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SOLIDS ANALYSIS SOLIDS ANALYSIS Prepared By Michigan Department of Environmental Quality Operator Training and Certification Unit

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SOLIDS ANALYSIS SOLIDS ANALYSIS NOTE: Page Numbers and Procedure Step Numbers Relate to the Operator Training and Certification Unit’s Laboratory Training Manual Available on the OTCU Website at

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Classification of Solids Suspended Solids Those solids that are non-filtrable with specified filters and are not volatilized at 103 degrees Celsius. Stuff that will not go through special filters and will not be lost when heated to dry the filter.

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Classification of Solids Suspended Solids Those solids that are non-filtrable with specified filters and are not volatilized at 103 degrees Celsius. Dissolved Solids Those solids which are in solution and are therefore filtrable. Stuff that DOES get through the filters

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Classification of Solids Suspended Solids Those solids that are non-filtrable with specified filters and are not volatilized at 103 degrees Celsius. Suspended Volatile Solids That portion of the suspended solids which are volatilized at 550 degrees C Dissolved Solids Those solids which are in solution and are therefore filtrable. Total Solids All of the solids present whether suspended or dissolved. Total Volatile Solids That portion of the total solids which are volatilized at 550 degrees C.

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TOTAL SUSPENDED AND VOLATILE SUSPENDED SOLIDS PROCEDURE TOTAL SUSPENDED AND VOLATILE SUSPENDED SOLIDS PROCEDURE The Suspended Solids are removed from a sample by filtration and weighed. (Gravimetric) The Solids are ignited at 550°C. The remaining solids are the Fixed (inorganic) solids. The loss on ignition is the Volatile (organic) solids. Standard Methods, 1997 Methods 2540 D (TSS) and 2540 E (VSS)

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2.11 Insert glass fiber filter FILTERING FLASK 2.12 Seat filter 2.13 Dry briefly 103 deg. C 2.13 Ignite in muffle furnace 550 deg. C for 15 minutes 2.14 Cool in drying oven briefly

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2.13 Ignite in muffle furnace 550 deg. C for 15 minutes 2.14 Cool in drying oven briefly 2.14 Cool in desiccator to room temperature

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Desiccator To Prevent Errors in Weighing of Crucibles by Providing a 0% Humidity Atmosphere While the Crucibles Cool to Room Temperature.

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Desiccator To Prevent Errors in Weighing of Crucibles by Providing a 0% Humidity Atmosphere While the Crucibles Cool to Room Temperature. (Indicating Desiccant is Required) Blue - Good Pink – Must Be Replaced or Recharged

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2.13 Ignite in muffle furnace 550 deg. C for 15 minutes 2.14 Cool in drying oven briefly 2.14 Cool in desiccator to room temperature 2.15 Weigh crucible

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Desiccation Time - Must Verify Cooling Time By Reweighing to Constant Weight. (Change Less Than 4% or 0.5 mg.) Repeat at Least 10 Times. Keep Data on File. Repeat Annually.

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2.13 Ignite in muffle furnace 550 deg. C for 15 minutes 2.14 Cool in drying oven briefly 2.14 Cool in desiccator to room temperature 2.15 Weigh crucible

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Ignite Cool Desiccate Weigh 2.16 Repeat Change Less Than 4% or 0.5 mg.

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2.21 Choose sample volume 2.5 to 200 mg 2.22 Thoroughly mix 2.23 Place crucible on vacuum flask, wet filter 2.2 Sample Analysis

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2.24 Pour sample in Gooch crucible Filter with vacuum Wash graduate, crucible, and filter with distilled water Dry crucibles plus solids for one hour at 103 º C.

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2.26 Dry crucibles plus solids for one hour at 103 º C Cool in desiccator to room temperature 2.28 Weigh crucible plus suspended solids.

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2.26. Drying 2.27 Desiccate 2.28 Weigh 2.29 Repeat Change Less Than 4% or 0.5 mg.

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2.31 Ignite in muffle furnace at 550 deg. C for 15 minutes 2.32 Cool in drying oven briefly 2.32 Cool in desiccator to room temperature 2.33 Weigh crucible plus ash Weight 2.3 Volatile Solids

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2.34 Repeat Change Less Than 4% or 0.5 mg. Ignite in muffle furnace at 550 deg. C for 15 minutes Cool in drying oven briefly Cool in desiccator to room temperature Weigh crucible plus ash.

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Suspended Solids Procedure Summary Suspended Solids Procedure Summary

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1. Insert glass fiber filter 2. Seat filter3. Dry briefly 103 deg. C 4. Ignite in muffle furnace 550 deg. C for 15 minutes 5. Cool in drying oven briefly 6. Cool in desiccator to room temperature 7. Weigh crucible TOTAL SUSPENDED AND VOLATILE SUSPENDED SOLIDS PROCEDURE

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8. Pour measured volume of sample in Gooch crucible. 9. Filter with vacuum. 10. Wash graduate, crucible, and filter with distilled water. 11. Dry crucibles plus solids for one hour at 103 º C. 12. Cool in desiccator to room temperature 13. Weigh crucible plus suspended solids. 14. Ignite in muffle furnace at 550 deg. C for 15 minutes 15. Cool in drying oven briefly 16. Cool in desiccator to room temperature 17. Weigh crucible plus ash.

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OTHER FILTER APPARATUS Filter Apparatus Used is Optional As Long As Specified Filters Are Used

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Suspended Solids Suspended SolidsCALCULATIONS

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Suspended Solids (mg/L) Wt. of Solids Sample Volume (grams) (mL) X gram X mL Wt. of Solids (grams) Sample Volume (mL) X 1,000,000 Wt. of Cruc. & Solids - Wt. of Cruc. Volume of Sample (grams) (mL) X 1,000,000 mg1000 1Liter

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Volatile Suspended Solids (mg/L) Wt. of Volatile Sample Volume (grams) (mL) X gram X mL Wt. of Volatile (grams) Sample Volume (mL) X 1,000,000 Wt. of Cruc. & Solids - Wt. of Cruc. & Ash Volume of Sample (grams) (mL) X 1,000,000 mg1000 1Liter

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SUSPENDED SOLIDS EXAMPLE PROBLEM Calculate suspended and volatile suspended solids in mg/L given the following data: Sample Volume= 25 mL Weight of Crucible= grams Weight of Crucible & Dry Solids= grams Weight of Crucible & Ash= grams Suspended Solids, mg/L = Wt. Dry Solids, grams Sample Volume, mL X 1,000,000 = g 25 mL X 1,000,000 = g 25 mL X 1,000,000 = 128 mg/L g

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SUSPENDED SOLIDS EXAMPLE PROBLEM Calculate suspended and volatile suspended solids in mg/L given the following data: Sample Volume= 25 mL Weight of Crucible= grams Weight of Crucible & Dry Solids= grams Weight of Crucible & Ash= grams Volatile Sus. Solids, mg/L = Wt. Volatile Solids, grams Sample Volume, mL X 1,000,000 = g 25 mL X 1,000,000 = g 25 mL X 1,000,000 = 104 mg/L g

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Work Calculations on Separate Paper Answers Given on Next Slides SUSPENDED SOLIDS PRACTICE PROBLEMS Calculate suspended and volatile suspended solids in mg/L given the following data: Weight of Crucible= grams Weight of Crucible & Dry Solids= grams Weight of Crucible & Ash= grams Volume of Sample Filtered= 50 mL

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SUSPENDED SOLIDS PRACTICE PROBLEM Calculate suspended and volatile suspended solids in mg/L given the following data: Weight of Crucible= grams Weight of Crucible & Dry Solids= grams Weight of Crucible & Ash= grams Volume of Sample Filtered= 50 mL Suspended Solids, mg/L = Wt. Dry Solids, grams Sample Volume, mL X 1,000,000 = g g 50 mL X 1,000,000 = g 50 mL X 1,000,000 = 90 mg/L

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Calculate suspended and volatile suspended solids in mg/L given the following data: Weight of Crucible= grams Weight of Crucible & Dry Solids= grams Weight of Crucible & Ash= grams Volume of Sample Filtered= 50 mL Volatile Sus. Solids, mg/L = Wt. Volatile Solids, grams Sample Volume, mL X 1,000,000 = g g 50 mL X 1,000,000 = g 50 mL X 1,000,000 = 76 mg/L SUSPENDED SOLIDS PRACTICE PROBLEM

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SUSPENDED SOLIDS (mg/L) Wt. Of Dry Solids (grams) Volume of Sample (mL) X 1,000,000 Wt. Of Vol. Sus. Solids (grams) Volume of Sample (mL) VOLATILE SUSPENDED SOLIDS (mg/L) X 1,000,000

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Total Solids Dewatered Sludge (Cake) Sludges

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SLUDGE SOLIDS PROCEDURE Evaporating Dish Total Solids – All of the Solids present whether Suspended or Dissolved. Total Solids – The Residue Remaining Upon Evaporation.

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SLUDGE SOLIDS PROCEDURE Evaporating Dish Preparation Ignite 2.11 Cool 2.12 Weigh 2.13

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SLUDGE SOLIDS PROCEDURE Total Solids Analysis Weigh 2.22 Add Sample 2.21 (25 to 50 grams)

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SLUDGE SOLIDS PROCEDURE Total Solids Analysis (cont.) Evaporate 2.23 Cool 2.25 Weigh 2.25 Dry Repeat < 4% or 50 mg

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SLUDGE SOLIDS PROCEDURE Volatile Solids Analysis Ignite (1 Hr.) 2.27 Cool 2.28 Weigh Repeat (30 min.) < 4% or 50 mg

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SLUDGE SOLIDS PROCEDURE Evaporating Dish Preparation Ignite 2.11 Cool 2.12 Weigh 2.13 Weigh 2.23 Add Sample 2.22 Total Solids Analysis Cool 2.26 Weigh Dry 2.25 Evaporate 2.24 Volatile Solids Analysis Ignite 2.27 Cool 2.28 Weigh 2.29

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SLUDGE SOLIDS PROCEDURE Evaporating Dish Preparation Ignite 2.11 Cool 2.12 Weigh 2.13 Weigh 2.23 Break Up Cake 2.31 Total Solids Analysis Cool and Weigh 2.34 Dry 2.33 Repeat (1 hour) Dewatered Sludge (cake)

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Percent Total Solids % = Amount in Question Total Amount Possible X 100% % Total Solids = Wt. Of (Dry) Solids Wt. Of (Wet) Sample X 100% % Total Solids = Dry Wet X 100% % Total Solids = (Dish & Dry) - (Dish) (Dish & Wet) - (Dish) X 100%

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Percent Volatile Solids % = Amount in Question Total Amount Possible X 100% % Volatile Solids = Wt. Of Volatile Solids Wt. Of Dry Solids X 100% % Volatile Solids = Dry - Ash X 100% % Volatile Solids = (Dish & Dry) - (Dish & Ash) (Dish & Dry) - (Dish) X 100% Dry

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Calculate the Percent Total Solids and Percent Volatile Solids of a sludge sample given the following data: Wt. of Dish= grams Wt. of Dish and Wet Sludge= grams Wt. of Dish and Dry Sludge= grams Wt. of Dish and Ash= grams % Total Solids = Wt. of Dry Solids, g Wt. of Wet Sludge, g X 100% = g g g g X 100% = 3.79 g g X 100% = X 100% = 4.0 %

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Calculate the Percent Total Solids and Percent Volatile Solids of a sludge sample given the following data: Wt. of Dish= grams Wt. of Dish and Wet Sludge= grams Wt. of Dish and Dry Sludge= grams Wt. of Dish and Ash= grams % Volatile Solids = Wt. of Volatile Solids, g Wt. of Dry Solids, g X 100% = g g g g X 100% = 1.97 g 3.79 g X 100% = X 100% = 52.0 %

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Work Calculations on Separate Paper Answers Given on Next Slides Total Solids Practice Problem Calculate the Percent Total Solids and Percent Volatile Solids of a sludge sample given the following data: Wt. of Dish= grams Wt. of Dish and Wet Sludge= grams Wt. of Dish and Dry Sludge= grams Wt. of Dish and Ash= grams

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Calculate the Percent Total Solids and Percent Volatile Solids of a sludge sample given the following data: Wt. of Dish= grams Wt. of Dish and Wet Sludge= grams Wt. of Dish and Dry Sludge= grams Wt. of Dish and Ash= grams % Total Solids = Wt. of Dry Solids, g Wt. of Wet Sludge, g X 100% = g g g g X 100% = 2.94 g g X 100% = X 100% = 3.6 % Total Solids Practice Problem

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Calculate the Percent Total Solids and Percent Volatile Solids of a sludge sample given the following data: Wt. of Dish= grams Wt. of Dish and Wet Sludge= grams Wt. of Dish and Dry Sludge= grams Wt. of Dish and Ash= grams % Volatile Solids = Wt. of Volatile Sludge, g Wt. of Dry Solids, g X 100% = g g g g X 100% = 1.50 g 2.94 g = X 100% = 51.0 % Total Solids Practice Problem

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Percent Total Solids % Total Solids = Dry Wet X 100% Percent Volatile Solids % Volatile Solids = Dry - Ash X 100% Dry

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Sludge Solids 6% 94% Water 100 # 6 # 94 # TOTAL SOLIDS 6 # ASH VOLATILE 70 % 30 % 4.2 # 1.8 #

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T O T A L D I S S O L V E D S O L I D S Page 134-1

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TOTAL DISSOLVED SOLIDS TDS Summary of Method Prepare Filter Apparatus and Evaporating Dish Filter Measured Volume of Sample Rinse Filter Apparatus Transfer ALL Filtrate to Evaporating Dish Evaporate to Dryness Dry Residue at 180° C Cool and Weigh Calculate TDS, mg/L

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TOTAL DISSOLVED SOLIDS TDS Calculation: TDS, mg/L = Wt. of Dry Solids, (gram) Volume of Sample, mL X 1,000,000 Wt. of Dry Solids = (Wt. Of Dried Residue & Dish) – (Wt. of Dish ) {See Example, Page 134-4}

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SOLIDS ANALYSIS SOLIDS ANALYSIS Prepared By Michigan Department of Environmental Quality Operator Training and Certification Unit

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