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Solids in water are defined as any matter that remains as residue upon evaporation and drying at 103 degrees Celsius. They are separated into two classes: suspended and dissolved.

Total Solids = + Dissolved Solids ( nonfil terable residue) (filterable residue)

Each of these has Volatile (organic) and Fixed (inorganic) components which can be separated by burning in a muffle furnace at 550 degrees Celsius. The organic components are converted to carbon dioxide and water, and the ash is left. Weight of the volatile solids can be calculated by subtracting the ash weight from the total dry weight of the solids. DOMESTIC

t 999,000 mg/L

Total Solids 1,000 mg/L

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Total Suspended Solids/Volatile Solids treatment (adequate aeration, proper F/M & MCRT, good return wasting rates) , and the capacity of the secondary . Excessivl:and The Total Suspended Solids test is extremely valuable in the analysis of polluted suspended solids in final effluent will adversely affect disinfection capacity . waters. It is one of the two parameters which has federal discharge limits at 30 Volatile component of final effluent suspended solids is also monitored. A ppm through enforcement of the . Solids are removed throughout low volatile percentage may indicate hydraulic overload. High volatile the treatment plant to prevent excessive solids discharge to the receiving stream, percentage may indicate an unusual industrial input and may indicate a which would contribute to lowering of dissolved oxygen available to life in the higher BOD reading; comparison must be made with other wastewater test water, and to eutrophication of the stream. results to determine the problem.

Expected Total Suspended Solids: Treatment Plant Significance Raw Domestic Wa stewaters: 200-400 ppm (60-80% Volatile) Wa stewater Secondary Effi uents: < 30 ppm (60-80% Volatile) Solids determinations are very important in evaluating the performance of plants, and in controlling the processes in the plant. Total Suspended Solids is performed most often on Raw Wastewater, Primary Effluent, Treatment Plant Control and Final Effluent-at processes. A composite sample is taken for the test. Problem: Higher than normal Total Suspended Solids concentration in final effluent Raw Wastewater: Entering the treatment plant, due to water velocity , all particulate solids are suspended. Their concentration in the water Test This Possible Cause Sample Also For Other Checks determines design of process units, degree of treatment needed, and indicates changes in influent . The volatile content of these Industrial high COD, Tot.Phos., IPP records suspended solids relates to the efficiency of pretreatment units, and indicates strength input NH3-N, DO Previous Operating Reports changes in the amount of organic content of the incoming wastewater. It Contact contributing industries will influence percent removals and control of secondary treatment, Raw & Prim.effluent COD, Tot.Phos., NH3-N, TSS/VS, DO frequency of primary sludge pumping, and the efficiency of the anaerobic Primary sludge pumping rate, frequency digester. DO, blower use in biological unit Sec.sludge blanket level Primary Effluent: Total Suspended Solids concentration of this water determines the load on secondary, and relates to the efficiency of primary Industrial toxic COD, NH3-N, DO Plant operating records shock Contact contributing industries treatment. Frequency and duration of primary sludge pumping will have a Raw pH, color, odor significant effect on the suspended solids content of the primary effluent. DO, blower use in biological unit Volatile content of suspended solids in primary effluent is composed of the Biomass microscopic examination particulate organic compounds that will be used directly by the organisms Floe formation in secondary for growth, to be removed through biological adsorption, and Settleability of secondary sludge Sludge TS cone .. blanket level then absorption into the bacterial cell. It will determine the bacterial growth rate, and effect aeration and mixed liquor concentration. lnplant recycle COD, Tot.Phos., Recycle flow records Return and waste pumping rates will be affected. Non­ input NH3-N, DO Recycle COD, Tot.Phos., NH3-N, TSS/VS, TS volatile particulates will also be adsorbed by the biomass, and separated from Plant flow records the water, but these do not aid in bacterial growth. DO biological unit Sec.sludge blanket level

Effluent: This suspended solids test is most important, for it Final.determines NPDES permit compliance. Total suspended solids concentration of final effluent will depend on the efficiency of secondary •l•l l'llAl II(.:AL MANUAi UI W All II WA Ml' I llY llOLIUO 1111 I 111

fHt lhl1 Don't allow the muffle furnace go over 550 degrees Celsius. f>o11lble CauH Stutiplu Al•o l'or Othor Chook11 Components in the fi lter paper may ignite; some inorganics in the sample

Hydraulic COD, Tot.Phos., Plant flow records may burn. At higher temperatures, some inorganics may burn. overload NH3-N, DO Influent water temp. • Do not open the furnace door after a sample has been placed in there for Rew & Prim.Eff. COD, Tot.Phos., NHrN. ignition. The extra oxygen that enters when the door is opened may TSS/VS, DO ignite it so forcefully that the sample gets blown out of the crucible. Prim.sludge TS cone. Sec.sludge blanket level, TS cone. Apparatus: lnplent operational COD, Tot.Phos., Coagulant feed rate, cone., type • drying oven control problem NH3-N, DO Jar Test • muffle furnace Chemical feed pump operation • Gooch crucibles Prim.sludge TS cone. • desiccator Prim.Eff. TSS cone. Sludge pumping frequency • glass fiber filters Mechanical: sludge collector • source of vacuum Mixed liquor cone. • filtering flask DO in biological unit • tongs Mixing in biological unit Sludge TS cone., blanket level Biomass microscopic examination Procedure: F/M ratio, MCRT, RAS rate, hydraulic lo'ading 1. Insert filter with rough side up in Gooch crucible. Rinse filter with distilled water, applying vacuum to seat. QC procedures Incorrect analysis 2. Dry filter Gooch at 103 deg.C for 1 hr. Refer to Standard Methods Burn in muffle& furnace for 15 minutes. Cool in desiccator. 3. Weigh Gooch/filter to the nearest mg.(tare weight) Analysis: Total Suspended Solids/Volatile Solids 4. Mix sample well so that aliquot used has a representative amount of solids. Transfer quantitatively; filter a known volume of sample (it is Quality Control: best to use the largest volume possible that will not blind the filter). • Mix the sample well; pour aliquot before it gets a chance to settle. Use 5. Dry in 103 deg.C oven for 1 hour. Cool in desiccator. Weigh again (dry graduated cylinder to measure sample volume. Transfer quantitatively weight). to Gooch Crucible (wash out any particles that are stuck on the inner 6. Burn in muffle furnace for 15 minutes (550 deg.C). Cool in desiccator. walls of the cylinder). If large, uncharacteristic pieces are in the sample, Weigh again (ashed weight) . remove them. 7. Calculate: • Be sure the analytical balance has been calibrated to standard weights - g) recently. Weights to the milligram are necessary. = dryweig ht(mg) - tare weight(m TSS (mg/L) x 1000 • Do not handle solids sample ceramics with fingers. Use tongs. ml. sample • Weigh only room temperature samples; allow warm samples to cool in

= ashed weig - weig t(mg) a desiccator. Fixed Solids (mg/L) ht(mg) tare h x 1000 ml. sample • To troubleshoot weight discrepancies, run a blank, using distilled water, along with the samples. Volatile Solids (mg/L) = TSS (mg/L) - Fixed Solids (mg/L) • As per Standard Methods, periodically dry, cool, weigh repeatedly till weight is constant. In this way, proper drying time can be established. = Volatile Solids Cmg/L) • Oven and furnace drying and burning temperatures are critical. A % Volatile Solids x 100 TSS (mg/L) calibrated thermometer should be permanently set into the drying oven. Periodically it should be checked with another calibrated thermometer. ='f'-"'11._.At II< Al MANIJAL tJI WA'• ll WAI 11 l Ill Ml' 11\Y •I I ,_,_•IO"======OllUt Mixed Liquor Total Suspended Solids Teet Thie Po11lble Cause Sample Aleo For Other Checks This is similar to the Total Suspended Solids test done on influent and effluent Industrial DO, pH Raw pH ; it is done routinely on mixed liquor and activated sludge at an toxic shock microscopic exam Floe formation Activated Sludge Treatment Plant. Normally, Total Solids tests are done on Settleability of Sec. sludge , but this is a less concentrated sludge, and the weight of the dissolved substances in it may be significant, so it is tested for solids in the same way as a lnplant recycle DO, TS Recycle flow records input Recycle COD, Tot.Phos., NH3·N, TSSNS. TS. wastewater sample is. Plant flow records Sludge blanket level

Treatment Plant Significance Hydraulic DO, TS Plant flow records overload Influent water temp. Raw & Prim.Eff. COD, Tot.Phos., NH3·N, The results of this analysis represents the weight of the organisms in the aeration TSS/VS, DO tank, the bacteria which remove the organic wastes from the water. These bacteria Prim.sludge TS cone. are settled out in the secondary and called Activated Sludge. Continually, Sludge blanket level some portion of this sludge is recycled back to aeration (Return Activated Sludge), Sludge TS cone. and the rest is wasted (Waste Activated Sludge). lnplant DO Coagulant feed rate, Mixed Liquor cone., type The Mixed Liquor is a suspended floe mass, and includes not only bacteria, but operational microscopic exam Jar Test also the adsorbed solids from the wastewater, as they are being digested by the Chemical feed pump operation bacteria. The Mixed Liquor Suspended Solids (MLSS) concentration is controllable Prim.sludge TS cone. by varying the RAS and WAS pumping rates, and this concentration will determine Prim.Eff. TSS cone. Sludge pumping frequency aeration rate, F/M ratio, sludge age MCRT. Human control over the biomass Mechanical: sludge pump, sludge & concentrationis a major advantage of operating an activated sludge treatmentplant. collector Volatile and Fixed percentages of the mixed liquor are used to determine biological Mixed liquor cone. efficiency and potential for waste removal. Sec.sludge TS cone. Sludge blanket level F/M ratio, MCRT, RAS rate, hydraulic loading Expected MLTSS concentration: 1500 - 4000 mg/L Expected TSS Activated Sludge : 5,000 - 30,000 mg/L (.5-3%) Incorrect analysis QC procedures Refer to Standard Methods

Treatment Plant Control

Analysis: Mixed Liquor Total Suspended Solids Problem: Mixed Liquor Total Suspended Solids other than normal concentration. Grab samples are taken forthis test. This is a Total Suspended Solids test, but

Test This because of the greater amount of solids, a Buchner Funnel is used for filtering the Possible Cause Sample Also For Other Checks sample. If Volatile Solids is to be determined, the filter paper m�st b� glass-fiber. The filter paper (plus solids) is removed from the funnel, dned m the oven, Industrial high DO, TS Prim: weighed and then burned, and weighed again. strength input Raw & Prim.Eff. COD, NH3-N, Tot.Phos, TSS/VS Quality Control: Blower use • RAS, WAS rate Mix sample thoroughly, and pour immediately! Sludge TS cone. • Be sure to dry the sample thoroughly. To check time needed , dry, cool , weigh, dry again, cool, weigh. Al MANllAl l'llAI Ill UI WA' 1lWA 1 l I\ c Ill Mlt 11\Y '•UlII)' •I I

• Sec Quality Control and Safety notes from Total Suspended Solids Total Solids/V ola.tile Solids section.

Apparat.us: Total Solids tests are done on concentrated wastewater sludges. The result will include both suspended and dissolved solids, and are usually registered as • drying oven percentages. Total solids tests are not done on process waste aters b�caus la ge • desiccator � � � � portion of the dissolved solids in wastewater samples may be morgarucs onginatmg • tongs from the carriage water, and not fromthe waste. In sludges, however, only a small • filtering flask portion of the solid weight is dissolved; almost all of it is suspe�ded. �ince • source of vacuum of this type of sample is extremely difficult, a suspended sohds test is not • buchner funnel practical, and the Total Solids test is performed. • filter paper with diameter at least 1 inch larger than funnel base

Procedure: Treatment Plant Significance 1. Dry filter paper in oven at 103 deg.C for one hour. If volatile solids weight is desired, burn in muffle furnace at 550 deg.C for 15 minutes; Anaerobic Di.gester Sludge: Total Solids test on Primary Sludge (digester cool in desiccator. influent) yields data on status of primary clari�cation and influe�t sludge 2. Weigh filter paper to nearest mg. (tare weight) pumping. Its concentration (plus Volatile Sohds percentage) w1ll a�ect 3. Insert filter into Buchner funnel. Fit in with filter paper folded neatly up _ performanceof anaerobic digester and, in turn, dewatenng_ and drymg uruts. sides of funnel; wet down with distilled water, using vacuum. With this and digested sludge Total Solids content, digester efficiency and 4. Filter a known volume of solids (largest volume that will not blind the % Reduction Volatile Solids can be calculated. filter), applying vacuum. Total Solids data is used to calculate supernatant and dewatering filtrate 5. Carefully remove filter from funnel; dry in oven at 103 deg.C for 1 return flows, and sludge pumping rates. Percent Volatile Solids in sludge refers hour; cool in desiccator; weigh again (dry weight). to eff iciency of pretreatment and chemical characteristics of plan! influent 6. If volatile solids weight is desired, burn in muffle furnace at 550 deg.C wastewater. Nonvolatiles in the digester are not usable by the orgarusms, and for20 minutes. Cool in desiccator. Weigh again (ash weight). 7. Ca lculate: reduce effective volume of the digester.

Aerobic Di.gester Sludge: The Total Solids tests have similar significance, = dry we g ht(mg) TSS (mg/L) i ht(rng) - tare weig x ml. sample 1000 but refer to condition of process in the secondary clarifier. Total Solids tests are also performedon digester supernatant.

= ashed weigh t(mg t(mg) Fixed Solids (mg/L) ) - tare weigh x 1000 ml. sample Expec ted TS Primary Sludge : 3-5 % Expec ted TS Anaerobically Digested Sludge : 7-10% Volatile Solids (mg/L) = TSS (mg/L) - Fixed Solids (mg/L) Expec ted TS Dewatered Sludge (A n.Dig.): 30-40% Expec ted TS Aerobically Digested Sludge : 2-5 % Expe cted TS Dewatered Sludge (Aer.Dig.): 6-9% = Volatile Solids (mg/L) % Volatile Solids x 100 TSS (mg/L) (!====�==���=� 1'1\AC 111 AL MAIHIAI Cll WA'd I WA 1111 c Ill Ml't l I Y

/'rob/em: ower than normal Total Solids concentration 111 St.:co11da1y Trec\.lmcnt. PJ,u\t Cont a-ol Sludge L l'r oblem: Lower then normal Total Solids concentration in Primary Sludge Test This Test This Possible Cause Sample Also For Other Checks Possible Cause Sample Also For Other Checks De nitrification microscopic exam TSS final effluent Denitrification vs Prim.Eff. TSS, DO (rising sludge) Sludge blanket level (rising sludge) Sludge pumping frequency RAS rate Settleability Sludge Coning Prim.Eff. TSS, DO Rising Sludge High influent vs Raw & prim.elf. COD, TSS, NH3-N, TS cone.Prim. Sludge at start of BOD load Tot. Phos. pumping cycle F/M ratio, MCRT, Sludge blanket depth Settleability, Final eff. TSS, COD, NH3-N, Tot.Phos. Hydraulic vs Plant Flow Overload Prim.Eff. TSS, COD, DO Hydraulic Plant flow overload Raw & prim.eff COD, TSS Mechanical Operation of sludge pump Settleability, RAS rate Malfunction Operation of sludge collector mechanism Industrial pH Settleability Incorrect Analysis QC Procedures toxic shock microscopic exam TSS final effl. Refer to Standard Methods Contact contributing industries

Incorrect Analysis QC procedures Refer to Standard Methods Problem: Lower than normal Total Solids concentration in Anaerobically digested sludge. Analysis: Total Solids/Volatile Solids WasteWater Sludge Test This Possible Cause Sample Also For Other Checks In Total Solids test, known volume is not taken. Instead, an evaporating dish Incomplete vs VA/A ratio is filled, wet weight, dry weight, ash weight is recorded . Percent Total Solids can digestion Gas production, % C02 then be determined. TSS supernatant Digester temperature, loading, mixing Quality Control: Prim.sludge vs Prim. sludge TS • If Total Solids is being performed on a water sample, rather than a concentration Plant Flow sludge sample, dry firstat 98 degrees Celsius till the visible water is out, too low Prim. sludge pumping frequency to prevent spattering, then turn up to 103 degrees Celsius. • See Quality Control in Total Suspended Solids section. Industrial vs Supernatant COD toxic shock Raw wastewater COD Past plant operating records Apparatus: • drying oven Incorrect Analysis QC procedures • muffle furnace Refer to Standard Methods • desiccator • tongs • evaporating dish 1'111\C'I H Al MANUAL fll WAI 11WA1111 <'Ill Ml 1 llY 11

Procedure: calibrations to measure the sludge level. In many treatment facilities it has lwcu Burn clean evaporating dish in muffle fu rnace for 15 minutes. Cool. replaced with the one liter graduated cylinder. Most often performed on Mixed I. Weigh dish to the nearest ten milligrams (tare weight). Liquor, a 30 minute settling test yields data on the performance of the secondary 2. Fill dish about 3/4 with sludge. Weigh again (wet weight) . clarifier, and it relates to the waste/microorganism balance in the aeration tank 3. Dry sludge in 103 deg.C oven overnight. Cool in desiccator. Weigh (F/M ratio). This along with the TSS test results helps to regulate the RAS rate. again (dry weight) . The Settling Test results can also project expectations for downstream sludge 4. Burn in muffle furnace at 550 deg.C. Cool in desiccator. Weigh again handling processes; the same test can be performed on Activated Sludge, and (ashed weight). thickened or digested secondary sludges. 5. Calculate: Expected Settled Volume (A ctivated Sludge) : 200-400 ml in 1 Liter cylinder. dry weight(g.) - tare wei�ht(g.) Expected SVI: near 100 Total Solids ( % ) = x 100 wet weight (g.) - tare weight (g.) Expec ted SDI: near 1

Total Solids (mg/L) = Total Solids (%) x 10,000 Treatment Plant Control (g ) Fixed Solids (%) = ashed �eigh t(g.) - tare w�i�ht . x 100 dry weight (g.) - tare we1g t (g.) Problem: Mixed Liquor settling too fast; pinpoint floe in final effluent.

Volatile Solids (%) = 100% - Fixed Solids (%) Test This Possible Cause Sample Also For Other Checks

Volatile Solids (mg/L) = Volatile Solids (%) x 10,000 Operational DO, ML TSS/VS Raw prim.aft, final eff.COD, TSS, Tot.phos. control problem F/M, MCRT, RAS rate, cone.sludge

Settleable Solids Problem: Mixed Liquor settling too slowly.

Settleability is a quick and easy inplant control test. The ability to settle solids Test This Possible Cause Sample Also For Other Checks fromwastewater has been the basis of treatment since the earliest days of pollution control, and results of this test are still important at Activated Sludge treatment Operational DO, ML TSS/VS Raw, prim.eff, final eff. COD, TSS, Tot.phos. plants, where the settling capacity of the secondary sludge is variable. control problem F/M, MCRT, RAS rate, cone.sludge Sec.sludge blanket level

Industrial DO, pH, microscopic raw pH Treatment Plant Significance toxic shock examination sludge cone., Final eff. pH, TSS/VS, COD, Tot.phos. The first settleability tests were performed on primary sludge, and results measured in ml/L. From this a calculation of sludge pumping rate was made. In Hydraulic DO, MLTSS/VS Influent flow, sludge cone., Prim.eff. TSS/VS, more recent years, calculations of primary sludge pumping rates are made based on overload COD, Tot.phos. Sludge cone .. final eff. TSS/VS, COD, an expected volume and Total Solids concentration of the sludge. Primary sludges Tot.phos. are generally easy to settle, and most often cause problems if pumping frequency is not adequate. Predominance of DO, microscopic Visual-bulking sludge Secondary sludge settleability tests are much more important today, particularly filamentous examination Finaleff., prim eff., TSSNS, COD, Tot. Phos., for activated sludge, which can be difficult to settle. The Mallory Settleometer is organisms NH3-N, Sec. sludge blanket level. F/M Ratio, MCRT, RAS rate, TS.sec.sludge designed for this use, and has a beaker-like shape (very much like a clarifier), with •I l'l\Al 11< Al MANUAi lll WA'• IL WA 1111 < I IL Mlt• I HY

Analysis: Settleable Solids - Mixed Liquor

Calculations of Sludge Volume Index and Sludge Density Index for treatment process control are done based on the settled volume of sludge, and approximate calculations for activated sludge concentration can be done.

Quality Control: • Collect sample and do test immediately or sludge will rise. • • Be sure sample has been well mixed before pouring into cylinder. • Solids which rise to the top surface are not disturbed, and are not to be Dissolved Oxygen considered settleable solids. • Keep temperature constant.

Apparatus: • settleometer or 1 L graduated cylinder Dissolved oxygen (DO) is one of the most important and useful water measure­ Procedure: ments. Though the oxygen concentration in air is about 21 % , in water it is only 1. Fill vessel to the total volume with mixed liquor as soon as possible after slightly soluble. ranges from 7 ppm in hot water to 15 ppm in taking sample. cold water and is 9 .2 ppm at 20 degrees Celsius and atmospheric pressure at sea 2. Allow solids to settle for 30 minutes. Mark sludge level. Graph settling level. Type and amount of biological activity in a water body will depend upon the rate. amount of dissolved oxygen present. Most microorganisms use free or dissolved oxygen for respiration. Oxygen depletion in natural water bodies caused by the addition of bacterial nutrients (wastewater or agricultural runoff) may limit life in that water. The ability ofthe stream's microbes to degrade any added nutrients will be limited by the amount of dissolved oxygen in the water. On the other hand, photosynthesis adds dissolved oxygen to the water as a waste by-product.

Treatment Plant Significance

The measurement of Dissolved Oxygen is the basis for the BOD test, and for oxygen uptake rate tests. Oxygen depletion in long, sluggish wastewater collection systems may lead to the formation of toxic atmospheres. Nitrogen, hydrogen sulfide, methane, are emitted because of anaerobic conditions in the water. Corrosion of concrete and metal surfaces is enhanced; depletion of oxygen in primary sludges will start anaerobic action, and lead to rising sludge. Oxygen solubility determines the rate at which oxygen will be absorbed by organisms in biological aeration, making it an important factor in the cost of aeration. Oxygen concentrationdetermines whether biological degradation of a waste will be aerobic or anaerobic. Decreased amounts of oxygen in activated sludge aeration tanks promotes the growth of filamentous organisms. A high concentration of

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