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Amperometric Titration Theory

Amperometric Titration Theory
Page 150

50081_Titration.fm

addition to adsorption, iodine can react with organic matter, forming carbon-iodine
bonds. This is one reason for the traditional preference of the back titration methods for
total chlorine in sewage treatment plant effluents.

Figure 3

Titration Curves Using Thiosulfate vs. PAO Titrants

a) Thiosulfate as Titrant

b) PAO as Titrant

Current (µAmp)

Volume Titrant (mL)

Summary of Contents for AutoCAT 9000

Page 2: ...50081_TTL fm...

Page 3: ...e Sensor 18 2 2 6 Installing the Electrode 19 2 2 7 Power Connection 19 2 2 8 Serial Printer and PC Connections 20 Operation 21 Section 3 Basic Operation 23 3 1 Instrument Display and Keypad 23 3 2 Au...

Page 4: ...cate of Analysis for Hach Reagents 41 Section 5 Collecting and Accessing Data 43 5 1 Using the AutoCAT 9000 for Amperometric Methods 43 5 2 AutoCAT Titration 43 5 2 1 Data Collection 43 5 2 1 1 Curren...

Page 5: ...tric Forward Titration 105 Sulfite Amperometric Back Titration 111 Total Oxidants Quick Two Step Amperometric Titration 119 Chlorite Quick Two Step Amperometric Titration 127 Manual Endpoint Determina...

Page 6: ...1 3 Errors Common to Total Chlorine Determinations 149 1 4 Shift of Endpoints Due to Sample Iodine Demand 151 1 5 Order of Reagent Addition 151 Appendix B Printer Installation and Setup 153 Appendix C...

Page 7: ...will use the signal word Danger Caution Note corresponding to the greatest hazard DANGER Indicates a potentially or imminently hazardous situation which if not avoided could result in death or serious...

Page 8: ...Page 6 50081_Safety fm...

Page 9: ...or 80 columns Detailed or condensed Graphic or no graphic Results QC check on results with visual warning Statistical calculations Units All standard units for samples results Titration Curve Up to 2...

Page 10: ...d Language Options English and Spanish General Specifications Casing Splashproof ABS plastic Graphic 128 x 128 dot LCD and alphanumeric keypad Dimensions H x W x D 380 x 230 x 450 mm 15 x 9 x 17 inch...

Page 11: ...ollowing the instructions in Section 2 on page 13 3 Review Basic Operation on page 23 to familiarize yourself with the user interface and the keypad navigation and command keys 4 Set the software para...

Page 12: ...00 1 Metal electrode dual platinum wire BNC plug 6 50082 10 1 Burette stand 5 mL red cover 7 50082 50 1 Bottle stopper for 500 mL and 1000 mL plastic titrant bottles 8 50085 00 1 Magnetic stir bar 9 5...

Page 13: ...rvisor allows users to edit titration and analysis parameters to fit specific needs A Supervisor level user can also assign a password to protect the data and customized settings from inadvertent chan...

Page 14: ...Page 12 50081_Introduction fm...

Page 15: ...operation The relative humidity should be between 20 and 80 do not allow moisture to condense on the instrument Note Retain the original packaging material Instruments returned for service should be s...

Page 16: ...Anti diffusion Tip 13 Electrode BNC Connector 4 Temperature Sensor 14 Temperature Sensor CINCH Connector 5 Dual Platinum Electrode 15 Bottle Stopper for Plastic Titrant Bottle 6 Support Rod for Electr...

Page 17: ...n 4 must be completed before any analyses can be performed 2 2 1 Attaching the Titrant Bottle Holder 2 2 2 Connecting the Electrode Head and Accessories 1 Slide the titrant bottle holder into the moun...

Page 18: ...op the supplied magnetic stir bar into the titration beaker and place the beaker on the titration platform Note The provided stir bar has been specifically selected for use with the AutoCAT 9000 A dif...

Page 19: ...p into a small hole on the electrode head Turn the locking collar turn clockwise to lock it in place Note Make sure that the tubing is connected to the correct point on the rotating valve indicated by...

Page 20: ...he burette stand and lock the burette into position 5 Thread the connectors of the remaining section of tubing into the top of the burette and into the corresponding receptacle on the rotating valve N...

Page 21: ...age 23 to enter basic user information in preparation for performing analyses to comply with Good Laboratory Practices Refer to Section 4 on page 33 for the software setup required prior to performing...

Page 22: ...0 Workstation and the 9 pin D connector used for the serial port found on most personal computers If your computer has a 25 pin D connector use a 9 pin to 25 pin adapter available at many computer sup...

Page 23: ...reactivos puede ser peligrosa Revise las fichas de seguridad de materiales y familiar cese con los procedimientos de seguridad antes de manipular productos qu micos GEFAHR Das Arbeiten mit chemischen...

Page 24: ...Page 22 50081_OperationStop fm...

Page 25: ...key until the desired character is displayed then release the key Press and hold to scroll from uppercase to lowercase letters Delete the character displayed above the screen cursor by pressing the D...

Page 26: ...isplayed menus To select highlight the desired item and press the CHECK MARK to confirm Selections can also be made by pressing the corresponding number 1 6 if available to the right of the selection...

Page 27: ...ins all of the adjustable calibration parameters Supervisors can choose to have the titrant concentration input manually or determined through embedded calibration GLP Archives provides access to the...

Page 28: ...leaning and conditioning procedure adjustable parameters direct measurement and electrode temperature sensor functions Title bar displays Electrodes Method indicates the method currently selected Conn...

Page 29: ...e CHECK MARK to record this code All future access to the Setup menu will require the input of this case sensitive code Note To establish the Supervisor code see Accessing Supervisor Mode on page 33 3...

Page 30: ...3 5 1 Select Optional PC Keyboard Select an optional external keyboard to connect to the 6 pin PS 2 receptacle located on the right hand side bottom edge of the instrument 1 Scroll to highlight PC Key...

Page 31: ...c 1 Highlight Beep 2 Press the CHECK MARK to confirm the selection 3 Press the UP or DOWN key 4 Press the CHECK MARK to validate and return to the Configuration Menu 3 3 9 Rules for Routine Access Use...

Page 32: ...to Factory Settings 2 Press the CHECK MARK or Press 1 to confirm the selection and return to the Setup menu 3 3 12 Exit This selection allows the user to exit the Setup menu and return to the main me...

Page 33: ...o change the Sub ID in Routine Mode select Display Method on the Main Menu screen In Supervisor Mode select Method Library on the Main Menu screen 2 From this screen both the Method and the Sub ID can...

Page 34: ...Basic Operation Basic Operation Page 32 50081_Operation fm...

Page 35: ...the titrant bottle or switching to a method requiring a different titrant Use the following procedures to set up the AutoCAT 9000 titrator software 1 Turn the instrument ON or if already in operation...

Page 36: ...ftware Setup for Electrode and Temperature Sensor Installation 1 From the Methods menu see How to Access the Menus on page 24 use the RIGHT and LEFT keys to tab to the Electrodes menu 2 Press 1 to sel...

Page 37: ...lectrode or 50087 00 temperature sensor 4 Press the CHECK MARK to validate 5 Press 1 to confirm 6 Remove the probe 7 Install the replacement probe 8 Input the serial number of the replacement probe 9...

Page 38: ...install position 5 Highlight Burette Volume Press the CHECK MARK to input or change 6 Highlight the desired burette Note The default software setting is 5 mL Press the CHECK MARK to validate 7 Highlig...

Page 39: ...Number and press the CHECK MARK to confirm 6 Input the replacement burette serial number and press the CHECK MARK to validate 7 Press 1 to confirm 8 Remove the burette and press the CHECK MARK to con...

Page 40: ...bottle Press the CHECK MARK to validate 5 Highlight Expiration Press the CHECK MARK to input or change 6 Use the alphanumeric keypad to input the month and year of the titrant expiration date located...

Page 41: ...ate for the required titrant press the CHECK MARK to validate Note If replacing depleted titrant the embedded procedure will automatically begin here 12 Press 1 to confirm 13 Ensure that the correct c...

Page 42: ...64mN in this example and press the CHECK MARK to validate Note The AutoCAT 9000 automatically stores installed titrants for later concentration updates or calibrations 4 Press 1 to select Enter Titra...

Page 43: ...equested 9 Use the alphanumeric keypad and navigation keys to input or change the titrant concentration Press the CHECK MARK to validate Note Product lots differ slightly in concentration See Section...

Page 44: ...Page 42 50081_SoftwareSetup fm...

Page 45: ...on Each category is described in the sections below 5 2 1 Data Collection The AutoCAT displays the titration curve current A vs titrant volume mL graphically in real time as it dispenses titrant and m...

Page 46: ...a 0 01 mL volume increment and a 1 00 mL predose In this case 1 00 mL of titrant is added prior to data collection and the final 0 50 mL is delivered during data collection The same number of points w...

Page 47: ...ll proceed directly from data collection to AEPD without the usual intervening zoom window Following AEPD the results are displayed and the user can accept the results or reprocess the data using eith...

Page 48: ...and analyzed by the instrument Using the dilution information the AutoCAT can automatically convert the concentration measured for the diluted sample into the concentration of the undiluted sample 5 2...

Page 49: ...standard deviation of the mean SMean is estimated using the following formula Where Rmax is the maximum value obtained from the replicate measurements Rmin is the minimum value obtained from the repli...

Page 50: ...e most recent result is always assigned to position 1 in the archive For example if the user performs a series of 10 separate chlorine analyses then the results for the most recent analysis will be st...

Page 51: ...Calibration Procedures 50081_CalibrationStopper fm Page 49 Section 6 Calibration Procedures...

Page 52: ...Page 50 50081_CalibrationStopper fm...

Page 53: ...n for all the results Each test is given a different number all of which are listed under the same Sample ID When starting a new sample a new ID is assigned The AutoCAT can accommodate any sample size...

Page 54: ...s been chosen for demonstration purposes only 4 Press 1 to select Edit titrant 5 Press the CHECK MARK to change the titrant concentration input mode 6 Highlight Calibrate Press the CHECK MARK to valid...

Page 55: ...ECK MARK to change the titrant lot number or proceed to step 13 13 Highlight Volume for Test 1 Press the CHECK MARK to change the calibration volume or proceed to step 14 Note The default volume for t...

Page 56: ...ype of end point determination Press the CHECK MARK for Automatic Proceed to step 22 or press DEL for Manual and proceed to step 20 20 Select two line segments one on each side of the titration end po...

Page 57: ...d method as defined If the concentration of the Iodine Standard Solution is significantly less than 0 0282 N it may be necessary to reduce the predose volume prior to titration Titrate to an amperomet...

Page 58: ...andard Solution 0 0282 N varies 1000 mL 23333 53 Phenylarsine Oxide PAO Titrant 0 00564 N varies 1000 mL 1999 53 Potassium Iodide SwifTest refill 0 10 g 50 g 1077 60 Sodium Thiosulfate Standard Soluti...

Page 59: ...ation for all the results Each test is given a different number all of which are listed under the same Sample ID When starting a new sample a new ID is assigned Rinse the electrode temperature probe a...

Page 60: ...ate 4 Press 1 to select Edit Titrant 5 Press the CHECK MARK to change the titrant concentration input mode 6 Highlight Calibrate Press the CHECK MARK to validate 7 The titrant concentration input mode...

Page 61: ...ged to reflect standardization or the Certificate of Analysis value for a new bottle 12 Highlight Lot No Press the CHECK MARK to change the titrant lot number or proceed to step 13 13 Highlight Volume...

Page 62: ...ss the CHECK MARK for Automatic and proceed to step 22 or press DEL for Manual and proceed to step 20 20 Select two line segments one on each side of the titration end point by positioning the cursors...

Page 63: ...rm a back titration to an amperometric end point 25 Press 1 to select New Test to run a replicate calibration Proceed to step 26 or select Press 2 to select End Analysis and store the titrant calibrat...

Page 64: ...l toll free Required Reagents Description Qty required per test Unit Cat No Arsenite Standard Solution 0 1000 N 1 00 mL 100 mL 28435 42 Sodium Bicarbonate 4 g 454 g 776 01 Iodine Standard Solution 0 0...

Page 65: ...e sample containers thoroughly with deionized distilled water after use to reduce the need for pretreatment 7 3 Handling Use separate dedicated sample containers that are labelled for free and total c...

Page 66: ...Page 64 50081_Sampling fm...

Page 67: ...Titration Procedures 50081_ProcedureStopper fm Page 65 Section 8 Titration Procedures...

Page 68: ...Page 66 50081_ProcedureStopper fm...

Page 69: ...unning a new test and a new sample Each test is a replicate run of the current or previous sample analysis The AutoCAT 9000 automatically tracks the results of a series of tests and automatically calc...

Page 70: ...ator effluent sample with a pipet and transfer to a 250 mL beaker containing the magnetic bar Note All containers must be pretreated for chlorine demand see Container Pretreatment on page 63 5 Dilute...

Page 71: ...10 Add 1 dose of pH 7 0 Phosphate Buffer Press the CHECK MARK to confirm Note Phosphate buffer is added to adjust the sample pH The precise amount added is not crucial for the accuracy or precision o...

Page 72: ...is method Sub ID Note These Sub ID parameters can be edited here as run time settings or from the Main Menu as described in Section 3 5 Note This step will be skipped if auto scaling software is enabl...

Page 73: ...and end of each segment Press the CHECK MARK to confirm changes or press DEL to return to the Zoom window Note For more information on manual EP determination see page 135 19 Press the CHECK MARK to a...

Page 74: ...refully place onto the AutoCAT stirrer platform Lower the electrode head onto the beaker rim Press the CHECK MARK to confirm 4 The analysis parameters that have been stored for the current Sub ID may...

Page 75: ...pe of end point determination Press DEL for Manual Note Automatic determination attempts to identify linear segments without user input and is not recommended for this method 8 Using the navigation ke...

Page 76: ...ugh the sample Press the CHECK MARK to continue 5 Purge nitrogen gas through the sample for 15 minutes When the timer beeps transfer the purged sample into a 250 mL beaker Add the magnetic stir bar No...

Page 77: ...gs or from the Main Menu as described in Section 3 5 Note This step will be skipped if autoscaling software is enabled 10 The Start Timer will begin allowing the electrode to stabilize before data is...

Page 78: ...nt by positioning the cursors at the beginning and end of each segment indicated by arrows Press the CHECK MARK to confirm changes or press DEL to return to the previous window Note For more informati...

Page 79: ...lace onto the AutoCAT titration platform Lower the electrode head onto the beaker rim Press the CHECK MARK to confirm 4 The analysis parameters that have been stored for the current Sub ID may be edit...

Page 80: ...ioning the cursors at the beginning and end of each segment Press the CHECK MARK to confirm changes or press DEL to return to the previous window Note For more information on manual EP determination s...

Page 81: ...and 4 with nitrogen while performing Titrations 1 and 2 Another measurement used to gauge ClO2 generator production is the ratio of Titration 2 to Titration 1 results This provides an estimate of any...

Page 82: ...g 100 g 167 26H Sodium Thiosulfate Solution 0 10 N varies 1000 mL 323 53 Required Apparatus Description Qty required per test Unit Cat No Beaker Glass 250 mL 1 each 500 46H Gas Washing Bottle 1 each 2...

Page 83: ...darken A distinction is drawn between running a new test and a new sample Each test is a replicate run of the current or previous sample analysis The AutoCAT 9000 automatically tracks the results of...

Page 84: ...transfer to a 250 mL beaker with the specified magnetic stir bar All containers must be pretreated for chlorine demand see Container Pretreatment on page 63 5 Place the sample onto the AutoCAT 9000 st...

Page 85: ...ine and press the CHECK MARK to change one of the analysis parameters or press 1 to confirm Note Any changes made will become the new default parameters for this method Sub ID Note These Sub ID parame...

Page 86: ...or more information on manual EP determination see page 135 18 Press the CHECK MARK to accept the analysis and proceed to Titr 2 or press DEL to return to the previous window to adjust the linear segm...

Page 87: ...AutoCAT stirrer platform Lower the electrode head onto the beaker rim Press the CHECK MARK to confirm 4 The analysis parameters that have been stored for the current Sub ID may be edited at this time...

Page 88: ...Manual Automatic determination attempts to identify linear segments without user input and is not recommended for this method 8 Using the navigation keys select two line segments one on each side of t...

Page 89: ...ple for 15 minutes When the timer beeps transfer the purged sample into a 250 mL beaker Add the specified magnetic stir bar Note If the nitrogen purge has already been performed press DEL to skip this...

Page 90: ...Menu as described in Section 3 5 Note This step will be skipped if autoscaling software is enabled 10 The Start Timer will begin to allow the electrode to stabilize before data is collected After the...

Page 91: ...d end of each segment indicated by arrows Press the CHECK MARK to confirm changes or press DEL to return to the previous window Note For more information on manual EP determination see page 135 14 Pre...

Page 92: ...ode head onto the beaker rim Press the CHECK MARK to confirm 4 The analysis parameters that have been stored for the current Sub ID may be edited at this time Highlight the appropriate line and press...

Page 93: ...line segments one on each side of the titration end point by positioning the cursors at the beginning and end of each segment Press the CHECK MARK to confirm changes or press DEL to return to the pre...

Page 94: ...used for Titrations 3 and 4 with nitrogen while performing titrations 1 and 2 Required Reagents Description Qty required per test Unit Cat No Phenylarsine Oxide PAO Titrant 0 00564 N varies 1000 mL 19...

Page 95: ...AT automatically tracks the results of a series of tests and automatically calculates the mean and standard deviation for all the results Each test is given a different number all of which are listed...

Page 96: ...sample beaker Note Use only the provided stir bar to minimize loss of chlorine 5 Place the sample onto the AutoCAT 9000 stirrer platform 6 Verify User Press the CHECK MARK to enter a new user or pres...

Page 97: ...ectrode head onto the beaker rim Press the CHECK MARK to confirm 12 The analysis parameters that have been stored for the current Sub ID may be edited at this time Verify Increment from Table 1 Genera...

Page 98: ...two line segments one on each side of the titration end point at the beginning and end of each segment Press the CHECK MARK to confirm changes or press DEL to return to the previous window Note For m...

Page 99: ...0 0600 1 50 2 00 0 0900 2 000 0 1500 Note These recommendations apply to Free Chlorine titrations correspond to data collection times typically under 5 minutes and provide adequate data points on bot...

Page 100: ...on This procedure permits determination of the Free Chlorine concentration in a water sample Free chlorine corresponds to that portion of chlorine existing either as elemental chlorine Cl2 hypochlorou...

Page 101: ...ation for all the results Each test is given a different number all of which are listed under the same Sample ID When a new sample starts a new ID is assigned The AutoCAT 9000 can accommodate any samp...

Page 102: ...orine The recommended amount of 1 00 mL is sufficient for about 1 mg L of total chlorine For higher concentrations a larger amount of PAO should be added Note For total chlorine concentrations below 0...

Page 103: ...hanges made will become the new default parameters for this method Sub ID Note These Sub ID parameters can be edited here as run time settings or from the Main Menu as described in Section 3 5 Note Th...

Page 104: ...he data 19 The AutoCAT 9000 will run the analysis based on the automatic selection of linear segments Note The automated analysis requires approximately 1 minute to complete 20 Press the CHECK MARK to...

Page 105: ...boratory techniques throughout the procedure Consult the Material Safety Data Sheet MSDS for specific reagent s information Table 1 Recommended Volume Increment Settings for Total Chlorine Back Estima...

Page 106: ...ation is derived from the difference in the amount of reductant originally added to the sample and the amount remaining prior to titration The chemical reactions are PhAsO PAO Cl2 2H2O PhAsO OH 2 2Cl...

Page 107: ...sts and automatically calculates the mean and standard deviation for all the results Each test is given a different number all of which are listed under the same Sample ID When starting a new sample a...

Page 108: ...to minimize loss of chlorine or iodine 5 Place the sample onto the AutoCAT stirrer platform 6 Highlight User and verify the user ID Press 1 to confirm and accept the displayed ID To change the user ID...

Page 109: ...HECK MARK to change one of the analysis parameters or press 1 to confirm Note Any changes made will become the new default parameters for this method Sub ID Note These Sub ID parameters can be edited...

Page 110: ...he linear segments and reanalyze the data 19 The AutoCAT will run the analysis based on the automatic selection of linear segments Note The automated analysis requires approximately 1 minute to comple...

Page 111: ...tion end point for proper analysis Adjusting the volume increment will proportionately adjust the data collection times and number of data points collected For example doubling the volume increment wi...

Page 112: ...solution including free elemental chlorine Cl2 hypochlorous acid HOCl hypochlorite OCl ion and chloramines NH2Cl NHCl2 etc among other species In the procedure an excess of potassium iodide is added t...

Page 113: ...is assigned The AutoCAT 9000 can accommodate any sample size Standard Methods recommends a default volume of 200 mL The volume can be adjusted to expand the test range The AutoCAT 9000 calculates the...

Page 114: ...e and swirl to mix Place the sample onto the AutoCAT 9000 stirrer platform Note Depending on sulfite concentration the titration may yield higher results for sulfite due to iodine demand See Table 1 o...

Page 115: ...st 1 Press 1 to confirm Press the CHECK MARK to enter a new sample volume 11 Add 1 SwifTest dispensation 0 1 g of potassium iodide KI Press the CHECK MARK to confirm Note KI is added in excess The pre...

Page 116: ...e analysis parameters or press 1 to confirm Note Any changes made will become the new default parameters for this method Sub ID Note These Sub ID parameters can be edited here as run time settings or...

Page 117: ...l EP determination see page 135 20 Press the CHECK MARK to accept the analysis Proceed to step 22 or press DEL to return to the previous window Zoom Range Determination Adjust the linear segments and...

Page 118: ...se good safety practices and laboratory techniques throughout the procedure Consult the Material Safety Data Sheet MSDS for specific reagent s information Table 1 Recommended Iodine Spike Volume for S...

Page 119: ...or by titrating the sample matrix prior to sulfite or sulfur dioxide addition For best results chlorine should be eliminated from the sample by UV irradiation The resulting value from the titration is...

Page 120: ...or distributor serving you www hach com techhelp hach com In the U S A Outside the U S A On the Worldwide Web E mail toll free Optional Apparatus Digital Titrator each 16900 01 Delivery Tubes straight...

Page 121: ...essing the Methods menu and pressing 7 to lighten or 0 to darken A distinction is drawn between running a new Test and a new Sample Each Test is a replicate run of the current or previous sample analy...

Page 122: ...50 mL beaker with the specified magnetic stir bar All containers must be pretreated for chlorine demand see Container Pretreatment on page 63 5 Place the sample onto the AutoCAT 9000 stirrer platform...

Page 123: ...ARK to change one of the analysis parameters or press 1 to confirm Note Any changes made will become the new default parameters for this method Sub ID Note These Sub ID parameters can be edited here a...

Page 124: ...re information on manual EP determination see page 135 18 Press the CHECK MARK to accept the analysis and proceed to Titration 2 or press DEL to return to the previous window to adjust the linear segm...

Page 125: ...irrer platform Lower the electrode head onto the beaker rim Press the CHECK MARK to confirm 4 The analysis parameters that have been stored for the current Sub ID may be edited at this time Highlight...

Page 126: ...titration end point by positioning vertical lines cursors at the beginning and end of each segment Press the CHECK MARK to confirm changes or press DEL to return to the Zoom window Note For more infor...

Page 127: ...oxide has a short residence time in most drinking water the total oxidant result mainly consists of the chlorite ion This method can therefore be employed as an acceptable surrogate operational contro...

Page 128: ...talOxidants fm HACH COMPANY WORLD HEADQUARTERS Telephone 970 669 3050 FAX 970 669 2932 FORTECHNICAL ASSISTANCE PRICE INFORMATION AND ORDERING Call 800 227 4224 Contact the HACH office or distributor s...

Page 129: ...atically tracks the results of a series of tests and automatically calculates the mean and standard deviation for all the results Each test is given a different number all of which are listed under th...

Page 130: ...user or press 1 to confirm Note This screen will be skipped if the User ID is disabled See Setting a User ID on page 27 5 Highlight Sample ID Press the CHECK MARK to enter a new sample ID or proceed t...

Page 131: ...not crucial for the accuracy or precision of the analysis 13 The timer will start This allows a short period of time for the reagents to mix before starting the titration 14 Lower the electrode head o...

Page 132: ...t two line segments one on each side of the titration end point by positioning vertical lines cursors at the beginning and end of each segment Press the CHECK MARK to confirm changes or press DEL to r...

Page 133: ...place onto the AutoCAT stirrer platform Lower the electrode head onto the beaker rim Press the CHECK MARK to confirm 4 The analysis parameters that have been stored for the current Sub ID may be edit...

Page 134: ...titration end point by positioning vertical lines cursors at the beginning and end of each segment Press the CHECK MARK to confirm changes or press DEL to return to the Zoom window Note For more info...

Page 135: ...iption Qty required per test Unit Cat No Phenylarsine Oxide PAO Titrant 0 00564 N varies 1000 mL 1999 53 Hydrochloric Acid Standard Solution 2 5 N 4 mL 100 mL 1418 32 Phosphate Buffer pH 7 with droppe...

Page 136: ...orite fm HACH COMPANY WORLD HEADQUARTERS Telephone 970 669 3050 FAX 970 669 2932 FORTECHNICAL ASSISTANCE PRICE INFORMATION AND ORDERING Call 800 227 4224 Contact the HACH office or distributor serving...

Page 137: ...these linear segment selections as large as possible in order to obtain the most accurate endpoint determination Note The AutoCAT will draw a best fit regression line through the data points between t...

Page 138: ...Page 136 50081_ManualEndpoint fm...

Page 139: ...L to view the titration curve 2 Press the CHECK MARK to accept BDL as the result 3 In this example Below Detectable Limit is stored with Test 1 for Sample 1 1 Press DEL to view the titration curve Exa...

Page 140: ...Page 138 50081_BDL fm...

Page 141: ...ual platinum electrodes DPE as shown in the procedure below to make them more responsive The frequency of use and the type of samples analyzed will dictate the frequency for electrode cleaning and con...

Page 142: ...f the same type and rating Time delay 1 A 250 V 5 Replace the fuse holder Ensure that it is oriented correctly and that the retaining tabs are engaged Note Replacement of the circuit board mounted sec...

Page 143: ...ct Titrants Burette functions Flush Lightly tap the tubing while the instrument is flushing to purge air bubbles from the system Titrant leaks Titrant leaks can also occur when the burette seals becom...

Page 144: ...o scaling is often successful on a second attempt Turn Auto scaling off set the current range and volume increment manually and re run the analysis Automated end point Determination The fitted end poi...

Page 145: ...uit Use only a dedicated electrical circuit for the AutoCAT 9000 Erratic operation The AutoCAT 9000 is sensitive to static electricity Surround the AutoCAT 9000 with a Faraday cage Move the instrument...

Page 146: ...ect the problem complete the following sequence 1 Verify that the desired method has been selected 2 Verify that the burette has been properly installed in the software 3 Verify that the correct titra...

Page 147: ...passing through a solution under an imposed potential when electrons are transferred from the reductant to the oxidant Current stops flowing if either the oxidant or reductant is consumed or is otherw...

Page 148: ...Use a conversion factor to convert normality to more tangible units such as mg L or ppm The precise conversion factor depends on the particular analyte and concentration units involved For example one...

Page 149: ...erference from color turbidity iron manganese or nitrite nitrogen However several of these factors may affect the determination of chlorine species when using amperometric methods This is a brief revi...

Page 150: ...amperometric methods for total chlorine Standard Methods section 4500 Cl D 1 b states that nitrites do not interfere in the forward titration methods Section 4500 Cl C 1 b the Iodometric Method II sta...

Page 151: ...I reagent volatilization of elemental iodine iodine or iodate IO3 contamination in the iodide reagent consumption of triiodide by sample components Potassium iodide reagent may be oxidized by the fol...

Page 152: ...anic matter forming carbon iodine bonds This is one reason for the traditional preference of the back titration methods for total chlorine in sewage treatment plant effluents Figure 3 Titration Curves...

Page 153: ...of the available methods The literature concerning the amperometric determination of total chlorine in salt water is somewhat confusing Several studies indicate the order of reagent addition KI and bu...

Page 154: ...Page 152 50081_Titration fm...

Page 155: ...o the serial PC Printer port located on the back panel of the AutoCAT 9000 see Figure 3 on page 19 Plug one end of the printer power adapter into a 110 V ac outlet and the other end to the printer Not...

Page 156: ...iled is enabled the printout will include the titrant certificate number concentration and install date and the electrode used 10 Highlight Curve Press the CHECK MARK to change 11 Enable or Disable Cu...

Page 157: ...Printer Installation and Setup Printer Installation and Setup 50081_PrinterInstallation fm Page 155 Software Setup Sample Printout DETAIL CURVE AND LINE FIT...

Page 158: ...Page 156 50081_PrinterInstallation fm...

Page 159: ...ing for titrant stopcock to sample with anti diffusion tip see Figure 1 on page 13 item 2 50082 40 Electrode dual platinum see Figure 1 on page 13 item 5 50086 00 Magnetic stir bar see Figure 1 on pag...

Page 160: ...Page 158 50081_ReplacementParts fm...

Page 161: ...on of Water and Wastewater 2350B 2 Atmospheric Exposure To avoid oxidation and loss of chlorine low level chlorine standards must be prepared under a high purity inert gas headspace Nitrogen and argon...

Page 162: ...trator A certificate of analysis for the PAO titrant is also available for download from www hach com Additionally the calibration curves for colorimetric chlorine analyses that are programmed into Ha...

Page 163: ...t through an RS232 serial port pairing dispensed titrant volume with current output Endpoint determination and results calculation were performed on the instrument using the instrument s embedded endp...

Page 164: ...ce interval times the standard deviation For seven replicates the Student s t value at the 99 confidence interval is 3 143 The experimental conditions and apparatus for this series of experiments was...

Page 165: ...pable of measuring chlorine concentrations of up to 5 mg L Additionally the instrument will automatically correct for sample dilutions enabling determinations above this stated range An assessment of...

Page 166: ...from standard volumetric flasks in that they have a wide mouth which makes it easier to transfer samples quickly to the titration beaker without excessive chlorine loss The sample volume accuracy achi...

Page 167: ...ion of the KI in solution to iodine otherwise false positive results can be obtained which again can be significant sources of error in low g L determinations Factors that catalyze conversion of KI to...

Page 168: ...2 Mohm water 2 All apparatus must be PET Teflon or glass 3 Do not use amber glass 4 Pre treat all apparatus for chlorine demand 5 Thoroughly rinse all apparatus after pre treatment 6 Use ultra high pu...

Page 169: ...Company customer service is an important part of every product we make With that in mind we have compiled the following information for your convenience 50081_GeneralInfoStop fm Page 167 General Info...

Page 170: ...Page 168 50081_GeneralInfoStop fm...

Page 171: ...1000 4 3 Radiated RF Electro Magnetic Fields EN 61000 4 4 IEC 1000 4 4 Electrical Fast Transients Burst EN 61000 4 5 IEC 1000 4 5 Surge EN 61000 4 6 IEC 1000 4 6 Conducted Disturbances Induced by RF...

Page 172: ...ce pursuant to Part 15 of the FCC Rules These limits are designed to provide reasonable protection against harmful interference when the equipment is operated in a commercial environment This equipmen...

Page 173: ...nd E mail to intl hach com or contact In Canada Latin America Africa Asia Pacific Rim Telephone 970 669 3050 FAX 970 669 2932 In Europe the Middle East or Mediterranean Africa HACH Company c o Dr Brun...

Page 174: ...24 U S A only Telephone 515 232 2533 FAX 515 232 1276 In Canada Hach Sales Service Canada Ltd 1313 Border Street Unit 34 Winnipeg Manitoba R3H 0X4 800 665 7635 Canada only Telephone 204 632 5598 FAX 2...

Page 175: ...r or attempted repair not authorized by Hach Company any product not used in accordance with the instructions furnished by Hach Company freight charges to return merchandise to Hach Company freight ch...

Page 176: ......

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