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Poly-W109.01 Polyphenolics in Pulp Mill Wastewaters By NCASI METHOD POLY W109.01 POLYPHENOLICS IN PULP MILL WASTEWATERS BY SPECTROPHOTOMETRY NCASI West Coast Regional Center November 2009 This page intentionally left blank. Acknowledgments This method was prepared by Ron Messmer, Senior Research Associate, and Diana Cook, Project Leader, at the NCASI West Coast Regional Center. Other assistance was provided by Jan Napack, Research Associate, also with the NCASI West Coast Regional Center. For more information about this method, contact: Diana Cook Project Leader NCASI West Coast Regional Center PO Box 458 Corvallis, OR 97339-0458 (541) 752-8801 [email protected] For information about NCASI publications, contact Publications Coordinator NCASI PO Box 13318 Research Triangle Park, NC 27709-3318 (919) 941-6400 [email protected] National Council for Air and Stream Improvement, Inc. (NCASI). 2009. Methods Manual. NCASI Method Poly W109.01: Polyphenolics in pulp mill wastewaters by spectrophotometry. Research Triangle Park, NC: National Council of the Paper Industry for Air and Stream Improvement, Inc. © 2009 by the National Council for Air and Stream Improvement, Inc. NCASI’s Mission To serve the forest products industry as a center of excellence for providing technical information and scientific research needed to achieve the industry’s environmental goals. i Disclaimer The mention of trade names or commercial products does not constitute endorsement or recommendation for use. This method is included in NCASI’s Methods Manual and is a modified Folin reagent method for tannin-lignin (polyphenols) determination in wastewater. It is included in the Methods Manual as a proposed method. Those electing to apply the method are strongly encouraged to conduct rigorous QA/QC or validation so that the quality of data generated can be evaluated. Please note that this proposed method is not suitable for use as a regulatory monitoring or compliance method. ii NCASI METHOD POLY W109.01 POLYPHENOLICS IN PULP MILL WASTEWATERS BY SPECTROPHOTOMETRY 1.0 Scope and Application 1.1 Method Poly W109.01 procedures utilize a spectrophotometer to measure the absorbance of light as it passes through a sample that has been prepared by reaction with TanniVer 3® Folin phenol reagent. Concentrations of all hydroxylated compounds (polyphenols) that give a proportional blue color are determined by comparison of the absorbance of the sample to the absorbance of tannic acid solutions of known concentrations. 1.2 This method has been validated at the single laboratory level in wastewater treatment plant influents, biologically treated effluents from pulp and paper mills, and receiving waters. Demonstration of method performance for specific matrix types is recommended. 1.3 The estimated minimum detection limit (MDL) achievable is instrument and light path length dependent and was found to be 0.02 mg/L in reagent water using a 10 mm light path length. This value is provided as guidance. Due to variables in instrumentation and matrix effects, each laboratory should establish its own MDL. The lower instrument calibration limit (LCL) for this method is approximately 0.08 mg/L. Lower calibration levels can be obtained by using an increased light path length. The concentration range used during a single method validation was from 0.08 to 8.0 mg/L. Sample values above 8.0 mg/L may be determined by quantitative dilution (Section 12.3). 2.0 Summary of Method 2.1 Sample Preparation A sample volume of preserved or unpreserved wastewater is prepared to a volume of 25 mL in a 40 mL vial or a 50 mL round bottom tube using reagent grade water for dilution. The amount of sample utilized depends on previous experience with the sample to obtain an absorbance within the range of the calibration curve (Section 7.4). Folin phenol reagent (0.5 mL) is added and mixed with each sample or each prepared calibration point. Immediately, 5.0 mL (5 g) of sodium carbonate-tartrate buffer solution is added and mixed with each sample or prepared calibration point. Samples are allowed to react for a minimum of 30 minutes at room temperature to produce a blue- to green- hued solution. 2.2 Quantitative Analysis The absorbance of the solution is measured with a spectrophotometer set at a wavelength of 700 nanometers (ηm). The corrected concentration of the sample is calculated using the linear regression equation (Section 12.1) determined for the six point calibration curve prepared using tannic acid and the dilution factor for the sample. 1 November 2009 NCASI Method Poly W109.01—Polyphenolics by Spectrophotometry 2.3 Quality Assurance Quality is assured through reproducible calibration and testing of sample preparation and the spectrophotometer system. Calibration is verified on each day of analysis by freshly preparing and analyzing a point from the calibration curve. A method blank is analyzed with each sample set (samples started through the process on a given day, to a maximum of 20), along with sample duplicates to ensure reproducibility in the matrix. A fortified sample is assessed to determine recovery in the matrix. A complete description of quality control procedures, calculations, and method performance criteria are listed in Sections 9, 12, and 17, respectively. 3.0 Definitions 3.1 These definitions are specific to this method, but conform to common usage as much as possible. 3.1.1 May – this action, activity, or procedural step is neither required nor prohibited 3.1.2 Method Detection Limit (MDL) – As defined by EPA (1), the MDL is the lowest concentration that can be identified at the 99% confidence level as being greater than background. 3.1.3 Must not – this action, activity, or procedural step is prohibited 3.1.4 Must – this action, activity, or procedural step is required 3.1.5 Should – this action, activity, or procedural step is suggested, but not required 4.0 Interferences 4.1 Reagents, glassware, and other sample processing equipment may contribute analytical interferences, resulting in inaccurate absorbance readings. Run method blanks initially and with each subsequent sample set to demonstrate that the reagents, glassware, and other sample processing hardware are free from interferents under the conditions of the method. 4.2 Any substance that will produce a reaction with the Folin phenol reagent has the potential to cause interference. Organic compounds such as hydroxylated aromatics, proteins, humics, and amines can produce false positives (2). Ferrous iron, sodium sulfite, manganese, nitrite, cyanide, bisulfite, sulfide, and hydroxylamine hydrochloride also give a positive response when reacted with the Folin phenol reagent (2,3). 4.2.1 Ferrous iron interference at 2 mg/L will produce an increase in absorbance equivalent to 1 mg/L as tannic acid. Interference from ferrous iron up to 20 mg/L can be eliminated by adding 200 mg sodium pyrophosphate before reagents are added to the prepared sample (3). November 2009 2 NCASI Method Poly W109.01—Polyphenolics by Spectrophotometry 4.2.2 Sodium sulfite interference at 125 mg/L will produce an increase in absorbance equivalent to 1 mg/L as tannic acid. Interference from sodium sulfite can be eliminated by adding 1 mL formaldehyde solution just before reagents are added to the prepared sample (3). 4.3 All glassware must be clean and free of scratches. Cells used for spectrophotometric measurement of samples must be free of all oil or residue that may cause interference in the absorbance measurement. It is recommended that the same cell be utilized for measurements of the calibration curve, daily calibration checks, blanks, and samples. 5.0 Safety 5.1 Each chemical compound should be treated as a potential health hazard. Exposure to these compounds should be reduced to a level protective of human health. This method does not address all safety issues associated with its use. The laboratory is responsible for maintaining a current awareness file of OSHA regulations regarding the safe handling of the chemicals specified in this method. A reference file of data handling sheets (MSDS) should also be made available to all personnel involved in these analyses. 5.2 The Folin phenol reagent solution is corrosive. It contains phosphoric (H3PO4) and hydrochloric acid (HCl) pH <2. Take appropriate measures to avoid contact with chemicals by wearing chemical-resistant gloves, eye protection, and other protective clothing. 5.3 The carbonate-tartrate buffer reagent solution is corrosive. It contains sodium carbonate and sodium tartrate. The pH of this solution is >13, and it should be prepared and used with caution. Take appropriate measures to avoid contact with the chemicals by wearing chemical-resistant gloves, eye protection, and other protective clothing. 5.4 All chemicals should be treated as potential health hazards. It is recommended that prudent practices for handling chemicals in the laboratory be employed (4). As with all samples, precautions should be taken to avoid exposure to potentially toxic, caustic, or nuisance odor compounds. 6.0 Equipment and Supplies Note: Brand names, suppliers, and part numbers are cited for illustrative purposes only. No endorsement is implied. Equivalent performance may be achieved using equipment and materials other than those specified here, but demonstration of equivalent performance that meets the requirements of this method is the responsibility of the laboratory. 6.1 A spectrophotometer with a tungsten lamp source and a 10 ηm spectral slit width is required. The instrument must be capable of emitting light at a selectable wavelength of 700 ηm with an operating range of 400 to 700 ηm. Verify that the spectrophotometer is calibrated correctly by following the directions from the manufacturer for your specific instrument. 3 November 2009 NCASI Method Poly W109.01—Polyphenolics by Spectrophotometry 6.2 Do not use glassware with any star fractures, chips, cracks, or severe scratches. All glassware should be washed with detergent, rinsed with tap water, and rinsed with deionized water prior to use.
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