This method describes a procedure for isolating d compounds from aqueous samples. Those I think would be even better than doing the extraction in the bottle, just for purposes of centrifuging since you have to limit the centrifuge speed on the bottles to prevent breaking them. The test methods page continues to expand and improve. No warranty express or implied is made as to the website accuracy, completeness, or applicability such as the age of a method and whether or not it applies to your project. Due to a lapse in appropriations, EPA websites will not be regularly updated. Latest Blog Posts from Separation Science.
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The method also describes concentration techniques suitable for preparing the extract for the appropriate determinative methods described in Section 4. Each analyst must demonstrate the ability to generate acceptable results with this method.
Organochlorine pesticides may dechlorinate, phthalate esters may exchange, and phenols may react to form tannates. These reactions increase with increasing pH, and are decreased by the shorter reaction times available in Method Method is preferred over Method for the analysis of these classes of compounds. However, the recovery of phenols may be optimized by using Method , and performing the initial extraction at the acid pH.
NOTE: Fritted glass discs are difficult to decontaminate after highly contaminated extracts have been passed through. Columns without frits may be purchased. Use a small pad of Pyrex? Prewash the glass wool pad with 50 mL of acetone followed by 50 mL of elution solvent prior to packing the column with adsorbent. A ground-glass stopper is used to prevent evaporation of extracts. Attach to concentrator tube with springs, clamps, or equivalent.
Snyder column - Two-ball micro Kontes K or equivalent. The following glassware is recommended for the purpose of solvent recovery during the concentration procedures requiring the use of Kuderna-Danish evaporative concentrators. Incorporation of this apparatus may be required by State or local municipality regulations that govern air emissions of volatile organics.
EPA recommends the incorporation of this type of reclamation system as a method to implement an emissions reduction program. Solvent recovery is a means to conform with waste minimization and pollution prevention initiatives. The bath should be used in a hood. Erlenmeyer flask - mL.
Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination.
Reagents should be stored in glass to prevent the leaching of contaminants from plastic containers. Dissolve 40 g NaOH in organic-free reagent water and dilute to mL. Other concentrations of hydroxide solutions may be used to adjust sample pH, provided that the volume added does not appreciably change e. Purify by heating to EC for 4 hours in a shallow tray, or by precleaning the sodium sulfate with methylene chloride.
If the sodium sulfate is precleaned with methylene chloride, a method blank must be analyzed, demonstrating that there is no interference from the sodium sulfate. Other concentrations of acid solutions may be used to adjust sample pH, provided that the volume added does not appreciably change e.
Slowly add 50 mL of H2SO4 sp. Hexane, C6H14, boiling point Cyclohexane, C6H12, boiling point Acetonitrile, CH3CN, boiling point Alternatively, if the entire contents of the sample bottle are to be extracted, mark the level of sample on the outside of the bottle. If high analyte concentrations are anticipated, a smaller sample volume may be taken and diluted to 1-L with organic-free reagent water, or samples may be collected in smaller sample bottles and the whole sample used.
See Method and the determinative method to be used for details on the surrogate standard solution and matrix spiking solution. Alternatively, use 1.
Use 60 mL of methylene chloride to rinse the cylinder or bottle and transfer this rinse solvent to the separatory funnel. If the sample was transferred directly from the sample bottle, refill the bottle to the mark made in Sec. Alternatively, pour the exchange solvent into the top of the Snyder column while the concentrator remains on the water bath in Sec. NOTE: Methylene chloride creates excessive pressure very rapidly; therefore, initial venting should be done immediately after the separatory funnel has been sealed and shaken once.
The separatory funnel should be vented into a hood to avoid exposure of the analyst to solvent vapors. If the emulsion interface between layers is more than one-third the size of the solvent layer, the analyst must employ mechanical techniques to complete the phase separation. The optimum technique depends upon the sample and may include stirring, filtration of the emulsion through glass wool, centrifugation, or other physical methods.
Collect the solvent extract in an Erlenmeyer flask. Combine the three solvent extracts. Serially extract three times with 60 mL of methylene chloride, as outlined in Secs.
Collect and combine the extracts and label the combined extract appropriately. Collect the dried extract in a K-D concentrator. Rinse the Erlenmeyer flask, which contained the solvent extract, with 20 - 30 mL of methylene chloride and add it to the column to complete the quantitative transfer. Prewet the Snyder column by adding about 1 mL of methylene chloride to the top of the column. Place the K-D apparatus on a hot water bath 15 - 20EC above the boiling point of the solvent so that the concentrator tube is partially immersed in the hot water and the entire lower rounded surface of the flask is bathed with hot vapor.
Adjust the vertical position of the apparatus and the water temperature as required to complete the concentration in 10 20 minutes. At the proper rate of distillation the balls of the column will actively chatter, but the chambers will not flood.
When the apparent volume of liquid reaches 1 mL, remove the K-D apparatus from the water bath and allow it to drain and cool for at least 10 minutes.
Concentrate the extract, as described in Sec. If sulfur crystals are a problem, proceed to Method for cleanup. The extract may be further concentrated by using the technique outlined in Sec.
Prewet the column by adding 0. Place the K-D apparatus in a hot water bath so that the concentrator tube is partially immersed in the hot water. Adjust the vertical position of the apparatus and the water temperature, as required, to complete the concentration in 5 - 10 minutes. When the apparent volume of liquid reaches 0. Remove the Snyder column, rinse the flask and its lower joints into the concentrator tube with 0.
During evaporation, the tube must be positioned to avoid water condensation i. Under normal procedures, the extract must not be allowed to become dry. If analysis of the extract will not be performed immediately, stopper the concentrator tube and store refrigerated. If the extract will be stored longer than 2 days it should be transferred to a vial with a PTFE-lined screw-cap or crimp top, and labeled appropriately.
Phenols may be analyzed, by Method , using a 1. Method also contains an optional derivatization procedure for phenols which results in a 0. Refer to Method for guidance on the cleanup procedures available if required. Extraction pH sequence may be reversed to better separate acid and neutral waste components. Excessive pH adjustments may result in the loss of some analytes see Sec.
EPA 3510C PDF
Separation Science offers free learning from the experts covering methods, applications, webinars, eSeminars, videos, tutorials for users of liquid chromatography, gas chromatography, mass spectrometry, sample preparation and related analytical techniques. We do approx samples incl extracted calibration curve and QC on a single day by 1 analist. Extraction pH is dependent on the target analytes, e. Latest Blog Posts from Separation Science.
SW-846 Test Method 3510C: Separatory Funnel Liquid-Liquid Extraction
I have sent an email to the MICE site to ask if the sample bottle can be considered equivalent to a separatory funnel so we can claim EPA Method C as the extraction method, or if we have to claim EPA Method microscale extraction method with modification to larger vial size. I doubt that our eps will invest a lot of money into costly automation, but knowing the options is better than not. Thu Mar 03, 8: The shaker table is a modification that I did to speed up the process. Sun Jul 03, Shaking for 10 minutes each time then 10 minutes in a centrafuge definitely helps separate the layers and for actual samples almost necessary for emulsion breaking I use a pipette to remove the organic layer.