solids analysis solids analysis prepared by michigan department of environmental quality operator...

SOLIDSANALYSIS

SOLIDSANALYSIS

Prepared ByMichigan Department of Environmental Quality

Operator Training and Certification Unit

SOLIDSANALYSIS

SOLIDSANALYSIS

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 SolidsClassification of SolidsSuspended 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 filtersand will not be lost when heated to dry the filter.



Dissolved SolidsThose solids which are in solution and are therefore filtrable.

Stuff that DOES get through the filters



Suspended Volatile SolidsThat portion of the suspended solids which are volatilized at 550 degrees C

Dissolved SolidsThose solids which are in solution and are therefore filtrable.

Total SolidsAll of the solids present whether suspended or dissolved.

Total Volatile SolidsThat portion of the total solids which are volatilized at 550 degrees C.

TOTAL SUSPENDEDAND

VOLATILE SUSPENDED SOLIDSPROCEDURE

TOTAL SUSPENDEDAND


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, 1997Methods 2540 D (TSS) and 2540 E (VSS)

2.11 Insert glass fiber filter

FILTERING FLASK

2.12 Seat filter2.13 Dry briefly 103 deg. C

2.13 Ignite in muffle furnace 550 deg. C for 15 minutes

2.14 Cool in drying oven briefly



2.14 Cool in desiccator to room temperature

DesiccatorDesiccator

To Prevent Errors in Weighing of Crucibles by Providing a 0% Humidity Atmosphere

While the Crucibles Cool to Room Temperature.

DesiccatorDesiccator

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 Pink – Must Be Replaced or Replaced or RechargedRecharged



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.



2.14 Cool in desiccator to room temperature 2.15 Weigh crucible

Ignite Cool Desiccate Weigh

2.16 Repeat

Change Less Than 4% or 0.5 mg.

2.21 Choose sample volume2.5 to 200 mg

2.22 Thoroughly mix

2.23 Place crucible on vacuum flask, wet filter

2.2 Sample Analysis

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.

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


2.28 Weigh crucible plus suspended solids.

2.26. Drying 2.27 Desiccate 2.28 Weigh

2.29 Repeat


2.31 Ignite in muffle furnace at 550 deg. C for 15 minutes



2.33 Weigh crucible plus ash.

2.28 Weight

2.3 Volatile Solids

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.

SuspendedSolids

ProcedureSummary

SuspendedSolids

ProcedureSummary

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 temperature7. Weigh crucible

TOTAL SUSPENDEDAND


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.

OTHER FILTER APPARATUSOTHER FILTER APPARATUS

Filter Apparatus Used is Optional As Long As

Specified Filters Are Used

SuspendedSolids

SuspendedSolids

CALCULATIONSCALCULATIONS

Suspended Solids (mg/L)

Wt. of SolidsSample 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

mg10001 Liter

10001

Volatile Suspended Solids (mg/L)

Wt. of VolatileSample 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

mg10001 Liter

10001

SUSPENDED SOLIDS EXAMPLE PROBLEM

Calculate suspended and volatile suspended solids in mg/Lgiven the following data:

Sample Volume = 25 mLWeight of Crucible = 18.1450 gramsWeight of Crucible & Dry Solids = 18.1482 gramsWeight of Crucible & Ash = 18.1456 grams

Suspended Solids, mg/L = Wt. Dry Solids, gramsSample Volume, mL

X 1,000,000

= 18.1482 g

25 mLX 1,000,000

= 0.0032 g25 mL

X 1,000,000

= 128 mg/L

- 18.1450 g

SUSPENDED SOLIDS EXAMPLE PROBLEM


Sample Volume = 25 mLWeight of Crucible = 18.1450 gramsWeight of Crucible & Dry Solids = 18.1482 gramsWeight of Crucible & Ash = 18.1456 grams

Volatile Sus. Solids, mg/L = Wt. Volatile Solids, gramsSample Volume, mL

X 1,000,000

= 18.1482 g

25 mLX 1,000,000

= 0.0026 g25 mL

X 1,000,000

= 104 mg/L

- 18.1456 g

Work Calculations on Separate PaperAnswers Given on Next Slides

SUSPENDED SOLIDS PRACTICE PROBLEMS


Weight of Crucible = 21.0256 gramsWeight of Crucible & Dry Solids = 21.0301 gramsWeight of Crucible & Ash = 21.0263

gramsVolume of Sample Filtered = 50 mL

SUSPENDED SOLIDS PRACTICE PROBLEM


Weight of Crucible = 21.0256 gramsWeight of Crucible & Dry Solids = 21.0301 gramsWeight of Crucible & Ash = 21.0263 gramsVolume of Sample Filtered = 50 mL

Suspended Solids, mg/L = Wt. Dry Solids, gramsSample Volume, mL

X 1,000,000

= 21.0301 g - 21.0256 g

50 mLX 1,000,000

= 0.0045 g50 mL

X 1,000,000

= 90 mg/L


Weight of Crucible = 21.0256 gramsWeight of Crucible & Dry Solids = 21.0301 gramsWeight of Crucible & Ash = 21.0263 gramsVolume of Sample Filtered = 50 mL

Volatile Sus. Solids, mg/L = Wt. Volatile Solids, gramsSample Volume, mL

X 1,000,000

= 21.0301 g - 21.0263 g

50 mLX 1,000,000

= 0.0038 g50 mL

X 1,000,000

= 76 mg/L

SUSPENDED SOLIDS PRACTICE PROBLEM

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

Total Solids

Dewatered Sludge (Cake)Dewatered Sludge (Cake)

SludgesSludges

SLUDGE SOLIDS PROCEDURESLUDGE SOLIDS PROCEDURE

Evaporating Dish

Total Solids – All of the Solids present whether Suspended or Dissolved.

Total Solids – The Residue Remaining Upon Evaporation.

SLUDGE SOLIDS PROCEDURE

Evaporating Dish Preparation

Ignite2.11

Cool2.12

Weigh2.13


Total Solids Analysis

Weigh2.22

AddSample

2.21

(25 to 50 grams)


Total Solids Analysis (cont.)

Evaporate2.23

Cool2.25

Weigh2.25

Dry2.24

2.26 Repeat< 4% or 50 mg


Volatile Solids Analysis

Ignite (1 Hr.)2.27

Cool2.28

Weigh2.29

2.30 Repeat (30 min.)< 4% or 50 mg

SLUDGE SOLIDS PROCEDUREEvaporating Dish Preparation

Ignite2.11

Cool2.12

Weigh2.13

Weigh2.23

AddSample

2.22


Cool2.26 Weigh

2. 26

Dry2.25

Evaporate2.24

Volatile Solids Analysis

Ignite2.27

Cool2.28

Weigh2.29


Evaporating Dish Preparation

Ignite2.11

Cool2.12

Weigh2.13

Weigh2.23

Break UpCake2.31


Cool and Weigh2.34

Dry2.33

Repeat (1 hour)2.35 -2.37

Dewatered Sludge (cake)Dewatered Sludge (cake)

Percent Total SolidsPercent Total Solids

% = Amount in Question Total Amount Possible

X 100%

% Total Solids =Wt. Of (Dry) Solids

Wt. Of (Wet) SampleX 100%

% Total Solids = Dry Wet

X 100%

% Total Solids =(Dish & Dry) - (Dish)(Dish & Wet) - (Dish) X 100%

Percent Volatile SolidsPercent Volatile Solids

% = Amount in Question Total Amount Possible

X 100%

% Volatile Solids =Wt. Of Volatile Solids

Wt. Of Dry SolidsX 100%

% Volatile Solids = Dry - Ash X 100%

% Volatile Solids =(Dish & Dry) - (Dish & Ash)

(Dish & Dry) - (Dish) X 100%

Dry

Calculate the Percent Total Solids and PercentVolatile Solids of a sludge sample given thefollowing data:

Wt. of Dish = 104.55 gramsWt. of Dish and Wet Sludge = 199.95 gramsWt. of Dish and Dry Sludge = 108.34 gramsWt. of Dish and Ash = 106.37 grams

% Total Solids = Wt. of Dry Solids, gWt. of Wet Sludge, g X 100%

= 108.34 g - 104.55 g199.95 g - 104.55 g X 100%

=3.79 g95.40 g X 100%

= 0.040 X 100%

= 4.0 %



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

= 108.34 g - 106.37 g108.34 g - 104.55 g X 100%

=1.97 g3.79 g X 100%

= 0.520 X 100%

= 52.0 %

Work Calculations on Separate PaperAnswers Given on Next Slides

Total Solids Practice Problem





% Total Solids = Wt. of Dry Solids, gWt. of Wet Sludge, g X 100%

= 109.46 g - 106.52 g187.16 g - 106.52 g X 100%

=2.94 g80.64 g X 100%

= 0.036 X 100% = 3.6 %




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

= 109.46 g - 107.96 g109.46 g - 106.52 g X 100%

=1.50 g2.94 g X 100%

= 0.510 X 100% = 51.0 %


Percent Total SolidsPercent Total Solids

% Total Solids = Dry Wet

X 100%

Percent Volatile SolidsPercent Volatile Solids

% Volatile Solids = Dry - Ash X 100%

Dry

Sludge

Solids6%

94%Water

100 #

6 #

94 #

TOTALSOLIDS

6 #

ASH

VOLATILE70 %

30 %

4.2 #

1.8 #

TOTALTOTAL

DISSOLVED

DISSOLVED

SOLIDS

SOLIDS

Page 134-1Page 134-1

TOTAL DISSOLVED SOLIDSTOTAL DISSOLVED SOLIDSTDSTDS

Summary of Method

Prepare Filter Apparatus and Evaporating DishFilter Measured Volume of SampleRinse Filter ApparatusTransfer ALL Filtrate to Evaporating DishEvaporate to DrynessDry Residue at 180° CCool and WeighCalculate TDS, mg/L

TOTAL DISSOLVED SOLIDSTOTAL DISSOLVED SOLIDSTDSTDS

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}

SOLIDSANALYSIS

SOLIDSANALYSIS

Prepared ByMichigan Department of Environmental Quality

Operator Training and Certification Unit

solids analysis solids analysis prepared by michigan department of environmental quality operator...

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