Summaries of Standard Operating Procedures (SOPs) for Test Method 310

This page last reviewed March 20, 2012


SOP MLD SAS01 (Last Revised: August 17, 2010)
This procedure is based on ASTM D2369-87 and U.S. EPA Method 24/24A. The gravimetric analysis is for the determination of total volatile material in a sample. An aliquot of product is weighed into an aluminum foil dish and heated in a forced-air oven at 110 C for 60 minutes. The total volatile material is the difference in weight of the sample before and after heating. The total VOC is subsequently corrected for non-VOC, low vapor pressure and exempt compounds in the final weight percent calculation.

SOP MLD SAS02 (Last Revised: August 18, 2010)
This procedure is based on ASTM D 1426-93 and U.S. EPA Method 300.7. Ammonia present in products at a concentration greater or equal to 0.1% w/w is determined by accurately weighing approximately 1.0 g of product in a 10 ml volumetric flask and brought to volume with 1-methoxy-2-propanol (MPA). A 1.0 ml aliquot of the dilution is transferred to a 100 ml volumetric flask and brought to volume with deionized water. Ion chromatography with a conductivity detector is used to analyze the ammonium ion (NH4+) in the solution via autosampler.

SOP MLD SAS03 (Last Revised: August 19, 2010)
The procedure is based on the Karl Fischer procedures specified in ASTM D 4017-96 and ASTM D 3792-91. The procedure determines water content in the product using Karl Fischer reagent integrated with a drying oven. An aliquot of 1 ml is accurately weighed into 1-methoxy-2-propanol (MPA) and diluted to 10.0 ml. An aliquot of 250 l of this solution is placed in a headspace vial and the moisture from the sample is carried from the oven into a titration vessel by a stream of dry, inert carrier gas (or dried ambient air). The moisture in the titration vessel is titrated continuously until the designated endpoint is reached. The Karl Fischer reagent is designed to eliminate the interferences of ammonium, amines, and reactive carbonyls.

SOP MLD SAS04 (Last Revised: August 19, 2010)
This procedure is based on U.S. EPA Method 24/24A, Part 60, Title 40, CFR, Appendix A and ASTM D3792-91.  This procedure determines water content in the product using gas chromatography/thermal conductivity detector. An aliquot of approximately 1 ml is accurately weighed into 1-methoxy-2-propanol and diluted to 10.0 ml. The solution is thoroughly mixed and the solids, if present, allowed to settle. A volume of 1 l is injected into a gas chromatograph. The gas chromatographic data system is programmed with the appropriate retention time and response factor for water using an external calibration procedure. This procedure may not be applicable for the following types of products: low water content (<5%), products containing aerosol propellants which co-elute with water, and products which form water as a by-product during the drying step (MLD SOP SAS01).

SOP MLD SAS05 (Last Revised: August 18, 2010)
This procedure describes a method for collection and analysis of aerosol propellant by gas chromatography/thermal conductivity detector. An aerosol container is pierced and the propellant is collected in one liter evacuated Tedlar bag.   This aliquot is injected into a gas chromatograph (GC) and the components of the propellant are identified.  Any exempt compounds present are quantified. Under the regulations, the following gaseous compounds are exempt from the definition of "Volatile Organic Compounds (VOC): carbon monoxide (CO), carbon dioxide (CO2), methane (CH4), ethane (C2H6), 1,1-difluoroethane (HFC-152a), 1,1,1-trifluoroethane (HFC-143a), trifluoromethane (HFC-23), and 1,1,1,2-tetrafluoroethane (HFC-134a).  The data produced from the GC is in volume based units, therefore density measurement is needed to convert the data into a mass based format. For more information see ARB Method 310, U.S EPA Method 18, U.S EPA Method 8240, ASTM D 859-88 and NIOSH 1400.

SOP MLD SAS06 (Last Revised:August 23, 2010)
This procedure qualitatively identifies compounds present in consumer products using a headspace gas chromatographic/mass spectrometer (GC/MS) technique.  Approximately 100 l of undiluted sample is introduced into a 40 ml headspace vial containing 4.0 ml of 10% water/polyethylene glycol 400 (PEG 400).  The vial is then sealed and placed into the headspace sampling unit.  The PEG 400 dispersant is used to insure that small variations in sample polarity will not affect the analyte(s) partition coefficient.  The vial is equilibrated to 80 C, pressurized to a constant pressure, and an aliquot of the headspace gas is injected into a GC/MS equipped with a 60m, 0.25 mm id. DB-VRX capillary column.

SOP MLD SAS07 (Last Revised: August 20, 2010)
This procedure determines exempt compounds acetone, ethanol (antiperpirants/deodorants), dichloromethane, perchloroethylene, 1,1,1-trichloroethane, p-chlorobenzotrifluoride, methyl acetate, glycols, and siloxanes, as well as non-exempt compounds generally found in consumer products.  An aliquot of 1 ml is accurately weighed into 1-methoxy-2-propanol and diluted to 10.0 ml. The solution is thoroughly mixed and the solids, if present, are allowed to settle. A volume of 1 l is injected into a gas chromatograph equipped with an FID. The data system is programmed with the appropriate retention times and response factors to automatically quantitate the analytes.

SOP MLD SAS09 (Last Revised: August 17, 2010)
This procedure determines the boiling point distribution in consumer products by gas chromatography to identify low vapor pressure-volatile organic compound components.  An aliquot of the pure (undiluted) sample is used for analysis, if possible.  If the sample is viscous or a solid, the sample is diluted or dissolved in approximately 1.4 ml of carbon disulfide.  The solution is thoroughly mixed. The sample is checked to ensure that it is not biphasic and/or the solid has completely dissolved.  A volume of 1 l is injected into a gas chromatograph equipped with an FID.  The data system is programmed to report the boiling distribution in list, plot and chromatogram formats.  The results indicate the percent of the sample mass that boiled at a given temperature as well as the initial boiling point and the final boiling point of the sample.

SOP MLD SAS12 (Last Revised: January 23, 2012)
This procedure is used to measure the aromatic hydrocarbons in multi-purpose solvents and paint thinners by multidimensional gas chromatography equipped with dual detectors, flame ionization and mass selective detector (FID/MSD). Depending on sample matrix, the sample can be analyzed neat or can be dissolved in hexane or cyclohexane prior to analysis. An aliquot of 0.1 μl of the sample (neat or dilute) is injected into the GC system. The total aromatic content is determined by measuring the peak area of C6 to C10+ aromatics with boiling points less than 270 degrees centigrade (C) as compared to the total area of the chromatogram.

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