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)
 FILTERING FLASK
2.11Insert glass 2.13 Dry briefly
fiber filter 2.12 Seat filter 103 deg. C

Ignite in muffle furnace

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

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

2.14Cool in desiccator
to room temperature 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.

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

2.14Cool in desiccator
to room temperature 2.15 Weigh crucible
 2.16 Repeat

Ignite Cool Desiccate Weigh

Change Less Than 4% or 0.5 mg.

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
2.24
vacuum.
2.25 Wash graduate,
crucible, and
filter with
distilled water.
Pour sample in
2.24
Gooch crucible.

2.26 Dry crucibles

plus solids
for one hour
at 103 C.
 2.26 Dry crucibles
plus solids
for one hour
at 103 C.

2.27 Cool in desiccator 2.28 Weigh crucible

to room temperature 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 2.32 Cool in drying oven

550 deg. C for 15 minutes briefly

2.32 Cool in desiccator 2.33 Weigh crucible

to room temperature plus ash.
 2.34 Repeat

Ignite in muffle furnace at

550 deg. C for 15 minutes

Cool in drying oven Cool in desiccator Weigh crucible

briefly to room temperature plus ash.

Change Less Than 4% or 0.5 mg.

Suspended
Solids
Procedure
Summary
 TOTAL SUSPENDED
AND
VOLATILE SUSPENDED SOLIDS
PROCEDURE

1. Insert glass 2. Seat filter 3. Dry briefly

fiber filter 4. Ignite in muffle furnace
103 deg. 550 deg. C for 15 minutes
C

5. Cool in drying oven

briefly 6. Cool in desiccator 7. Weigh crucible
to room temperature
 9. Filter 10. Wash graduate,
with crucible, and
vacuum. filter with
distilled water.
8. Pour measured 11. Dry crucibles plus solids
volume of for one hour at 103 C.
sample in
Gooch crucible.

12. Cool in desiccator 13. Weigh crucible plus

to room temperature suspended solids.

14. Ignite in muffle furnace at

550 deg. C for 15 minutes

15. Cool in drying oven 16. Cool in desiccator 17. Weigh crucible
briefly to room temperature 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 1000 mL

X
Sample Volume (mL) 1 gram 1 Liter

Wt. of Solids (grams)

X 1,000,000
Sample Volume (mL)

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

Wt. of Volatile (grams) X 1000 mg 1000 mL

X
Sample Volume (mL) 1 gram 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

Wt. Dry Solids, grams

Suspended Solids, mg/L = X 1,000,000
Sample Volume, mL

= 18.1482 g - 18.1450 g
X 1,000,000
25 mL

0.0032 g
= X 1,000,000
25 mL

= 128 mg/L
 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
X 1,000,000
25 mL

0.0026 g
= X 1,000,000
25 mL

= 104 mg/L
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 = 21.0256 grams

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

Wt. Dry Solids, grams

Suspended Solids, mg/L = X 1,000,000
Sample Volume, mL

= 21.0301 g - 21.0256 g
X 1,000,000
50 mL

0.0045 g
= X 1,000,000
50 mL

= 90 mg/L
 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

Volatile Sus. Solids, mg/L = Wt. Volatile Solids, grams X 1,000,000

Sample Volume, mL

= 21.0301 g - 21.0263 g
X 1,000,000
50 mL

0.0038 g
= X 1,000,000
50 mL

= 76 mg/L
 SUSPENDED SOLIDS (mg/L)

Wt. Of Dry Solids (grams)

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

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

Cool
Ignite 2.12
2.11

Weigh
2.13
 SLUDGE SOLIDS PROCEDURE

Total Solids Analysis

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

Total Solids Analysis (cont.)

Evaporate Dry Cool

2.23 2.24 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

2.30 Repeat (30 min.)

Weigh < 4% or 50 mg
2.29
 SLUDGE SOLIDS PROCEDURE
Evaporating Dish Preparation

Ignite Cool Weigh

2.11 2.12 2.13
Total Solids Analysis

Add
Sample Weigh
2.22 2.23

Evaporate Dry Cool

2.24 2.26 Weigh
2.25
2. 26
Volatile Solids Analysis

Ignite Cool
Weigh
2.27 2.28
2.29
 SLUDGE SOLIDS PROCEDURE
Dewatered Sludge (cake)
Evaporating Dish Preparation

Ignite Cool Weigh

2.11 2.12 2.13

Total Solids Analysis

Break Up
Weigh
Cake
2.23
2.31

Repeat (1 hour)
2.35 -2.37
Dry Cool and Weigh
2.33 2.34
 Percent Total Solids
Amount in Question X 100%
% =
Total Amount Possible

Wt. Of (Dry) Solids

% Total Solids = X 100%
Wt. Of (Wet) Sample

Dry X 100%
% Total Solids = Wet

(Dish & Dry) - (Dish)

% Total Solids = - (Dish) X 100%
(Dish & Wet)
 Percent Volatile Solids
Amount in Question X 100%
% =
Total Amount Possible

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)
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

Wt. of Dry Solids, g X 100%

% Total Solids = 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 = 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

Wt. of Volatile Solids, g

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

108.34 g - 106.37 g
=
108.34 g - 104.55 g X 100%
1.97 g
= X 100%
3.79 g

= 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 = 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

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

Wt. of Dry Solids, g X 100%

% Total Solids = 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 = 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

Wt. of Volatile Sludge, g X 100%

% Volatile Solids = Wt. of Dry Solids, g

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

1.50 g
= X 100%
2.94 g

= 0.510 X 100% = 51.0 %

 Percent Total Solids
Dry
% Total Solids = X 100%
Wet

Percent Volatile Solids

Dry - Ash X 100%
% Volatile Solids = Dry
 Sludge
100 #
4.2 #

94 # 94% Water
70 %
6#
VOLATILE

TOTAL
6# 6%Solids
SOLIDS 1.8 #
30 %
ASH
 A L
O T E D
T L V
S O S
I S I D
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