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## 2-Bromo-3,3,3-Trifluoropropene Spectra

HLS study number: WAG0006

Version ID: Final

Issue date: 26 July 2012Huntingdon Life Sciences WAG0006

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## Sponsor and Test Facility

Sponsor 

### American Pacific Corporation 3883 Howard Hughes Parkway Suite 700 Las Vegas NV 89169 USA

Test facility 

### Huntingdon Life Sciences Eye Research Centre Eye Suffolk IP23 7PX UK

NMR spectrometry London Metropolitan University (subcontracted) Institute for Health Research and Policy 166-220 Holloway Road London N7 8DB UK

The NMR spectrometry was performed unde r the supervision of Dr Annie Bligh (Responsible Analyst). The laboratories ar e not a member of the UK GLP compliance
programme.Huntingdon Life Sciences WAG0006

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## Table of Contents

Sponsor and Test Facility ......................................................................................................

. 2

Compliance with Good Laboratory Practice............................................................................ 4

Quality Assurance Statement ................................................................................................. 5

Contributing Scientists ........................................................................................................

.... 6

Summary........................................................................................................................

......... 7

1. Introduction ...................................................................................................................

. 8

1.1 Objective ............................................................................................................ 8 1.2 Regulatory compliance....................................................................................... 8 1.3 Study schedule................................................................................................... 8 1.4 Maintenance of records...................................................................................... 8

2. Test Substance .............................................................................................................. 9

3. Experimental Procedures............................................................................................. 10

3.1 Ultraviolet/visible absorption spectrum............................................................. 10 3.1.1 Apparatus ............................................................................................. 10 3.1.2 Procedure ............................................................................................. 10 3.1.3 Results.................................................................................................. 10 3.1.4 Conclusion............................................................................................ 10

3.2 Infrared spectrum ............................................................................................. 14 3.2.1 Apparatus ............................................................................................. 14 3.2.2 Procedure ............................................................................................. 14 3.2.3 Results.................................................................................................. 14 3.2.4 Conclusion............................................................................................ 14

3.3 Nuclear magnetic resonance spectrum............................................................ 16 3.3.1 Apparatus ............................................................................................. 16 3.3.2 Procedure ............................................................................................. 16 3.3.3 Results.................................................................................................. 16 3.3.4 Conclusion............................................................................................ 16



## List of Annexes

Annex 1 Eye Research Centre GLP Compliance Statement 2011 .............................. 18Huntingdon Life Sciences WAG0006

6 

## Contributing Scientists

2-Bromo-3,3,3-trifl uoropropene: Spectra

Study management

P Sydney BSc MSc Study Director Product Chemistry

Other responsible staff

L Lawson MChem Scientist Product Chemistry

B Turner BSc Scientist Product ChemistryHuntingdon Life Sciences WAG0006

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## Summary

Spectral analysis was pe rformed to aid in the characteris ation of the test substance, 2-Bromo-3,3,3-trifluoropropene.

Ultraviolet/visible, infrared and nuclear magnetic resonance spectra were recorded and found to be consistent with the assi gned structure of the molecule.Huntingdon Life Sciences WAG0006

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## 1. Introduction

1.1 Objective

Spectral analysis was pe rformed to aid in the characteris ation of the test substance, 2-Bromo-3,3,3-trifluoropropene.


## 1.2 Regulatory compliance

The study was conducted in accordance with accepted principles in order to meet the requirements of Commission Re gulation (EC) No. 440/2008 and the OECD Guidelines for the Testing of Chemicals. 

## 1.3 Study schedule

Study initiation date : 09 November 2011

Experimental start date : 22 November 2011

Experimental completion date : 03 July 2012

Study completion date : 26 July 2012



## 1.4 Maintenance of records

Primary data from the tests, and a copy of the final report, are stored in the archives of Huntingdon Life Sciences.Huntingdon Life Sciences WAG0006

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## 2. Test Substance

Identity: 2-Bromo-3,3,3-trifluoropropene

Chemical structure: F
F
F CH 2

Br



### CAS number: 1514-82-5

Appearance: Clear liquid w ith a slight yellow tint

Storage conditions: Room temperature

Lot number: KgF080

Purity: 99.9% excluding stabilisers

Stabilisers:

Expiry date: 01 August 2012

Date received: 12 September 2011Huntingdon Life Sciences WAG0006

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## 3. Experimental Procedures

3.1 Ultraviolet/visible absorption spectrum

3.1.1 Apparatus

Camspec M550 UV-Visible Spectrophotometer

Calibration: Wavelength scale calibrated using holmium glass filter. Absorbance scale calibrated agai nst acidified potassium dichromate solution.

3.1.2 Procedure

Definitive ultraviolet/visible (UV/vis) absorpti on spectra for 2-Bromo-3,3,3-trifluoropropene were measured in purified water, 0.1M aque ous hydrochloric acid and 0.1M aqueous sodium hydroxide under the following conditions. The solu tions contained acetonitrile (5% v/v) to aid dissolution.

Concentration: 250 mg/l

Cell type: Quartz

Cell path length: 1 cm

Scan range: 200 - 400 nm

Bandwidth: 2 nm

The corresponding blank solvent syst ems were used as references as appropriate. Preliminary spectra had indicated no absorb ance between 400 and 800 nm.

3.1.3 Results

The spectra are shown in Figures 1 to 3. So me low wavelength absorbance was evident, but there were no significant ab sorption wavelength maxima ( λ max 

### ) above solvent cut-off wavelengths (approximately 210 nm for neutra l and acidic media; 220 nm for the basic medium).

3.1.4 Conclusion

The UV/vis spectra were consistent with the assigned structure of 2-Bromo-3,3,3- trifluoropropene.Huntingdon Life Sciences WAG0006

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### Figure 1 UV/vis spectrum of 2- Bromo-3,3,3-trifluoropropene (250 mg/l in purified water)

0.00 0.20 0.40 0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00

200 220 240 260 280 300 320 340 360 380 400Absorbance

Wavelength, λ (nm)Huntingdon Life Sciences WAG0006

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### Figure 2 UV/vis spectrum of 2- Bromo-3,3,3-trifluoropropene (250 mg/l in 0.1M aqueous HCl)

0.00 0.20 0.40 0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00

200 220 240 260 280 300 320 340 360 380 400Absorbance

Wavelength, λ (nm)Huntingdon Life Sciences WAG0006

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### Figure 3 UV/vis spectrum of 2- Bromo-3,3,3-trifluoropropene (250 mg/l in 0.1M aqueous NaOH)

0.00 0.20 0.40 0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00

200 220 240 260 280 300 320 340 360 380 400Absorbance

Wavelength, λ (nm)Huntingdon Life Sciences WAG0006

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## 3.2 Infrared spectrum

3.2.1 Apparatus

Cary 630 Fourier Transform - Infrared (FT-IR) Spectrometer.

Calibration: Wavelength scale calibrated against a polystyrene film.

3.2.2 Procedure

The infrared (IR) absorption spectrum of 2-Br omo-3,3,3-trifluoropropene was recorded over the scan range 4000 to 500 cm -1 

### (Figure 4). The instrumental parameters were as follows:

Resolution: 4.0 cm -1 

### Number of scans: 64

3.2.3 Results

The spectrum showed the presence of characteristic absorption bands as follows:

Frequency (cm -1 ) Observation Assignment

1635 Weak, sharp band C=C stretching

1500 - 1000 Series of strong, sharp bands C-F stretching C-H deformation, in-plane

<1000 Series of weak/medium, sharp bands C-Br stretching C-H deformation, out-of-plane



### 3.2.4 Conclusion

The IR spectrum was consistent with th e assigned structure of 2-Bromo-3,3,3- trifluoropropene.15 Huntingdon Life Sciences WAG0006Figure 4 IR spectrum of 2-Bromo-3,3,3-trifluoropropeneHuntingdon Life Sciences WAG0006

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## 3.3 Nuclear magnetic resonance spectrum

3.3.1 Apparatus

Bruker Avance 500 MHz Nuclear Magneti c Resonance (NMR) Spectrometer.

Calibration: The spectrometer was internally calib rated relative to tetramethylsilane (TMS).

3.3.2 Procedure

A solution of 2-Bromo-3,3,3-trifluoropropene was prepared in deuterochloroform. A
1 

### H-NMR spectrum (Figure 5) was obtained us ing the conditions liste d on the spectrum.

3.3.3 Results

Details of the spectral data are given in the following table:

Chemical shift (ppm) relative to TMS Assignment

6.5, 6.0 =C H 2
7.3, 1.5 Solvent signals



### 3.3.4 Conclusion

The NMR spectrum was consistent with the assigned structure of 2-Bromo-3,3,3- trifluoropropene.Huntingdon Life Sciences WAG0006

17Figure 5 NMR spectrum of 2-Bromo-3,3,3-trifluoropropeneHuntingdon Life Sciences WAG0006

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### Annex 1 Eye Research Centre GLP Compliance Statement 2011