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, DOCUMENT RESUME _ED 147 190 SE .023 378 TITLE Effluent Monitoring Procedures: Nutrients. Student . _ Reference Manual.- :INSTITUTION Environientail Protection Agency, Washington, D.C. Office- of Water Programs. REPORT WO EPA-430-1-76-006 'PUB DATE Jun 76 s . ,NOTE 503p.; for related documents, see SE '023 377-383 EDRSPRICE MF-$1.00 HC-$27.45 Plus Postage. DESCRIPTORS *Educational Programs; Environmental Education; *InetrUctional,Materiaist Laboratory Equipment; *Laboratoti Techniguee-;*Pollution; 'Post Secondary EduOatioil Skill Development; *Water Pollution. Control IDENTIFIERS *Waste Water Treatment ABSTRACT This isoneof several shortter -courses--developed oassistinthetraining: -Ofwaste Water -treatmentplantoperational ersonnel in thetests, Meesureeente,_andreport preparation required Or coMpliancewiththeir_ NPDES_Permita. The _Student. Reference Manual re___Vea:--by for laboritory applicatida of Ment---OPerating-protedUres' foreffluent monitoring-.Eadi lesson i_specifiC objectifre, description of the'analySiS4: and the of the proCadate. =Parameters of this course -rincInde phOSPhOrtie, Chemical Oxygen Demand, Kjeldahl 'reten,Oil, 'and= Greeit.. (CS) sue_ ******** *6666******* ***10 **** *******_**** )ot4sents_aa4tiied_byERIC ,,inc many inicing nn materials-iot avail_able -Othersources._ERIC 1, 1_Orert,iitort * :oobtain copy_iiailft§)e.teteithglese, _ifeat'of ,"argfial* rePrOdi4ibilityFie Often, encountered end,_thiss AffeCte: the quality * the, iitarafiche- .and:hattOopy--,, - '', ieprogingf-44-**_iiikee',' 0014-ley-,,. *- _*liii-fillaq. 'Docuilent:Repo4,0tioil $_erviCe_0,044.:,-spas Wheat- * _.,i1.0,-onei-hie for the Oakity of--doCuitent.:ReproductiOnt * _supplied-by- bit' 'i:te. tie Willi- that can _,fia- ;Rita froa_ the Iitiginai. * ****4*************************************4.************************** EP 430/1-76406 U S DEPARTMENT OF MEALTM, EDUCATION A WELFARE NATIONAL INSTITUTE OF EDUCATION THIS DOCUMENT HAS BEEN REPRO. DUCEO EXACTLY AS RECEIVED FROM THE PERSON OR ORGANIZATION ORIGIN- ATING IT POINTS OF VIEW OR OPINIONS STATED DO NOT NECESSARILY REPRE SENT OFFICIAL NATIONAL NSTITUTE OF EDUCATION POSITION OP POLICY 'PERMISSION TO REPRODUCE THIS MATERIAL HAS BEEN GRANTED BY Bernardijkrp TO TIIE EDUCA 7 ION L RESOURCES INFORMATION CENTER IERICI AND 111111114111111 USERS OF it* ERIC 3YS FEM STUDENT REFERENCE MANUAL 37-EicrV1kaNickEN TA L -PROTEC 110 NA-GLENCY_ PFICE OF WATER PROGRAM OPERATIONS %.) 2 s , : EPA-430/1-76-006 June 1976 EFFLUENTMONITORING PROCEDURES:NUTRIENTS This course is designed for the treatment plantoperi-tor:or, technician who,isrequireCto-MonitCr effluent discharges under-a National Pollutant Discharge Elimination System (NPDES) _Perm% and who has.had,little or-no previous experience in 0 wastewater analysis. fht:COurse includet:protedurOt for MeasuilhOotallihosphorus (as P), theMical-0XYgen.DeMand,Aieldahl-(Total)-.Nitrogen, ,Ammonia (as N) ofKjeldahl N and M,ionia NNitrate-Nitrite (as II), Nitrite (as N), Nitrate (as Oib-y,differendi.nfAitfate-Aitite=M,andliittteltiind Oil and-Grease, Thecoutite=alto'inCluAet-fieddedures!10related tkIlls=,usinvalpictoolopmetOiand;Orpparing'vCilibration, , : During the course, thestudint.4111.,,petfcimran-40Proved analYtical-prOdedure for each: Of-t*me-aiiW.eimnts. At'the conclusion, he will be.giVen-a-certifititte-Verifiing,which, .measurements he perfOilmed in a satisfactory manner. U.S. ENVIRONMENTAL PROTECTION AGENCY Office of Water Program Operations TRAINING PROGRAM 3 DISCLAIMER Reference to commercial productsOrade names, or manufacturers is for purposes of example and illustration.\ Such references do not constitute endorsement by the Office of Water Program Operations, U.S. Environmental Protection Agency. CONTENTS Analytical Procedures Outline Number Use of a Spectrophotometer 1 Preparation of.Calibration Graphs 2 Determination of Total Phosphorus (as P) or of 3 Orthophosphate (as P), Single Reagent Method Determination of Chemical Oxygen Dethane 4 Determination of Total ljeldahl Nitrogen 5 Nitrogen, AmmoniOetermination, 6 Determination of Nitrate-Nitrite Nitrogen and of 7 Nitrate Nitrogen, CadmiumReduction Method Determination of Oil andiGrease 8 Other A3proved Analytical Procedures Determination of Ammonia by an Ammonia Selective 9 Ion Electrode - A PROTOTYPE FOR DEyELOPMENT,OF ROUTINE OPERATIONAL PROCEDURES for the cb USE OF A SPECTKOPHOT METER as applied in WASTEWATER TREATMENT FACILITIES andin the MONITORING OFEFFLUENT WASTEWATERS National Training Center __- Municipal Operations and Training Division Office of Water Program Operations U.S. Environmell Protection Agency EFFLUENT MONITORING PROCEDURE: Use of a Spectrophotometer This operational procedurewas developed by: i.< NAME Charles R. Feldmann ADDRESS EPA-WPO-National Training *ter, Cincinnati, OF. 45268 POSITIONChemist - Instructors EDUCATION AND TECHNICAL BACKGROUND 4v B.S. - Chemistry M.S. - Chemistry 1-1/2 years Industrial Chemist , 4 years, college Chemistry Instructor 1-1/2 years DHEW - Air Pollution Program, Chemist 4-1/2 years DI - EPA, Chemist-Instructor "Page No. 1-3 EFFLUENT MONITORING PROCEDURE: Use of a Spectrophotometer 1. Analysis Objectives: The user of the attached effluent monitoring procedure will learn how to use the Bausch and Lomb Spectftnic 20 Spectrophotometer for making colorimetric measurements. _2. BriefDescription'of Analysis: In-the-field_Of_water pollution_analnia, manyLdeterMinationtIam____ based on measurinn the intensity of color at a patticular wavelength. In general, color is formed in the sample by some sort of preliminary treatment such as distillation or digestion, and then adding.a color developing reagent. The intensity of the color formed is related-to the amount of material (such as phosphorus) in the sample. As part. of the analysis, col& is also-developed-in a series of-standards; in each of the standards is a known amount of the material (such as phosphorus) of interest. A calibration curve is made using the color intensities of the individual-standards and the-corresponding amounts of material present.The amount of material present in the sample is determined using the calibration curve. A Bausch and Lomb Spectronic 20 Spectrophotometer is an instrument used to measure the color intensities of the standards and sample. The word absorbance is associated with the words color intensity; i.e., a sample or standard which has a low color intensity will also have a low absorbance. Sourceof Procedure: Spectronic 20 Spectrophotometer Operating Manual, 'Bausch & Lomb, Rochester, New York 14602 PRRIOn of a particular brand name does not constitute endorsement by the U.S. Environmental Protection Agency ti ,"a EFFLUENT MONITORING PROCEDURE: Use of a Spectrophotometer General Description of Equipment Used in theProcess A. Capital 1. One Bausch and Lomb Spectronic 20 Spectrophotometer 2. One manufacturer's manual for the spectrophotometer 3. Still,or other source of distilled water 4. Hotplate 5. One spectrophotometer cell - A set of cells-may be, used only if tht7tills are optically matched. One cell would be used for each solution. B. Reusable 1. Brash--(for cleaning- spectrophotometer cell) 2. Laboratory apron 3. Safety glasses 4. One pen or pencil 5. Notebook or-data sheet (see page 1-23) for recording data 6. Brush (for dusting spectrophotometer) 7. One 2 liter beaker 8. One 250 ml beaker 9. One glass stirring rod 10. One 2 liter glass stoppered bottle 11. One visible phototube (Bausch and Lomb catalog number 33-29-71) 12. One infrared phototube (Bausch and Ldmb catalog number 33-29-72) 13. One infrared filter (Bausch and Lomb catalog number 33- 29 -18) 14. Ten soft tissues (for wiping the cells) 15. One plastic squeeze distifled water bottle 16. Sink or 1 liter container for rinsing solutions 17. One 1 cm cell (tc fit the Spectronic 20) C. Consumable 1. Soap 2. Sodium dichromate, Na2Cr207 3. Concentrated sulfuric acid, d2SO4 Items A4, B7 through B10,and Cl through"C3 are for cleaning the spectrophotometer cell. z-, === = ff,,== Page No. 1-6 c EFFLUENT MONITORING PROCEDURE:, Use of a Spectrophotometer 9 SCALE PILOT LIGHT WAVELENGTH CONTROL SAMPLE HOLDER WAVELENGTH COVER SCALE SAMPLE COMPARTMENT LIGHT CONTROL POWER SWITCH/ZERO CONTROL 10 FIGURE 1 I soh4,7,1''14 41, c / / 0 'A O uf , 4.r4/. 4,1,A441 `"r-'2..= L "r-f EFFLUENT MONITORING PROCEDURE: Use of a Spectrophotometer 4* ra = BOTTOM OF SPECTRONIC 20 FIGURE 4 16 Page No1-9 __ _ _ 1:14 \ EFFLUENT MONITORING PROCEDURE: Use of a Spectrophotometer BOTTOM OF SPECTRONIC 20 19 FIGURE .5 - - EFFLUENT MONITORING PROCEDURE:.Use of:a Spectrophoto6eter c3) FILTER FILTER HOLDER. BOTTOWOF 20 4 'r' R-FIGURE6 '171 21 Page No. 11i. s t EFFLUENT MONITORING PROCEDURE:Use of a Spectrophotometer Page No. 1-12 'TRAINING OPERATING-_-PROCEDURES STEP SEQUENCE -INFORMATION/OPERATING GOALS/SPECIFICATIONS GUIDE NOTES A. Equipment Preparation -1. Cell cleaning 1. Clean the Bausch:& Lomb la. For the rest of this,effluent monitoring pro- . Spectron-ic-20-Spectro,----_cedure-the-abbretriatriorpes-21V-w41-1-be-tisech photometer test tube(cell. 2. Spec 20 cleaning 1. Clean the Spec 20. la. It should be free of dust, dirt, and spilled chemicals. lb. The Spec 20 should be stored in an area where there is.no danger that chemicals will, be spilled on it. lc. The plastic cover sUpplied with the Spec 20 should be covering the instrument whenever it is not in use. 2.-If the power cord is plugged into a Wall, outletremove it. Phototube 1. Check whether the proper la. See section C for 4nstructions on changing the phgtotub is in place. phototube
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