SOLIDS ANALYSIS Prepared By Michigan Department of Environmental Quality

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 Unit’s
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 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)
2.11 Insert glass
fiber filter
FILTERING FLASK
2.12 Seat filter
2.13 Ignite in muffle furnace
550 deg. C for 15 minutes
2.13 Dry briefly
103 deg. C
2.14 Cool in drying oven
briefly
2.13 Ignite in muffle furnace
550 deg. C for 15 minutes
2.14 Cool in desiccator
to room temperature
2.14 Cool in drying oven
briefly
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
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
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
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
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
2.24 Filter with
vacuum.
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.
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.
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 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.
OTHER FILTER APPARATUS
Filter Apparatus Used is
Optional As Long As
Specified Filters Are Used
Suspended
Solids
CALCULATIONS
Suspended Solids (mg/L)
1000 mg
Wt. of Solids (grams)
X
(mL)
1 gram
Sample Volume
1000 mL
X
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)
1000 mg
Wt. of Volatile (grams)
X
(mL)
1 gram
Sample Volume
1000 mL
X
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
X 1,000,000
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
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 grams
21.0301 grams
21.0263 grams
50 mL
Wt. Dry Solids, grams
X 1,000,000
Sample Volume, mL
21.0301 g - 21.0256 g
=
50 mL
=
0.0045 g
50 mL
= 90 mg/L
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
Weigh
2. 26
Volatile Solids Analysis
Ignite
2.27
Cool
2.28
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
Dry
% Total Solids =
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
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