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TS-ZF02NT 

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Study Report 

Title: Characterization of Test Substance Oxygen Functional Group Distribution 

Report Date: October 30, 2014

File Reference: 

Principal Investigator(s): {

} 

Testing Facility: {

} 

Sponsor: {

EPA Reference: TS-ZF02NT 
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TS-ZF02NT 

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Study Report 

Characterization of Test Substance Oxygen Functional Group Distribution 

Introduction: 

X-ray photoelectron spectroscopy is used in conjunction with chemical derivitization to 

examine the distribution of oxygen containing functional groups 

} present in the Sponsor’s Test Substance. 

1) Purpose & Scope: 

This study provides characterization data on the distribution of oxides present in the 

Sponsor’s Test Substance in normal liquid suspensions (Test Solution). This summary is to 

be used to inform chemical identification processes {,

}. 

2) Administrative Organization: 

This report was prepared by principal investigator, { based upon chemical 

derivitization and subsequent XPS analysis carried out by {

}. 

3) Test Substance: 

The study was conducted on the TS-ZF02NT new chemical substance (Test Substance) 

without confounding { typical of the 

final formulation. 

4) Principle and Study Design: 

X-ray photoelectron spectroscopy is a surface sensitive technique (5-10nm) using the binding 

energies of core level electrons to determine elemental surface composition and oxidation 

state of a material. For {

} fitting becomes ambiguous and derivitization of specific oxide functional groups 

with Fluorinated tags (which are more sensitive in the XPS) is needed for quantification. A 

separate sample is needed for each oxide being assayed. Further details may be found in the 

attached report. 

5) Sample Handling and Preparation:

The new chemical substance was provided to { } and prepared under his 

direction after the pilot centrifugation process, but {

} 
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TS-ZF02NT 

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was mounted to a blank 200mm wafer used for shipment purposes only. The prepared sample 

was enclosed in a standard 200mm wafer case, and taped closed with FAB tape. Final 

packaging and transfer to the UPS carrier was by { } Shipping and 

Receiving. The sample was shipped intact, in a secure container to the Testing Facility. 

6) Study Results:

{

} 

Appendices: 

1. { } 
Report Prepared by:

The goal of this project was to characterize the oxygen functional group distribution in films prepared 

from Type B using chemical derivatization coupled to X-ray photoelectron 

spectroscopy (XPS).

XPS Overview. 

X-ray photoelectron spectroscopy (XPS) is a surface analytical technique (top 5-10 nm) used for 

elemental analysis of samples under ultra-high vacuum conditions (10-8-10-9 Torr). Both identification 

and quantification of the atomic composition is achieved by incident X-rays of a specific photon energy 

causing core level electrons of a sample to eject at various kinetic energies. Since each element has a 

unique set of core electron binding energies, the specific kinetic energy at which a particular core level 

electron is ejected will allow for elemental identification while the number of detected electrons at this 

particular energy will enable the quantification of this element relative to other elements in a given 

sample. 

Initial Survey Scan. 

XPS analysis typically begins with a scan across a wide range of energies to identify the elements present 

in a particular sample at concentrations greater than 1%. In a survey spectrum, the energy is reported as 

binding energy. For the sample analyzed, Type-B, the only elements 

identified were , indicating that there were no contaminants containing other 

elements and the coating of completely covered the underlying substrate. 
Quantitative Analysis.

Chemical Derivatization 

Chemical derivatization is a labeling technique used to tag specific functional groups on a surface. Three 

derivatizing reagents, all containing fluorine, can be used to tag 

The reactions are carried out in the vapor phase to minimize purification 

and work-up steps. The % fluorine (1s) for each derivatization reaction can be quantified using XPS and 
stoichiometrically used to determine the percentage of each oxygen functional group. The derivatization 

reactions are outlined below: 

Analysis of Oxygen Functional Group Distribution 

Type B samples were run in triplicate for each chemical derivatization 

reaction. The highest concentration of tagged oxygen functional group was observed for the 

 synthesis method or the preparation 

procedure. Regardless, all derivatization reactions were observed to have good precision, with a 

standard deviation of ± 0.1%.