3.0 DETECTION LIMIT 3.1. See Procedure ALQAP Procedure for the Determination of Uncertainty
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1 1.0 IDENTIFICATION 1.1. SM 2540D Total Suspended Solids dried at C. 2.0 APPLICABLE MATRIX 2.1. Drinking Water 3.0 DETECTION LIMIT 3.1. See Procedure ALQAP Procedure for the Determination of Uncertainty 4.0 SCOPE AND APPLICATION 4.1. The method applies to the determination of total suspended solids in drinking water Total Suspended Solid is defined as a portion of solids that is retained by crucible filter. 5.0 SUMMARY OF THE TEST METHOD 5.1. A well-mixed sample is filtrated through a crucible filter and the residue retained in the filter is dried to a constant weight at 103ºC - 105ºC. The increase in weight of the filter represents the total suspended solids. 6.0 DEFINITIONS 6.1. Total Suspended Solid - a portion of solids that is retained by weighted crucible filter Method Blank Is used to check possible contamination in equipment and supplies used in the measurement process. 7.0 INTERFERENCES 7.1. Large floating particles or submerged agglomerates of materials should be removed if not representative For samples high in dissolved solids, thoroughly wash the filter after filtration of sample with deionized water to ensure removal of dissolved material Samples with two-phases or three-phases must be kept homogeneous during transfer to crucible Samples with high mineral concentration of calcium, magnesium, chloride or sulfate may be hygroscopic and require prolonged drying, followed by proper desiccation and rapid weighing. 8.0 SAFETY 8.1. Regular laboratory safety equipment should be used at all times during the analysis including gloves, safety glasses and laboratory coat. 9.0 EQUIPMENT & SUPPLIES 9.1. Glass fiber filters without organic binder 9.2. Gooch Crucible, 25mL 40mL capacity, with Gooch crucible adapter Filtration apparatus. (Section 23.1) 9.4. Suction Flask (Section 23.1) 9.5. Drying Oven, for operation at 103 C C 9.6. Desiccator, provided with a desiccant containing color indicator of moisture concentration or an instrumental indicator Analytical balance, capable to weighing to 0.10 mg. Page 1 of 7
2 9.8. Magnetic stirrer with TFE stirring bar Wide bore pipets or graduated cylinder REAGENT & STANDARD Reagent Water: Deionized Water 11.0 SAMPLE COLLECTION, PRESERVATION SHIPMENT AND STORAGE Samples should be collected in plastic or glass bottles If storage is required stored samples should be at 4 C Bring to room temperature before analysis QUALITY CONTROL Every tenth sample should be analyzed in duplicate. If the batch has less than ten samples always analyze one sample in duplicate Duplicate determinations should agree within precision acceptance limit generated by the laboratory Method blank required at the beginning of every batch. Results should be less than method detection limit CALIBRATION AND SATANDARIZATION Perform internal calibration of analytical balance every day of use Verify balance calibration using calibrated Class A weights PROCEDURE Preparation of Crucible Insert disk with wrinkled side up into crucible Apply vacuum and wash disk with three successive 20 ml portions of reagent grade water Dry crucible and filter in a drying oven at C for one hour. Cool in a desiccator Repeat cycle of drying, cooling, desiccating and weighing until a constant weight is obtained or until weight change is less than 4% of the previous weight Record constant weight in Logbook Form 005A. Refer to Section Store in a desiccators until needed Sample Procedure Record Crucible ID in Logbook Form 074 Page 2. Refer Section Assemble filtering apparatus and filter and begin suction (Section 23.1). Wet filter with reagent water to sit it. Stir sample with a magnetic stirrer at a speed to shear larger particles While stirring, pipet measured volume into the seated glass-fiber filter. For homogeneous samples pipet from the approximate midpoint of container but not in the vortex Choose a point both middepth and midway between wall and vortex Or when the sample is well mixed transfer sample to graduated cylinder to measure sample and then transfer to crucible Pipet sample volume yield between 2.5 and 200 mg of sample. If sample contains large amount of solids less volume of sample can be used. Page 2 of 7
3 Wash filter with three successive 10 ml volumes of reagent water. Allow complete drainage between washings. Continue suction for 3 minutes after filtration is complete. If more than 10 minute are required to complete filtration, decrease sample volume Remove the crucible with filter from the filtration apparatus Record volume of sample filtrated in Logbook Form 074 Page 2. Refer to Section Dry for at least one hour at C in an oven. Cool in a desiccator and weigh Repeat the cycle of drying, cooling, desiccating and weighing until a constant weight is obtained or until the weight change is less than 4% of the previous weight Record crucible weight in Logbook Form 074 Page 2. Refer Section DATA ANALYSIS AND CALCULATIONS Mg total suspended solids / L = (A B) X 10 6 sample volume in ml. A= weight of crucible, filter and dried residue g. B= weight of empty crucible and filter g Relative % Difference (RPD) Between Sample Duplicate: RPD = (Sample Result Sample Duplicate Result) x 100 (Sample Result + Sample Duplicate Result)/ METHOD PERFORMANCE Refer to laboratory Method Quality Performance Data files POLLUTION PREVENTION Pollution Prevention should be the management first option When wastes cannot he feasibly reduced at the source recycling is the next best option See Procedures ALGAP DW 004 Laboratory Waste Disposal, ALGAP DW 012 Sample Storage and Disposition DATA ASSESMENT AND ACCEPTANCE CRITERIA FOR QUALITY CONTROL MEASURES See Procedure ALQAP DW Statistical Control Procedure, ALGAP DW 002- Procedure of Non-Conforming Results 19.0 CORRECTIVE ACTIONS FOR OUT OF CONTROL DATA See Procedure ALQAP DW Corrective and Preventive Actions 20.0 CONTIGENCIES FOR HANDLING OUT OF CONTROL OR UNACCEPTABLE DATA See Procedures ALQAP DW Statistical Control Procedure, ALGAP DW 002 Procedure of Non-Conforming Results 21.0 WASTE MANAGEMENT See Procedures ALGAP DW 004 Laboratory Waste Disposal, ALGAP DW 012 Sample Storage and Disposition. Page 3 of 7
4 22.0 REFERENCES Standard Method for the Examination of Water and Wastewater - SM 2540D SM 4020 Quality Assurance/ Quality Control ISO Standard Puerto Rico Dept. of Health Regulation for Drinking Water Manual for the - Certification of Laboratories Analyzing Drinking Water PRDOH TABLES, DIAGRAMS, FLOWCHARTS Figue 1 Filtration System Page 4 of 7
5 23.2. Figure 2 - Logbook Form 005 A Page 5 of 7
6 23.3. Figure 2 - Logbook 074 Page 1 Page 6 of 7
7 23.4. Figure 2 - Logbook 074 Page CHANGE HISTORY 10/10/13 REV. A First Issued 09/04/14 REV. B Correction of all quality manual procedure id used as reference. 09/16/16 REV. C Updated reference in section 22.0 Page 7 of 7
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