Request No.:102570 Analyst: GJM

Charge No.: 20006799.0040

Notebook No.:21400

Log-in Date:11/18/2008

Analysis Report

To: Al Arnold, Carol Grubb Dept./Loc.: RD3-D207

From: G.J. Meixsell/D. J. Nagy/Ann Kotz Dept./Ext.: ETC-GAS/12416/15438

Date: 12/08/08 Lab Name: Polymer Separations

Subject: Molecular Weight Analysis by High Resolution Low Mass GPC analysis

Sample No.: BA-100

Summary

Sample BA-100, the reaction of pthalic acid and poly(ethylene glycol 200), was submitted for molecular weight 

distribution via Low Mass Gel Permeation Chromatography (LW-GPC) analysis to determine if the sample adheres 

to Schedule 9 polymer regulations. The sample was analyzed using a Waters Corporation Alliance 2795 HPLC 

with THF as a mobile phase @ 35oC 1mL/min; sample was diluted to approximately 0.4%wt in fresh THF prior to 

separation. Sample result is relative to a poly(ethylene glycol) calibration curve ranging from 62 daltons up to 

1,900K daltons. In addition to GPC, MALD/I analysis was performed to provide additional support information 

regarding structure and mass assignment. Molecular weight and molecular weight distribution results are 

summarized below.

 Results Summary Table #1

Sample Id Mn Mw Slice MW Cumulative

% >348d

Slice MW Cumulative 

% <1000d

Slice MW Cumulative 

% <500d

BA-100 (GPC Result 317 353 51.95 % * 99.89% 92.28%

BA-100 MALD/I 

Result

419 464 74.3 % **

*see attached xls file containing slice log Mw information

**see ppt file containing MALD/I data

BA-100 Slice MW 

table and Calibration Curve.xlsx

Mp vs Area (No 

referecne peak) C. Grubb.pdf

BA-100 MWD 

Result C. Grubb.pdf

 
Results and Discussion:

The GPC data exhibits 50% of the distribution’s mass is greater than 348 daltons which indicates that the sample is 

polymeric in accordance to Schedule 9. Furthermore, no more than 20% by weight of molecules are of the same 

molecular weight by GPC separation. Additionally, the MALD/I data indicates that greater than 74.3% of the 

distribution is greater than 348daltons with average repeat units of 5.1 and 5.5 EO/molecule; the addition of the 

repeat EO unit can be easily observed on the MALD/I plot. See tables and plots below for details.
MALD/I Summarized Slice Component Results

GPC Run Conditions:

Instruments: Waters Alliance 2795 Separation Module

Column: Waters Styragel HR 0.5, 300 x 7.8mm

Detector Waters 2414 DRI @ 35C

Mobile Phase: Isocratic 100% THF ACS grade

Calibration Curve Narrow PEG Standards

Flow Rate: 1 ml/minute

Injection Volume: 100 μL

Data System: Waters Empower Software
Description of Low-Mass GPC- Molecular Weight Report

Sample Information:

Sample identification, file name, and other administrative information are given at the top of page of this report.

Molecular Weights:

Below the header information on page 1 is a summary of all the appropriate molecular weight distribution data. 

Molecular weight averages are reported relative to a poly(styrene) calibration. The most commonly used molecular 

weights are the number-average (Mn) and weight-average (Mw). The polydispersity is the ratio of Mw / Mn and is a 

measure of the broadness of the molecular weight distribution. 

Molecular Weight Distribution:

In the middle of the page is the differential molecular weight distribution graph of weight-fraction versus 

log(molecular weight). The x-axis usually covers several orders of magnitude in molecular weight, such as from 100 

(10E2.0) to 100,000 (10E5.0) daltons. Overlaid with the differential molecular weight distribution curve is the 

cumulative molecular weight distribution plot of cumulative weight-fraction versus log(molecular weight). This type 

of plot is used to determine weight percent less than or greater than a specific molecular weight. The y-axis is 

displayed in the range from 0 to 100 and the x-axis covers the same range in mass as the differential molecular 

weight distribution curve.

GPC Chromatogram:

On the bottom of the page is the raw GPC chromatogram of differential refractive index (DRI) signal versus elution 

time is shown on page 1. Detector signal is plotted as a function of elution time in minutes. Materials with 

decreasing molecular weight elute with increasing retention time. The narrow peak on the chromatogram is toluene, 

which is added to each sample as an internal standard. The dotted lines are the areas under the peak area being 

integrated.