SOP TSS & TVSS Revision No.3b Date: 1/07/11 Page 1 of 8
STANDARD OPERATING PROCEDURE SOP Description Total Suspended Solids
Document Name TSS & TVSS Revision #3b
0dffae8ee692508c7bf2883348be124c.doc
Method: SM 18-20 2540D ELAP Code: 9065 Technology: Grav
2018 年 4 月 3 日
Approved By: ______Group Supervisor
______QA Officer
______Technical Director
Monroe County Environmental Laboratory ID 10373 1574 Lakeshore Blvd. Rochester, NY 14617
DOCUMENT CONTROL Annual Review of this SOP has been performed and reflects current practice NUMBER:______Signature: ______Date:______Initials: ______Date:______Signature: ______Date:______
Signature: ______Date:______“ORIGINAL” Watermark Must Be Visible ORIGINAL
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1. Identification of Test Method: Total Suspended Solids and Total Volatile Suspended Solids via glass microfiber filter dried at 103-105° C and fired at 550 ° C. EPA 160.2
2. Matrix: Non-potable water
3. Detection Limit: 5 mg/L (Dilution Factor x 2.5) Derived from a minimal amount of residue on a glass filtered of 1mg and 200mL sample filtered. Detection limits will vary depending sample volume filtered through the filter. 1mg/L: derived from 1mg and 1000mL sample 2mg/L: derived from 1mg and 500mL sample 4mg/L: derived from 1mg and 250mL sample
4. Scope and Application: Non Potable waters including surface water, groundwater, industrial and domestic waste water, effluents and polluted waters.
5. Summary of Method: A well-mixed sample is filtered through a weighed standard glass-fiber filter/ Gooch filter. The residue on the filter is dried to a constant weight at 103 to 105 °C. The increase in weight in the filter unit represents the suspended solids. The sample residue on its filter combination is ignited at 500 50 °C to a constant weight. The weight lost on ignition is the volatile solids.
6. Definitions:
Residue, non-filterable, is defined as those solids which are retained by a glass fiber filter and dried to constant weight at 103-105ºC.
Blank: Reagent water taken through the same analytical process as samples.
LCS: Laboratory control sample.
Run: A run is defined as all samples that are analyzed together in on batch on one day.
MDL: Method detection limit. The concentration of analyte that can be differentiated from zero
with 95% confidence.
7. Interferences:
a. Filtration apparatus, glass-fiber filter, pre-washing, post washing, and drying temperature are specified because these variables have been shown to affect the results.
b. Exclude large floating particles or submerged agglomerates of non-homogeneous materials from the sample if it is determined that their inclusion is not representative.
D:\Docs\2017-12-14\0dffae8ee692508c7bf2883348be124c.doc SOP TSS & TVSS Revision No.3b Date: 1/07/11 Page 3 of 8 C. Limit the sample size to that yielding no more than 200mg residue because excessive residue on the filter may form a water-entrapping condition..
8. Safety: Use protective eye gear (safety glasses with eye shields) and gloves. Analysts should follow the lab’s Chemical Hygiene Plan (CHP) with lab coat and glasses as well.
9. Equipment and Supplies: a. Glass fiber filter, Whatman 934-AH (21mm-gooch, 90mm-buchner funnel) b. Rubber crucible holder for receiving Gooch crucibles and filters c. Oven capable of maintaining 104 C +/-1 C d. Muffle furnace capable of maintaining 550º C e. Desiccator with anhydrous CaSO4 (Drierite) or indicating Silica get dried at 104 deg. C over night for cooling Gooch crucibles and filters to room temperature. f. Analytical Balance or balance capable of weighing to the nearest 0.0001 gram. g. Vacuum, suction and filtered water trap. h. Large tongs for holding Gooch crucible. i. Flat end forceps or tweezers for lifting filters. j. 100 and 250 ml graduated cylinders.
10. Reagents and Standards: a. LCS: 0.2000g NaCl + 0.2000g Celite / Diatomaeous earth to 2.0 L distilled water.
11. Sample Collection, Preservation, Shipment and Storage: Store in plastic or glass containers. a. Hold in refrigeration at 4° C until analyzed. b. Analyze samples samples soon after they are received, to avoid microbiological decomposition of solids. Samples must be analyzed within 7 days.
12. Quality Control (QC): a. Method Blank: One blank sample run or batch. b. Duplicates: 10% of samples should be repeated1 for precision purposes. c. LCS: One per batch or twenty samples, whichever more frequent.
13. Calibration and Standardization: No instrument. Ovens are checked once daily for proper temperature. The analytical balance is checked daily.
14. Procedure: Preparation of Clean Gooch with fiber filters : a. Cleaning of dirty gooches: - take filter out of used gooch - soak the gooches in a pan with 1-2 tsp of Alconox till ready to clean. - fill sink with hot water, put in gooches and scrub each with brush and rinse - put gooches in basket and rinse again - put gooches in a pan and dry for 10 to 20min., or until dry b. Place the glass fiber filter, wrinkled side up, into a clean labeled Gooch crucible. c. Place crucible and filter unit in rubber holder hooked up to vacuum apparatus. d. While vacuum is applied, wash filter with three 20 mL portions of distlled water, suction dry. e. Dry in an oven at 103-105 °C for an hour before use, and / or store in oven at 103-105 ºC D:\Docs\2017-12-14\0dffae8ee692508c7bf2883348be124c.doc SOP TSS & TVSS Revision No.3b Date: 1/07/11 Page 4 of 8 until use. f. Fire crucible and filter in muffle furnace for 15 minutes at 550° C. If volatile solids are to be measured. If volatile solids are not required remove the crucibles from the 103-105° C. cooling a minimum of 1 hour. Leave jar lid open for 5 minutes to prevent build up of vacuum pressure. Close jar lid.
Sample Preparation : Take sample bottles out of cold storage and warm to room temperature.
Sample Analysis: a. Cool prepared labeled Gooch crucibles with filter in a desiccator for one hour to reach room temperature. b. Prepare bench worksheet with date and analyst. c. Weigh crucibles on analytical balance to the nearest 0.0001 gram, placing in a pan for storage before analysis. d. Place Gooch crucible in rubber holder on vacuum apparatus and wet filter with 10 ml of distilled water. Turn on vacuum to seal filter to crucible. e. Shake sample vigorously, inverting at least 3 times, to evenly distribute any suspended or settled material in the sample bottle. Use a pipette for volume of 25mL (or less) or 100 - 250 mL graduated cylinder. f. Filter as much sample as the filter can handle. Try to filter enough volume to obtain a minimum of 1.0 mg suspended solids on the filter disk. If the filtration rate begins to drop, stop adding sample. Enter volume amount used (ml sample) under sample identification on bench worksheet. g. After all trace of sample has run through the crucible and filter apparatus, rinse the cylinder three times with approximately 10 –12 ml distilled water and pour on the filter to wash the filter of all dissolved sample. Allow vacuum to dry the crucible and filter in place for a few minutes. h. Turn off suction. Carefully remove crucible and filter unit from apparatus with large tongs and place unit in pan while all samples are being processed. i. After all samples are filtered, place pan with crucible and filter units in a 103-1050 C oven for 1 hour. Record time samples entered drying oven, and the time samples are removed. j. Remove crucible and filter unit from pan used to retain crucibles in the oven with tongs and place in desiccator to cool to room temperature. This cooling should take at least 1 hour, with a maximum of 10 Gooches per desiccator. k. Weigh crucible on analytical balance to 0.0001g. l. Through the analysis of a constant weight study it has been proven that 1 hour single weight determination is acceptable and meet the required method of weighing to constant weight within 0.0005 gms. See M:\LAB\QC\GROUP\Manual Wet Chem \ Constant_Weight_TSS.xls. m. Note that if the you are unable to filter enough sample through the Gooch filter to meet the minimum 1.0 mg weight change you must report the result with an elevated detection limit or repeat the sample at a greater volume using the 9cm test below.
Aeration Pads: (9cm glass microfiber filter) a. Label each pads with a # using Ferric Chloride b. Burn for 5 minutes in muffle furnace (acts as a fixative for Ferric Chloride reducing bleed)
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c. Place a filter on Buchner funnel with wrinkled surface up and rinse pad with three successive 20mL volumes of distilled water. d. Place filters in a pan and put in a 103 – 105 ºC oven for 1hour. You may skip this step if time allows for completion in muffle furnace. e. Fire filters (muffle furnace 500 ºC) for 20 minutes. f. Place filters in a dessicator for an hour before use, and / or store in a dessicator until used.
PROCESS FOR VOLATILE SUSPENDED SOLIDS a. Complete either TSS Gooch Crucible or 9cm Pad analysis as outline above. After recording weight of dried residue and filter and crucible at 103-105° C. Place crucible and filter unit or 9cm filter directly into muffle furnace (5500C) for 15 minutes. b. Take crucible and filter unit out of oven and cool slightly before placing in desiccator to cool to room temperature. NOTE: Leave desiccator lid ajar for approximately 5 minutes to prevent pressure build up from heat. Experience has shown that a drying and cooling time of 1 hour each is sufficient. c. Weigh crucible and filter to nearest 0.0001 gram, enter weight of ignited Crucibleand filter or 9 cm filter in appropriate field on bench worksheet. d. Through the analysis of a constant weight study it has been proven that 1 hour single weight determination is acceptable and meet the required method of weighing to constant weight within 0.0005 gms. See Q:\QC\Manual Wet Chem \ Constant_Weight_TSS.xls. e. Subtract the average ignited crucible weight from the average dry crucible weight to obtain the volatile solids weight. Complete calculations (See calculation below)
Calculations: Calculate non-filterable residue as follows:
Non – filterable residue, mg/L = ( A – B ) x 1,000 C A = weight of filter (or filter and crucible) + residue in mg B = weight of filter (or filter and crucible) in mg C = mL of sample filtered
Calculate Volatile non-filterable residue as follows:
Volatile Non – filterable residue, mg/L = ( A – B ) x 1,000 C A = weight of filter (or filter and crucible) + residue 103-105° c in mg B = weight of filter (or filter and crucible) in mg + Ash residue 550° c in mg C = mL of sample filtered
15. Method Performance: Method performance is assessed through participation in the ELAP accreditation program.
D:\Docs\2017-12-14\0dffae8ee692508c7bf2883348be124c.doc SOP TSS & TVSS Revision No.3b Date: 1/07/11 Page 6 of 8 16. Pollution Prevention: The less is better philosophy is used.
17. Data Assessment and Acceptance Criteria for Quality Control Measures:
Method Blanks - Analysis of Laboratory reagent grade water is carried throught the entire process. These results are recorded and must be below the method reporting limits for a run to be acceptable. This applies to all aspects of analysis and applies to both TSS and Volatile analysis for both Gooch crucible analysis and 9 cm Buchner filter method.
LCS - Laboratory control samples are analyzed minimally one per sample batch. They are prepared internally and use diatomaceous earth as the suspended fraction for the analysis. Sodium Chloride is added at the same concentration. This acts as a positive interference, measuring method competency. Recovery limits are set through internal QC monitoring and limits generated minimally on an annual basis. Do to the nature of suspended solids and non homogeneous mixtures, failed LCS’s should be repeated using Gooches from the same batch as which the samples were analyzed. If the second LCS fails the run should be voided and the associated samples repeated. Limits may be found in Q:\QC\Solid\ss(Year).xls Current Limits are also listed on the sheet used for recording tare weights.
18. Corrective Actions for Out of Control Data: Follow the procedure outlined in v:\usr\shared\Logel\xldata\ QC FLOW CHART.
19. Contingencies for Handling Out-of-Control or Unacceptable Data: Follow the procedure outlined in v:\usr\shared\Logel\xldata\ QC FLOW CHART.
20. Waste Management: The laboratory is responsible in complying with all Federal, State and local regulations governing waste management, particularly the hazardous waste identification rules and land-disposal restrictions. Compliance with all sewage discharge permits and regulations is required. The “Less is Better” philosophy is encouraged. The reference for waste disposal is Prudent Practices in the Laboratory, NRC, 1995. There are no hazardous wastes associated with this method. Therefore, all waste can be discarded down the drain.
21. References a. 1998. Clesceri, L.S., A.E. Greenberg and A.D. Eaton (editors). Standard Methods for the Examination of Water and Wastewater, 20th edition. b. Prudent Practices in the Laboratory
22. Validation Data: Certification is maintained through DOH ELAP Proficiciencies.
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Revision History: Revision Date Author Change Rev 3 8/29/07 SAG/SG New SOP Format
Rev3a 2/29/08 PG/SAG 7.0 Added interferences Added detection limit for methods Added QC definition for blanks and LCS Added instruction for preparation of LCS Added frequency requirement for LCS 14.l. Removed weighing to constant weight and added path to QC study 14. m . Added requirement of minimum change of 1.0 mg weight change adding reanalyze sample on 9 cm pad if Gooch crucible clogs before 1.0 mg weight change Added calculation for TVSS 17.0 Added QC reuirements for both Method Blanks and LCS for TSS and TVSS analysis
Rev3b. 1/07/11 SAG
Distribution List:
Assigned Person/Area Copy # QA\QC 1 Solids 2
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The analysts identified below have read this method and have agreed to implement this method for future analysis.
Analyst(s):
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