ANALYTICAL SOLUTIONS FOR THE PETROCHEMICAL INDUSTRY

| | | | ANALYTICAL SOLUTIONS FOR THEPETROCHEMICAL INDUSTRYLearn more about our products for the Petrochemical industry by visiting sigma-aldrich.com/petro2 Analytical Solutions for the Petrochemical IndustrySample PreparationSOLID PHASE MICROEXTRACTION (SPME)Solid phase microextraction is an innovative, solvent-free sample preparation technology that is fast, economic and versatile.• One step sampling, extraction and enrichment technique for 100% solvent free, organic trace analysis• Microsampling technique for small or precious samples and difficult matrices, such as oils (via the headspace)• New configurations allow automated fiber exchange, leading to fast method development and higher sample throughput.SPME uses a fiber coated with a liquid (polymer), a solid (sorbent), or a combination of both. The fiber coating removes the compounds from your sample by absorption in the case of liquid coatings or adsorption in the case of solid coatings. The SPME fiber is then inserted directly into the gas chromatograph for desorption and analysis.Comparison of Oxygenates in Gasoline, Direct Injection vs. SPMEMin0 0.5 1 1.5 2 2.5 3 3.5 4 4.5uV0500010000150002000025000EthanolButaneIPAPentanen-Propanol5SPMEMin0 0.5 1 1.5 2 2.5 3 3.5 4 4.5uV0500010000150002000025000EthanolButaneIPAPentanen-Propanol5Direct InjectionChromatograms normalized. Field samplers are also available.SPME Fast Fiber Assemblies (FFA)The SPME Fast Fit Assemblies (FFA) are a new configuration of SPME fibers that allow the automated exchange of SPME fibers by the Multi Fiber EXchange (MFX) System* on a CTC CombiPAL™ type autosampler. This enables: • Automated screening for optimal SPME phase selectivity in method development• Extraction of samples with a variety of different SPME phase chemistries for analyte polarity range enhancement• The ability for unattended desorption of multiple fibers to be loaded with samples from field sampling and air monitoring campaigns • SPME-FFAs are complemented by new holders for field sampling, passive air sampling and new storage devices for shipping and storing the FFAs.*available through Gerstel GmbH & Co KGFor additional product information and video demonstration, visit sigma-aldrich.com/spmePartner with Sigma-Aldrich for high-quality products specialized for the Petrochemical Industry.The oil industry fuels the global economy by meeting the demand for petroleum, natural gas, biofuels and petrochemicals. Its success depends upon safe, reliable and efficient processes to ensure that consumers receive a consistent flow of high-quality products. For decades, Sigma-Aldrich has provided the highest quality of reliable analytical solutions to help researchers, process managers and quality analysts meet their measurement challenges. From characterizing raw crude oil and natural gas, to monitoring the production of refined chemicals and determining the quality of alternative fuels, Sigma-Aldrich offers a broad range of products to the energy and chemical industries.As a leading solutions provider to the petrochemical industry, we are learning the challenges customers face. We offer innovative product solutions to monitor the quality of petrochemical products and to comply with industry standards – in the laboratory and online in the process environment. Our petrochemical analysis solutions include moisture determination, speciality gas chromatography (GC) columns that quantitate trace contaminants in petrochemical streams, sample preparation devices and analytical standards to insure accurate analysis of the diverse components of a sample. In this brochure we provide a summary of proven tools and consumables for sample preparation and analysis in petrochemical laboratories.This brochure is designed to illustrate typical workflow associated with analytical processes, with all the information broken down into sections such as: • Sample preparation • Columns for GC• Solvents• Standards • Karl Fischer Titration• Safety Applications3sigma-aldrich.com/petrobag. It employs the technique of flash vaporization to vaporize the sample in a continuous flow of inert gas which carries the sample to the sampling tube. After enough time has elapsed, typically less than five minutes, the tube is removed from the ATIS and analyzed using the appropriate analytical technique for that adsorbent tube.For more information, visit sigma-aldrich.com/atisSOLID PHASE EXTRACTION (SPE)Use SPE for aliphatic/aromatic hydrocarbon split and total petroleum hydrocarbons (TPH), as well as polychlorinated biphenyl (PCB) analysis in waste oils.Dual Layer Florisil®/Sodium Sulfate SPE Products for Hydrocarbon Oil Index • Retention Mechanism: Normal-phase or adsorption• Sample Matrix Compatibility: Organic solutions • Florisil particle size – 60/100 mesh (150–200 µm); Na2SO4 Purity – 99.99+%, density – 2.68 g/mL• Suitable for the determination of the hydrocarbon oil index in water (in such locations as surface, waste and sewage treatment plants) by GC-FID analysis according to European Standard EN ISO 9377-2 : 2000 This is a dual layer SPE tube (available in both glass and polypropylene hardware) that contains Na2SO4 (upper layer) and Florisil (magnesium silicate, lower layer) separated and packed with PTFE frits (glass tubes) or PE frits (PP tubes). The Na2SO4 layer aids in removing aqueous sample residues that may hinder Florisil performance and/or subsequent GC analysis.Glass SPE hardware allows users to reactivate Florisil through heating at 140 °C, 16 hours. Both tubes can be used in conjunction with Visiprep™ Large Volume Sampler (Cat. No. 57275) and Visiprep SPE Vacuum Manifolds for processing larger volume samples.Supelclean™ Sulfoxide SPE for PCB Extraction From Oils• Retention Mechanism: Normal-phase (PCB retention is facilitated via interaction between the electrophilic sulfur and the pi-electron cloud of the PCBs)• Sample Matrix Compatibility: Hexane extracts of transformer, waster and mineral oil• Developed specifically for the extraction of polychlorinated biphenyls (PCBs) from transformer, waste and mineral oilThis unique tube (available in both glass and polypropylene) consists of a patent pending silica-bonded sulfoxide SPE phase that offers a simple and efficient sample prep method for identifying PCBs at quantitation limits of 0.5 ppm.When using the polypropylene SPE tube version, a large volume reservoir is recommended for increasing SPE volume headspace. The glass SPE version is of unique design and is threaded on the mouth of the SPE tube; this allows for a screw-top cap and female luer plug to reduce moisture contamination during shipment and storage.For additional product information, visit sigma-aldrich.com/speSPE Product Ordering InformationCat. No. Hardware Description Frit Material Bed Weight Tube Volume Pack Size52582-U Glass Dual Layer Florisil SPE Tube PTFE frit Bed A 2g (Florisil), Bed B 2g (Na2SO4) 6 mL 4854116-U Polypropylene Dual Layer Florisil SPE Tube PE frit Bed A 2g (Florisil), Bed B 2g (Na2SO4) 6 mL 4855252-U Glass Supelclean Sulfoxide SPE Tube PE frit 6 g 20 mL 3055253-U Polypropylene Supelclean Sulfoxide SPE Tube PE frit 3 g 6 mL 5CALIBRATIONATIS – Adsorption Tube Injection SystemFeatures of this system include the ability to:• Inject calibration standards onto adsorbent tubes, to calibrate your analytical system• Inject surrogates and system monitoring compounds onto adsorbent tubes before or after sampling• Remove moisture from tubes prior to analysis (dry purging)• Connect an air-sampling bag to the outlet of the ATIS to vaporize a calibration standards prior to assure complete vaporisationThe ATIS provides a quick and efficient way to transfer calibration standards or samples onto an adsorbent tube or into a gas sampling 28521-U ATIS Adsorbent Tube Injector System 230V4 Analytical Solutions for the Petrochemical IndustryStandardsANALYTICAL STANDARDS FOR PETROCHEMICAL ANALYSISSigma-Aldrich offers a comprehensive line of pure standards (neats) and also single- and multi-component petrochemical solutions suitable for all analytical methods. Many of our standards are formulated to meet the prescribed recommendations of ASTM, or international bodies (including DIN, EN and ISO), as well as other international organizations.The quality and consistency of our products are supported by our ISO 9001:2000 certification. Double accreditation according to ISO/IEC 17025 and ISO Guide 34 is the highest achievable quality standard for the production of certified reference materials (CRMs). All standards are tested for purity, supported by a Certificate of Analysis. Neats and Solutions• ASTM® Petroleum Standards• Gasoline Range Organics (GRO)• Biodiesel• BTEX• DIN Standards• Diesel Range Organics (DRO)• Bioethanol• Olefins• Paraffins• Gas Calibration Standards• Fuel Oil• Inorganic standards for AAS, ICP and XRF• Underground Storage Tank (UST)• Hydrocarbons• Jet Fuel• Petroleum Refinery Reformates• GPA Standards• PNA/PONA/PIANO Mixtures• Wear Metal Standards• Organometallic Oil Solutions• Sulfur StandardsPhysical Properties• Viscosity• Colour Reference Solution• Conductivity• Density• Melting PointMatrix Materials• Soil Matrix Materials• Water Pollution/Waste Water MaterialsBiological Reference Materials• Microorganisms (CFU)For additional product information, visit sigma-aldrich.com/standardspetrochemistryCustom Standards ServicesWe also offer custom formulation, testing and packaging services for those times when a stock product will not work for your specific application. To request a quotation for a custom formulation, visit sigma-aldrich.com/standardsPARAGON VISCOSITY CERTIFIED REFERENCE MATERIALSWith almost 20 years of experience in the production and certification of quality reference materials, Paragon Scientific has become a leading producer of CRMs for viscosity measurement and has developed an international reputation synonymous with quality, affordability and first-class customer service. The company was the first to offer “Gold Standard” CRMs for a wide range of viscosity measurement applications. The range of more than 600 CRMs includes a wide variety of petrochemical and viscosity certified reference materials. Petrochemical Industry Certified Reference Materials• Gas oil certified for Cold Filter Plugging Point (CFPP)• Cloud point• Distillation using ASTM/IP and EN test method protocols• Flash point using ASTM D92 (Cleveland open cup flash point) and ASTM D93 (Pensky Marten closed cup flash point)• Freezing point• Fuels testing• Pour pointParagon Scientific also offers a growing range of CRMs for many important parameters that are widely measured across the petrochemical industry. These include the following important analytical techniques:• Color, density, flash point, refractive index, Total Acid Number (TAN) and Total Base Number (TBN)Specialized Analytical Reagents and ViscometersLithium Chloride Electrolyte, available in convenient 30 mL bottles, is manufactured and certified compliant for the ASTM method, ‘Standard Test Method for Acid Number of Petroleum Products by Potentiometric Titration’.A wide range of calibrated glass calibrated viscometers are available, supplied with or without a full ISO-IEC 17025 Certificate of Calibration. All are manufactured in accordance with ASTM D445, D446 and ISO 3104, 3105. Available with a UKAS 17025 certificate of calibration or non-calibrated.For more details, visit sigma-aldrich.com/paragonStandards ExplorerStandards Explorer provides a fast and efficient access to our extensive product line using keyword searching with name, CAS number, molecular formula or official methods.sigma-aldrich.com/standards_explorer5sigma-aldrich.com/petroPetrocol® DH OctylPetrocol DH 50.2Petrocol DHPetrocol DH 150Petrocol 2887Petrocol EX2887SPB®-1 SULFUREquity®-1SLB®-5msPTA-5HT-5 (aluminum clad)SPB-1000Nukol™Carbowax® AmineSUPELCOWAX® 10SLB-IL59SLB-IL60SP™-2380TCEPSLB-IL100SLB-IL111ChiralCarboxen®-1010 PLOTCarboxen-1006 PLOTSupel-Q PLOTAlumina sulfate PLOTAlumina chloride PLOTMol Sieve 5A PLOTBentone® 34/DNDP SCOTTCEP SCOTBMEA SCOTSqualane SCOTFluorcol™ and Krytox® Packed ColumnsGPA Packed ColumnsMicropacked ColumnsDetailed Hydrocabon Analysis (DHA) l l l lSimulated Distillation (Sim Dis) l l lFuels by Pattern Recognition l lAromatics in Fuel lOxygenates in Fuel l l l lSulfur Compounds in Fuel l l l lImpurities in Fuel l l lNatural Gas, Natural Gas Liquids l lHopanes (Triperpenes) lSolvents l l lC1-C5 Alkanes, Alkenes, Alkynes l lImpurities in Ethylene lImpurities in Propylene lAromatics l l l l lImpurities in Toluene l l lXylene Isomers l l l lMineral Spirits l lChlorinated Solvents l l lPesticides l lFluorocarbons l l lAlcohols l l l l lGlycol Ethers (Cellosolves), Diols, Glycols l l l lFormalin lKetones l l l l lCarboxylic Acids as Methyl Esters l l lDicarboxylic Acids as Dimethyl Esters l lTall Oil Fatty Acid as Methyl Esters l lEsters and Ethers l l l lImpurities in MTBE l l l lTerpenes l l l l l lAmines l l l lAromatic Amines (Anilines) l l l lSulfur Compounds l l l lDissolved Gas Analysis (DGA) lGases, Light Hydrocarbons l l l l l lProcess Analyzers l l l l lGC AnalysisGC COLUMNSSupelco offers a full-line of capillary gas chromatography (GC and GC-MS) columns, including ionic liquid, MS-grade, Fast GC, PLOT and SCOT columns, and also includes the most complete line of packed GC columns and components. These columns can be used for analyses such as purity, boiling point composition, aromatics, light hydrocarbons, fluorocarbons and sulfur-containing compounds in petroleum products using all techniques including GCxGC.Supelco GC Columns for Petroleum and Petrochemical ApplicationsDid you know?The Gas Chromatography Accessories and Gas Purification/Management Products brochure is a valuable resource for anyone who performs GC. It includes items (septa, liners, ferrules, solvents, syringes, vials, purifiers and much more) for the entire technology workflow.For more information or to obtain literature on GC columns and accessories, visit sigma-aldrich.com/gc6 Analytical Solutions for the Petrochemical IndustryIONIC LIQUID GC COLUMNSExclusive to Supelco, these columns utilize unique ionic liquid stationary phases. The IL column can be used in the first or second dimension in GCxGC to provide unique selectivity choices. They are less susceptible to damage from moisture and/or oxygen in the extracts. With a variety of different IL phases available, most with higher operating temperatures compared to traditional polysiloxane polymer or PEG GC columns, IL GC columns give additional separation power for difficult samples.Two phases are highly applicable to the petrochemical industry:• SLB-IL111 column is extremely polar and provides significant chromatographic improvement over existing columns for analytes containing double and/or triple bonds. Orthogonal selectivity to non-polar columns also provides unique separations for GCxGC applications • SLB-IL60 column has selectivity similar to traditional wax columns, but with lower bleed and is different enough to provide a unique elution pattern. ApplicationBenzene and Other Aromatics in Reformulated GasolineThe SLB-IL111 can be used in a single column configuration to determine benzene in reformulated gasoline, resolving oxygenates, such as ethanol or MTBE, from aliphatics, other aromatics, oxygenates and any internal standards. The following chromatogram shows reformulated gasoline with ethanol as the oxygenate and two internal standards. A 60 m SLB-IL111 column was able to provide the resolution of benzene from all other components. Also note that the heavy constituents (methylnaphthalenes, peaks 15 and 16) elute in a timely manner with great peak shapes. This method using Ionic Liquid GC is an excellent alternative to the current, lengthy, two-(packed) column, switching approach.For more information on ionic liquid GC columns and further applications, visit sigma-aldrich.com/il-gc column: SLB-IL111, 60 m x 0.25 mm I.D., 0.20 µm (28928-U) oven: 50 °C (3 min), 15 °C/min to 265 °C (5 min) inj. temp.: 250 °C detector: FID, 275 °C carrier gas: helium, 30 cm/sec injection: 0.5 µL, 200:1 split liner: 4 mm I.D., split type, wool packed single taper FocusLiner™ design sample: Premium unleaded gasoline, plus ethanol at 20% (v/v) and two internals each at 4% (v/v) Min4 6 8 10 12 14 161 2345678910111213141516Min23455.2 5.4 5.6 5.8 6.0 6.21. C5-C11 Hydrocarbons2. Ethanol3. Benzene4. 2-Butanol5. Methyl ethyl ketone6. Toluene7. Ethylbenzene8. p-Xylene9. m-Xylene10. o-Xylene11. 1,2,4-Trimethylbenzene12. 1,2,3-Trimethylbenzene13. 1,2,4,5-Tetramethylbenzene14. Naphthalene15. 2-Methylnaphthalene16. 1-MethylnaphthalenePeak IDs (black = aliphatic; red = aromatic; blue = alcohol; green = int. std.)7sigma-aldrich.com/petroSolventsPETROCHEMICAL APPLICATIONSEach part of the workflow requires different grades of solvent. The table below provides the suggested minimum grade solvent that should be used within each stage of an application. Minimum grade suitable for:SPE CHROMASOLV® HPLC / CHROMASOLV PlusHPLC CHROMASOLV Plus / CHROMASOLV HPLC LC-MS LC-MS CHROMASOLVGC and GC-MS applications (e.g. VOC and SVOC)Capillary GC / PRA Grade*Metal speciation TraceSELECT®Air monitoring sample preparations ACS / Reagent Grade*PRA = Pesticide Residue AnalysisComplete details and specifications for these solvents can be found at sigma-aldrich.com/solventsHYDRANAL® Reagents for Karl Fischer Titration• Karl Fischer titration is designed specifically for the determination of moisture.• Karl Fischer titration is prescribed for measuring the water content of petroleum and related products in several standard methods from ASTM, DIN and ISO.• HYDRANAL service laboratory proved its expertise for testing and calibration and achieved accreditation according to ISO/IEC 17025:2005. Petroleum specific products are available:• HYDRANAL Solver (Crude) Oil (Cat. No. 34697) is a reagent for volumetric water determination in oils• HYDRANAL Coulomat Oil (Cat. No. 34868) is a reagent for the coulometric water determination in oils• HYDRANAL Water Standard Oil (Cat. No. 34694) is a mineral-oil based matrix standard for Karl Fischer titration in oils. This standard is tested against NIST SRM 2890.TECHNICAL GUIDELINES FOR PETROLEUM APPLICATIONSTo achieve reproducible results for water content using the Karl Fischer (KF) titration method, two fundamental preconditions are required: • Preliminary homogenization of samples using a homogenizer or ultrasound• Complete dissolution or at least fine dispersion of the sample in the KF working medium for complete extraction of waterItems to note:• Crude oil and petroleum products have limited solubility in methanol• Adding chloroform and/or xylene improves sample solubility• Chloroform dissolves the hydrocarbons, while xylene dissolves the bituminous compounds• In addition to the co-solvent, some samples may require an extraction time before start of titration• Formulated oils may cause problems due to the additives• When additives interfere, an indirect titration with a Karl Fischer oven is possibleWe offer various application reports for water content determination in crude oil and petroleum products. These are available upon request from our HYDRANAL experts at hydranal@sial.com. Application support, advice on choice of reagents or any technical question about Karl Fischer titration can also be requested at this address. Examples of HYDRANAL application reports for water content determination in crude oil and petroleum products that are available upon request, include:• L108 – Crude oil• L111 – Fuel oil, heavy• L148 – Crude oil (coulometric)• L412 – Greases• L531 – Oils, with additives• L545 – Lubricating oilA complete list of HYDRANAL applications are available at sigma-aldrich.com/hydranalHYDRANAL-MOISTURE ON-SITE TEST KITThe HYDRANAL-Moisture Test Kit (Cat. No. 37858) enables the determination of the amount of water in colorless liquid samples. This ready-to-use test kit can be inserted on site, for example, directly at a solvent or fuel tank and it is likewise suitable for use in laboratories that do not have a Karl Fischer titrator.Each HYDRANAL-Moisture Test Kit includes: • HYDRANAL-Titrant E (Cat. No. 34732)• HYDRANAL-Solvent E (Cat. No. 34730)• HYDRANAL-Standard 5.00 (Cat. No. 34813)• A syringe to measure out the sample• A bottle acting as titration vessel8 Analytical Solutions for the Petrochemical IndustrySafetyDECOMMISSIONING OF OIL RIGSDuring the demolition of oil rigs, workers can be exposed to isocyanates during the welding processes. The ASSET™ EZ4-NCO Dry Sampler was specifically developed to effectively monitor occupational exposure to isocyanates and can be used to check if personal protection equipment is adequate.ASSET EZ4-NCO Dry Sampler for IsocyanatesFeatures and Benefits• Low detection limits and high capacity, with sampling times from 5 minutes up to 8 hours for true Time Weighted Average (TWA) determinations• Stable derivatization using dibutylamine (DBA) – no refrigeration or infield extraction is needed• Complete derivatization of particles, preventing underestimation of isocyanates• Compliance with ISO17734-1 “Determination of organonitrogen compounds in air using liquid chromatography and mass spectrometry – Part 1: Isocyanates using dibutylamine derivatives”Description Qty. Cat. No.Sampling DeviceASSET EZ4-NCO Dry Sampler 10 505027-U 5028-U Sample KitIncludes 2 samplers, 1 calibration fitting and 2 tube adapters2 5047-UAnalytical ColumnsLC-MS-MS Ascentis® Express C18, 5 cm x 2.1 mm, 2.7 µm particles1 53822-ULC-MS Ascentis Express C18, 15 cm x 4.6 mm, 2.7 µm particles1 53829-UAnalytical StandardDBA Isocyanate Mix (acetonitrile:methanol, 99:1, varied conc), 6 x 1 mLIsocyanic acid-di-n-butylamine (ICA-DBA) 1 µg/mL Ethyl isocyanate-di-n-butylamine (EIC-DBA) 1 µg/mL Hexamethylene diisocyanate-2(di-n-butylamine) (HDI-2(DBA)) 1 µg/mL Isophorone isocyanate-2(di-n-butyl amine) isomer 1 (IPDI-2(DBA)) 1 µg/mL Isophorone isocyanate-2(di-n-butyl amine) isomer 2 (IPDI2-2(DBA)) 0.4 µg/mL 4,4’-Methylenediphenyl diisocyanate-2(di-n-butylamine) (4,4’-MDI-2(DBA)) 1 µg/mL Methyl isocyanate-di-n-butylamine (MIC-DBA) 1 µg/mL Phenyl isocyanate-di-n-butylamine (PhI-DBA) 1 µg/mL Propyl isocyanate-di-n-butylamine (PIC-DBA) 1 µg/mL 2,4-Toluene diisocyanate-di-n-butylamine (2,4-TDI-2(DBA)) 1 µg/mL 2,6-Toluene diisocyanate-2(di-n-butylamine) (2,6-TDI-2(DBA)) 1 µg/mL40141-Ud9-DBA Isocyanate Internal Standard Mix, 6 x 1 mLIsocyanic acid-di-n-butylamine-d9 (ICA-DBA- d9) 1 µg/mL Ethyl isocyanate-di-n-butylamine-d9 (EIC-DBA-d9) 1 µg/mL Hexamethylene diisocyanate-2(di-n-butylamine-d9) (HDI-2(DBA-d9)) 1 µg/mL Isophorone diisocyanate-2(di-n-butylamine-d9) isomer 1 (IPDI-2(DBA-d9)) 1 µg/mL Isophorone diisocyanate-2(di-n-butylamine-d9) isomer 2 (IPDI2-2(DBA-d9)) 0.28 µg/mL 4,4-Methylenediphenyl diisocyanate-2(di-n-butylaine-d9) (4,4’-MDI-2(DBA-d9)) 1 µg/mL Methyl isocyanate-di-n-butylamine-d9 (MIC-DBA-d9) 1 µg/mL Phenyl isocyanate-di-n-butylamine-d9 (PhI-DBA-d9) 1 µg/mL Propyl isocyanate-di-n-butylamine-d9 (PIC-DBA-d9) 1 µg/mL 2,4-Toluene diisocyanate-2(di-n-butylamine-d9) (2,4-TDI-2(DBA-d9)) 1 µg/mL 2,6-Toluene diisocyanate-2(di-n-butylamine-d9) (2,6-TDI-2(DBA-d9)) 1 µg/mL40142-UDBA Isocyanate Standard Kit, 2 x 1 mLIncludes 1 mL of DBA Isocyanate Mix and 1 mL of d9-DBA Internal Standard Mix40143-UAIR SAMPLINGAir sampling products conforming to ASTM, NIOSH, OSHA, US EPA, California Air Resources Board (CARB) and European methods are all included in the Sigma-Aldrich offering. Consistency and reproducibility are met through our stringent quality control testing. Many of the adsorbents we manufacture are proprietary and have unique and superior performance characteristics; examples of these materials include carbon molecular sieves and graphitized carbons.The range includes active, passive and whole air samplers.Active sampling is performed by drawing air through a type of adsorbent media such as an ORBO™ tube, thermal tube, filter or impinger using an air pump. Passive sampling is achieved when contaminated air enters the device by diffusion onto the adsorbent media inside the device. A whole air sample is collected when the air is drawn into some sort of vessel (e.g. Tedlar® bag, glass bulb or a canister).Table of Air sampling product selection Active Passive Whole AirVOCs Thermal desorption tubesradiello™, SPME Tedlar bags, Supel Inert Film bagsSVOC ORBO and solvent desorption tubesradiello, SPME Tedlar bags, Supel Inert Film bagsPermanent Gases (e.g. CO)— radiello Supel Inert foil bagsIsocyanates ASSET EZ4-NCO — —Carbonyls eg AldehydesDNPH sampling tubesradiello Tedlar bags, Supel Inert Film bagsAcidic compoundsFilters with cassettes: Glass Fiber, PTFE, PVC, MCEradiello (HCL, HF)—The Supelco Air Methods Guide is a resource of sampling and analytical methods for more than 1000 compounds in air. Air monitoring of many matrices – workplace, indoor, ambient and source – are integrated into this one easy-to-read reference.For more information and to download the guide, visit sigma-aldrich.com/airmonitoringPASSIVE SAMPLINGradiello™radiello is a passive/diffusive sampling personal monitoring device that is easily mounted near to the breathing zone. The radial design of this product offers higher capacity and faster uptake/sampling rates than traditional passive monitors. Applications include BTEX, VOCs, NO2, SO2, HF, aldehydes, ozone, H2S, ammonia, HCl, phenols, 1,3-butadiene and isoprene. Some additional advantages are:• Compact, portable, unobtrusive and inexpensive • Offers indication of average pollution levels over time periods of 8 hours to weeks/months • Requires no supervision, is noiseless and can be used in hazardous environments 9sigma-aldrich.com/petro• Low cost allows for sampling at multiple locations (e.g., for highlighting pollution “hotspots”; or determining long term data trends in a specific geographical area) • Amenable to indoor air analysis and outdoor ambient air analysisTo conduct each radiello analysis, the following materials are required:• radiello Triangular Support Plate RAD121 (pk of 20) • radiello Clips RAD195 suspending radiello triangular support plate (pk of 20) • radiello Barcode Labels RAD190 (pk of 198) • radiello Empty Storage Tubes RAD1992 polypropylene (with stopper), volume 12 mL (pk of 100) Choose the matrix and packing by application from the table below. Matrix and Packing by ApplicationCat. No. Application Desorption Technique Matrix and Packing Diffusive Body NeededRAD147 Phenolic Compounds Thermal desorption matrix SS net (100 mesh, 4.8 mm diam.), Tenax-TA,RAD120 white, configured for general use, pk of 20RAD172 Ozone (O3), Acidified 3-methyl-2-benzothiazoli-none hydrazone hydrocloride (MBTH)microporous PE tube with 4,4'-dipyridylethylene coated silicaRAD1201 blue, configured for sampling light sensitive compounds, pk of 20RAD170 Hydrogen Sulfide (H2S) Solvent (water) and buffers microporous PE coated with zinc acetateRAD120 white, configured for general use, pk of 20RAD166 HF, NO2 and SO2 Water (for NO2 and SO2), IC eluate (for HF)microporous PE impregnated with wet TEARAD1201 blue, configured for sampling light sensitive compounds, pk of 20RAD169 HCl Desorption with deionized water SS net with silica gel (100–400 µm particle size)RAD120 white, configured for general use, pk of 20RAD145 BTEX and VOCs Thermal desorption SS net (3 x 8 µm, 4.8 mm diam.), CarbographRAD1202 yellow, configured for reduced sampling rates, pk of 20RAD130 BTEX and VOCs CS2 Desorption SS net (100 mesh, 5.8 mm diam.), activated with activated charcoal (30–50 mesh)RAD120 white, configured for general use, pk of 20RAD168 Ammonia (NH3) Desorption with deionized water microporous PE impregnated with phosphoric acidRAD1201 blue, configured for sampling light sensitive compounds, pk of 20RAD165 Aldehydes Solvent desorption with ACN SS net with 2,4-DNPH coated FLORISIL®RAD1201 blue, configured for sampling light sensitive compounds, pk of 20Full application details can be found at sigma-aldrich.com/radiello-applicationsACTIVE SAMPLINGSupel™-Inert Gas Sampling BagsIf you need to sample whole air, gas sampling bags are widely recognized as cost-effective alternatives to Summa canisters for sampling volatile organic compounds (VOCs), and light and permanent gases.Abrasion Resistant Supel-Inert Film BagsUsed for low VOC and sulfur background levels.• No detectable background levels of DMAC (Dimethylacetamide) and phenol, giving an inertness similar to Tedlar® for a wide range of compounds• Are suitable for up to 2-day sampling and analysis for most VOC’s and many sulfur* compounds for up to 24 hours• Are chemically inert to most acids, aliphatic and aromatic organic compounds, chlorinated solvents and alcohols*Use foil bags for storing hydrogen sulfideWe have expanded our gas sampling bag line to include our Supel-Inert film as an economic alternative for the industry standard Tedlar® material, and now also offer Supel-Inert Foil bags that are aluminium lined. Supel-Inert Film is a proprietary fluoropolymer developed specifically for air sampling applications.Supel-Inert Foil Gas Sampling BagsThese are suitable for sampling low molecular weight compounds such as carbon monoxide (CO), carbon dioxide (CO2) and permanent gases.• Multilayer foil composition composed of two outer layers of aluminum film providing a great barrier to gases permeating through the walls of the bag• Only foil bag material that can hold hydrogen sulfide for long periods, from 5 to 7 days• Sample stability up to 5 days for most recommended compounds• Chemically inert with moisture and light protection• Not recommended for low ppm VOC’s due to background levels (use Film bags)10 Analytical Solutions for the Petrochemical IndustrySupel™-Inert Gas Sampling BagsSupel-Inert FilmSupel-Inert Multi-Layer FoilPush/Pull Lock Valve (PLV)1 L 30213-U 30237-U 2 L 30214-U 30238-U5 L 30215-U 30239-U 10 L 30216-U 30240-U25 L* 30217-U —Screw Cap Valve (SCV) 1 L 30221-U 30226-U2 L 30222-U 30227-U5 L 30223-U 30228-U 10 L 30224-U 30229-U25 L* 30225-U —* Part numbers relate to a pack of 10 sampling bags, except 25 L offering, which are a pack of 5 sampling bagsBoth bag types use Thermogreen® polymer septa and are available with two valve fitting options: Push-Lock Valve (PLV) and Screw Cap Valve (SCV). Both include a septum for spiking or aliquot retrieval by a syringe. Thermogreen polymer has the industry’s lowest bleed, thus preventing any sample contamination from the septum.For more information, visit sigma-aldrich.com/gassamplingbagsFILTERS/MEMBRANESThese filters and accessories are cited in numerous Occupational Health and Safety Administration (OSHA) and National Institute of Occupational Safety and Health (NIOSH) methods in the US, and the analogous bodies in Europe. They are universally respected for quality and reliability.Whatman® QM-A Quartz FiltersHigh-purity quartz (SiO2) microfiber filters are used for air sampling in acidic gases, stacks, flues and aerosols, particularly at high temperatures up to 500 °C and in PM-10 testing Technical Note PM10 Filters. Because of the low level of alkaline earth metals, ‘artifact’ products of sulfates and nitrates (from SO2 and NO2) are virtually eliminated. QM-A, sequentially numbered according to EPA standards, is suitable for most applications.sigma-aldrich.com/qmaquartzfiltersWhatman High-purity Glass Microfiber Extraction Thimbles High-purity glass microfiber thimbles manufactured from 100% pure borosilicate glass are available for specialized applications. The thimbles are completely free of binders or additives and can be used at temperatures up to 500 °C or when using solvents incompatible with cellulose thimbles. These thimbles are also used in pollution monitoring techniques (0.8 µm nominal particle retention). Typical thickness is 1.7 mm.Features and Benefits • Available in a range of sizes and wall thicknesses to suit your application • Designed to fit most commercially available Soxhlet extractors • No binders are added Applications • Smoke stack gas monitoring sigma-aldrich.com/extractionthimblesWhatman Air Sampling Filters – EPM2000EPM 2000 has been developed especially for use in high volume PM-10 air sampling equipment that collects atmospheric particulates and aerosols. It is manufactured from 100% pure borosilicate glass of special purity enabling detailed chemical analysis of trace pollutants to take place with the minimum of interference or background.Whatman EPM 2000 was selected by the EPA to be the standard filter for use in the nationwide network of HiVol air samplers. Sheets are individually numbered to facilitate identification.sigma-aldrich.com/whatman11sigma-aldrich.com/petroWhatman Polymeric Membrane FiltersWhatman Cyclopore® membranes are true pore size microporous membranes featuring sharp cut-off and reproducible microfiltration performance characteristics of track etched membranes. The smooth flat membrane ensures particles are retained on the surface so that they are easily visible under a microscope. Cyclopore membranes are manufactured from a pure polymeric film using proprietary Whatman technology to produce a precision membrane filter with a closely controlled pore size distribution. They are free of contaminants and have very low levels of nonspecific protein binding. The polycarbonate membranes are hydrophilic and are available in a choice of diameters and pore sizes. The polyester membranes are resistant to most organic solvents, amides and halogenated hydrocarbons. This broad chemical compatibility makes them suitable for the detection of particles in many corrosive fluids.Features and BenefitsLow affinity for stains provide a higher optical contrast and make visibility under a microscope easy. There is a true surface capture which provides easy examination of samples and short analysis times. The totally transparent membranes have negligible absorption and adsorption of the filtrate and are non-hygroscopic. With low tare weights, there is no particle shedding which provides an ultra-clean filtrate, and the membranes are biologically inert. Applications • Air monitoring of Trace elements • Analytical methods - Gravimetric analysis, densitometry, emission spectroscopy, x-ray fluorescence and infrared analysis sigma-aldrich.com/pmembranefilterWhatman PM 2.5 Air Monitoring MembraneWhatman PM 2.5 filters are used for particulate matter detection in air. PM 2.5 - refers to particulate matter greater than 2.5 µm in diameter. The presence of particles in ambient air is the main cause of urban smog and can lead to respiratory illness. sigma-aldrich.com/whatmanGLASS SAMPLING TUBES FOR CARBONYL SAMPLINGORBO™-555 Solvent Desorption Tubes • Low pressure drop enables use at high sampling rates of 1.5 – 2.0 L/min, even with personal sampling pumps • High purity LpDNPH adsorbent for greater accuracy in trace analysis • Manufactured in a controlled, low carbonyl environment • Low background The ORBO-555 is a 6 mm O.D. x 110 mm length dual-bed LpDNPH glass sampling tube, containing 300 mg of LpDNPH in the front section, and 150 mg in the back section. The back section functions as a back-up bed for incidences of breakthrough that are sometimes associated with single bed DNPH cartridges in higher concentration environments, or when you are not certain of the concentration. The tube has a low pressure drop which enables use at high sampling rates of 1.5–2.0 L/min, even with personal sampling pumps.BPE-DNPH Solvent Desorption Tubes Carbonyl sampling with built-in Ozone scrubber• High purity adsorbent for better accuracy and trace analysis• High sensitivity, low background• Low pressure drop, enables use at high sampling rates (1.5–2 L/min) • New packaging, for maximum sample integrity • Manufactured in a controlled environment • Meet EPA, OSHA, NIOSH and ASTM specificationsThe BPE-DNPH cartridge is dual-layered and is comprised of silica gels impregnated with trans-1,2-bis (2-pyridyl), ethylene (BPE) as the top layer and the bottom layer of DNPH coated silica gel that collects carbonyls for analysis. The BPE converts the ozone into a DNPH derivative for either analysis, or simply for scrubbing ozone from your sample, depending on your choice of extraction method. This sampler is not affected by high humidity.Solvent Desorption Tubes for CarbonylsCat. No. Description Bed PackingTube Volume/DimensionsPack Size54020-U ORBO™ 555 LpDNPH bed A 300 mg (DNPH-coated silica), bed B 150 mg (DNPH-coated silica) with W,W,W separators6 mm O.D. × 105 mm L2054278-U BPE-DNPH Cartridgebed B 270 mg (DNPH-coated silica), bed A 130 mg (2-BPE coated silica)3 mL 1054279-U BPE-DNPH Cartridgebed A 130 mg (2-BPE coated silica), bed B 270 mg (DNPH-coated silica3 mL 50Order/Customer Service: sigma-aldrich.com/order Technical Service: sigma-aldrich.com/techservice Development/Custom Manufacturing Inquiries safcglobal@sial.com Safety-related Information: sigma-aldrich.com/safetycenterWorld Headquarters 3050 Spruce St. St. Louis, MO 63103 (314) 771-5765 sigma-aldrich.comEnabling Science to Improve the Quality of LifePNU807551093©2013 Sigma-Aldrich Co. LLC. All rights reserved. SIGMA, SAFC, SIGMA-ALDRICH, ALDRICH and SUPELCO are trademarks of Sigma-Aldrich Co. LLC, registered in the US and other countries. FLUKA is a trademark of Sigma-Aldrich GmbH, registered in the US and other countries. Ascentis, Carboxen, Equity, Petrocol, SLB, SPB, Thermogreen and TraceSELECT are registered trademarks of Sigma Aldrich Co. LLC. CHROMASOLV and HYDRANAL are registered trademarks of Sigma-Aldrich Laborchemikalien GmbH. ASSET, Fluorcol, Nukol, ORBO, SP, Supel, Supelclean and Visiprep are trademarks of Sigma-Aldrich Co. LLC. ASTM is a registered trademark of American Society for Testing and Materials. Carbowax is a registered trademark of Union Carbide. CombiPAL is a trademark of CTC Analytics. Cyclopore is a registered trademark of Whatman International Ltd. Florisil is a registered trademark of U.S. Silica Company. FocusLiner is a trademark of SGE Analytical Science Pty Ltd. Krytox and Tedlar are registered trademarks of E. I. du Pont de Nemours and Company. radiello is a trademark of Fondazione Salvatore Maugeri IRCCS. Whatman is a registered trademark of GE Healthcare. Sigma-Aldrich, Sigma, Aldrich, Supelco, Fluka and SAFC brand products are sold by affiliated Sigma-Aldrich distributors. Purchaser must determine the suitability of the product(s) for their particular use. Additional terms and conditions may apply. Please see product information on the Sigma-Aldrich website at www.sigmaaldrich.com and/or on the reverse side of the invoice or packing slip.CARBONYL ANALYSIS BY HPLCAscentis® Express C18 and RP-Amide Ascentis Express HPLC columns, through the use of Fused-Core® particle technology, can provide you with both the high speed and high efficiencies of sub-2 µm particles while maintaining lower backpressures. The combination of high efficiency and low backpressure in conjunction with robustness benefits UPLC® (or other ultra high pressure system) users as well as conventional HPLC users.Ascentis Express Particles2.7 µm 5 µm0.5 µm1.7 µm2.7 µm Solid Core0.6 µm3.3 µm5 µm Solid CoreFor more information, visit sigma-aldrich.com/expressAnalysis of 21 Aldehyde/Ketone DNPH Derivatives Using Ascentis RP-AmideThis application demonstrates the suitability of the Ascentis RP-Amide for the analysis of 21 aldehyde ketone derivatives. column: Ascentis RP-Amide, 15 cm x 4.6 mm I.D., 3 µm particles (565322-U) mobile phase A: 60:40, water:acetonitrile mobile phase B: 25:75, water:acetonitrile flow rate: 1.5 mL/min. temp.: 30 °C det.: UV at 360 nm injection: 10 µL sample: as listed in mobile phase gradient: Min %A %B 0 100 0 5 100 0 25 40 60 40 0 100 60 0 1001. Dinitrophenylhydrazine (100 µg/mL)2. Formaldehyde-2,4-DNPH (40 µg/mL)3. Acetaldehyde-2,4-DNPH (29 µg/mL)4. Acetone-2,4-DNPH (23 µg/mL)5. Acrolein-2,4-DNPH (24 µg/mL)6. Propionaldehyde-2,4-DNPH (23 µg/mL)7. Crotonaldehyde-2,4-DNPH (20 µg/mL)8. 2-Butanone-2,4-DNPH (10 µg/mL)9. Butyraldehyde-2,4-DNPH (20 µg/mL)10. Benzaldehyde-2,4-DNPH (15 µg/mL)11. Cyclohexanone-2,4-DNPH (10 µg/mL)12. Isovaleraldehyde-2,4-DNPH (18 µg/mL)13. Valeraldehyde-2,4-DNPH (18 µg/mL)14. o-Tolualdehyde-2,4-DNPH (14 µg/mL)15. m-Tolualdehyde-2,4-DNPH (14 µg/mL)16. p-Tolualdehyde-2,4-DNPH (14 µg/mL)17. Hexaldehyde-2,4-DNPH (16 µg/mL)18. 2,5-Dimethylbenzaldehyde-2,4-DNPH (13 µg/mL)19. Heptaldehyde-2,4-DNPH (19 µg/mL)20. Octaldehyde-2,4-DNPH (19 µg/mL)21. Nonaldehyde-2,4-DNPH (19 µg/mL)22. Decylaldehyde-2,4-DNPH (19 µg/mL)123456 78910,11121315,1614171819 20 21220 10 20 30 40 50 60Min column: Ascentis Express C18, 10 cm x 4.6 mm I.D., 2.7 µm (53827-U) mobile phase: 60:40, water:acetonitrile flow rate: 2 mL/min. temp.: 30 °C det.: UV at 360 nm injection: 5 µL sample: waterIsocratic Analysis of Aldehydes/Ketone DNPH on Ascentis Express C181.0 2.0 3.0 4.0 5.0 6.0Min123456 78910 1112 13RNHNHN+O-ON+O - O1. Formaldehyde-2,4-DNPH2. Acetaldehyde-2,4-DNPH3. Acetone-2,4-DNPH4. Acrolein-2,4-DNPH5. Propionaldehyde-2,4-DNPH6. Crotonaldehyde-2,4-DNPH7. 2-Butanone-2,4-DNPH8. Butyraldehyde-2,4-DNPH9. Benzaldehyde-2,4-DNPH10. Valeraldehyde-2,4-DNPH11. m-Tolualdehyde-2,4-DNPH12. Hexaldehyde-2,4-DNPH13. Methacrolein-2,4-DNPHBPE-DNPH – Acetonitrile (3 mL) Extraction column: Ascentis Express C18, 15 cm x 4.6 mm I.D., 2.7 µm particle mobile phase: 55:45 acetonitrile:water (4 min), gradient to 90% acetonitrile at 13 min (5 min hold) flow rate: 0.5 mL/min det.: UV 360 nm injection: 10 µL0 2 4 6 8 10 12 14 16 18Min0200400mAU 24135BPEDNPH0 2 4 6 8 10 12 14 16 18Min010mAU 241 3BPE DNPHAir SampleCartridge Blank1. Formaldehyde-DNPH2. Pyridine-2-aldehyde-DNPH*3. Acetaldehyde-DNPH4. Acetone-DNPH5. Hexanal-DNPH*Peak 2 is a marker for ozone presence.