Otto Prohaska

1
New Technology for Sulfur Detection

• Otto Prohaska
• Science and Technology Group
• Otto.Prohaska_at_PerkinElmer.com

2
PerkinElmer Instruments

• Analytical Instrument Manufacturer
• GC, GC/MS, HPLC
• ICP-OES, ICP-MS, AA
• UV/Vis, FTIR, FT Imaging
• Research new technologies
• New instrument development for total and
  speciated sulfur monitoring
• New sulfur detection technology patents filed

3
Summary of Key Technical Results

• Resolution - 0.15 pgmS/s sample used for the
  study thiophene
• Response Time - PWHM 0.95 sec
• Selectivity - versus HCs is gt 106
• Precision - lt 3 for 10 runs
• Stability - drift lt 5 per day
• Interferents - lt 0.3 for nitrogen, phosphorous,
  chlorine compounds
• Linear Dynamic Range - 105 (concentration range
  with linear response)

4
Thiophene Response with PKI and SCD Detectors
Amount Injected 0.5 uL Concentration 200 ppm
Thiophene Split Ratio 1001 PWHM1.4
s Signal/Noise 4700 Peak Asymmetry factor at 5
1.22
Amount Injected 0.5 uL Concentration 200 ppm
Thiophene Split Ratio 1001 PWHM1.2
s Signal/Noise 5400 Peak Asymmetry factor at 5
1.3
200
600
500
SCD Signal(mV)
PKI Detector Response
100
400
300
2.22
2.26
2.30
2.20
2.25
2.30
Time (min)
5

Sulfur Compound Standard from Sievers Results
with PKI Detector
3
1 Dimethyl Sulfide 2 Ethyl Methyl Sulfide 3
Thiophene 4 Toluene Solvent
PKI Detector Response
2
1
4
Time(min)
6
Gasoline Sample
0 Unidentified Sulfur Compound 1 Thiophene 2
2-Methyl Thiophene 3 3-Methyl Thiophene 4 2-Ethyl
Thiophene 5 Alkyl Thiophene 6 BenzoThiophene 7
Methyl Benzothiophene 8 Dimethyl Benzothiophene
Time(min)
7
Gasoline Response with PKI and SCD Detector
7
1
1 Thiophene 2 2-Methyl Thiophene 3 3-Methyl
Thiophene 4 Alkyl Thiophene 5 Benzo-Thiophene 6
Methylbenzo-Thiophene 7 Dimethyl Benzo- Thiophene
5
6
PKI Detector Response
2
4
3
1 Thiophene 2 2-Methyl Thiophene 3 3-Methyl
Thiophene 4 Alkyl Thiophene 5 Benzo-Thiophene 6
Methylbenzo-Thiophene 7 Dimethyl Benzo- Thiophene
5
7
1
6
2
SCD Signal(mV)
4
3
Time(min)
8
Long Term Stability - Gasoline
9
Total Sulfur Measurement in Gasoline
PKI Detector Response
10
Summary of Key Technical Results

• Resolution - 0.15 pgmS/s sample used for the
  study thiophene
• Response Time - PWHM 0.95 sec
• Selectivity - versus HCs is gt 106
• Precision - lt 3 for 10 runs
• Stability - drift lt 5 per day
• Interferents - lt 0.3 for nitrogen, phosphorous,
  chlorine compounds
• Linear Dynamic Range - 105 (concentration range
  with linear response)