SOLIDS

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

SOLIDS
ANALYSIS
NOTE: Page Numbers and Procedure Step Numbers
Relate to the Operator Training and Certification Units
Laboratory Training Manual Available on the OTCU
Website at www.michigan.gov/deqoperatortraining

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.

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

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.

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 550C.
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)

Insert glass
fiber filter

2.11

FILTERING FLASK

2.12

Seat filter

Ignite in muffle furnace

550 deg. C for 15 minutes

2.13

2.13

Dry briefly
103 deg. C

Cool in drying oven

briefly

2.14

Ignite in muffle furnace

550 deg. C for 15 minutes

2.13

Cool in desiccator
to room temperature

2.14

Cool in drying oven

briefly

2.14

Desiccator
To Prevent Errors in Weighing of Crucibles by
Providing a 0% Humidity Atmosphere
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.
(Indicating Desiccant is Required)

Blue - Good

Pink Must Be
Replaced or
Recharged

Ignite in muffle furnace

550 deg. C for 15 minutes

2.13

Cool in desiccator
to room temperature

Cool in drying oven

briefly

2.14

2.14

2.15

Weigh crucible

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.

Ignite in muffle furnace

550 deg. C for 15 minutes

2.13

Cool in desiccator
to room temperature

Cool in drying oven

briefly

2.14

2.14

2.15

Weigh crucible

2.16 Repeat

Ignite

Cool

Desiccate

Change Less Than 4% or 0.5 mg.

Weigh

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

Filter with
vacuum.

2.24

2.25

Pour sample in
Gooch crucible.

Wash graduate,
crucible, and
filter with
distilled water.

2.24

2.26

Dry crucibles
plus solids
for one hour
at 103 C.

2.26

2.27

Cool in desiccator
to room temperature

Dry crucibles
plus solids
for one hour
at 103 C.

2.28 Weigh crucible

plus suspended
solids.

2.29 Repeat

2.26. Drying

2.27 Desiccate

2.28 Weigh

Change Less Than 4% or 0.5 mg.

2.28 Weight

2.3 Volatile Solids

2.31

Ignite in muffle furnace at

550 deg. C for 15 minutes

2.32

Cool in desiccator
to room temperature

2.32

Cool in drying oven

briefly

2.33

Weigh crucible
plus ash.

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.

Suspended
Solids
Procedure
Summary

TOTAL SUSPENDED
AND
VOLATILE SUSPENDED SOLIDS
PROCEDURE

1. Insert glass
fiber filter

2. Seat filter

5. Cool in drying oven

briefly

3. Dry briefly
103 deg.
C

6. Cool in desiccator
to room temperature

4. Ignite in muffle furnace

550 deg. C for 15 minutes

7. Weigh crucible

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 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.

OTHER FILTER APPARATUS

Filter Apparatus Used is

Optional As Long As
Specified Filters Are Used

Suspended
Solids

CALCULATIONS

Suspended Solids (mg/L)

Wt. of Solids (grams) X 1000 mg
1 gram
Sample Volume (mL)

1000 mL
1 Liter

Wt. of Solids (grams)

X 1,000,000
Sample Volume (mL)

Wt. of Cruc. & Solids Wt. of Cruc. (grams)

Volume of Sample (mL)

X 1,000,000

Volatile Suspended Solids (mg/L)

Wt. of Volatile (grams) X 1000 mg
1 gram
Sample Volume (mL)

1000 mL
1 Liter

Wt. of Volatile (grams)

X 1,000,000
Sample Volume (mL)

Wt. of Cruc. & Solids Wt. of Cruc. & Ash (grams)

X 1,000,000
Volume of Sample (mL)

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
18.1482 g - 18.1450 g

25 mL

0.0032 g
25 mL

= 128 mg/L

X 1,000,000

X 1,000,000

X 1,000,000

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 X 1,000,000

Sample Volume, mL

18.1482 g - 18.1456 g

25 mL

0.0026 g
25 mL

= 104 mg/L

X 1,000,000

X 1,000,000

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

Work Calculations on Separate Paper

Answers Given on Next Slides

SUSPENDED SOLIDS PRACTICE PROBLEM

Calculate suspended and volatile suspended solids in mg/L
given the following data:
Weight of Crucible
Weight of Crucible & Dry Solids
Weight of Crucible & Ash
Volume of Sample Filtered

Suspended Solids, mg/L

- 21.0256 g

50 mL

21.0256 grams
21.0301 grams
21.0263 grams
50 mL

Wt. Dry Solids, grams

Sample Volume, mL
21.0301 g

=
=
=
=

0.0045 g
50 mL

= 90 mg/L

X 1,000,000

X 1,000,000

X 1,000,000

SUSPENDED SOLIDS PRACTICE PROBLEM

Calculate suspended and volatile suspended solids in mg/L
given the following data:
Weight of Crucible
Weight of Crucible & Dry Solids
Weight of Crucible & Ash
Volume of Sample Filtered

Volatile Sus. Solids, mg/L

=
=
=
=

21.0256 grams
21.0301 grams
21.0263 grams
50 mL

= Wt. Volatile Solids, grams X 1,000,000

Sample Volume, mL

21.0301 g

- 21.0263 g

50 mL

0.0038 g
50 mL

= 76 mg/L

X 1,000,000

X 1,000,000

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)

Total Solids
Sludges
Dewatered Sludge (Cake)

SLUDGE SOLIDS PROCEDURE

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

SLUDGE SOLIDS PROCEDURE

Evaporating Dish Preparation

Ignite
2.11

Cool
2.12

Weigh
2.13

SLUDGE SOLIDS PROCEDURE

Total Solids Analysis

Add
Sample
2.21
(25 to 50 grams)

Weigh
2.22

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

SLUDGE SOLIDS PROCEDURE

Volatile Solids Analysis

Cool
2.28

Ignite (1 Hr.)
2.27

Weigh
2.29

2.30 Repeat (30 min.)

< 4% or 50 mg

SLUDGE SOLIDS PROCEDURE

Evaporating Dish Preparation

Cool
2.12

Ignite
2.11

Weigh
2.13

Total Solids Analysis

Add
Sample
2.22

Evaporate
2.24

Weigh
2.23

Cool
2.26

Dry
2.25

Volatile Solids Analysis

Ignite
2.27

Cool
2.28

Weigh
2. 26

Weigh
2.29

SLUDGE SOLIDS PROCEDURE

Dewatered Sludge (cake)
Evaporating Dish Preparation

Cool
2.12

Ignite
2.11

Weigh
2.13

Total Solids Analysis

Break Up
Cake
2.31

Weigh
2.23

Repeat (1 hour)
2.35 -2.37
Dry
2.33

Cool and Weigh

2.34

Percent Total Solids

% =

Amount in Question X 100%

Total Amount Possible

% Total Solids =

Wt. Of (Dry) Solids

X 100%
Wt. Of (Wet) Sample

% Total Solids =

% Total Solids =

Dry X 100%
Wet

(Dish & Dry)

(Dish & Wet)

- (Dish)
- (Dish)

X 100%

Percent Volatile Solids

% =

Amount in Question X 100%

Total Amount Possible

% Volatile Solids =

Wt. Of Volatile Solids

X 100%
Wt. Of Dry Solids

Dry - Ash
% Volatile Solids =
Dry

X 100%

(Dish & Dry) - (Dish & Ash)

% Volatile Solids =
X 100%
(Dish & Dry) - (Dish)

Calculate the Percent Total Solids and Percent

Volatile Solids of a sludge sample given the
following data:
Wt. of Dish
Wt. of Dish and Wet Sludge
Wt. of Dish and Dry Sludge
Wt. of Dish and Ash

% Total Solids =

= 104.55 grams
= 199.95 grams
= 108.34 grams
= 106.37 grams

Wt. of Dry Solids, g X 100%

Wt. of Wet Sludge, g
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 %

Calculate the Percent Total Solids and Percent

Volatile Solids of a sludge sample given the
following data:
Wt. of Dish
Wt. of Dish and Wet Sludge
Wt. of Dish and Dry Sludge
Wt. of Dish and Ash

% Volatile Solids =

= 104.55 grams
= 199.95 grams
= 108.34 grams
= 106.37 grams

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 %

Total Solids Practice Problem

Calculate the Percent Total Solids and Percent

Volatile Solids of a sludge sample given the
following data:
Wt. of Dish
Wt. of Dish and Wet Sludge
Wt. of Dish and Dry Sludge
Wt. of Dish and Ash

= 106.52 grams
= 187.16 grams
= 109.46 grams
= 107.96 grams

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
Wt. of Dish and Wet Sludge
Wt. of Dish and Dry Sludge
Wt. of Dish and Ash

% Total Solids =
=

= 106.52 grams
= 187.16 grams
= 109.46 grams
= 107.96 grams

Wt. of Dry Solids, g X 100%

Wt. of Wet Sludge, g

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

Calculate the Percent Total Solids and Percent
Volatile Solids of a sludge sample given the
following data:
Wt. of Dish
Wt. of Dish and Wet Sludge
Wt. of Dish and Dry Sludge
Wt. of Dish and Ash

% Volatile Solids =
=

= 106.52 grams
= 187.16 grams
= 109.46 grams
= 107.96 grams

Wt. of Volatile Sludge, g X 100%

Wt. of Dry Solids, g

109.46 g - 107.96 g
109.46 g - 106.52 g X 100%
=

1.50 g
2.94 g

= 0.510 X 100%

X 100%

= 51.0 %

Percent Total Solids

% Total Solids =

Dry
X 100%
Wet

Percent Volatile Solids

% Volatile Solids =

Dry - Ash X 100%

Dry

Sludge

100 #

4.2 #
94 #

6#

94% Water

6%Solids

6#

TOTAL
SOLIDS

70 %
VOLATILE

1.8 #
30 %
ASH

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

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

TOTAL DISSOLVED SOLIDS

TDS
Calculation:
Wt. of Dry Solids = (Wt. Of Dried Residue & Dish) (Wt. of Dish )

Wt. of Dry Solids, (gram) X 1,000,000

TDS, mg/L = Volume of Sample, mL

{See Example, Page 134-4}

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