tp

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 www.michigan.gov/deqoperatortraining

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. 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. 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

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

15. 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

16. 2.24 Pour sample in
Gooch crucible.
2.24 Filter with
vacuum.
2.25 Wash graduate,
crucible, and
filter with
distilled water.
2.26 Dry crucibles
plus solids
for one hour
at 103 º C.

17. 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. 2.26. Drying 2.27 Desiccate 2.28 Weigh
2.29 Repeat
Change Less Than 4% or 0.5 mg.

19. 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.
2.28 Weight
2.3 Volatile Solids

20. 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.

21. Suspended
Solids
Procedure
Summary

22. 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
TOTAL SUSPENDED
AND
VOLATILE SUSPENDED SOLIDS
PROCEDURE

23. 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.

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
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
mg
1000
1 Liter
1000
1

27. 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
mg
1000
1 Liter
1000
1

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 = 18.1450 grams
Weight of Crucible & Dry Solids = 18.1482 grams
Weight of Crucible & Ash= 18.1456 grams
Suspended Solids, mg/L = Wt. Dry Solids, grams
Sample Volume, mL
X 1,000,000
= 18.1482 g
25 mL
X 1,000,000
=
0.0032 g
25 mL
X 1,000,000
= 128 mg/L
- 18.1450 g

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 = 18.1450 grams
Weight of Crucible & Dry Solids = 18.1482 grams
Weight of Crucible & Ash= 18.1456 grams
Volatile Sus. Solids, mg/L = Wt. Volatile Solids, grams
Sample Volume, mL
X 1,000,000
= 18.1482 g
25 mL
X 1,000,000
=
0.0026 g
25 mL
X 1,000,000
= 104 mg/L
- 18.1456 g

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 = 21.0256 grams
Weight of Crucible & Dry Solids = 21.0301 grams
Weight of Crucible & Ash = 21.0263 grams
Volume of Sample Filtered = 50 mL

31. SUSPENDED SOLIDS PRACTICE PROBLEM
Calculate suspended and volatile suspended solids in mg/L
given the following data:
Weight of Crucible = 21.0256 grams
Weight of Crucible & Dry Solids = 21.0301 grams
Weight of Crucible & Ash = 21.0263 grams
Volume of Sample Filtered = 50 mL
Suspended Solids, mg/L = Wt. Dry Solids, grams
Sample Volume, mL
X 1,000,000
= 21.0301 g - 21.0256 g
50 mL
X 1,000,000
=
0.0045 g
50 mL
X 1,000,000
= 90 mg/L

32. Calculate suspended and volatile suspended solids in mg/L
given the following data:
Weight of Crucible = 21.0256 grams
Weight of Crucible & Dry Solids = 21.0301 grams
Weight of Crucible & Ash = 21.0263 grams
Volume of Sample Filtered = 50 mL
Volatile Sus. Solids, mg/L = Wt. Volatile Solids, grams
Sample Volume, mL
X 1,000,000
= 21.0301 g - 21.0263 g
50 mL
X 1,000,000
=
0.0038 g
50 mL
X 1,000,000
= 76 mg/L
SUSPENDED SOLIDS PRACTICE PROBLEM

33. 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

34. Total Solids
Dewatered Sludge (Cake)
Sludges

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

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

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

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

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

40. 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
2. 26
Dry
2.25
Evaporate
2.24
Volatile Solids Analysis
Ignite
2.27
Cool
2.28
Weigh
2.29

41. 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)
2.35 -2.37
Dewatered Sludge (cake)

42. 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%

43. 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

44. Calculate the Percent Total Solids and Percent
Volatile Solids of a sludge sample given the
following data:
Wt. of Dish = 104.55 grams
Wt. of Dish and Wet Sludge = 199.95 grams
Wt. of Dish and Dry Sludge = 108.34 grams
Wt. of Dish and Ash = 106.37 grams
% Total Solids =
Wt. of Dry Solids, g
Wt. of Wet Sludge, g
X 100%
=
108.34 g - 104.55 g
199.95 g - 104.55 g
X 100%
=
3.79 g
95.40 g X 100%
= 0.040 X 100%
= 4.0 %

45. Calculate the Percent Total Solids and Percent
Volatile Solids of a sludge sample given the
following data:
Wt. of Dish = 104.55 grams
Wt. of Dish and Wet Sludge = 199.95 grams
Wt. of Dish and Dry Sludge = 108.34 grams
Wt. of Dish and Ash = 106.37 grams
% Volatile Solids =
Wt. of Volatile Solids, g
Wt. of Dry Solids, g
X 100%
=
108.34 g - 106.37 g
108.34 g - 104.55 g
X 100%
=
1.97 g
3.79 g X 100%
= 0.520 X 100%
= 52.0 %

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 = 106.52 grams
Wt. of Dish and Wet Sludge = 187.16 grams
Wt. of Dish and Dry Sludge = 109.46 grams
Wt. of Dish and Ash = 107.96 grams

47. Calculate the Percent Total Solids and Percent
Volatile Solids of a sludge sample given the
following data:
Wt. of Dish = 106.52 grams
Wt. of Dish and Wet Sludge = 187.16 grams
Wt. of Dish and Dry Sludge = 109.46 grams
Wt. of Dish and Ash = 107.96 grams
% Total Solids = Wt. of Dry Solids, g
Wt. of Wet Sludge, g
X 100%
=
109.46 g - 106.52 g
187.16 g - 106.52 g
X 100%
=
2.94 g
80.64 g
X 100%
= 0.036 X 100% = 3.6 %
Total Solids Practice Problem

48. Calculate the Percent Total Solids and Percent
Volatile Solids of a sludge sample given the
following data:
Wt. of Dish = 106.52 grams
Wt. of Dish and Wet Sludge = 187.16 grams
Wt. of Dish and Dry Sludge = 109.46 grams
Wt. of Dish and Ash = 107.96 grams
% Volatile Solids =
Wt. of Volatile Sludge, g
Wt. of Dry Solids, g X 100%
=
109.46 g - 107.96 g
109.46 g - 106.52 g
X 100%
=
1.50 g
2.94 g X 100%
= 0.510 X 100% = 51.0 %
Total Solids Practice Problem

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

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

51. 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:
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}

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