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Hach AutoCAT 9000 Скачать руководство пользователя страница 45

Collecting and Accessing Data

50081_AutomatedTitration.fm

Page 43

Section 5

Collecting and Accessing Data

5.1 Using the AutoCAT 9000 for Amperometric Methods

The following analysis procedures, based on Standard Methods, are embedded directly
in the instrument software:

•

Forward titration for free chlorine

•

Forward titration for total chlorine

•

Back titration for total chlorine

•

Forward titration for chlorine dioxide

Hach sells pre-standardized titrants, prepared according to Standard Methods, for both
forward and back titrations. The 0.00564 N phenylarsine oxide titrant (Cat. No. 1999-53)
has a shelf life of >1 year in the unopened bottle. The unopened 0.0282 N Iodine
Standard Solution titrant (Cat. No. 23333-53) is stable for 6 to 12 months.

Periodically recalibrate the titrants after opening to ensure accuracy. Dispense reagents
directly from the product bottle to eliminate contamination from transferring them to
separate containers.

5.2 AutoCAT Titration

AutoCAT 9000 functions can be separated into three categories: (1) data collection,
(2) end point determination, and (3) calculation. Each category is described in the
sections below.

5.2.1 Data Collection

The AutoCAT displays the titration curve (current (µA) vs. titrant volume (mL))
graphically in real time, as it dispenses titrant and measures the current. After the
titration is complete, the user can choose between a fully automated or manual routine to
determine the end point. Following end point determination, the AutoCAT 9000
automatically calculates the analyte concentration.

The titration curve is constructed by plotting the measured current as a function of the
volume of titrant added. Several parameters, which must be set prior to data collection,
are available to control the data collection process. These parameters include the
(1) current range, (2) volume increment, (3) predose volume, and (4) Auto-scaling.

5.2.1.1 Current Range

Current Range allows the user to set the maximum current (in µA) expected for a
particular titration. The AutoCAT 9000 allows four possible settings (2 µA, 20 µA,
200 µA, and 1 mA) for the current range. The default setting (20 µA) setting is adequate
for most purposes. The 2 µA setting is recommended when analyzing samples with
concentration less than 0.600 mg/L Total Chlorine.

Note:

The 200-µA and 1-mA settings are available for experimental use, and are not

recommended for most titrations.

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Содержание AutoCAT 9000

Страница 1: ...50081 18 Chlorine Amperometric Titrator Hach Company 2002 2003 2007 All rights reserved Printed in the USA pks 4 07 3ed...

Страница 2: ...50081_TTL fm...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

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

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

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

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

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

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

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

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

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

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

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

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

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

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

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

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

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

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

Страница 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...

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

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

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

Страница 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...

Страница 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...

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

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

Страница 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...

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

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

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

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 176: ......

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