SOLIDS

TITLE
Determination of the Solids in water

INTRODUCTION Water and waste water consists of pure water along with various dissolved, colloidal and suspended contaminants. The suspended contaminants in turn may be settle able or non settle able. These may be either organic or inorganic in nature. Strictly speaking, all matter except the water contained in liquid materials is classified as solid matter

DEFINITION The usual definition of solids however refers to the matter that remains as residue upon evaporation and drying at 103- 1050C

EXPLANATION All materials that exert significant vapor pressure at such temperatures are, of course, lost during the evaporation and drying procedures. The residue or solids remaining represent only those materials present in a sample that have a negligible vapor pressure at 105 0C. In the same way that a solid holds its shape, the atoms inside of a solid are not allowed to move around too much. This is one of the physical characteristics of solids. Atoms and molecules in liquids and gases are bouncing and floating around, free to move where they want. The molecules in a solid are stuck. The atoms still spin and the electrons fly around, but the entire atom will not change position. Solids can be made up of many things. They can have pure elements or a variety of compounds inside. When you get more than one type of compound in a solid it is called a mixture. Most rocks are mixtures of many different compounds. Concrete is a good example of a manmade mixture.

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CLASSIFICATION OF SOLIDS

1. DETERMINATION OF TOTAL SOLIDS (TS)

Definition It refers to the material residue left in a dish or vessel after evaporation of a sample and its subsequent drying in an oven at a defined temperature. Total solids include total suspended solids and total dissolved solids. Purpose During TSS determination if the suspended material clogs the filter and prolongs filtration we can estimate the TSS by calculating the difference between the total solids and total dissolved solids. For this purpose total solids are measured. In addition to this, this method can be applied for the determination of moisture content and total solid material in a wastewater, sludge or any other sample. Scope This procedure is applicable to waters of wide range of quality including surface water, industrial and domestic effluents, treated wastewaters etc. In addition to these samples, this method can also be applied for the analysis of moisture content in sludges, soil etc.

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Interferences Sampling, sub-sampling, and pipeting two-phase samples may introduce serious errors. Homogenization of sample before sampling and use of wide-mouth pipette eliminates the error; Exclude large floating particles or submerged agglomerates of non-homogeneous materials from the sample if it is determined that their inclusion is not representative; Highly mineralized waters containing hygroscopic constituents may interfere. Prolonged drying and rapid weighing may reduce this error; Excessive solids may form water-trapping crust, which can be avoided by limiting the sample to produce 0.2 g residue; To aid in the quality assurance, analyze samples in duplicate.

Sampling and Storage Obtain an appropriate quantity of sample in a glass or plastic bottle; If suspended matter adheres to the container walls prefer glass container; Analyze sample as soon as possible. If preservation required, store it at 40C to avoid biological degradation; Preferably analyze with 24 hours and in no case after 7 days. Bring sample to room temperature before analysis.

Apparatus Muffle furnace for operating at 550 0C; Desiccator provided with a desiccant containing a color indicator of moisture concentration; Drying oven, for operation at 180 0C; Analytical balance capable of weighing 0.1 mg; Magnetic stirrer
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Wide-mouth pipettes; Evaporating dishes of 100 mL capacity; Graduated cylinder Low-form beaker

Procedure If volatile solids are to be measured, ignite cleaned evaporating dish at 550 0C for 1 hour in a muffle furnace; If only total dissolved solids are to be measured, heat clean dish to 1800C for 1 hour in an oven; Store and cool the in desiccator until needed. Weigh immediately before use. Choose sample volume to yield between 2.5 and 200 mg dried residue. Pipette a measured volume of well-mixed sample to a pre-weighed evaporating dish; Evaporate to dryness in the drying oven. If necessary add successive sample portions to the same dish after evaporation; Dry evaporated sample for at least 1 hour in an oven at 103 to 105 0C; Cool in a desiccator to balance temperature, and weigh; Repeat drying cycle of drying, cooling, desiccating, and weighing until a constant weight is obtained or until weight loss is less than 4% of previous weight or 0.5 mg, whichever is less; When weighing dried sample, be alert to change in weight due to air exposure and/or sample degradation.

Calculation TS, mg/L = Where: A= weight of dried residue + dish, g

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(A B) X 1000 Sample volume, mL

B=

weight of dish, g

2. DETERMINATION OF TOTAL SUSPENDED SOLIDS (TSS)

Definition It refers to the solid material in water or wastewater sample, which is retained by a filter of 2.0 m (or smaller) nominal size under specified conditions.

Purpose TSS is an important parameter in wastewater treatment. The data obtained from this test is used in the design of wastewater treatment plants. In addition to this, TSS is a parameter mentioned in NEQS, which is to be reported by industries under SMART.

Scope This pr0Cedure is applicable to waters of wide range of quality including surface water, industrial and domestic effluents, treated wastewaters etc.

Interferences Sampling, sub-sampling, and pipeting two-phase samples may introduce serious errors. Homogenization of sample before sampling and use of wide-mouth pipette eliminates the error; Exclude large floating particles or submerged agglomerates of non-homogeneous materials from the sample if it is determined that their inclusion is not representative; Excessive solids may form water-trapping crust, which can be avoided by limiting the sample to produce 0.2 g residue; For samples with high TDS thoroughly wash the filter to ensure removal of dissolved material; To aid in the quality assurance, analyze samples in duplicate.

Sampling and Storage Obtain an appropriate quantity of sample in a glass or plastic bottle; If suspended matter adheres to the container walls prefer glass container;
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Analyze sample as soon as possible. If preservation required, store it at 4 0C to avoid biological degradation; Preferably analyze with 24 hours and in no case after 7 days. Bring sample to room temperature before analysis.

Apparatus Muffle furnace for operating at 5500C; Desiccator provided with a desiccant containing a color indicator of moisture concentration; Drying oven, for operation at 103 to 105 0C; Analytical balance capable of weighing 0.1 mg; Magnetic stirrer. Wide-mouth pipettes; Glass fiber filter disks without organic binder; Filtration apparatus; Suction flasks sufficient capacity for sample size selected; Aluminum weighing dishes.

Procedure Preparation of glass fiber filter disk: Insert disk with wrinkled side up into filtration apparatus; Apply vacuum and wash disk with three successive 20 mL volumes of distilled water. Continue suction to remove all traces of water and discard washings; Remove filter from filtration apparatus and transfer to an inert aluminum weighing dish; Dry the glass fiber filter disk in an oven at 103 to105 0C for 1 hour. If volatile solids are to be measured, ignite at 550 0C for 15 minutes in a muffle furnace; Cool in a desiccator to balance temperature and weigh; Repeat cycle of drying or igniting, cooling, desiccating, and weighing until a constant weight is obtained or until weight change is less than 4% of the previous weighing or 0.5 mg, whichever is less. Store in a desiccator until needed;

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Choose sample volume to yield between 2.5 and 200 mg dried residue. If volume filtered fails to meet minimum yield, increase the sample volume up to 1 L. If more than 10 minutes are required for complete filtration, increase the filter size or decrease sample volume;

Assemble filtering apparatus and filter and begin suction. Wet filter with a small volume of distilled water to seat it; Pipette a measured volume of well-mixed sample onto the seated glass fiber filter disk (predried and weighed) with applied vacuum; Wash with three successive 10 mL volumes of distilled water, allowing complete drainage between washings, and continue suction for about 3 minutes after filtration is complete. Samples with high TDS may require additional washings;

Carefully remove filter from filtration apparatus and transfer to an aluminum weighing dish; Dry for at least 1 hour at 103 to105 0C in an oven, cool in a desiccator to balance temperature and weigh; Repeat drying cycle of drying, cooling, desiccating, and weighing until a constant weight is obtained or until weight loss is less than 4% of previous weight or 0.5 mg, whichever is less.

Calculation TSS, mg/L = (A B) X 1000 Sample volume, mL Where: A= B= weight of dried residue + filter, g weight of filter, g

3. DETERMINATION OF TOTAL DISSOLVED SOLIDS (TDS)

Definition It refers to the portion of solids present in water or wastewater that passes through a filter of 2.0 m (or smaller) nominal pore size under specified conditions. The principal ions contributing to TDS are carbonate, bicarbonate, chloride, sulfate, nitrate, sodium, potassium, calcium and magnesium. TDS in water may originate from natural sources, sewage effluent discharges, urban
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runoff, or industrial effluent discharges.

Purpose TDS is measured in waters and wastewaters because they influence other qualities of water, such as taste, hardness, corrosion and etc. Its amount in water is a consideration for the suitability of that water for drinking and other purposes. Scope This procedure is applicable to waters of wide range of quality including surface water, industrial and domestic effluents, treated wastewaters etc.

Interferences Sampling, sub-sampling, and pipeting two-phase samples may introduce serious errors. Homogenization of sample before sampling and use of wide-mouth pipette eliminates the error; Highly mineralized waters containing hygroscopic constituents may interfere. Prolonged drying and rapid weighing may reduce this error; Excessive solids may form water-trapping crust, which can be avoided by limiting the sample to produce 0.2 g residue; To aid in the quality assurance, analyze samples in duplicate.

Sampling and Storage Obtain an appropriate quantity of sample in a glass or plastic bottle; Analyze sample as soon as possible. If preservation required, store it at 4 0C to avoid biological degradation; Preferably analyze with 24 hours and in no case after 7 days. Bring sample to room temperature before analysis.

Apparatus Muffle furnace for operating at 550 0C; Desiccator provided with a desiccant containing a color indicator of moisture concentration; Drying oven, for operation at 180 0C; Analytical balance capable of weighing 0.1 mg;
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Magnetic stirrer with TFE stirring bar; Wide-mouth pipettes; Glass fiber filter disks without organic binder; Filtration apparatus; Suction flasks sufficient capacity for sample size selected; Evaporating dishes of 100 mL capacity.

Procedure: Preparation of glass fiber filter disk: Insert disk with wrinkled side up into filtration apparatus; Apply vacuum and wash disk with three successive 20 mL volumes of distilled water. Continue suction to remove all traces of water and discard washings; If volatile solids are to be measured, ignite cleaned evaporating dish at 550 0C for 1 hour in a muffle furnace. If only total dissolved solids are to be measured, heat clean dish to 1800C for 1 hour in an oven; Transfer into a desiccator and store there until needed. Weigh immediately before use. Choose sample volume to yield between 2.5 and 200 mg dried residue. If more than 10 minutes are required for complete filtration, increase the filter size or decrease sample volume; Pipette a measured volume of well-mixed sample onto the seated glass fiber filter disk with applied vacuum; Wash with three successive 10 mL volumes of distilled water, allowing complete drainage between washings, and continue suction for about 3 minutes after filtration is complete; Transfer total filtrate to a pre-dried and weighed evaporating dish and evaporate to dryness in a drying oven; If filtrate volume exceeds dish capacity add successive portions to the same dish after evaporation; Dry after evaporation for at least 1 hour in an oven at 180 0C, cool in a desiccator to balance temperature, and weigh; Repeat drying cycle of drying, cooling, desiccating, and weighing until a constant weight is obtained or until weight loss is less than 4% of previous weight or 0.5 mg, whichever is less.
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Calculation TDS, mg/L = (A B) X 1000 Sample volume, mL Where: A= B= weight of dried residue + dish, g weight of dish, g

4. DETERMINATION OF SETTLE ABLE SOLIDS (SS)

Definition Settleable solids is the term applied to the material settling out of suspension within a defined period. Purpose This parameter gives us information about the amount of suspended mater on surface water, domestic and industrial wastewater which is settle able under gravitational force. In other words, this is the portion of solids in a water sample which can be removed from water under gravitational force.

Scope This procedure is applicable to waters of wide range of quality including surface water, industrial and domestic effluents, treated wastewaters etc.

Interferences Sampling and sub-sampling may introduce serious errors. Homogenization of sample before sampling eliminates the error.

Sampling and Storage: Obtain an appropriate quantity of sample in a glass or plastic bottle; If suspended matter adheres to the container walls prefer glass container; Analyze sample as soon as possible. If preservation required, store it at 4 oC to avoid biological degradation; Preferably analyze with 24 hours and in no case after 7 days. Bring sample to room temperature before analysis.

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Apparatus: Imhoff cone

Procedure: Fill an Imhoff cone to the 1-L mark with a well mixed sample; Settle for 45 min, gently agitate sample near the sides if the cone with a rod or by spinning; Settle 15 min longer and record volume of settleable solids in the cone as mL/L; If the settled matter contains pockets of liquid between large settled practical, estimate volume of these and subtract from volume of settled solids The practical lower limit of measurement depends on sample composition and generally is in the range of 0.1 to 1.0 mL/L; Where a separation of settle able and floating materials occurs, do not estimate the floating material as settle able matter; Replicates usually are not required.

5. DETERMINATION OF FIXED AND VOLATILE SOLIDS (F&VS)

Definition Fixed solids is the term applied to the residue of total, suspended or dissolved solids after ignition for a specified time at a specified temperature; And Volatile solids is the term used for the weight lost on ignition of above sample. Purpose In wastewater treatment technologies Volatile Suspended Solids (VSS) are considered to depict the biomass of wastewater. Hence, its determination is helpful in the design of a secondary wastewater treatment system; Fixed solids are considered to be the inorganic constituents of wastewater. Thus, the determination of fixed solids in a wastewater gives an estimate of inorganic constituents of wastewater. Scope This procedure is applicable to waters of wide range of quality including surface water, industrial and domestic effluents, treated wastewaters etc.
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Interferences Determinations of total, fixed and volatile solids do not distinguish precisely between inorganic and organic matter because the loss on ignition is not confined to organic matter. It includes losses due to decomposition or volatilization of some mineral salts. Sampling and Storage Obtain an appropriate quantity of sample in a glass or plastic bottle; If suspended matter adheres to the container walls prefer glass container; Analyze sample as soon as possible. If preservation required, store it at 4 oC to avoid biological degradation; Preferably analyze with 24 hours and in no case after 7 days. Bring sample to room temperature before analysis. Procedure Ignite residue to constant weight in a muffle furnace at a temperature of 550 oC; Ignite a blank glass fiber filter along with samples; Usually, 15 to 20 minute ignition is required for 200 mg residue. Let dish or filter disk cool partially in air until most of the heat has been dissipated; Transfer to a desiccator for final cooling in a dry atmosphere. Do not overload desiccator; Weigh dish or disk as soon as it has cooled to balance temperature; Repeat cycle of igniting, cooling, desiccating, and weighing until a constant weight is obtained or until weight change is less than 4% or 0.5 mg, whichever is less. Weight loss of the blank filter is an indication of unsuitability of a particular brand or type of filter for this analysis. Calculation VS, mg/L = (A B) X 1000 Sample volume, mL FS, mg/L = (B C) X 1000 Sample volume, mL Where: A= B= C= weight of dried residue + dish or filter before ignition, g weight of residue + dish or filter after ignition, g weight of dish or filter, g
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OBSERVATIONS AND CALCULATIONS

Total Solids B = (Initial wt. of China Dish) A = (Final wt. of China Dish after evaporation, Drying and Cooling) Total Solids = (A - B)x1000/ml of sample

Suspended Solids B = (Weight of Filter Paper) A = (Weight of Filter Paper after drying) Suspended Solids = (A - B)x1000/ml of sample

Dissolved Solids B = (Initial wt. of China Dish) A = (Final wt. of China Dish after evaporation, Drying and Cooling) Dissolved Solids = (A - B)x1000/ml of sample

Volatile Suspended Solids B = (Weight after ignitian) A = (Weight before ignitian) Volatile Suspended Solids = (A - B)x1000/ml of sample
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Fixed Suspended Solids B = (Weight after ignitian) C = (Weight of Cruicible) Fixed Suspended Solids = (B - C)x1000/ml of sample

Settleable Solids Settleable Solids from Imhoff Cone

Comments:

Questions: 1) Why sample is evaporated at 1800C for dissolved solids?

2) What is the WHO guideline value for total solids?

3) Define volatile solids?

4) What is a gravimetric method?

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5) Why some solids settle down after somw time?

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