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1-Identification of Activated Sludge And

1-Identification of Activated Sludge And

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PII: S0043-1354(97)00334-5

Wat. Res. Vol. 32, No. 4, pp. 1240±1254, 1998 # 1998 Elsevier Science Ltd. All rights reserved Printed in Great Britain 0043-1354/98 $19.00 + 0.00

IDENTIFICATION OF ACTIVATED SLUDGE AND WASTEWATER CHARACTERISTICS USING RESPIROMETRIC BATCH-EXPERIMENTS
M H. BROUWER1*, A. KLAPWIJK1* and K. J. KEESMAN2

Department of Environmental Technology, Wageningen Agricultural University, Bomenweg 2, NL-6703 HD Wageningen, The Netherlands and 2Department of Agricultural Engineering and Physics, Wageningen Agricultural University, Bomenweg 4, NL-6703 HD Wageningen, The Netherlands
1

(First received June 1996; accepted in revised form August 1997) AbstractÐThis paper presents a procedure to obtain activated sludge kinetics and wastewater characteristics from respirometric batch-experiments. For identi®cation of state variables and model parameters a modi®ed version of the ASM no. 1 that describes the oxygen uptake rate of the nitri®cation process and organic matter elimination was used. It is demonstrated that the maximum nitri®cation rate of activated sludge and the concentration nitri®able nitrogen, and the rapid hydrolysis rate together with the concentration slowly biodegradable organic compounds can be estimated accurately. Suggestions to improve identi®ability problems are given. It is concluded that the proposed method o€ers possibilities to follow changes in sludge capacities, for both heterotrophic and autotrophic micro-organisms, and wastewater composition. # 1998 Elsevier Science Ltd. All rights reserved Key wordsÐactivated sludge, identi®cation, respirometry, batch-experiments, characterization, biokinetic parameters, wastewater composition

NOMENCLATURE iXB kH K r rend S X Y mm Indices S1 and S2 S i NH and NO A1 and A2 H max spec mass N per mass COD in biomass (gN gCOD ) rate of hydrolysis (hÀ1) half-saturation coecient: for heterotrophic biomass (mgCOD lÀ1); for autotrophic biomass (mgN lÀ1) respiration rate (mgO2 lÀ1 hÀ1) initial endogenous respiration rate (mgO2 lÀ1 hÀ1) soluble substrate concentration (mgCOD lÀ1) particulate substrate concentration (mgCOD lÀ1) yield coecient (mgCOD mgÀ1 COD) maximum speci®c growth rate (hÀ1) index relative to readily biodegradable organic compound 1 and 2 index relative to slowly biodegradable organic compounds index relative to inert matter index relative to ammonia or nitrite index relative to autotrophic biomass Nitrosomonas or Nitrobacter index relative to heterotrophic biomass index relative to maximum rate index relative to speci®c rate
À1

INTRODUCTION

For modelling as well as control purposes of wastewater treatment plants, information about the wastewater composition and activated sludge characteristics is essential.
*Author to whom all correspondence should be addressed.

The traditional way of analyzing wastewater composition is based on relatively simple physicalchemical methods. Filters are used to distinguish the soluble, colloidal and suspended fractions. The physical-chemical method is, however, not processrelated and therefore not able to fractionate the readily and slowly biodegradable part. This makes wastewater characterization by the physical-chemical method less suitable for model simulation or control purposes. Recent studies were done to gain knowledge about activated sludge and wastewater characteristics from a so-called respirogram (Kappeler and Gujer, 1992; Spanjers and Keesman, 1994; Spanjers and Vanrolleghem, 1995; Vanrolleghem and Van Daele, 1994; Dochain et al., 1995; Vanrolleghem et al., 1995). A respirogram is obtained in a batch assay where a sample of wastewater, or a compound which can be biologically oxidized, is added to a batch-vessel which contains a volume of endogenous respiring activated sludge. After addition the respiration rate is measured over a period of time. The collected data compose a dynamic respiration rate pro®le which provides good means to determine wastewater characteristics and activated sludge kinetics. This paper presents the evaluation of a series of respirograms gained from the municipal wastewater treatment plant Nijmegen (The Netherlands). The

1240

be given unique values''. A small eigenvalue (li) corresponds with a relatively large uncertainty in the direction of the associated (Vi) vector. ammonia was converted to nitrite by Nitrosomonas and nitrite was converted to nitrate by Nitrobacter. In that case. 1 seven combinations of the ®ve original parameters were structurally identi®able. Readily biodegradable organic substrate was split up into two fractions (SS1 and SS2) (Spanjers and Vanrolleghem. Additionally. Parameter uncertainty evaluation Dochain et al.. the problem of highly correlated parameters was disturbing the uniqueness of the parameter estimates. Dochain et al. The key question of the identi®ability analysis was de®ned by Dochain et al. from given single output data y E RN and in this case the available OUR data. The question arises: ``can the parameters.. to give the model parameters a unique value. The following modi®cations and assumptions were introduced: . In this particular case: e(tkvy) = OUR à R (tk.j is large as compared to other elements in this column.. given a set of measured state variables. Due to correlation's the estimated parameters may vary over a broad range and little physical meaning can be given to the parameters obtained. for instance. Vanrolleghem et al. 1987) was used. . Eigenvalue decomposition of the covariance matrix is de®ned by: ” NV ˆ L V T Cov y …2† MODEL PARAMETER IDENTIFICATION Structural and practical identi®ability In the calibration of model parameters identi®ability analysis plays an important role. . 1995) or on the type and quality of available data (practical identi®ability. Nitri®cation was modelled as a two-step process. with the available experimental data. 1994).. still producing a satisfying ®t between the experimental data and model predictions. the analysis could also have been performed with the Fisher Information Matrix. Notice that in equation 1 the term s2 e stems from the output data and since it is a scalar it can be interpreted as a scaling factor. . via parameter estimation?'' Herein a distinction was made in identi®ability on the basis of the model structure only (structural identi®ability.vy)2 as the pre(tk) À OU dicted OUR response at time instant tk as a function of y. an element Vi. (1995) showed that from a modi®ed ASM no. The elements of L indicate whether a parameter combination. Hydrolysis was modelled as ®rst-order kinetics (Sollfrank and Gujer. (1995). as in Vanrolleghem et al. a change in one parameter can be compensated by a proportional shift in another parameter. If. Let us recall very brie¯y the theory to study the practical identi®ability of model parameters.. E RP. 1 (Henze et al..y). In the case of a parameter that is structurally identi®able it is not ensured that this parameter is also practically identi®able. the corresponding parameter value is dicult to estimate accurately.. 1991). Slowly biodegradable organic substrate (XS) was. converted to SS2.. À T ÁÀ1 Cov yN ˆ s2 …1† e X X where s2 to be estie is the residual € error variance 2 and X is the mated from 1aN À p N kˆ1 e…tk jy† Jacobian matrix de(tkvy)/dyj with k = 1. COD and BOD5. 1995. ACTIVATED SLUDGE MODEL Modi®ed IAWQ-model In order to investigate the identi®ability of biokinetic parameters and biodegradable wastewater components a modi®ed version of the ASM no. for four types of models. In their modi®ed model no nitri®cation nor denitri®cation were considered and the deathregeneration concept was abandoned. a€ects the sum of squares... Vanrolleghem et al. Lukasse et al. with OU à R (tk. Consequently. due to hydrolysis.p. The ”N uncertainty in least-squares parameter estimates y Where V is an orthogonal matrix of eigenvectors and L is a diagonal matrix with eigenvalues. 1995). (1995) as follows: ``Can we expect. Dochain et al. 1996). given the weights of the associated eigenvector.. They concluded.N and j = 1. In other words: for this parameter the respirogram is non-informative and consequently a wide range of parameter values can be used to describe the experimental data. is given by the covariance matrix of the estimates. (1995) studied the structural identi®ability of kinetic models describing the activated sludge process from the assumption that only respiration data were available. A useful tool to analyze the precision of parameter estimates is the eigenvalue decomposition of the covariance matrix (Vanrolleghem et al.. NH4-N. the obtained wastewater fractions were compared with the measured analytical data: Nkj-N.Use of respirometry to characterise sludge 1241 primary goal was to investigate the identi®ability of biokinetic model parameters and initial state variables from a wastewater respirogram only. XTX directly. . that only a smaller set of the combinations of the original parameters were structurally identi®able.. (1995) showed that when a limited set of data is used for parameter estimation.

Because one of the goals is to assess the biological characteristics of the wastewater. the maximum nitri®cation rate (speci®c for Nitrosomonas) could be measured with an excess of exogenous substrate described by the following equation:   1 rNHmax ˆ iXB ‡ m XB. Aerate the sludge for the time period until endogenous respiration rate is reached. 1. Model used for simulation wastewater respirogram j 1 2 3 4 5 6 process component -> i 1 SS1 À Y1H 2 SS2 3 XS 4 SO YH À 1À YH ÀYA1 À 3X43 YA1 ÀYA2 À 1X14 YA2 YH À 1À YH 5 SNH ÀiXB ÀiXB ÀiXB À Y1 A1 6 SNO Process rate SS1 mm.A2 SS2 mm. This may be sludge from the aeration tank or return sludge. 1990). Dochain et al. Spanjers and Vanrolleghem. The experimental procedure was as follows: 1. . The respirometer is classi®ed as a continuous ¯ow-through measurement which uses the DO concentration in the liquid phase to calculate the respiration rate of the activated sludge (Spanjers et al.1242 H. The time period to aerate the sludge before it reaches the endogenous state depends on the loading regime of the plant and the spot where the sludge was sampled.75 l). Ammoni®cation. 1994. also called the endogenous respiration (Spanjers and Klapwijk. Not incorporated in the model were: . the sample is returning to the batch vessel..bacter on SNO endogenous respiration autotrophs and heterotrophs Hydrolysis XS À Y1H ÀiXB À Y1 A2 -1 1 -1 rend kHXS . From Table 1 it can be seen that the oxygen uptake rate is composed of: . EXPERIMENTAL PROCEDURE The experimental set-up consisted of a batch-vessel (3 l) which was directly attached to a continuous respirometer (RA-1000. . The modi®cations were introduced because the ASM no. oxidation of nitrite (SNO) to nitrate . 1994). After passing the respiration vessel (0. expressed in COD). oxidation of readily biodegradable organic compound 1 (SS1) present in wastewater . Denitri®cation. These parameters were left out of consideration because the experiments performed didn't allow their estimation. After the endogenous rate is reached a known volume of pre-aerated wastewater can be added to the batch vessel containing the activated sludge.. like mm and XB (for both autotrophs and heterotrophs) were structurally unidenti®able from respiration data (Dochain et al. one can follow the course of the measured respiration rate.. 1990). Due to the short term of this speci®c batch-experiment the endogenous respiration was assumed to be constant. as such. 1996). 2. Manotherm)..A1 SNO mm. Roughly the sludge should be aerated for a period of 2 h without feed (Spanjers and Klapwijk. because dissolved oxygen was non-limiting in the performed experiments. 1. Add a known volume of sludge to the batch-vessel. Brouwer et al. The peristaltic pump of the respirometer is continuously taking a sample of activated sludge (24 l/h) from the batch vessel.H2 KS2 ‡SS2 XBH growth heterotrophs on SS1 growth heterotrophs on SS2 growth N. The sample of wastewater has to be aerated ®rst to prevent a oxygen .A1 and XB. For instance. oxidation of ammonia (SNH.A1 were combined to one measurable parameter rNHmax.. present in wastewater) to nitrite . Due to the short term of the experiment and the low S0/ X0-ratio used (S0 and X0 were the initial substrate and biomass concentration. Hydrolysis of slowly hydrolysable organic matter according to ASM no. Measuring principle.A1 In this equation iXB. it is important that the activated sludge is respiring in the absence of the exogenous substrate. decay respectively growth of biomass were dicult to obtain. 1993. To detect this state. Table 1. because this process was assumed to be instantaneous (Henze et al. An important feature before the addition of substrate can take place is the state of respiration of the activated sludge. 1995).H1 KS1 ‡SS1 XBH SNH mm.somonas on SNH growth N. mm.A2 KNO ‡SNO XB. 1987). oxidation of readily biodegradable organic compound 2 (SS2) present in wastewater and formed by hydrolysis of slowly biodegradable organic compounds (XS) . . Due to the use of a single DO-electrode the measuring frequency is limited by the response rate of the DO-electrode (Spanjers and Klapwijk. where the dissolved oxygen at the inlet and outlet are measured.A1 …3† YA1 m. endogenous respiration Parameter reduction The model consisted of a large amount of parameters and process variables. iXB was assumed to be 0. . The amount of parameters was therefore reduced by combining non-identi®able parameters to structurally identi®able parameter combinations (Vanrolleghem and Verstraete. 1990) and is ®xed at once a minute. YA1.086 gN gCODÀ1 (Henze et al. Some of the parameters.A1 KNH ‡SNH XB. 3. was not able to produce a satisfying ®t between modelled and measured respiration data. Hereby the activated sludge is continuously recirculating. Growth and decay processes of autotrophic and heterotrophic biomass. 1995).

9 l of pre-settled wastewater to 1. The poor identi®ability is con®rmed by the sensitivity plot (d/dy*y) of the parameters concerned.Use of respirometry to characterise sludge Table 2. At the municipal wastewater treatment plant of Nijmegen. A double nitrogen tailing is previously recognized by Ossenbruggen et al. the complete respirogram is acquired. (1996). For all six respirograms the model is used to estimate the model parameters and state variables. However. 11. 4. When only a very few data points are related to the substrate induced respiration rate. as no saturation behaviour can be observed. Experimental conditions Date (June 1993) 16 18 21 23 24 25 MLSS (g/l) 1. 2 the measured and modelled total respiration rate (16 June 1996) and the estimated respiration rates for the ®ve wastewater components are shown.95 1. From the matrix of eigenvectors (Appendix A) we see that the vectors with the smallest eigenvalues (column 10.5 19. i.58 7. no information is retained to di€erentiate between rSs1max and (1-YH)KS1.39 Temp (8C) 20. Notice. (1996) suggested to reduce the amount of model parameters by giving them ®xed values. this will not guarantee both parameters can be separately estimated with the same accuracy. When the respiration rate has returned to the initial rate. for instance rSs1 (Fig.5 20 COD (mgCOD/l) 311 247 363 364 344 387 BOD5 (mgCOD/l) 160 160 170 185 180 210 S0/X* 0 (gCOD/gCOD) 0. A double tailing is created when the conversion rate of nitrite into nitrate (Nitrobacter) is lower than ammonia into nitrite (Nitrosomonas) and consequently nitrite is accumulated.69 7.3). Directly after the addition of wastewater to the activated sludge the respiration rate increases and within two minutes the maximum respiration rate is reached.6 1.76 pH (À) 6. 1(a±f) shows a respirogram with a double nitrogen tailing. Results of an eigenvalue decomposition of the covariance matrix of the estimated parameters are given in Appendix A.43YA1)KNH and (1.59 1. RESULTS AND DISCUSSION Figure 1 shows the six respiration rate curves gained after the addition of wastewater to the batch-vessel containing endogenously respiring sludge. listed in Table 3. Reduction of unknown model parameters also can be achieved by the performance of isolated substrate respirograms.7 1. From Fig.43-YA1) KNH. Those parameters which were not sensitive to the model output were given a ®xed value and consequently the remaining model parameters could be obtained with higher accuracy.14-YA2)KNO (roughly.69 1. After the addition of wastewater the respiration rate will increase due to the oxidation of organic and nitrogen compounds. Observe that Fig. The ®gures contains rough data. With a sequential addition of synthetic substrates of nitrite and ammonia the biokinetic parameters of autotrophic bacteria can be deduced seperately. The parameter combination (1-YH)XS and kH can be estimated very precisely in combination. 3(a±d) the derivatives of the residuals to the parameters and state variables become visible and it is shown that for some parameters only a small part of the curve is sensitive for a change of the residual of the estimate. Consequently. A similar e€ect can also be seen from Fig. 12 and 13) contains the following dominant weights on the parameters and initial state variables: (1-YH)Ss1. from Fig. Identi®ability analysis The model contains 9 biokinetic parameters and 4 initial state variables.057 0. these parameters/states are dicult to obtain with the given experimental data set. a series of respirometric batch-experiments were performed on 6 di€erent days. The batch-experiments were commenced by transferring 0. They suggested the use of an optimal experimental design. the rate before adding wastewater (taking dilution with wastewater into account). 3(d) that the high sensitive peaks of (1-YH)XS and kH coincides and thus these parameters cannot be identi®ed seperately in this particular experimental setup. The modelled respiration rate matches the measured respiration rate. 5. Another approach was suggested by Vanrolleghem et al. 1) and moreover. In this case only the ®rst order constant rSs1max/(1-YH)KS1 can be estimated.088 0. In this approach the calibrated biokinetic parameters for autotrophic bacteria can . furthermore. Their results indicate that the parameter variances could be decreased by a factor of 2 when an amount of substrate is injected at an optimally chosen time instant during the experiment.9 7. elements >0.099 1243 drop in the batch-vessel which will a€ect the measured respiration rate.5 21 21 20. To improve the reliability of estimation Lukasse et al.e.097 0.091 0. The Nijmegen plant has a plug-¯ow con®guration and is mainly treating domestic wastewater.62 7. In Fig. The applied S0/X0ratio equals the ratio as it enters the ®rst compartment of the full-scale installation. (1995).103 0. 3(b) for rNHmax and (3. The experimental conditions are presented in Table 2.5 l of return sludge in a batch-vessel of 3 l. Results of the identi®ability analysis are summarized in Table 4. rSs1max and the saturation coecients (3.23 6.

Brouwer et al. Fig 1. (a)±(c).1244 H. .

Use of respirometry to characterise sludge 1245 Fig. . Wastewater respirograms obtained at 6 di€erent days. 1.

.. Kappeler and Gujer worked at a very high S0/X0 ratio which resulted in a considerable population shift among the fast-growing/low-anity organisms (Grady et al. The threshold between low and high ratios of S0/X0 is not strictly de®ned but may be considered between an interval of 2 and 4 as a correct estimation (Chudoba et al. be used as default settings..103 (Table 2).43-YA1) KNH (1. rSmax and (1-YH)KS (in the case of one readily biodegradable organic compound) and the wastewater components: (1YH)XS. Biokinetic parameters With the objective to obtain biokinetic constants from batch cultivated biodegradation experiments it is demonstrated that the applied S0/X0 is extremely important (Chudoba et al.43-YA1)SNH. 1991) and 20 mgCOD/l (Henze et al. The parameter values found are readily in agreement with values reported in literature using similar calibration techniques (Spanjers and Vanrolleghem.. 4 and Fig. The wastewater treatment plants generally work at very low actual S0/X0 ratios. The applied actual S0/X0 ratio varied between 0.h) (mgCOD/l) (mgCOD/l) (mgNH4-N/l) (mgNO2-N/l) (1/h) state variable SS1* SS2* X S* SNH* parameter combination (1-YH) SS1 (1-YH) SS2 (1-YH) XS (3. 1994. 1994). The S0/X0 ratio determines whether catabolism or anabolism prevails. This signi®cantly reduces the number of unknown parameters for parameter calibration of a wastewater respirogram. 5 mgCOD/ l (Sollfrank and Gujer. In order to ®nd representative kinetic parameters it is important to work at low S0/X0 ratios.h) (mgCOD/l. YA1 and YA2).5 to 4 mgCOD/l (Kappeler and Gujer.14-YA2) KNO - …iXB ‡ Y1 †mmYA1 XBYA1 A1 * Under the assumption of known biomass yield (YH.h) (mgNO2-N/l. When anabolism prevails. Brouwer et al. Novak et al. However. 1992).43-YA1) SNH unit (mgCOD/l) (mgCOD/l) (mgCOD/l) (mgNH4-N/l) mmYH1 XBH mmYH2 XBH …iXB ‡ Y1 †mmYA2 XBYA2 A2 (1-YH) KS1 (1-YH) KS2 (3. Wastewater respirogram (16 September 1993) with measured and modelled respiration rates. parameter combinations and state variables parameter rSs1max rSs2max rNHmax rNOmax KS1* KS2* KNH* KNO* kH parameter combination 1 YH 1 1 YH 2 unit (mgCOD/l. halfsaturation coecients found by other research groups show signi®cantly higher values: 2. 1987).. Di€erences found can be explained by the applied experimental conditions. (1-YH)SS and (3. Model parameters. Spanjers and Vanrolleghem. Therefore it is expected that the observed biokinetic parameters will represent true values.h) (mgNH4-N/l. 1994). The estimated biokinetic heterotrophic parameters are given in Fig.. 1992. 5.1246 H. Table 3. organisms have sucient substrate for their growth and cell multiplication dominates above storage and accumulation phenomena.057 and 0. The only model parameters left to estimate are kH. 1992). Fig. 1996). 2.

due to a low pH on June 16 and 24 (Table 2) inhibition of the nitri®cation rate could have been occurred. From this type of respirogram it is obvious that no information regarding the conversion of nitrite can be obtained. rNHmax and rSs2max rSs2max and (1-YH)Ss2 Identi®ability Bad (1-YH)Ks1 and rSs1max (1. Spanjers and Vanrolleghem (1995) observed.14-YA2)KNO (1-YH)Ss1 and (3. Identi®ability classi®cation of a combination of biokinetic model parameters and initial state variables for this speci®c experimental design (Fig. In the case of inhibition of nitri®cation due to a decreasing pH. However. . at the applied S0/X0 ratio of 0. the wastewater appeared to be inhibitory to nitri®cation.43-YA1)KNH Figure 6 and Fig. Taking into account the poor identi®ability of rNOmax (Appendix A). special care should be paid to these values. The maximum conversion rate shows a high variation for both nitrifying organisms.43-YA1)SNH and (1-YH)XS.05. (3. Inhibition of nitri®cation was not veri®ed. (1-YH)XS. 7 graphically show the time variation in the speci®c maximum substrate elimination rate for Nitrosomonas and Nitrobacter. On June 23 and 24 the observed respirogram shows only one tailing. 1) Good (1-YH)XS and kH rNHmax. the maximum nitri®cation rate for both organisms are Fig 3(a)±(b) caption overleaf.Use of respirometry to characterise sludge 1247 Table 4.

Brouwer et al. . Fig. Fig. 3.1248 H. 4. Estimated speci®c maximum substrate elimination rates for heterotrophic organisms (95% error bounds). Sensitivity plot of the model parameters and state variables.

1991.06).67).18 and YA2=0. 5. 8. The estimated values are in the range of previous works. 1995). the area of the curve which is attributed to oxidation of XS is estimated larger and a smaller area is attributed to the oxidation of SNH which results in an overestimation of XS and underestimation of SNH. except on June 24. Estimated speci®c maximum substrate elimination rate for Nitrosomonas and Nitrobacter (assumed YA1=0. (95% error bounds). in many activated sludge models hydrolysis of slowly biodegradable organic substrate is simpli®ed to a ®rst order conversion. 6. Spanjers and Vanrolleghem. Hence. Di€erences can be explained by the medium or temperature which is used to obtain the hydrolysis rate. Consequently. The hydrolysis rate of slowly biodegradable organic substrate is given in Fig.Use of respirometry to characterise sludge 1249 Fig. Estimated half-saturation coecients readily biodegradable compounds SS1 and SS2 (assumed YH=0. (95% error bounds). In some cases a di€erent time scale is used. Because it is not possible to deduce the hydrolysis rate of slowly biodegradable COD from a 2-h experiment it is suggested to characterize the hydrolysis process as fast hydrolysis (Sollfrank and Gujer. According to the ASM no. underestimated. The hydrolysis shows a rather constant rate. 1 the hydrolysis constant kH slightly depends on the biomass concentration but mainly relies on temperature. . Fig.

7.06). (95% error bounds).18 and YA2=0. (1994) Kappeler and Gujer (1992) Sollfrank and Gujer (1991) Sollfrank and Gujer (1991) Spanjers and Vanrolleghem (1995) kH (h ) 0. Fig. Estimated half-saturation ammonia and nitrite coecients (assumed YA1=0. Brouwer et al.73±2. Estimated hydrolysis rate of slowly biodegradable organic substrate (95% error bounds). Reported ®rst order hydrolysis rates Authors This study San Pedro et al.17 0.17 to 0.14 0. Table 5. 8.75 1.1250 H. Fig. (8C) 19.05 to 0.4 À1 temp.04 2.21 0.5±21 20 14 10 20 20 time scale OUR ``short-term'' medium wastewater starch wastewater wastewater wastewater wastewater OUR ``short-term'' .

Estimated organic wastewater fractions: XS.67.67). Wastewater composition A basic problem of the experimental set-up used is the fact that addition of wastewater in the batch vessel led to a delayed increase of the respiration rate in the attached respirometer. assumed XBH and measured total COD. Because the maximum respiration rate was reached within 2 min after the addition we think the possible error made was almost negleglible. With the assumption of YH=0. or by applying mass balances for both vessels as done by Spanjers and Vanrolleghem (1994). via N-incorporation into biomass. Ss1.67. 9. compared to measured total COD. The assumption that the initial substrate concentration could be calculated from the injection at time zero was incorrect. and Fig. The estimated and analytical measured wastewater composition are given in Fig. . indirectly. Table 5 lists the values of hydrolysis rates which are reported by several authors and their experimental designs used.Use of respirometry to characterise sludge 1251 Fig. Cumulated total COD calculatedfor YH=0.5 and 0. This phenomenon could be corrected by injecting the sample of wastewater in both batch and respiration vessel in appropriate amounts (equal dilutions). e‚uent COD (Xi + Si) and BOD5 (assumed YH=0. the concentration nitri®able nitrogen. Ss2. For the estimation of di€erent wastewater fractions the heterotrophic yield (YH) determines the absolute concentration of COD and. 9. 10.

SS2. Smets B. Jr. They ®rst calculated YA1 from a dosage of known amount of ammonia and used this value to obtain the ammonia concentration from the wastewater experiment. Dochain D. Sci. 742±748. Spanjers and Vanrolleghem (1995) found values in good agreement with the ammonia concentration found by analysis. Therefore we would like to stress that it is very important to keep the pH constant at a non-inhibiting level. with the addition of a sequence or mixture of synthetic substrates. From identi®ability analysis it is found that from a wastewater respirogram the maximum nitri®cation rate of activated sludge and the concentration nitri®able nitrogen. and the hydrolysis rate in combination with the concentration slowly biodegradable organic compounds can be estimated accurately for the given system and experiment.18 and YA2=0. 11). XS. Fig.06). 1992).56 were found.5 corresponds more reasonable to the measured values. and Chudoba J.. 11. P. 10 it can be seen that an applied YH of 0..36 and 0.. Vanrolleghem P. Di€erences could be explained by a poorly controlled pH during the experiment (Table 2). Estimated and analyzed nitrogen wastewater fractions: SNH (nitri®able nitrogen) and NH4-N and Nkj-N (assumed YA1=0. F. and Daele van D. It is recommended REFERENCES Chudoba P. . which is a€ecting the estimated maximum oxidation rates and consequently the in¯uent composition. In this paper it is suggested that the biokinetic parameters be obtained separately. 26. Automation of the procedure could make it possible to follow changes of activated sludge as well as wastewater characteristics in time and is therefore recommended. Xi+Si (inert COD) and XBH are somewhat higher than the analytical measured total COD (Fig. 29. The estimated nitri®able nitrogen concentration shows some inconsistency with the nitrogen found from chemical analysis (Fig. Capdeville B.1252 H. (1992) Explanation of biological meaning of the S0/X0 ratio in batch cultivation. CONCLUSIONS that the results of an eigenvalue decomposition of the covariance matrix related to given respirograms be evaluated. The reliability of estimation of model parameters and state variables depends on the respiration pro®le and chosen model structure. 2571±2578. The assessed biokinetic parameters can then be used as default values which favour the estimation of the remaining unknown model parameters. taking into account that 20% of the in¯uent COD exist of biomass (Henze. Techn. (1995) Structural identi®ability of biokinetic models of activated sludge respiration. it is demonstrated that respirometric batch-experiments are a useful tool in obtaining some activated sludge and wastewater characteristics. From Fig. Res. Wat. and Barbeau D. 743±751. (1996) Variability in kinetic parameter estimates: a review of possible causes and a proposed terminology. S. the estimated cumulated organic fractions SS1. Finally. Wat. Res. To improve the identi®ability of wastewater composition the number of unknown model parameters should be reduced. Acknowledgements ÐThe authors wish to thank Anneke Rinia and Ron Blokzijl for their assistance in the research carried out. 10). 30(3). Wat. Jacques Segers and Dennis Piron from ``Zuiveringsschap Rivierenland'' are thanked for their cooperation during the research. Brouwer et al. Grady C. YA1 values of 0.

Sci. 29. Wat. A. Sci. Wat.. 13th IFAC World Congress. and Verstraete W. Wat. and Klapwijk A. and Matsuo T. Novak N. Wat. Kappeler J. Gujer W.. R. 171±180. 34(2). 1253 Sollfrank U. 125±139. 1011±1016. Appendix overleaf. and Marais G. Tech. Lukasse L. anoxic and aerobic conditions. Henze M. Sci. and Keesman K. (1996) Grey-box identi®cation of dissolved oxygen dynamics in activated sludge processes. Spanjers H. Res. Vanrolleghem P. (1993) Simultaneous biokinetic characterization of heterotrophic and nitrifying populations of activated sludge with an on-line respirographic biosensor. Henze M. 25. 243±253. pp..Use of respirometry to characterise sludge Henze M. 30. Wentzel M. and Vanrolleghem P. Tech.. (1994) Optimal experimental design for structure characterization of biodegradation models: on-line implementation in a respirographic biosensor. (1996) Respirometry in control of the activated sludge process. 2561± 2570. Spanjers H. 939±953. Wat. A. Proc. Wat. Copenhagen. Tech. and Dochain D. A. Van Daele M. (1994) Evaluation of the rate of hydrolysis of slowly biodegradable COD (SBCOD) using starch as substrate under anaerobic. (1987). 30. J.P. Grady C. J.L. Gujer W.1.. Wat. Activated Sludge Model No. Mino T. Sci. Spanjers H. July 1996. Lewis. IAWPRC. Spanjers H. 26 July±3 August. Tech. Marais G. Keesman K. (1992) Characterization of wastewater for modelling of activated sludge processes. 23. On-line meter for respiration rate and short-term biochemical oxygen demand in the control of the activated sludge process. Wat. (1994) Estimatiom of maximum speci®c growth rate of heterotrophic and autotrophic biomass: a combined technique of mathematical modeling and batch cultivations. J. 25. (1994). and Gujer W. (1995) Respirometry as a tool for rapid characterization of wastewater and activated sludge. v. Wat. and Klapwijk A. and Gujer W.. 1±15. Vanrolleghem P. Sci. Tech. Scotland. 117±126. Sci. S. 2. Sci. Vanrolleghem P. Conference on Control Applications. (1992) Estimation of kinetic parameters of heterotrophic parameters under aerobic conditions and characterization of wastewater for activated sludge modelling. Wat. 24±26 August.v. and Matsuo T. 1992. San Pedro D.. Activated sludge Model No. 377±387.. Matsuo T. Glasgow. J. Larrea L. 611±118. and Wanner J. Tech. Identi®cation of wastewater biodegradation kinetics. Proc. Proceedings 3th IEEE. Japan. C. 30. Preprint for IAWQ Specialised Seminar on Modelling and Control of Activated Sludge Processes. C. (1995) Practical identi®ability of a biokinetic model of activated sludge respiration. Spanjers H. Mino T. 30.. (1994). Sci. In Advances in Water Pollution Control. 31(2). and Dold P. (1994). IAWQ Scienti®c and Technical Reports. pp. 1057±1066. (1990). Tech. 5th IAWPRC Workshop. 105±114.1. Tech. 191±199... Wat. IAWPRC Scienti®c and Technical Report No. (1991) Characterization of domestic wastewater for mathematical modelling of the activated sludge process. Sci. and Van Daele M. and Straten van G. A. 1995. Res. 28. A. Londen. Yokohama and Kyoto. Spanjers H. and Vanrolleghem P.. A.. 50th Purdue Industrial Waste Conference. Tech. (1996) Assesment of a two-step nitri®cation model for activated sludge.. Vanrolleghem P. . Gustaf O.R. Ossenbruggen P.

53 1.27 0.26 0.30 0.02 À0.43-YA1)KNH (1.37 1.28 0.01 0.03 À0.13 À0.95 À0.06 À0.06 0.07 0.04 À0.42 À0.23 À0.08 0.00 À0.20E + 05 À0.00 À0.21 À0.03 À0.51 À0.13 À0.14 0.84 0.25 0.15 1.80E + 04 À0.00 À0.23 0.07 À0.02 À0.29 0.01 9.07E + 01 À0.22 0.02 À0.08 À0.59E + 00 .43 À0.21 0.13 À0.02 À0.14 0.36 0.00 0.09 À0.02 À0.02 0.02 3.04 À0.08 0.02 0.00 0.01 0. (1-YH)Ss1 (1-YH)Ss2 (1-YH)Xs kH rNHmax rNOmax (3.04 0.01 0.01 0.18 0.39 0.26 À0.03 À0.35 À0.02 0.00 0.02 0.12 0.29 À0.05 À0.24 À0.30 À0.30 À0.00 0.11 0.01 0.00 0.10 À0.01 À0.00 0. Brouwer et al.19 0.07 À0.21 À0.66 À0.98E + 03 0.81 0.06 0.55 À0.16 0.1254 APPENDIX A Eigenvalue Decomposition of the Covariance Matrix H.22 À0.16 0.17 0.14 0.60E + 03 À0.04 À0.08 1.12 0.01 8.02 À0.02 À0.01 À0.02 À0.64 0.11 0.00 0.23 0.34 0.10E + 04 0.13 À0.01 0.29 0.08 À0.23 0.57 0.34 0.24 À0.05 À0.74E + 02 À0.17 0.91 0.07 0.67 2.05 À0.75 0.74 0.26 0.01 0.03 À0.03 0.03 À0.04 7.30 0.25 0.28 À0.04 0.43-YA1)SNH rSs2max (3.08 0.00 0.18 À0.01 À0.45 0.06 À0.46E + 04 0.14-YA2)KNO (1-YH)Ks1 (1-YH)Ks2 rSs1max Eigenvalues 0.47 À0.01 0.59 À0.05 À0.01 À0.09 0.70 0.48E + 02 0.02 0.01 0.35E + 03 À0.03 À0.03 4.30 À0.00 0.01 À0.03 3.06 À0.21 À0.91 À0.06 0.14 À0.24 1.04 À0.08 À0.05 À0.01 0.05 À0.22 À0.27 0.04 0.22E + 03 0.18 2.25 À0.06 0.13 0.01 0.61 À0.53E + 04 0.

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