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

2. 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

3. 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.

4. 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

5. 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.

6. 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)

7. 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

8. 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

9. 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.

10. 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

11. 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

12. 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.

13. 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

14. 2.16 Repeat
Ignite
Cool
Desiccate
Weigh
Change Less Than 4% or 0.5 mg.

15. 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

16. 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.

17. 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.

18. 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.

19. 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.

20. 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.

21. Suspended
Solids
Procedure
Summary

22. 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

23. 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

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

25. Suspended
Solids
CALCULATIONS

26. 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)

27. 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)

28. 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

29. 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

30. 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

31. 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

32. 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

33. 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)

34. Dewatered Sludge (Cake)
Total Solids
Sludges
Dewatered Sludge (Cake)

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

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

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

38. 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

39. 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

40. 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

41. 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

42. 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)

43. 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)

44. = 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 %

45. = 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%
= %

46. 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

47. = 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 %

48. = 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%

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

50. 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

51. TOTAL DISSOLVED SOLIDS
Page 134-1

52. 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

53. 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}

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