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New Technology for Sulfur Detection Otto Prohaska Science and Technology Group Otto.Prohaska@PerkinElmer.com
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PerkinElmer Instruments Analytical Instrument Manufacturer GC, GC/MS, HPLCGC, GC/MS, HPLC ICP-OES, ICP-MS, AAICP-OES, ICP-MS, AA UV/Vis, FTIR, FT ImagingUV/Vis, FTIR, FT Imaging Research new technologies New instrument development for total and speciated sulfur monitoringNew instrument development for total and speciated sulfur monitoring New sulfur detection technology – patents filed
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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 > 10 6 Precision - < 3% for 10 runs Stability - drift < 5% per day Interferents - < 0.3% for nitrogen, phosphorous, chlorine compounds Linear Dynamic Range - 10 5 (concentration range with linear response)
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Amount Injected 0.5 uL Concentration: 200 ppm Thiophene Split Ratio: 100:1 PWHM=1.4 s Signal/Noise = 4700 Peak Asymmetry factor at 5 % =1.22 Thiophene Response with PKI and SCD Detectors PKI Detector Response 300 400 500 600 2.222.262.30 100 200 2.202.252.30 SCD Signal(mV) Time (min) Amount Injected 0.5 uL Concentration: 200 ppm Thiophene Split Ratio: 100:1 PWHM=1.2 s Signal/Noise = 5400 Peak Asymmetry factor at 5 %=1.3
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1 2 3 4 1 Dimethyl Sulfide 2 Ethyl Methyl Sulfide 3 Thiophene 4 Toluene Solvent PKI Detector Response Time(min) Sulfur Compound Standard from Sievers: Results with PKI Detector
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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)
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1 2 3 4 5 6 7 1 Thiophene 2 2-Methyl Thiophene 3 3-Methyl Thiophene 4 Alkyl Thiophene 5 Benzo-Thiophene 6 Methylbenzo-Thiophene 7 Dimethyl Benzo- Thiophene Gasoline Response with PKI and SCD Detector PKI Detector Response 1 Thiophene 2 2-Methyl Thiophene 3 3-Methyl Thiophene 4 Alkyl Thiophene 5 Benzo-Thiophene 6 Methylbenzo-Thiophene 7 Dimethyl Benzo- Thiophene SCD Signal(mV) Time(min) 1 2 3 4 5 6 7
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Long –Term Stability - Gasoline
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Total Sulfur Measurement in Gasoline Total Sulfur Measurement in Gasoline PKI Detector Response Time(min) Total Sulfur Content:195 ppm Sample size: 0.005 uL Analysis Time: 0.1 min 500 0.050.100.150.20 400 300
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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 > 10 6 Precision - < 3% for 10 runs Stability - drift < 5% per day Interferents - < 0.3% for nitrogen, phosphorous, chlorine compounds Linear Dynamic Range - 10 5 (concentration range with linear response)
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