What Is The Fastest Route to High Quality Data? AxION DSA: Quality data without chromatography or sample preparation. AxION 2 TOF MS and AxION DSA
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1 What Is The Fastest Route to High Quality Data? Imagine being able to take virtually any sample and run it directly through a Time-of-Flight Mass Spectrometer No complicated method development No time-consuming sample preparation No necessary up-front chromatographic separation AxION DSA: Quality data without chromatography or sample preparation How much faster could you run an analysis? How much more would you be able to get done? How much easier would life become? Kai Robinson M.App.Sc. Product Specialist - Chromatography 1 Direct Sample Analysis (DSA) PerkinElmer AxION 2 TOF MS and AxION DSA 2 AxION DSA (Direct Sample Analysis) Instant sample introduction Ionization occurs within the enclosed portion of the DSA system, at the entrance to the mass analyzer, generating clean molecular ions without any required sample prep or chromatographic separations Faster analysis times By eliminating multiple steps from the workflow, a typical analysis can be condensed from ~ minutes to just seconds Immediate results With accurate mass, the AxION DSA/TOF system records true molecular ions, presenting perfectly clear, easy-to-read data without any complicated post-processing 3 4 information rich results in less time
2 Automated Sample Holder Liquid Inlet Auxiliary Gas Inlet Automated sample trays for fast, consistent ionization of liquid and solid samples N 2 Nebulization Gas Inlet (N 2 ) Heater Sample Corona Needle 5 6 Disposable sample holders available The AxION 2 TOF MS Mass Accuracy 2 ppm Wide linear dynamic range (10 5 ) Fast acquisition ~ Hz, perfect for fast UHPLC Isotopic patterns, mass accuracy and resolution 6,7*8%'*9:*%;);*:<=>< * * * * *?()@*8%'*9:*%;);*>AB*.,#1#".,#1,-".,#1,-,/".,+1,-".,+1,-##".,.1.".,.1#&".,.1#./-".,&1#$".,&1#$#*" No ions lost due to scanning ALL IONS ALL THE TIME 7 No sensitivity loss with fast scan speed Constant sensitivity with increasing number of ions 10X increased sensitivity with TrapPulse technology Time-of-Flight MS technology Provides exact mass performance for clear, unambiguous results to quickly identify, quantify, qualify 8 " #$ "%" #& "'"(" & ")" " #* "%" #& "'"(" + ")" +" " #+ "%" #, "'"(" - "" " #& "%" #- "'")" $ "" " #, "%" #& "'"(" * ")". "" " +# "%" #& "'"" " / "%" #- "'"(" + ")" 0 "" " * "%" #, "'"(" #+ ")"" " #$ "%" #& "'"(" & ")" " #* "%" #& "'"(" + ")" +" " #+ "%" #, "'"(" - "" " #& "%" #- "'")" $ "" "#$%&'(")*+&''*$%',-./,"* "#$%&'(")*+&''*&##.$�* +1$,2%3*(',4,1(#*3('4$(5./,"'* " #$ "%" #& "'"(" & ")"
3 How do you test for pesticide residues like Carbamates? Liquid Samples, 3 ppm Carbamate Pesticides spiked in Orange Juice Carbamates Pesticides listed in ascending order of m/z: Methomyl, Aldicarb, Carbaryl, Propoxur, Carbofuran, Aldicarb-sulfone, Mercaptodimethur and Carbofuran-3-hydroxy Mass RET ( ) Curve Amplitude m/z PerkinElmer s new iqt GC/MS/MS Emerging Techniques; Hyphenated Technologies for Polymer and Biofuel Application Scott Fraser (PhD) National Product Specialist Thermal & Elemental Analysis 11 Releasing this August PerkinElmer
4 Hyphenation Possibilities Modification of Sample Environment Tracks physical changes in the sample by adjusting the environmental conditions Thermal UV DSC-UV, STA-UV Mechanical-UV/Humidity DMA-UV DMA-Humidity Can give an accurate representation of materials under given conditions representative of storage, processing, different markets etc. Evolved Gas Analysis Evolved Gas Analysis refers to measurements made on gases released from a sample being tested by a thermal analyzer. Can determine water content in food stocks/pharmaceuticals, presence of volatiles, contaminants, breakdown products etc. Evolved Gas Analysis Why Hyphenate? Evolved Gas Analysis: TGA as a Source Because sometimes it s not enough to know when something happened; need to know what it was as well. TGA Mass was lost FTIR Contains gases with certain functional groups present vs. time (temperature) GCMS What were those gases Gas is evolved in the TGA Formed in different ways either volatilization, pyrolysis, combustion, reactions etc. Data here is Mass Loss vs. Temperature or time Can determine the number of weight loss events and then monitor the off gases in secondary analysis system Quantitative for the amount of gas produced Often a complex mixture of gases 15 Complete picture in real time 16
5 Evolved Gas Analysis: FTIR as a Secondary Analysis Evolved Gas Analysis: GCMS/MS as a Secondary/Tertiary Analysis FTIR provides information on gases functional groups Solvent levels Detection of pseudo-polymorphs and hydrates Detection of degradation/reaction products Reaction mechanism insights Tells us what came off in a thermal event giving insight into: 17 reaction mechanism reaction by-products which solvents are present understanding of the decomposition process Residual solvent at low levels for validation of loss on drying. Contaminants at low levels Identification of solvates obtained in crystallization process Forensic concerns on combustion Can run units in stand alone mode Higher mass range, soft ionization, and chemical ionization with oxygen resistant filament in the MS 18 The Transfer Line 19 The mass flow controller and filtering system provides a Constant Gas Flow through the system. Therefore Constant Gas Pressure and Constant Gas Speed are guaranteed. The Transfer Line guarantees Constant Gas Temperature Zero mass principle ensures minimal turbulence and residue formation in line Temperature range up to 3 C Simple operation; digitally controlled Polymer Safety Case Study: Polycarbonate and EVA 20
6 TGA Results TGA + FTIR Results EVA 2 Mass Loss Events 2 nd event seems complex most likely a gas mixture Polycarbonate 1 Mass Loss Event Highly reproducible %T Wavenumber Name Coadded Spectrum at C (Temperature based Extra Coadded Spectrum at C (Temperature based Extra Coadded Spectrum at C (Temperature based Extra Coadded Spectrum at C (Temperature based Extra GCMS Results Biopolymer Case Study; Recycling and Biowaste Elution Time (min)* Likely Compound* 2.42" Benzene" 2.87" Toluene" 3.55" Ethyl-Benzene" 3.65" p-xylene" 3.84" Styrene" 4.16" 1-methylethyl-Benzene" 4.66" Phenol" 4.81" Alpha-Methyl Styrene" 5.89" p-cresol" 7.14" 4-ethyl Phenol" 7.98" 3-propyl Phenol" 8." m-tert-butyl, Phenol" 10.32" p-isopropenyl-phenol" 13.68" 2,3 dihydro, 2-methyl Benzofuran" 14.45" Hexadecane, " 23 24
7 TGA Thermogram for Biowaste Sample EGA Event #1 Weight Remaining (%) Thermogram Derivative Weight Remaining (%) Temperature ( C) Temperature ( C) 26 EGA Event #2 EGA Event #3 Weight Remaining (%) Weight Remaining (%) Temperature ( C) Temperature ( C) 27 28
8 Conclusions Hyphenation opens up the possibility for obtaining more information on a single sample Complex samples can also be deconvaluted, and different breakdown conditions can be examined Forensically, samples with little known information can be categorized or even deduced utilizing hyphenated technology Thankyou For Your Attention Scott Fraser PhD National Product Specialist Thermal & Elemental Analysis PerkinElmer For the Better Level 2, Building 5, Brandon Office Business Park, 5 5 Springvale Rd, Glen Waverley Australia 31 (Ph): (Mobile): Scott.Fraser@perkinelmer.com PerkinElmer
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