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**SOLIDS ANALYSIS Prepared By**

Michigan Department of Environmental Quality Operator Training and Certification Unit

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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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**VOLATILE SUSPENDED SOLIDS Methods 2540 D (TSS) and 2540 E (VSS)**

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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**fiber filter 103 deg. C 550 deg. C for 15 minutes briefly**

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

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**550 deg. C for 15 minutes briefly to room temperature**

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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**While the Crucibles Cool to Room Temperature.**

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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**550 deg. C for 15 minutes briefly to room temperature**

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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**550 deg. C for 15 minutes briefly to room temperature**

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

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

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**vacuum. crucible, and filter with distilled water. Gooch crucible.**

2.25 Wash graduate, crucible, and filter with distilled water. 2.24 Pour sample in Gooch crucible. 2.26 Dry crucibles plus solids for one hour at 103 º C.

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**plus solids for one hour at 103 º C. 2.28 Weigh crucible**

2.26 Dry crucibles plus solids for one hour at 103 º C. 2.27 Cool in desiccator to room temperature 2.28 Weigh crucible plus suspended solids.

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

2.28 Weigh Change Less Than 4% or 0.5 mg.

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**2.3 Volatile Solids 550 deg. C for 15 minutes briefly**

2.28 Weight 2.3 Volatile Solids 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.

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**Change Less Than 4% or 0.5 mg. 2.34 Repeat 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. Change Less Than 4% or 0.5 mg.

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Suspended Solids Procedure Summary

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**VOLATILE SUSPENDED SOLIDS**

TOTAL SUSPENDED AND VOLATILE SUSPENDED SOLIDS PROCEDURE 1. Insert glass fiber filter 2. Seat filter 3. 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

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10. Wash graduate, crucible, and filter with distilled water. 9. Filter with vacuum. 8. Pour measured volume of sample in Gooch crucible. 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 16. Cool in desiccator to room temperature 17. Weigh crucible plus ash. 15. Cool in drying oven briefly

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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 CALCULATIONS

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**Suspended Solids (mg/L)**

Wt. of Solids (grams) 1000 mg 1000 mL X X Sample Volume (mL) 1 gram 1 Liter Wt. of Solids (grams) X 1,000,000 Sample Volume (mL) - Wt. of Cruc. Wt. of Cruc. & Solids (grams) X 1,000,000 Volume of Sample (mL)

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**Volatile Suspended Solids (mg/L)**

Wt. of Volatile (grams) 1000 mg 1000 mL X X Sample Volume (mL) 1 gram 1 Liter Wt. of Volatile (grams) X 1,000,000 Sample Volume (mL) - Wt. of Cruc. & Ash Wt. of Cruc. & Solids (grams) X 1,000,000 Volume of Sample (mL)

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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 Wt. Dry Solids, grams Suspended Solids, mg/L = X 1,000,000 Sample Volume, mL = g g X 1,000,000 25 mL g = X 1,000,000 25 mL = mg/L

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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 Wt. Volatile Solids, grams Volatile Sus. Solids, mg/L = X 1,000,000 Sample Volume, mL = g g X 1,000,000 25 mL g = X 1,000,000 25 mL = mg/L

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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 Work Calculations on Separate Paper Answers Given on Next Slides

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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 Wt. Dry Solids, grams Suspended Solids, mg/L = X 1,000,000 Sample Volume, mL g g = X 1,000,000 50 mL g = X 1,000,000 50 mL = 90 mg/L

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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 Wt. Volatile Solids, grams Volatile Sus. Solids, mg/L = X 1,000,000 Sample Volume, mL g g = X 1,000,000 50 mL g = X 1,000,000 50 mL = 76 mg/L

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**SUSPENDED SOLIDS (mg/L) VOLATILE SUSPENDED SOLIDS (mg/L)**

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

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**Dewatered Sludge (Cake)**

Total Solids Sludges Dewatered Sludge (Cake)

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**SLUDGE SOLIDS PROCEDURE**

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

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**SLUDGE SOLIDS PROCEDURE**

Evaporating Dish Preparation Cool 2.12 Ignite 2.11 Weigh 2.13

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**SLUDGE SOLIDS PROCEDURE**

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

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**SLUDGE SOLIDS PROCEDURE**

Total Solids Analysis (cont.) Evaporate 2.23 Dry 2.24 Cool 2.25 2.26 Repeat < 4% or 50 mg Weigh 2.25

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**SLUDGE SOLIDS PROCEDURE**

Volatile Solids Analysis Cool 2.28 Ignite (1 Hr.) 2.27 2.30 Repeat (30 min.) < 4% or 50 mg Weigh 2.29

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**SLUDGE SOLIDS PROCEDURE**

Evaporating Dish Preparation Ignite 2.11 Cool 2.12 Weigh 2.13 Total Solids Analysis Add Sample 2.22 Weigh 2.23 Evaporate 2.24 Dry 2.25 Cool 2.26 Weigh 2. 26 Volatile Solids Analysis Cool 2.28 Ignite 2.27 Weigh 2.29

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**SLUDGE SOLIDS PROCEDURE Dewatered Sludge (cake)**

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

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**Percent Total Solids - - Amount in Question Total Amount Possible % =**

% = X 100% Wt. Of (Dry) Solids % Total Solids = X 100% Wt. Of (Wet) Sample Dry Wet X 100% % Total Solids = - (Dish & Dry) (Dish) % Total Solids = - X 100% (Dish & Wet) (Dish)

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**Percent Volatile Solids**

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

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**= 4.0 % Wt. of Dry Solids, g % Total Solids = X 100%**

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 Wt. of Dry Solids, g % Total Solids = X 100% Wt. of Wet Sludge, g g g = X 100% g g 3.79 g = X 100% 95.40 g = X 100% = 4.0 %

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**= 52.0 % Wt. of Volatile Solids, g % Volatile Solids = X 100%**

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 Wt. of Volatile Solids, g % Volatile Solids = X 100% Wt. of Dry Solids, g g g = X 100% g g 1.97 g = X 100% 3.79 g = X 100% = %

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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 Work Calculations on Separate Paper Answers Given on Next Slides

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**= 3.6 % Total Solids Practice Problem Wt. of Dry Solids, g**

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 Wt. of Dry Solids, g % Total Solids = X 100% Wt. of Wet Sludge, g g g = X 100% g g 2.94 g = X 100% 80.64 g = X 100% = 3.6 %

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**= 51.0 % Total Solids Practice Problem Wt. of Volatile Sludge, g**

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 Wt. of Volatile Sludge, g % Volatile Solids = X 100% Wt. of Dry Solids, g g g = X 100% g g 1.50 g = X 100% 2.94 g = % = X 100%

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**Percent Volatile Solids**

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

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**100 # 4.2 # 94 # 6 # 6 # 1.8 # Sludge 70 % 30 % ASH 94% Water TOTAL 6%**

VOLATILE TOTAL SOLIDS 6 # 6% Solids 1.8 # 30 % ASH

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**TOTAL DISSOLVED SOLIDS**

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

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**SOLIDS ANALYSIS Prepared By**

Michigan Department of Environmental Quality Operator Training and Certification Unit

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