flow mL/min :450
Solvent delay : 4 minute

9. Sampling Technique:

Mix well before the taking the sample

10. Procedure:

10.1 De- sulphonation of PAS Granule/ PAS Liquid

10.1.1 Weight around 500 mg of PAS liquid/ PAS Granule in a 20ml screw cap vial
10.1.2 Add 3ml 4M Sulphuric acid (7.8) also add 3-4 anti-bumping granules to avoid glass vial
rupture and tightly close the lid.
10.1.3 Heat it on a hotplate for 2 hours under a fume hood
10.1.4 Cool and add 5ml of n-Pentane using a plastic syringe through the septa and shake
10.1.5 Allow to separate and transfer the Pentane layer to another vial using a plastic
syringe/dropper
Unilever R&D – Unilever Method of Analysis (UMA)
Version: DD-Mon-YYYY
UMA-#### UMA TITLE
Page 4 of 5

10.1.6 Add 3ml of 15% sodium hydroxide solution (7.9) to pentane layer, stopper and shake gently
10.1.7 Transfer the top pentane layer to another vial containing 5 ml of water and shake gently
10.1.8 Transfer the pentane layer using a syringe/dropper another vial containing 2g of anhydrous
sodium sulphate
10.1.9 Collect the pentane layer and analyse it on GC-FID

11. Calculations & Expression of Results:

Integrate the peaks with zero threshold

12. Raw and Processed Data:

Figure 1: FID Chromatogram of PAS Liquid 27%

C12

C14

Figure 2: FID Chromatogram of PAS Granule

C12

C14
Unilever R&D – Unilever Method of Analysis (UMA)
Version: DD-Mon-YYYY
UMA-#### UMA TITLE
Page 5 of 5

13. Quality Assurance and Control:

Not available

14. Special Cases and Notes:

Not available

15. References:

UOP Method 673-06

16. Annexes:

Not available

You might also like

pFad - Phonifier reborn

Pfad - The Proxy pFad of © 2024 Garber Painting. All rights reserved.

Note: This service is not intended for secure transactions such as banking, social media, email, or purchasing. Use at your own risk. We assume no liability whatsoever for broken pages.


Alternative Proxies:

Alternative Proxy

pFad Proxy

pFad v3 Proxy

pFad v4 Proxy