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Operating Instructions Part 1: Part 2: General Information Functional

1. 42 11 Meter Setup 43 11 1 Selecting the language 43 11 2 Setting the date time 44 TL3 GSC ceenucawweu eas aed ee nen 44 11 4 System info eee 45 12 Updating method data 46 13 RS 232 C interface 48 13 1 Principle course of the remote control 48 13 2 Command list 0 0 0 0 00 2 eee 48 13 3 Output format of measured values 49 13 4 Data transmission 00 00 ee ee 49 13 5 Pin assignment 0 00008 49 14 Maintenance 50 14 1 Changing the lamp 0 50 14 2 Actions to take if a cell is broken 50 15 Technical Data 51 16 What to do if 53 p 1 Overview 1 1 Description of the operating elements r an CSB 4650 7 Chemischer Sauerstoffbeds Meinberg 1500 mg CSB 414mm TT Zu So A e as Z WY Z UV cel 2 Anil robel sung Mischen m he moreaktor mind i in ein Reaktions K vette wird hei amp nitzen l kiWette geben am Verschlu anfassen Display Menu call Enter key Scroll key Recess for MemoChip Absorbance measure ment key Concentration measure ment key Notch for cell alignment Round cell shaft Storage space for anal ysis regulations short form Cover with integrated on off switch OOF O8OH
2. 44 11 Meter Setup Call up the system info menu item Sample display 45 12 Updating method data You will always find the latest method data for your photometer on the Internet A method update contains all new test sets and methods respectively Additionally minor modifications of already existing methods are transferred with it With a method update you receive all new methods and at the same time can easily and conveniently update all method data The software provided for downloading contains the program file and method data It can be downloaded from our homepage with a mouse click The files are packed in a self decompressing archive file exe or in a zip file zip and can be decompressed after the download Carry out the update as follows 46 To download and update the photometer method data via the built in RS232 interface you need the following PC Win 95 or higher with Internet connection PC cable available as an accessory An exe or zip file from the Internet contains the UpdateMethodData exe program file and 6 method data files pls6md xxx pls12md xxx plspekmd xxx nova30md xxx nova60md xxx nova400md xxx xxx version Switch on the photometer open the cover Switch on the PC Download from the Internet the software including the method data exe or zip and copy it into a separate directory or on a floppy disk Decompress the exe
3. Call up the reset submenu Confirm with Select the reset menu item Confirm with e An AQA reset is performed 26 8 Analytical Quality Assurance AQA 8 2 Photometer monitoring AQA1 8 2 1 Entering PhotoCheck standards A Spectroquant PhotoCheck is required to perform the photometer monitoring AQA1 At least 1 standard must be input We recom mend however to input all available standards Press to call up the setup menu Call up the meter setup submenu Call up the AQA functions submenu Input the password Call up the AQA standards submenu and the following display appears Call up the PhotoCheck submenu Select between input Input the theoretical value absorbance from the lot certificate of Spectroquant PhotoCheck output Print display theoretical values erase Erase theoretical values e The erase and output menu items only appear 2 after at least one standard has been input 27 8 Analytical Quality Assurance AQA Example 445 1 nm theoretical value absorbance 0 200 admissible tolerance 0 020 28 Select with amp Quit via the menu item return Confirm with amp Input the theoretical value 445 1 Confirm with amp If the standard is already stored this value appears on the display Input the tolerance with amp Confirm with amp PhotoCheck standard 445 1 is input Select the nex
4. Insert the round cell with barcode into the round cell shaft until it clicks into place Align the line mark to the notch of the photometer The photometer reads the barcode of the round cell and automatically selects the relevant method After approx The measured value appears on the display 2S e Ifthe select method menu is displayed align the 2 line mark of the round cell to the notch of the photometer 4 Measuring the Concentration 4 2 Measuring using tests without barcode manual method sele When measuring using cell tests without barcode the method must be selected manually The last method set up manually appears on the display Select the required method with amp Confirm with amp After approx The measured value appears on the display 2S 5 Measuring the Absorbance Transmission 5 1 Switching to the Absorbance Transmission measuring mode Call up the setup measuring mode by actuating amp Inthe setup menu call up the abs trm submenu Selection of the measuring mode absorbance transmission 5 2 Measuring the absorbance or transmission Call up the absorbance or transmission measuring mode depending on the selection in the abs trm menu by actuating GD Measuring mode absorbance Measuring mode transmission e The transmission measurement is not described 2 separately in the following example as it operates i
5. 04 2004 ba75430e01 ww C2 25 688 04 Chemischer Sauerstoffbeda Vari WTW MeBbereick a 1500 mg CSB J7 inuten photoLab Operating Instructions Part 1 General Information Part 2 Functional Description gt Contents 1 Photometers I 1 1 Photometry au dicen tence tind eatensawens cases Il 1 2 The Photometers 2 22222 Ill 2 Photometric Test Kits II 2 1 Basic Principle 222 cexaxteverenevsdsinansaseesnnt Ill 2 1 1 Spectroquant Cell Tests III 2 1 2 Spectroquant Reagent Tests IV 2 2 Notes for Practical Use IV 2 2 1 Measuring Range IV 2 2 2 Influence of pH V 2 2 3 Influence of Temperature V 2 2 4 Time Stability V 2 2 5 Influence of Foreign Substances VI 2 2 6 Dosing of Reagents VI 2 2 Shelf life of the Reagents VII 3 Sample Preparation VII 3 1 Taking Samples VII 3 2 Preliminary Tests o ccceiscecdesorseneneecaune ve VII 2 3 DUGON ecr nee VIII 3 4 Filtration 0 0 0 VIII 3 5 Homogenization ses cesceenay nase anne IX 3 6 Decomposition iiiscss cavers vananaveranaeccnates IX 4 Pipetting System XI 5 Analytical Quality Assura
6. 14598 F 1 00 mg l 0 15 mg l 19814 10 0 mg I 1 2 mg l 19814 Formaldehyde Cell Test 14500 HCHO 5 00 mg I 0 50 mg l see prep instr Formaldehyde Test 14678 HCHO 4 50 mg I 0 50 mg l see prep instr Gold Test 14821 _ Au 6 0 mg I 0 6 mg l 70216 Hardness see Total Hardness Cell Test Hydrazine Test 09711 NoH 1 00 mg I 0 10 mg l see prep instr Hydrogenperoxide Cell Test 14731 H203 10 0 mg I 1 0 mg l see prep instr lodine Test 00606 lo 4 00 mg l 0 40 mg l see prep instr Iron Cell Test 14549 CombiCheck 30 14677 Fe 1 00 mg l 0 15 mg l 19781 Iron Cell Test 14896 Fe 25 0 mg I 2 5 mg l 19781 Iron Test 14761 CombiCheck 30 14677 Fe 1 00 mg l 0 15 mg l 19781 Iron Test 00796 CombiCheck 30 14677 Fe 1 00 mg l 0 15 mg l 19781 Lead Cell Test 14833 CombiCheck 40 14692 Pb 2 00 mg l 0 20 mg l 19776 Lead Test 09717 CombiCheck 40 14692 Pb 2 00 mg l 0 20 mg l 19776 Magnesium Cell Test 00815 Mg 40 0 mg I 4 0 mg l 19788 Manganese Cell Test 00816 CombiCheck 30 14677 Mn 1 00 mg l 0 15 mg l 19789 Manganese Test 14770 CombiCheck 30 14677 Mn 1 00 mg l 0 15 mg l 19789 Molybdenum Cell Test 00860 _ Mo 0 50 mg I 0 05 mg l 70227 Monochloramine Test 01632 _ Clo 5 00 mg l 0 50 mg l see prep instr Nickel Cell Test 14554 CombiCheck 40 14692 Ni 2 00 mg l 0 20 mg l 09989 Nickel Test 14785 CombiCheck 40 14692 Ni 2 00 mg l 0 20 mg l 09989 Nitrate N1 25 CombiCheck 20 14675 NO3 N 9 0 mg l 0
7. Method Parameters 7 2 Selecting the unit The preset unit is mg l It can be changed to mmol l Call up the unit submenu Using amp scroll to mmol l Confirm with amp 20 8 Analytical Quality Assurance AQA Analytical quality assurance AQA can be performed The AQA mode must be activated in the photometer in two steps In the delivery state it is switched off AQA1 Photometer monitoring The AQA mode is activated AQA2 Total system monitoring with by inserting the AQA MemoChip standard solutions monitoring of the total system using standard solutions AQA2 e The total system monitoring AQA2 is a by using a menu to select 2 pie check using standard solu monitoring of the photometer AQA1 monitoring of the total system using standard If this is performed successfully it also includes solutions AQA2 photometer monitoring AQA1 See also part General information for further information on Analytical Quality Assurance AQA 8 1 Activating AQA To switch on the photometer open the cover 8 1 1 Activating AQA using the AQA MemoChip Place the AQA MemoChip in the recess on the photometer The following display appears e The action of placing the AQA MemoChip in the 2 recess directly activates the AQA2 check see section 8 3 4 wo 2 WO A AQS 8 1 2 Activating AQA via the menu guide Press amp Call up the
8. No of test kit Schwefels ure Mercury ll sulfate sulfuric acid Details regarding contents ccc ne acide sulfurique Designation of test kit i Special cell in optical quality acido solforico Additional reagent s Some cell tests e g COD or nitrite already contain all the necessary reagents in one and the same cell and the sample must merely be added using a pipette Release 07 03 Identification mark for the Be i Een correct insertion into the cell 14690 compartment of the photo we i Bar code for identification meter CSB COD Ri in the photometer MERCK Quecksilber ll sulfat Mercurio solfato ico 7 91146 9080 01 61333567 wi ie 7 In other tests however for reasons of chemical com and masking agents that suppress or minimize the influence of interfering ions The colour reactions are in most cases based on modified classical in many cases also normed analytical procedures Details on the respective refe rence procedures are stated in the package insert or else in the parameter overview Risk phrases Highly precise dosage of _ the reagent patibility it is necessary to separate the test into two or three different reagent mixtures In these test kits it is necessary to add in addition to the sample the dosage reagent to the cell reagent gt 2 Photometric Test Kits 2 1 2 Spectroquant Reagent Tests The principle behind the reagent tests is t
9. 020 mg of bromine vy Preparation of the bromine standard solution Pipette 10 ml KIO KI standard solution into a 100 ml volumetric flask add 2 0 ml of H SO 0 5 mol l art 1 09072 leave to stand for 1 min and then add NaOH 2 mol l art 1 09136 dropwise approx 1 ml until the solution just loses its colour Subsequently make up the solution to the mark with distilled water The concentration of the solution is 2 00 mg l bromine y Stability The KIO stock solution remains stable for 4 weeks when stored in a cool place The KIO3 KI standard solution can be used for 5 hours when stored in a cool place The dilute bromine standard solution remains stable for a maximum of 5 minutes y Reagents required 1 02404 0100 Potassium iodate volum standard 1 05043 0250 Potassium iodide GR 1 09072 1000 Sulfuric acid 0 5 mol l 1 09136 1000 Sodium hydroxide solution 2 mol l XX Standard solution of free chlorine Preparation of a stock solution of free chlorine First prepare a 1 10 dilution using a sodium hypo chlorite solution containing approximately 13 of active chlorine For this pipette 10 ml of sodium hypochlorite solution into a calibrated or confor mity checked 100 ml volumetric flask and then make up to the mark with DI water v Precise assay of the stock solution for free chlorine Pipette 10 0 ml of the stock solution into a 250 ml ground glass stoppered conical flask containing 60 ml of DI water Subse
10. 10 10 20 Nickel Cell Test 14554 no 20 20 20 Nickel Test 14785 no 20 20 20 Nitrate N1 25 no 0 2 20 Nitrate Cell Test 14542 no 0 4 20 Nitrate Cell Test 14563 no 0 2 20 Nitrate Cell Test 14764 no 0 5 20 Nitrate Cell Test 00614 no 2 20 Release 07 03 XVI gt Suitability of Test Kits for Testing Salt Water l Test kit Art Seawater Limit of tolerance salts in k E Nitrate Test 14773 no 0 4 20 Nitrate Test 09713 no 0 2 20 Nitrate Cell Test salt water 14556 yes 20 20 Nitrate Test salt water 14942 yes 20 20 Nitrite N4 25 yes 20 20 15 Nitrite Cell Test 14547 yes 20 20 15 Nitrite Test 14776 yes 20 20 15 Nitrogen total see Total Nitrogen Cell Test Oxygen Cell Test 14694 no 10 5 1 Ozone Test 00607 no 10 10 10 Ozone Test 14732 no 10 10 10 pH Cell Test 01744 yes Phenol Cell Test 14551 yes 20 20 15 Phenol Test 00856 yes 20 20 20 Phosphate P4 25 yes 5 10 10 Phosphate P total P4 25 no 1 10 10 Phosphate P5 25 yes 20 20 20 Phosphate P total P5 25 yes 5 20 20 Phosphate Cell Test 14543 yes 5 10 10 Phosphate Cell Test P total 14543 no 1 10 10 Phosphate Cell Test 14729 yes 20 20 20 Phosphate Cell Test P total 14729 yes 5 20 20 Phosphate Cell Test 00616 yes 20 20 20 Phosphate Test 14848 yes 5 10 10 Phosphate Test 00798 yes 15 20 10 Phosphate Cell Test 14546 yes 20 20 20 Phosphate Test 14842 yes 20 20 20 Potassium Cell Test 14562 yes 20 20 20 Potassium Cell Test 00615 yes 20 20 20 Residual Hardness Cell Test 14683 no 0
11. 12 0 mg l 1 0 mg l 19812 Ammonium Cell Test 14559 CombiCheck 70 14689 NH N 50 0 mg l 5 0 mg l 19812 Ammonium Test 14752 CombiCheck 50 14695 NH N 1 00 mg l 0 10 mg l 19812 Ammonium Test 00683 CombiCheck 70 14689 NH N 50 0 mg l 5 0 mg l 19812 AOX Cell Test 00675 AOX 1 00 mg l 0 10 mg l 00680 BOD Cell Test 00687 Oo 210 mg l 20 mg l 00718 Boron Cell Test 00826 B 1 00 mg l 0 15 mg l 19500 Boron Test 14839 B 0 400 mg I 0 040 mg l 19500 Bromine Test 00605 Bro 4 00 mg l 0 40 mg l see prep instr Cadmium Cell Test 14834 CombiCheck 30 14677 Cd 0 500 mg l 0 060 mg l 19777 Cadmium Test 01746 Cd 0 250 mg l 0 010 mg l 19777 Calcium Cell Test 00858 Ca 75 mg I 7 mg l 19778 Calcium Test 14815 Ca 80 mg I 8 mg l 19778 Chlorine Cell Test 00595 Clo 4 00 mg I 0 40 mg l see prep instr Chlorine Cell Test 00597 Clo 4 00 mg I 0 40 mg l see prep instr Chlorine Test 00598 Clo 4 00 mg I 0 40 mg l see prep instr Chlorine Test 00602 Clo 4 00 mg I 0 40 mg l see prep instr Chlorine Test 00599 Clo 4 00 mg I 0 40 mg l see prep instr Chlorine Test 14828 Clo 4 00 mg I 0 40 mg l see prep instr Chlordioxide Test 00608 ClO 4 00 mg I 0 40 mg l see prep instr Chlorine dioxide Chlorine Clo 2 50 mg I 0 25 mg l see prep instr Ozone Test 14732 Chloride Cell Test 14730 CombiCheck 20 14675 Cl 60 mg l 10 mg l 19897 CombiCheck 10 14676 25 mg l 6 mg l 19897 Ch
12. 6 5 5 7 SG 6 4 20 7 8 5 8 7 4 DTR if not available short circuit CTS and RTS 9 49 p 14 Maintenance 14 1 Changing the lamp Switch off the photometer and disconnect it from Connect the plug of the new lamp the power line Screw the lamp cover on again Carefully turn up the photometer and park it safely Set up the photometer again and connect it to the Screw off the lamp cover on the underside of the power line photometer Press and hold amp i Let the lamp of the photometer cool down Switch on the meter open the cover and after the following display appears release Pull out the plug Unscrew the screw Remove the lamp with its holder by pulling it gently upwards Do not touch the new light bulb of the N photometer Insert a new preset lamp and screw it tight using the screw 14 2 Actions to take if a cell is broken the liquid After it is dry check the photometer N Do not rotate the photometer to pour out Letthe cell shaft dry Perform a photometer monitoring see section 8 2 The photometer has a draining mechanism under the cell shaft that when operated correctly prevents any liquid coming into contact with electronic components Switch off the photometer close the cover and disconnect it from the line power Let the liquid drain off Carefully remove any pieces of glass e g using
13. 64 1026 Further investigational concentrations may be pre pared from the stock solution exactly determined according to the procedure described above by diluting accordingly Vv Stability When stored in a cool place refrigerator the stock solution remains stable for at most one day The further diluted solutions investigational concentrations must be used immediately vy Reagents required 1 09099 1000 lodine solution 0 05 mol 12 1 0 1 N solution Sodium sulfide hydrate approx 35 GR Sodium thiosulfate solution 0 1 mol l 0 1 N solution Sulfuric acid 25 GR Zinc iodide starch solution GR Water GR 1 06638 0250 1 09147 1000 1 00716 1000 1 05445 0500 1 16754 9010 Release 07 03 Standard solution sulfite Preparation of a standard solution Dissolve 1 57 g of sodium sulfite GR and 0 4 g of Titriplex Ill GR with DI water in a calibrated or conformity checked 1 volumetric flask and make up to the mark The stock solution prepared according to this procedure has a concentration of 1000 mg l sulfite Further investigational concentrations may be prepared from this stock solution by diluting accordingly vy Stability When stored in a cool place refrigerator the stock solution remains stable for only one day Vv Reagents required 1 06657 0500 Sodium sulfite GR 1 08418 0100 Titriplex Ill GR 1 16754 9010 Water GR Standard solution of a surfactants Preparation of a
14. 9 mg l 19811 Nitrate Cell Test 14542 CombiCheck 20 14675 NO3 N 9 0 mg l 0 9 mg l 19811 XVIII Release 07 03 gt Spectroquant CombiCheck and Standard Solutions CombiCheck Art Test kit Art standards Nitrate Cell Test 14563 Nitrate Cell Test 14764 Nitrat Cell Test 00614 Nitrate Test 14773 Nitrate Test 09713 Nitrate Cell Test 14556 Nitrate Test 14942 Nitrite N4 25 Nitrite Cell Test 14547 Nitrite Test 14776 Nitrogen total s Total Nitrogen Cell Test Oxygen Cell Test 14694 Ozone Test 00607 DH Cell Test 01744 Phenol Cell Test 14551 Phenol Test 00856 Phosphate P4 25 Phosphate P5 25 Phosphate Cell Test 14543 Phosphate Cell Test 14729 Phosphat Cell Test 00616 Phosphate Test 14848 Phosphate Test 00798 Phosphate Cell Test 14546 Phosphate Test 14842 Potassium Cell Test 14562 Potassium Cell Test 00615 Residual Hardness Cell Test 14683 Silicate Silicic Acid Test 14794 Silicate Silicic Acid Test 00857 Silver Test 14831 Sulfate Cell Test 14548 Sulfat Cell Test 00617 Sulfate Cell Test 14564 Sulfate Test 14791 Sulfide Test 14779 Sulfite Cell Test 14394 Sulfite Test 01746 Surfactants anionic Cell Test 14697 Tin Cell Test 14622 TOC Cell Test 14878 TOC Cell Test 14879 Total Hardness Cell Test 00961 Total Nitrogen Cell Test 14537 Total Nitrogen Cell Test 00613 Total Nitrogen Cell Test 14763 Zinc Cell Test 00861 Zinc Cell Test 14566 Z
15. both photometer monitoring AQA1 and system moni toring AQA2 e For the total system monitoring AQA2 a 2 change of the time interval n weeks even retroactively applies to monitoring processes that are already running Changing the number of measurements n measurements does not affect monitoring processes already running Thus individual numbers of measurements can be set for different methods AQA interval n weeks The AQA interval n weeks is only effective if the n weeks setting is active for the AQA mode function The specified number of n weeks applies to the photometer with AQA1 all methods with AQA2 Inthe AQA intervals menu call up the n weeks submenu After an interval has expired the following conse quences become effective Warning and loss of AQA identification Locking of the method for concentration measure ments as long as the locking is active Setting ranges Photometer monitoring AQA1 1 to 52 weeks default 12 weeks or 1 to 9999 measurements default 1500 Monitoring of the total system using standard solu tions AQA2 1 to 52 weeks default 4 weeks or 1to 9999 measurements default 100 e Withthe n measurements setting a difference measurement see section 7 1 2 is counted as one measurement only Inthe AQA configuration menu call up the AQA intervals submenu According to the selection in the AQA mode menu a fixed t
16. bottle The dose metering cap colour green volume 0 025 ml blue 0 050 ml can be used in cases when the solid substance or mixture is free flowing In all other cases the substances are dosed using the microspoon colour grey volume 0 01 ml green 0 03 ml blue 0 1 ml Release 07 03 gt 2 Photometric Test Kits 2 2 7 Shelf life of the Reagents The Spectroquant test kits can be kept for up to three years when stored cool and dry A few tests have a shorter shelf life 18 or 24 months or must else be stored in the refrigerator The exception here are all COD cell tests which must be stored pro tected from light then the three year shelf life is guaranteed The expiry date is printed on the outer label The shelf life may become shortened when the reagent bottles are not reclosed tightly after use gt 3 Sample Preparation Sample preparation covers all the steps necessary before the actual analysis can be performed 3 1 Taking Samples The taking of samples is the first and most impor tant step on the way to obtaining the correct ana lysis result Not even the most exact method of analysis can correct any mistakes made in the taking of the sample The objective of the sampling proce dure is to gain a sample with a representative com position The most important precondition for gain ing a representative sample is the identification of the suitable sampling site Here it must be borne in mind that the
17. clock is empty and has to be replaced Send the photometer to the service department for this The MemoChip is not recognized by the photometer though it is in the recess during switching on Operate the photometer with line power see chapter 3 COMMISSIONING Repeat the procedure Inform the service department The connected printer is off line Switch on the printer or pull out the interface cable The message remove cell appears on the display although no cell is inserted Clean the cell shaft with a damp lint free cloth If the error message still appears return the photometer to the service depart ment Replace the lamp see chapter chapter 14 MAINTENANCE No zero adjustment is stored in the meter for the cell Perform zero adjustment see chapter chapter 11 ZERO ADJUSTMENT No data is stored in the photometer for the selected method Update method data see chapter chapter 12 UPDATING METHOD DATA During a difference measurement the method was changed between the first and second measurement During a difference measurement the method must remain identical Hardware error Send the photometer to the service department Replace the lamp see chapter chapter 14 MAINTENANCE If the error message remains send the meter to the service department 53
18. file with a double click or decompress the zip file with Winzip Connect the serial interfaces of the PC and photometer with the cable Start the UpdateMethodData exe program file by double clicking The Update Method Data window appears In the upper half of the window there is the name of your photometer among other things behind it there is the method version in brackets e g 8 00 All method data are reloaded into the photom eter with the update The old method data are overwritten by this Click on the Search meter button The program automatically recognizes the connected photometer Another Update Method Data window appears Click on the Start button to start the method download The process takes approx 3 minutes You can terminate it at any time by clicking on the Cancel button In this case however the download has to be carried out once again completely so that the photometer can save the method data and is operative 12 Updating method data During the download the following display appears on the photometer screen After the download confirm the Data successfully downloaded message The download is finished The photometer returns to the concentration measuring mode You can check whether the new method data are 2 stored in the photometer To do so proceed as follows Inthe setup menu call up the meter setup submenu Call up the system info menu item Sample
19. following display appears Call up the correction funct submenu Select the correction function blank value turbidity correct Confirm with amp 9 1 Blank value The blank value reagent blank value for each method is stored in the photometer When the blank value function is active the stored value is ignored and the measured value of a self prepared reagent blank solution is used instead This procedure increases the measuring accuracy for some tests for more information see part Analytical procedures A blank value is always stored for the method that was just called up A maximum of 10 measured blank values can be stored each of which is permanently assigned to a method A blank value remains stored until it is erased menu item erase blank value or overwritten The reset setup function sets the blank value to off The stored blank values however remain stored The reset total function resets all settings and blank values at once If a measured blank value is stored and the blank value function is active for a method this blank value is used for determining the measured value and the measured value is documented accordingly The blank value function is not active when delivered 37 p 9 Correction functions Measuring the concentration with a blank value Press to call up the concentration measuring mode The value measured against the prepared blank solu tio
20. meter setup submenu The meter setup submenu appears with the AQA func tions menu item preselected Confirm with amp 21 8 Analytical Quality Assurance AQA A password request appears If the input was incorrect After the password has been successfully input the AQA configuration submenu appears 22 A separate password protects settings of the AQA configuration against unauthorized access Changing the password see section 8 1 5 Input the password with Only numeric characters are allowed Default 0000 Confirm with amp Repeat the input 2 If you have forgotten the password contact the service department Call up the AQA mode function Default off no monitoring Select AQA mode off nweeks n measurements Confirm with amp Inthe setup menu call up the AQA check submenu Selection of the AQA mode meter system e The menu item meter only appears after the 2 corresponding PhotoCheck standards have been input see section 8 2 1 8 Analytical Quality Assurance AQA 8 1 3 Changing AQA intervals AQA intervals specify the interval between two AQA checks A fixed time interval n weeks or a number of measurements n measurements can be specified as the interval The respective values that were input remain stored even if they are not activated Additionally two separate intervals can be set up for
21. mg I 15 mg l 70730 Ca 2 50 mg l 0 30 mg l 19778 Si 2 50 mg l 0 25 mg l 70236 0 375 mg l 0 040 mg l 70236 Si 25 0 mg I 2 5 mg l 70236 Ag 1 50 mg I 0 20 mg l 19797 SO 100 mg l 15 mg l 19813 SO 100 mg l 15 mg l 19813 SO 500 mg l 75 mg l 19813 SO 100 mg l 15 mg l 19813 S 0 75 mg I 0 08 mg l see prep SO 12 5 mg l 1 5 mg l see prep SO 30 0 mg l 1 0 mg l see prep MBAS 1 00 mg l 0 20 mg l see prep Sn 1 25 mg l 0 13 mg l 70242 TOC 40 0 mg l 3 0 mg l 09017 TOC 400 mg I 30 mg l 09017 Ca 75 mg l 7 mg l 19778 N 5 0 mg l 0 7 mg l see prep N 5 0 mg l 0 7 mg l see prep N 50 mg l 7 mg l see prep Zn 0 500 mg l 0 050 mg l 19806 Zn 2 00 mg l 0 40 mg l 19806 Zn 1 25 mg 0 20 mg l 19806 c 1000 mg l analyte compare with O Sensor instr instr instr instr instr instr instr instr instr instr Instructions for the Preparation of Standard Solutions Standard solution of bromine acc to DIN EN ISO 7393 Preparation of a KIO stock solution Ina 1000 ml volumetric flask dissolve 1 005 g of KIO art 1 02404 in 250 ml of distilled water Subsequently make up to the mark with distilled water v Preparation of a KlO Kl standard solution Transfer 8 90 ml of the KIO stock solution to a 1000 ml volumetric flask add approx 1g of KI art 1 05043 and make up to the mark with distilled water 1 ml of this solution is equivalent to 0
22. mm 13 8 mm Recess for MemoChip Display Graphical display 128 x 64 pixels Connections Digital inter RS 232 C 9 pin socket to connect face to PC or printer Power supply 2 pin socket to connect the plug in power supply unit Data storage Cyclical memory to record 500 measured values FCC Class A Equipment Statement Note This equipment has been tested and found to comply with the limits for a Class A digital device 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 equipment generates uses and can radiate radio frequency energy and if not installed and used in accordance with the instruction manual may cause harmful interference to radio communications Operation of this equipment in a residential area is likely to cause harmful interference in which case the user will be required to correct the interference at his own expense 52 Software settings when delivered Measured value 1 number blank value is Off turbidity correct Off language English Date of the last valid invalid not yet measured AQAI check AQA1 interval 12 weeks AQA2 interval 4 weeks AQA password 0000 AQA mode Off Lock measurement if Off AQA2 expired Checks to be measured none with AQA1 AQA2 values none Settings after reset total Measured value storage and setup re
23. new date as well Selecting the menu item return returns to the menu item blank value Before measuring and storing erase the old blank value 9 1 3 Erasing blank values A measured blank value is erased via the menu item erase blank value 39 p 9 Correction functions Select the erase blank value menu item After confirming with E the erase blank value menu opens e lhe erase blank value menu item first appears 2 after a blank value has been measured Select between all Erase all stored blank values single Erase individual stored blank value e Each stored blank value is displayed with the 2 date of the blank value measurement and the relevant method designation Select the blank value with amp Erase the displayed blank value with e Select the erase menu item with amp Confirm with amp 9 1 4 Recalling blank values Select the recall blank values menu item with amp Confirm with amp Select the blank value with amp Return with amp 40 9 Correction functions 9 2 Turbidity correction Turbidity correction is used in sample solutions that The turbidity correct function is not active when deliv contain finely distributed suspended particles The ered Suspended particles cause a light absorption This leads to incorrect too high measured values e This function is not necessary or useful in all The function remains permanently switche
24. nme 17 7 1 1 Changing the citation form 17 7 1 2 Performing a difference measurement 18 7 2 Selecting the unit 005 20 8 Analytical Quality Assurance AQA 21 8 1 Activating AQA 0 eee 21 8 1 1 Activating AQA using the AQA MemoChip ce ee eee 21 8 1 2 Activating AQA via the menu guide 21 8 1 3 Changing AQA intervals 23 8 1 4 Locking the system 25 a Contents 8 1 5 Changing the password 26 8 1 6 Performing an AQA reset 26 8 2 Photometer monitoring AQA1 27 8 2 1 Entering PhotoCheck standards 27 8 2 2 Download of PhotoCheck standards 29 8 2 3 Erasing PhotoCheck standards 29 8 2 4 Performing Photometer monitoring 30 8 3 Total system monitoring with standard solutions AQA2 war rn sah anaana anaana 32 8 3 1 Entering standards 32 8 3 2 Output of standards 34 8 3 3 Erasing standards 35 8 3 4 Monitoring of the total system using standard solutions 35 9 Correction functions 37 9 1 Blank value 0 cee eee 37 9 1 1 Activating the blank value measurement Ese_ uwrix se ee ee eee 38 9 1 2 Measuring the blank value 39 9 1 3 Erasing blank values 39 9 1 4 Recalling blank values 40 9 2 Turbidity correction 0000 41 10 Zero adjustment
25. of measure ments before each AQA2 check The currently set number of measurements for the AQA2 check is saved for the active method and output in the report individually section 8 3 4 Inthe AQA intervals menu call up the n measure ments submenu To return without change press E9 three times Enter the number of measurements for AQA meter with amp confirm with Enter the number of measurements for AQA system with amp confirm with 24 8 Analytical Quality Assurance AQA 8 1 4 Locking the system The function system locked is effective if fora moni As a result a concentration measurement is not tored method possible for this method no AQA check was performed the AQA check system has expired Call up the system locked submenu Select the menu item with amp Confirm with amp 25 8 Analytical Quality Assurance AQA 8 1 5 Changing the password When delivered the default password is 0000 This password can be changed as follows Call up the change password submenu Confirm with Input the required password e g 0700 with amp Confirm with amp Input the password once again Confirm with amp 8 1 6 Performing an AQA reset If the Analytical Quality Assurance is to be switched off completely or reset to the delivery state this can be made via the reset function in the AQA configuration submenu
26. 01 0 01 0 01 Silicate Silicic Acid Test 14794 yes 5 10 5 Silicate Silicic Acid Test 00857 no 5 10 245 Silver Test 14831 no 0 1 5 Sodium Cell Test 00885 no 10 1 Sulfate Cell Test 14548 yes 10 20 Sulfate Cell Test 00617 yes 10 20 Sulfate Cell Test 14564 yes 10 20 Sulfate Test 14791 no 0 2 0 2 Sulfide Test 14779 no 0 5 1 1 Sulfite Cell Test 14394 no 20 20 20 Sulfite Test 01746 no 20 20 20 Surfactants anionic Cell Test 14697 no 0 1 0 01 10 Tin Cell Test 14622 yes 20 20 20 TOC Cell Test 14878 no 0 5 10 10 TOC Cell Test 14879 no 5 20 20 Total Hardness Cell Test 00961 no 2 2 1 Total Nitrogen Cell Test 14537 no 0 5 10 Total Nitrogen Cell Test 00613 no 0 2 10 Total Nitrogen Cell Test 14763 no 2 20 Zinc Cell Test 00861 no 20 20 1 Zinc Cell Test 14566 no 10 10 10 Zinc Test 14832 no 5 15 15 TE Release 07 03 XVII gt Spectroquant CombiCheck and Standard Solutions CombiCheck Art Other standards Art Confidence interval tolerance Test kit Art Evalu ation Spec value for as the standard Alcohol Cell Test 14965 C2H30H 3 g l 0 3 g l 09008 Aluminium Test 14825 CombiCheck 40 14692 Al 0 75 mg l 0 08 mg l 19770 Ammonium A5 25 CombiCheck 10 14676 NH N 4 00 mg l 0 30 mg l 19812 Ammonium Cell Test 14739 CombiCheck 50 14695 NH N 1 00 mg l 0 10 mg l 19812 Ammonium Cell Test 14558 CombiCheck 10 14676 NH N 4 00 mg l 0 30 mg l 19812 Ammonium Cell Test 14544 CombiCheck 20 14675 NH N
27. 1 4 Selecting and calling up the menu items To switch on the photometer open the cover Press amp The following display appears Example The documentation menu item is preselected in the setup menu gt Select a menu item e g meter setup Press The following display appears The meter setup menu item is preselected gt Call up the meter setup submenu by pressing amp The required menu item is selected using amp called up using amp Selection lists Changes to the settings are accepted after confir mation by pressing Current settings are marked by Change to other configuration levels by Selecting the menu item return Pressing Scroll with Character input by using the character to be input is shown in reverse video Confirm each input with 2 Safety This operating manual contains basic instructions to be followed in the commissioning operation and main tenance of the meter Consequently all responsible personnel must read this operating manual before 2 1 Authorized use working with the meter The operating manual must always be available in the vicinity of the meter The photometer is authorized exclusively for analyzing substances in water and aqueous solutions using round cells or rectangular cells special optical glass Observe the technical specifications of the cel
28. 1000 mg l hydrazine Further investigational concentrations may be prepared from this stock solution by diluting accordingly Vv Stability When stored in a cool place refrigerator the stock solution and the further diluted investiga tional solutions remain stable for one day Vv Reagents required 1 04603 0100 Hydrazinium sulfate GR 1 16754 9010 Water GR Release 07 03 Standard solution of iodine acc to DIN EN ISO 7393 Preparation of a KIO stock solution Ina 1000 ml volumetric flask dissolve 1 005 g of KIO art 1 02404 in 250 ml of distilled water Subsequently make up to the mark with distilled water v Preparation of a KIO KI standard solution Transfer 5 60 ml of the KIO stock solution to a 1000 ml volumetric flask add approx 1g of Kl art 1 05043 and make up to the mark with distilled water 1 ml of this solution is equivalent to 0 020 mg of iodine vy Preparation of the iodine standard solution Pipette 10 ml KIO KI standard solution into a 100 ml volumetric flask add 2 0 ml of H2SO0 0 5 mol l art 1 09072 leave to stand for 1 min and then add NaOH 2 mol l art 1 09136 dropwise approx 1 ml until the solution just loses its colour Subsequently make up the solution to the mark with distilled water The concentration of the solution is 2 00 mg l iodine y Stability The KIO stock solution remains stable for 4 weeks when stored in a cool place The K
29. 8O 1 2 Identifying the connectors Power pack amp Connection for power pack RS 232 interface p 1 Overview 1 3 Short manual The short manual lists all of the steps necessary to determine the concentration of a sample and to activate AQA2 at a glance 1 3 1 Measuring the concentration To switch on the photometer open the cover The photometer performs a check Self Check of the entire system and then switches automatically to the concentration measuring mode Measuring mode concentration Insert the round cell with barcode in the round cell e shaft until it clicks into place J Align the line mark to the notch of the photometer The IM message measuring appears e lithe select method menu is displayed align the 2 line mark of the round cell to the notch of the photometer The measured value appears on the display Measured values outside the specified measuring range are output in small numerals Repeat the measurement Press 1 3 2 Activating AQA2 Place the AQA MemoChip in the recess on the photometer The following display appears The action of placing the AQA MemoChip in the recess directly activates the AQA check without m oe b having to press any key A AQS Standard concentrations and tolerances are 2 listed in the table Spectroquant CombiCheck and standard solutions in the part General information b 1 Overview
30. IO3 KI standard solution can be used for 5 hours when stored in a cool place The dilute iodine standard solution remains stable for a maximum of 5 minutes vy Reagents required 1 02404 0100 Potassium iodate volum standard 1 05043 0250 Potassium iodide GR 1 09072 1000 Sulfuric acid 0 5 mol l 1 09136 1000 Sodium hydroxide solution 2 mol l XXIII Instructions for the Preparation of Standard Solutions Standard solution of ozone Standard solution of total nitrogen acc to DIN EN ISO 7393 Preparation of a KIO stock solution Ina 1000 ml volumetric flask dissolve 1 005 g of KIO art 1 02404 in 250 ml of distilled water Subsequently make up to the mark with distilled water v Preparation of a KIO KI standard solution Transfer 14 8 ml of the KIO stock solution to a 1000 ml volumetric flask add approx 1g of KI art 1 05043 and make up to the mark with distilled water 1 ml of this solution is equivalent to 0 010 mg of ozone Vv Preparation of the ozone standard solution Pipette 20 ml KIO KI standard solution into a 100 ml volumetric flask add 2 0 ml of H SO 0 5 mol l art 1 09072 leave to stand for 1 min and then add NaOH 2 mol l art 1 09136 dropwise approx 1 ml until the solution just loses its colour Subsequently make up the solution to the mark with distilled water The concentration of the solution is 2 00 mg l ozone v Stability The KIO stock solution remains stable
31. If the message reoccurs inform the service department After approx 4s Insert the L2 cell ir After approx 1s 30 8 Analytical Quality Assurance AQA After successful light barrier testing the PhotoCheck standards test solutions are measured Example After approx 3 sS Absorbance test OK Insert a cell with the test solution 445 1 The photometer measures the absorbance of the test solution and compares the result with the value entered Or error message Insert the next test solution Cancel To cancel the check means no release for the next meter AQA Interval Error elimination 1 Repeat the measurement insert the cell again 2 If necessary perform a zero adjust ment and repeat the check 3 Exchange the test solution each packet contains two identical test solutions Use a new Spectroquant Photo Check packet 5 Quit and have the photometer checked in the factory The absorbance test is terminated if an error message occurs and the meter is not released On switching on the warning message AQA interval expired appears until the AQA was successfully performed or the AQA mode was switched off Example Report output AQA check meter AQA1 26 08 97 10 23 operator AQA interval 12 weeks AQA check AQA1 ok L check ok test sol meas unit theor val tolerance result value 445 1 0 211 A 0 200 0 020 ok 31 8 Analytical Qual
32. am provides an overview regarding internal quality assurance aspects Test for the overall system Checking the handling operations 3 Suspend the bottom Carefully pipette 3 ml of Heat the reaction cell in n Swirl the cell after sediment in the cell by the sample into a reaction the thermoreactor at 10 minutes swirling sahen htly with the 148 C for 2 hours Influence of the sample Test for recovery Release 07 03 XII gt 5 Analytical Quality Assurance AQA 5 2 1 Checking the Photometer As soon as the photometer is activated it is running a Self Check This means the hardware and the soft ware of the photometer is checked and compared with internal standards The photometer itself is checked in the AQA 1 mode using the Spec troquant PhotoCheck The pack includes round cells containing stable test solutions secondary standards for checking the photometer at the 445 525 and 690 nm wavelengths The test solutions are measured in a reference photometer monitored with primary standards and the absorbance values are documented in the package insert These desired values with the permissible tolerances are entered into the photometer or else handwritten into the con trol chart For the measurement the cell is placed in the compartment for the round cell and identified by 5 2 2 Checking the Overall System Test for the overall system includes checking the working equipment and checking
33. ances or water insoluble samples decomposi tion using concentrated acids and other agents is in dispensible Corresponding examples are described in the Application Compendium obtainable from your local Merck representative see Appendix a collection of analytical specifications for real samples The necessity for decomposition can be checked according to the following diagram Procedure Measurement Result B AandB idential Decomposition _ No Yes No decomposition necessary necessary For wastewater with a consistent composition this check as a rule need be carried out only once It is however advisable to check the result periodically Release 07 03 gt 4 Pipetting System Positive displacement pipettes permit an exact dosage of the sample volume and a precise measurement of sample and reagent volumes and of the volumes of water for dilution purposes Pipettes of varying volumes and also ones with a fixed volume are available Sources of error and hints on how to avoid them Closely follow the instructions for use contained with the pipette in question Check the pipetted volumes by weighing using analytical scales weighing accuracy 1 mg 1 ml of water at 20 C 1 000 g 1 mg Check the pipetted volume using Spectroquant PipeCheck this is a photometric check of the pipette and scales are not necessary See section AQA Avoidance of spread effects by rinsing the pipette s
34. arentheses indicate the range in which the theoretical value should move Confirm with amp Input the tolerance 0 7 mg l with amp Confirm with amp Both standard and tolerance values have been over written Confirm with 33 8 Analytical Quality Assurance AQA 8 3 2 Output of standards The current list of stored standards is output via the RS 232 interface PC printer or via the display Select the outout submenu Confirm with Select the output medium jo display jo printer PC serial interface Select with amp Confirm with E9 to start the download Example Report output AQA check system AQA2 26 08 97 13 57 system locked on method unit theor val tolerance AQA date 14554 mg l 2 00 0 20 24 08 97 14555 mg l 5000 400 26 08 97 34 8 Analytical Quality Assurance AQA 8 3 3 Erasing standards Erasing the method specific standard solutions leads to the change of the measured value identification from AQA2 to AQA1 with activated AQA mode Call up the standard solutions submenu Select the menu item erase with amp Confirm with amp Select the standard to be erased with amp Erase with 8 3 4 Monitoring of the total system using standard solutions The AQA2 check can be performed after it has been e ForAQA2 with the setting n measurements we activated see section 8 1 2 recommend to check and if n
35. ay appears Call up the method parameters submenu Input the method number Confirm with amp Select the menu item with amp Call up the parameter by pressing e 16 7 Method Parameters 7 1 Citation form 7 1 1 Changing the citation form O o o M Example Change the citation form from NH N to NH4 Call up the citation submenu Using scroll to NH Confirm with amp 17 p 7 Method Parameters 7 1 2 Performing a difference measurement Difference measuring is possible for some methods e g Iron III Ca Mg Hardness e For more information on this see part Analysis 2 specifications Example Determination of iron Il and iron III Enter method 106 Confirm with Call up the citation menu item The current setting Fe Using scroll to Fe Il Fe IIA Confirm with amp Citation form Fe Il Fe IIIA is set Change to measuring by pressing Start the 1st measurement by inserting cell 1 18 b 7 Method Parameters After approx 2 S After approx 2 S The 1st measured value appears on the display amp Fe Remove cell 1 Press amp Start the 2nd measurement by inserting cell 2 The 2nd measured value appears on the display Iron Il Continue to the display of both measured values using E9 Display of both measured values as asummary 19 p 7
36. ct the safety of both the user and the environment as well as the equipment 2 2 3 Qualification of the personnel The personnel responsible for the commissioning operation and maintenance must have the necessary qualifications for this work If the personnel do not have the required skills they have to be instructed 2 2 4 Technical state of the meter lt is the responsibility of the operator to continuously observe the overall technical condition externally recognizable deficits and damage as well as alter ations to the operational behavior of the meter If safe operation is no longer possible the equipment must be taken out of service and secured against inadvertent operation Non compliance with the safety instructions will result in the loss of any warranty claims Furthermore it must be ensured that the personnel read and completely understand the present operating manual Safe operation is no longer possible if the equipment has been damaged in transport the equipment has been stored under adverse conditions for a lengthy period of time the equipment is visibly damaged the equipment no longer operates as prescribed If you are in any doubt please contact the supplier of the photometer 3 Commissioning The photometer operates at an environmental temper Before putting the photometer into service wait until it ature of 5 C to 40 C During transport from coldto has adapted to the new environm
37. cted since the resultant error is lower than 2 The addition of larger quantities should be duly con sidered by adjusting the sample volume accordingly The specified pH values for the sample solution and wherever applicable for the measurement solution are defined in the respective package inserts and in the analysis instructions in chapter 3 of the manual Absorbance 10 20 30 40 Temperature C Absorbance 30 60 Reaction time minutes 2 Photometric Test Kits 2 2 5 Influence of Foreign Substances Foreign substances in the sample solution can raise the measurement value as a result of an amplification of the reaction or lower the measurement value as a result of a prevention of the reaction A quantification of the effects is stated in tabular form in the respective package inserts for the most important foreign ions The tolerance limits have 2 2 6 Dosing the Reagents Small amounts of liquids are dosed by counting the number of drops from the leakproof bottle Larger amounts of liquids are dosed with the piston syringe enclosed with the respective test kit Handling Depress the piston of the syringe to the zero position Place the tip of the syringe firmly on the leakproof attach ment of the bottle Turn the bottle with the piston syringe 180 so that the piston syringe is positioned underneath the bottle In some cases in which an exact dosage of gene rally small quant
38. d Input the date using amp Erase the input using Confirm with amp Select the output medium jo display jo printer PC serial interface Select the menu item with amp Confirm with to start the memory download Each data record appears individually on the display beginning with the data record just measured The display shows no of meas value citation date time meas value D number unit method designation Where necessary AQA ID e g AQA2 Scroll with p 6 Documentation Memory download to printer PC Memory download to the serial interface Display of the transmitted no of measured value continuation display beginning with the last measured value Cancel with e Sample printout 003 14541 10 02 98 11 56 33 t 80 mg l COD 002 14541 10 02 98 11 54 21 t 70 mg l COD 001 14729 03 02 98 18 30 53 TOS mg l PO4 P 6 3 Download of the methods list The stored methods are downloaded to the printer PC via the serial interface Call up the outout methods submenu The following parameters can be set all Download of all stored methods Select the menu item with amp Start the download with amp 15 p 7 Method Parameters The following parameters can be set in the method parameters menu citation unit To switch on the photometer open the cover Press E9 The following displ
39. d Path length of the cell in cm c Concentration of the analyte in mol l Release 07 03 gt 1 Photometers The photometers that belong to the Spectroquant Analysis System differ from conventional photo meters in the following important aspects The calibration functions of all test kits are elec tronically stored The measurement value can be immediately read off from the display in the desired form The method is selected via the AutoSelect function bar code on the cells on the AutoSelector for reagent tests gt 2 Photometric Test Kits The photometers possess AQA Analytical Quality Assurance functions to assure the quality of the measurement New methods can be downloaded from our homepage www merck de and stored permanently in your photometer For technical data and instructions for use please refer to the section Function description 2 1 Basic Principle By means of reagents the component of a sample to be analyzed is converted into a coloured compound in a specific reaction The reagents or reagent mix tures contain in addition to the reagent selective for the parameter to be determined a number of auxi liary substances that are essential for the course of the reaction These include for example buffers for adjusting the pH to the optimal value for the reaction 2 1 1 Spectroquant Cell Tests The most important part of these test kits is the cell Cat
40. d difference is equal to the concen tration of analyte of addition solution that was added the recovery rate is 100 If the difference is less than 90 then a matrix interference is present The block temperature compensates for any heat lost due to insufficient heat transfer XIV Release 07 03 5 Analytical Quality Assurance AQA 5 4 Definition of Errors It is obvious that measurement results as a rule may be associated with errors This applies equally to standardized methods of analysis reference methods and to routine analysis The discovery and the minimization of errors must be the objective here A distinction is made between systematic errors and random errors Systematic errors are present when all the results of an analysis deviate from the true value with the same algebraic sign Examples here include a wrong sam ple volume a wrong pH a wrong reaction time a sample matrix influence etc Systematic errors thus affect the accuracy of the method of analysis Accuracy Deviation of the measured concentra tion from the true concentration Random errors manifest themselves in the form of a wide range of deviation of the results of a given sam ple These can be kept to a minimum by ensuring good operating techniques and multiple determina tion with calculation of the mean values Random errors make the result of the analysis unreliable they influence the precision Precision Dispersion of th
41. d on after it 2 methods Ifthe turbidity correction is active the has been activated Values that were measured using photometer automatically decides whether to turbidity correction are given an identifier in the perform the function or not depending on the display and in the documentation printout and method storage Inthe correction funct menu call up the turbidity correct submenu The following display appears The turbidity correct function appears Select the on menu item with amp Confirm with amp Press to call up the concentration measuring mode Insert the measuring cell After approx Display of the measured value with turbidity correction 2 S switched on Identified by TC Warning of excessive turbidity If the turbidity absorbance of 0 100 A is exceeded the meter displays the measured value together with a warning 41 p 10 Zero adjustment Zero adjustment is necessary after changing the lamp after the error message PhotoCheck AQA1 occurs on initial commissioning if the photometer was mechanically stressed e g percussion transport if the ambient temperature changed by more than 5 C since the last zero adjustment at least every six months Only perform the zero adjustment against 2 distilled water in an optically perfect cell Press E9 Inthe setup menu call up the meter setup submenu The following display appea
42. display the software version is irrelevant here The method version here 19 00 has to agree with the method version for your photometer in the Update Method Data window during the download Error messages Message Meaning Remedy No meter found Connection PC photo Tightly connect the cable to the meter out of order or not serial interfaces of the PC and available photometer Use the correct cable Photometer not recognized Select the photometer manually 47 p 13 RS 232 C interface Via the interface data can be output to a printer and exchanged with a personal computer PC For this the following items are available as accesso ries Printer cable Printer Interface cable Communication software 13 1 Principle course of the remote control String to meter Reply from meter Operating mode S lt CR gt gt lt CR gt Remote remote control Command xx see 15 2 Reply string command xx lt CR gt Remote remote control command list CLOC lt CR gt Concentration measurement e The keyboard of the photometer is locked in the 2 remote operating mode 13 2 Command list Command Function S Begin communication CLOC Switchover to normal operation concentration measurement CDAT anz Reads out stored measured values anz number of the measured values to be output CMES MMM Measurement and transmission of the concentration value with date time MMM method
43. e following display appears Call up the documentation menu with amp The following functions can be selected no of meas value reset the number download memory total from date output methods all lists of the respective submenus 12 b 6 Documentation 6 1 Resetting the number of the measured value Call up the no of meas value submenu yes The numbering of the measured values starts again with 001 default no Consecutive numbering of the measured values from 001 to 999 Select the menu item with amp Confirm with amp 6 2 Download memory The measured value storage can be selectively down loaded to either the display or serial interface The selection of the output medium is made after the specification of the sorting criteria Call up the download memory submenu The download memory menu item only appears 2 after at least one measurement has been performed The following sorting criteria can be set total all stored measured values from date all measured values from a special date Select the menu item with amp Confirm with amp 13 p 6 Documentation Selecting total Selecting from date Memory download to display 14 Select the output medium jo display jo printer PC serial interface Select the menu item with amp Confirm with to start the memory downloa
44. e results among each other Release 07 03 The following diagram illustrates the aspects of accuracy and precision Accuracy poor Precision poor Major errors have been made Accuracy good Precision poor Calculation of the mean values from at least three or better even more parallel determina tions yields an approximation of the true value Accuracy poor Precision good The high degree of precision mis takenly indicates a correct value Accuracy good Precision good The ideal objective XV Suitability of Test Kits for Testing Salt Water Test kit Art Seawater Limit of tolerance salts in Naci NaNO Alkohol Cell Test 14965 no Aluminium Test 14825 yes 10 20 20 Ammonium A5 25 yes 20 10 15 Ammonium Cell Test 14739 no 5 5 5 Ammonium Cell Test 14558 yes 20 10 15 Ammonium Cell Test 14544 yes 20 15 20 Ammonium Cell Test 14559 yes 20 20 20 Ammonium Test 14752 no 10 10 20 Ammonium Test 00683 yes 20 20 20 AOX Cell Test 00675 no 0 4 20 20 BOD Cell Test 00687 yes 20 20 20 Boron Cell Test 00826 yes 10 20 20 Boron Test 14839 no 20 5 20 Bromine Test 00605 no 10 10 10 Cadmium Cell Test 14834 no 10 10 10 Cadmium Test 01745 no 1 10 1 Calcium Cell Test 00858 no 2 2 1 Calcium Test 14815 yes 20 20 10 Chlorine Cell Test 00595 no 10 10 10 Chlorine Cell Test 00597 no 10 10 10 Chlorine Test 00598 no 10 10 10 Chlorine Test 00602 no 10 10 10 Chlorine Test 00599 no 10 10 10 Chlorine Test 14828 no 10 10 10 Ch
45. e sample must be diluted accordingly so that it lies ideally in the middle of the effective range least error measurement Method In photometry it is conventional practice to measure against the reagent blank value Here the analysis is carried out blind i e without any analyte added Instead of the sample volume the corresponding quantity of distilled or DI water is used This reagent blank value is already electronically stored in the system photometers meaning that a separate mea surement is not necessary It is possible however to enhance the accuracy of the determination at the measuring range limit by measuring against a self prepared reagent blank solution for adjustment see Function description Blank value correction There are however also cases in which the colour intensity of the solution and thus the absorbance drop off again at very high analyte concentrations These exemplary cases are listed in the table below The values indicated in the display are correct up to the concentrations specified in the third column and false measuring values are obtained above these concentrations In such a case it is necessary to con duct a plausibility check by running preliminary tests using test strips or dilution Correct indica Colour change tion of result up to sample conc Ammonium 25 mg l 250 mg l 100 mg l 5000 mg l 30 mg l 4 mg l 25 mg l 25 mg l 100 mg l 5 mg l turquoise instead of gr
46. e substance in question this absorption occurs at a specific wavelength Incident light Transmitted light The wavelength is selected from the overall spectrum of white light emitted by a tungsten halogen lamp using narrow band interference filters or other mono chromators The intensity of the absorption can be characterized using the transmittance T or respectively T in percent GLP Good Laboratory Practice AQA Analytical Quality Assurance T I lo lo Initial intensity of the light Intensity of the transmitted light If the light is not absorbed at all by a solution then this solution has a transmittance of 100 a com plete absorption of the light in the solution means 0 transmittance The measure generally used for the absorption of light is the absorbance A since this correlates directly with the concentration of the absorbing sub stance The following connection exists between absorbance and transmittance A logT Experiments by BOUGUER 1693 1758 and LAMBERT 1728 1777 showed that the absorbance is dependent on the thickness of the absorbing layer of the cell used The relationship between the absor bance and the concentration of the analyte in ques tion was discovered by BEER 1825 1863 The com bination of these two natural laws led to the deriva tion of Lambert Beer s law which can be described in the form of the following equation Molar absorptivity in molxcm
47. e syringe tightly Hold the syringe upright and Filter the contents of the filtered with the syringe into the front side of the slowly depress the piston syringe into the intended glass membrane filter attachment upwards until the membrane vessel filter is fully wetted free of air bubbles 3 5 Homogenization As a measure to ensure that a representative sample sample must be homogenized This must be can be taken in the presence of suspended matter in carried out using a magnet stirrer 2 minutes at the water sample in question for certain parameters 700 900 rpm and taking the sample while stirring for example COD total content of heavy metals the cf DIN 38402 A30 3 6 Decomposition Water borne substances can be present in the sample for investigation in a variety of forms as the ion bound more or less solidly in a complex or as a solid substance opel OH Solid substance Release 07 03 gt 3 Sample preparation The manner in which the sample is pretreated en ables the three proportions to be distinguished from each other This can be illustrated using a copper containing wastewater sample as an example Example Filtration Total content Solid Substances Cu OH Complexes Cu EDTA Complexes Cu EDTA lons Cu2 lons Cu2 Result A Result B Dissolved proportion Dissolved proportion lons Cu2 Result C Proportion lonogenic Complex Solid Substances Total content Decompositi
48. ecessary change The following display appears the currently set number of measurements before each AQA check 8 1 3 CHANGING AQA INTERVALS Insert cell with prepared solution ready to be measured e g using Spectroquant a CombiCheck The photometer reads the barcode identifies the method and performs the AQA2 check 35 8 Analytical Quality Assurance AQA After approx 2 S 36 AQA check OK Or error message Repeat the check lf the error is repeated perform troubleshooting of the error See Analytical Quality Assurance in part General information e The system AQA2 check must be performed 2 separately for each method monitored The release is stored with the date and the specified interval The AQA2 interval system set up for the respective method begins again Example Report output AQA mode n weeks AQA check system AQA2 26 08 97 11 02 operator AQA interval 4 weeks method meas unit theor val tolerance result value 14554 1 95 mg l 2 00 0 20 ok Example Report output AQA mode n measurements AQA check system AQA2 26 08 97 11 02 operator AQA interval 100 measurements method meas unit theor val tolerance result value 14554 1 95 mg l 2 00 0 20 ok I 9 Correction functions To switch on the photometer open the cover Press E9 Inthe setup menu call up the meter setup submenu The following display appears The
49. edure is calculated as follows Final volume total volume Initial volume sample volume F The analytical result is subsequently multiplied by the dilution factor A calculation can be dispensed with when the dilu tion is programmed into the photometer The dilution number See the table at the right is entered and the measurement value is subsequently calculated correctly and immediately displayed for settings see Function description Method parameters Dilution All dilutions should be made in such a way that the measurement value lies in the middle of the measur ing range As a rule the dilution factor should never be greater than 100 In the event that yet larger dilu tions become necessary all the same then this must be done in two separate steps Example Step 1 Make up 2 ml of sample to 200 ml with destilled water Dr 100 dilution number 1 99 Take 5 ml of the above solution and make up to 100 ml Dr 20 dilution number 1 19 The dilution factor for the total dilution is calcu lated by multiplying the individual dilutions DF total Dr4 X Dro 100 X 20 2000 dilution number 1 1999 Step 2 Simplified procedure Dilutions up to 1 10 can also be prepared without volumetric flasks in a glass beaker measuring the volumes of the sample and the dilution water using a previously calibrated positive displacement pipette see table below for instructions Desired Volume of V
50. eeding 30 C generally influence the stability of the compound that is formed in the reaction The optimal temperature for the colour reaction is stated in the package inserts of the respective Spectro quant test kits Attention After thermic decomposition proce dures the determination of COD or total contents of nitrogen phosphorus or metal a sufficient waiting time must be allowed for to permit the solution cool to room temperature 2 2 4 Time Stability Most of the colour reactions require a certain time to reach the maximum colour intensity The solid curve in the figure at the right gives a schematic impression of a typical time course The behaviour of relatively instable colour reactions with time is shown by the dotted curve The reaction time specified in the working instruc tions refers to the period of time from the addition of the last reagent until the actual measurement In addition the package inserts for the individual test kits also state the time interval in which the measure ment value does not change The maximum time interval is 60 minutes this time should not be ex ceeded even in the case of stable colour reactions Release 07 03 1 mol l raises the pH dropwise testing the pH with suitable indicator strips after each drop is added The addition of the acid or lye results in a dilution of the test solution When up to five drops are added to 10 ml of sample the change in the volume can be negle
51. een CT Ammonium turquoise instead of green CT Ammonium turquoise instead of green CT Ammonium turquoise instead of green Chlorine CT Fluoride CT Copper yellow instead of red O C Q _ O on Q lt brownish yellow instead of violet light blue turquoise instead of blue Copper CT Phenol Silver light blue turquoise instead of blue weakening of colour Concentration no change flocculation Release 07 03 gt 2 Photometric Test Kits 2 2 2 Influence of pH Chemical reactions follow an optimal course only within a certain pH range The reagents contained in the test kits produce an adequate buffering of the sample solutions and ensure that the pH optimal for the reaction in question is obtained Highly acidic pH lt 2 and strongly alkaline pH gt 12 solutions can prevent the pH from being adjusted to an optimal range since under certain circumstances the buffering capacity of the test kit reagents may not be sufficient In such cases the pH must be corrected by adding diluted sulfuric acid 0 5 mol l lowers the pH or diluted sodium hydroxide solution 2 2 3 Influence of Temperature The temperature of the sample solution and reagents has a varying influence on the colour reaction and thus on the measurement result The typical tempe rature course is illustrated in the figure at the right If the sample temperature is lower than 15 C false low results must be reckoned with Temperatures exc
52. eitspr fung electrical safety test Keine visuellen M ngel keine Grate keine losen Teile und Befestigungen no visual flaws no burrs no loose parts and fastenings Freigabe release Datum Date AN Gy a T Bitte verwahren Sie dieses Dokument sorg itig Please add this document to your files Pr fer inspector XI gt 5 Analytical Quality Assurance AQA The certificate for the test kit available for each lot produced documents the quality of the reagents Chargenzeitifikat Lot Certitiente contained In the test kit Spectroquant CSB K vettentest Spectroquant COD Cell Test ee Sollwert Messergebniss Messbereich Target value Result Measuring Range BES mel CSECOD Standard Standard mg l CSB COD mg l CSB COD 13 I as o n Expiry date In I 10 18 Photometer Referenz Reference Wellenl nge Wavelength sm 180 178 MERCK I 180 ooe 20 208 200 28 Datum Date 11 05 00 114895_00428852 300 Kalibrierfunktion Calibration Function Sollwert Chargenwert Target value Lot value 00 i 400 sd J Ordinatenabschnitt Ordinate segment es 29 O Reag blindwert Reagent blank l Tolerance 1 600 0 020 1618 lo Steigung Slope Tolerance 1 00 0 03 7 9 ertrauensbereich Confidence interval P 95 Fee 1 aD nu IRRE ee VT The calculated function must agree within specified tolerances with the function electronically sto
53. ental conditions warm surroundings condensation can form resulting see also chapter 15 TECHNICAL DATA in the malfunction of the meter 3 1 Preparing the photometer Place the photometer on a hard flat surface and Battery operation protect it against intensive light and heat Charge the battery for approx 5 hours before the Line operation initial commissioning To do this Plug the original power pack into the socket on the Plug the original power pack into the socket on photometer the photometer Plug the power pack into the line socket Plug the power pack into the line socket and Switch on the photometer open the cover then the battery will be charged During battery operation or when the meter is at a standstill for longer periods of time the battery runs down This can result in your photometer no longer being ready for operation When the following symbol is displayed charge the battery i 3 2 Switching on the photometer To switch on the photometer open the cover The photometer performs a check Self Check of the entire system and then switches automatically to the concentration measuring mode Self check of the photometer Automatic change to the measuring mode After approx concentration 5 s 4 Measuring the Concentration Call up the concentration measuring mode by actuating Measuring mode concentration 4 1 Measuring using cell tests
54. eter When dealing with sample solutions of an unknown concentration it is advisable to establish whether the sample concentration is indeed within the specified measuring range ideally roughly in the middle of the range Release 07 03 Preliminary tests enhance the analytical reliability and make the determination of the necessary dilution ratios in the case of high concentrations easier Merckoquant Test Strips are very well suited for preliminary tests VII gt 3 Sample Preparation 3 3 Dilution Ee Dilution of samples is necessary for two reasons The concentration of the parameter under investi gation is too high i e it lies outside the measuring range Other substances contained in the sample inter fere with the determination matrix interference false high or false low results may ensue The following auxiliaries are absolute prerequisites for the dilution of the sample Volumetric flasks of varying sizes e g 50 100 and 200 ml Positive displacement pipette Distilled or DI water Only dilutions carried out with these auxiliary pro ducts are of sufficient reliability in the area of trace analysis to which photometry belongs for the sim plified procedure see below An important aspect here is that once the volumetric flask has been filled up to the mark with distilled water the flask is closed and the contents are thoroughly mixed The dilution factor Df resulting from the dilution proc
55. everal times with the solution to be pipetted Always exchange the pipette tip Draw up the liquid slowly and depress piston completely to discharge the liquid gt 5 Analytical Quality Assurance AQA The objective of analysis must always be to determi ne the true content of the analyte in question as accurately and precisely as possible Analytical Quality Assurance represents a suitable and indispensible method by which the quality of the user s own work can be assessed errors in the mea surement system diagnosed and the comparability with the results obtained using the respective refe rence methods demonstrated Details regarding the necessity of AQA can be found in the memorandum M 704 of the German Abwasser technische Vereinigung ATV Wastewater technical Association and in the corresponding self con trol self monitoring regulations of the German federal states available in english Causes for errors can include the working materials used the handling and or the sample under investigation These errors have effects on both the accuracy and precision of the results obtained 5 1 Quality Control at the Manufacturer Photometers and photometric test kits possess spe cifications that are adhered to and above all else also documented by the manufacturer The certificate for the photometer enclosed with each device documents the quality of the measuring device Release 07 03 Endprifu
56. for 4 weeks when stored in a cool place The KIO3 KI standard solution can be used for 5 hours when stored in a cool place The dilute ozone standard solution remains stable for a maximum of 5 minutes y Reagents required 1 05043 0250 Potassium iodide GR 1 09072 1000 Sulfuric acid 0 5 mol l 1 09136 1000 Sodium hydroxide solution 2 mol l XXIV Standard solution of phenol Preparation of a standard solution Dissolve 5 36 g of glycine GR with DI water in a calibrated or conformity checked 1 1 volumetric flask and make up to the mark The stock solution prepared according to this procedure has a concentration of 1000 mg l total nitrogen Further investigational concentrations may be prepared from this stock solution by diluting accordingly Vv Stability When stored in a cool place refrigerator the stock solution remains stable for one week The diluted investigational concentrations must be used immediately v Reagents required 1 04201 0100 Glycine GR 1 16754 9010 Water GR Preparation of a standard solution Dissolve 1 00 g of phenol GR with DI water in a calibrated or conformity checked 1 1 volumetric flask and make up to the mark The stock solution prepared according to this procedure has a concentration of 1000 mg l phenol Further investigational concentrations may be prepared from this stock solution by diluting accordingly vy Stability When stored in a cool place refrigerator the stock
57. g l formaldehyde vy Precise assay of the standard solution stock solution for formaldehyde Pipette 40 0 ml full pipette of the formaldehyde stock solution of approximately 1000 mg l into a 300 ml ground glass conical flask and add 50 0 ml buret of iodine solution 0 05 mol l and 20 ml of sodium hydroxide solution 1 mol l Leave to stand for 15 minutes and subsequently add 8 ml of sulfuric acid 25 GR Add 1 ml of zinc iodide starch solution and subsequently titrate to the end point with sodium thiosulfate solution 0 1 mol l v Calculation of the exact content of the formaldehyde solution C1 consumption of sodium thiosulfate solution 0 1 mol l C2 quantity of iodine solution 0 05 mol l mg l Formaldehyde C2 C1 x 37 525 Further investigational concentrations may be pre pared from the stock solution exactly determined according to the procedure described above by diluting accordingly vy Stability When stored in a cool place refrigerator the stock solution remains stable for one week After this time the stock solution must be determined anew and the corresponding value must be duly accounted for in the further use The further dilu tion solutions investigational concentrations must be used immediately vy Reagents required 1 04003 1000 Formaldehyde solution min 37 GR 1 09099 1000 lodine solution 0 05 mol 12 1 0 1 N solution 1 09147 1000 Sodium thiosulfate solution 0 1 mol l 0 1 N
58. hat the reagents necessary for the colour reaction are com bined in the form of liquid concentrates or solid substance mixtures In these tests a few drops of the respective reagent concentrate are added to for 2 2 Notes for Practical Use example 5 ml of sample This means that there is no need to dilute the sample which in turn enhances the sensitivity of the detection The making up of a sample in a volumetric flask to a defined volume usual in conventional photometry can be dispensed with _ 2 2 1 Measuring Range The intensity of the colour of a solution measured as the absorbance is proportional to the concentration of the respective analyte only within a specific range This measuring range effective range is electro nically stored in the photometers for each individual test kit See overview table in section 1 3 Below the specified measuring range either a different cell or else another procedure must be used The lower limit of the measuring range either takes the form of nonlinearity of the calibration curve as shown in the figure below or else is given by the limit of detection The limit of detection of a given analytical method is the lowest concentration that differs from the zero concentration with a defined probability e g 99 The upper limit of the measuring range is charac terized by there no longer being any linear correlation between analyte concentration and absorbance In such a case th
59. id 25 GR Titrate with a 0 02 mol l potassium permanganate solution until the colour changes to pink v Calculation of the exact content of the hydrogen peroxide concentration Consumption of potassium permanganate ml x 34 02 content of hydrogen peroxide in mg l Further investigational concentrations may be pre pared from the stock solution exactly determined according to the procedure described above by diluting accordingly vy Stability When stored in a cool place refrigerator the stock solution and the further diluted investiga tional solutions remain stable for one day vy Reagents required 1 09122 1000 Potassium permanganate solution 0 02 mol l 0 1 N 1 07209 0250 Perhydrol 30 GR 1 00716 1000 Sulfuric acid 25 GR 1 16754 9010 Water GR Release 07 03 XXVI C O per Q N 7 C O per Q C LL Edition 03 2004 Order no BA41107d05 General instructions Notes on this operating manual To ensure that you become rapidly acquainted with your photometer the first chapter contains an overview and a short manual of the meter The second chapter contains notes for the safe operation of the photometer Chapter 3 describes the commissioning of the photom eter The remaining chapters provide a comprehensive description of the functions and technical data of the photometer Symbols used indicates notes that you must read for N your own safety the safety
60. ime interval n weeks or anumber of measurements n measurements is setinthe AQA intervals Menu Ifthe AQA mode function is switched off the 2 AQA intervals submenu is not available To return without change press E9 three times Enter the time interval for AQA meter with confirm with 23 8 Analytical Quality Assurance AQA AQA interval n measurements The AQA interval n measurements is only effective if the n measurements setting is active for the AQA mode function The AQA2 check starts the monitoring for one method at a time The specified number of measurements applies to the instrument with AQA1 total number of measure ments performed independent of whether AQA2 is active for some parameters each method an AQA check will then be performed for with AQA2 Thus it is possible to define individual numbers of measurements for different methods The measurements are counted separately for each monitored method The monitoring intervals of AQA2 monitoring processes already started for other methods are not affected by changing the number of measurements Thus the number of measurements can be set for further methods no matter which monitoring processes were started before When an AQA2 check is performed the 2 number of measurements last set in the AQA intervals menu is automatically taken over Therefore you should check and if necessary change the currently set number
61. inc Test 14832 CombiCheck 20 14675 CombiCheck 80 14738 CombiCheck 20 14675 CombiCheck 20 14675 CombiCheck 10 14676 CombiCheck 20 14675 CombiCheck 10 14676 CombiCheck 20 14675 CombiCheck 10 14676 CombiCheck 80 14738 CombiCheck 20 14675 CombiCheck 10 14676 CombiCheck 10 14676 CombiCheck 10 14676 CombiCheck 20 14675 CombiCheck 10 14676 CombiCheck 50 14695 CombiCheck 50 14695 CombiCheck 70 14689 CombiCheck 40 14692 Self prepared recommended concentration Release 07 03 Evalu Confidence interval Other ation Spec value for tolerance as the standard Art NO3 N 9 0 mg l 0 9 mg l 19811 NO3 N 25 0 mg l 2 5 mg l 19811 NO3 N 100 mg l 10 mg l 19811 NO3 N 9 0 mg l 0 9 mg l 19811 NO3 N 9 0 mg l 0 9 mg l 19811 NO3 N 1 50 mg l 0 15 mg l 19811 NO3 N 8 0 mg l 0 8 mg l 19811 NO N 0 300 mg I 0 030 mg l 19899 NO N 0 300 mg I 0 030 mg l 19899 NO N 0 50 mg l 0 05 mg l 19899 O3 0 6 mg l O 4 00 mg l 0 40 mg l see prep pH 7 0 0 2 09407 Phenol 1 25 mg l 0 13 mg l see prep C6H5OH 2 50 mg l 0 25 mg l see prep PO P 0 80 mg l 0 08 mg l 19898 PO P 8 0 mg l 0 7 mg l 19898 PO P 0 80 mg l 0 08 mg l 19898 PO P 15 0 mg l 1 0 mg l 19898 8 0 mg l 0 7 mg l 19898 PO P 50 0 mg l 5 0 mg l 19898 PO P 0 80 mg l 0 08 mg l 19898 PO P 50 0 mg l 5 0 mg l 19898 PO P 15 0 mg I 1 0 mg l 19898 PO P 15 0 mg I 1 0 mg l 19898 K 25 0 mg l 4 0 mg l 70730 K 150
62. ities of reagent is called for it is necessary to conduct the dosage procedure using a positive displacement pipette this is described in detail in the analysis instructions Solid substances are dosed either with the dose metering cap or with microspoons that are integrated VI been determined for the individual ions they may not be evaluated cumulatively Suitability for use in salt water A tabular survey see pages XVI XVII provides infor mation on the suitability of the tests in connection with salt water and also on the tolerances for salt concentrations Cy re When using a dropping bottle it is imperative that the bottle be held vertically and the reagent be slowly added dropwise approx 1 drop per second Otherwise the correct drop size will not be achieved and the amount of reagent will be incorrect ry i E Slowly withdraw the piston downwards to the required volume orientation aid upper edge of the piston ring In the event that air bubbles are dra wn into the syringe with the reagent the syringe contents must be pressed back into the bottle and the filling process repeated Once the syringe has been fil led free of air bubbles turn the bottle with the piston syringe 180 back to the original posi tion Remove the filled piston syringe from the attachment of the bottle and carefully inject the contents into the reaction vessel into the screw cap of the respective reagent
63. ity Assurance AQA 1 8 3 Total system monitoring with standard soluti 8 3 1 Entering standards The standards compiled in the table Spectro quant CombiCheck and standard solutions see part General information are already stored method specifically in the photometer These values can be overwritten For total system monitoring AQA2 only one standard per test can be stored at a time The input of a standard is only complete with the input of the tolerances for finding it again i e it is then first stored no premature quitting Press to call up the setup menu Call up the meter setup submenu Call up the AQA functions submenu Input the password Call up the AQA standards submenu and the following display appears 32 4 ia i awe u A ONS ALG po uw lt N N a S pets N Y Call up the standard solutions submenu Select between input Enter standards output Print display standards erase Erase standards Displays the last selected method Select the method with amp Confirm with Input the standards 8 Analytical Quality Assurance AQA Example Method 14729 with a preset theoretical value of 15 0 mg l and tolerance of 1 0 mg l CombiCheck 80 Change to theoretical value 8 mg l tolerance 0 7 mg l CombiCheck 20 Confirm with Enter the new theoretical value e g 8 0 mg l with Values in p
64. k Type Meter safety Battery opera tion optional Power consump tion in line oper ation EMC Climatic class Ambient temper ature Allowable rela tive humidity Test certificate approx 2 3 kg battery version 2 8 kg EN 61010 IEC 1010 EN 61010 1 class 3 Friwo FW6798 11 8363 Friwo Part No 1810502 Input 230 V 10 50 Hz 25 VA Output 12 V 1540 mA Friwo FW6798 11 8365 Friwo Part No 1769227 Input 120 V 10 60 Hz 24 VA Output 12 V 1540 mA compulsory for meters with UL cUL test certificates FRIWO FW 75550 15 Friwo Part No 1822367 Input 100 240 V 50 60 Hz 400 mA Output 15 VDC 1A EN 60950 Built in battery NiCad recharge able battery 7 2 V 2200 mAh operating time with new fully charged battery typical 40 hours with 10 measurements per hour trickle charging in line operation approx 5 h charging time fora discharged battery total discharge protection max 1300 mA EU directive 89 336 EEC EN 61326 1 EN 61000 3 2 A14 EN 61000 3 3 FCC class A 2 VDI VDE 3540 Storage 25 C to 65 C Operation 5 C to 40 C Annual mean 75 30 days year 95 other days 85 CE 51 gt 15 Technical Data On off switch actuated by opening closing the lid of the cell shaft cover Operating elements Silicon keyboard with 4 function keys Cell shaft for round cells flat cell floor external internal diameter 16
65. language menu The available languages are listed in the language of the respective country in the photometer When Russkij is selected as the language the Cyrillic alphabet is used for the user guidance Method designation and ID numbers are always displayed in Latin script For output to the RS 232 C interface Cyrillic characters are converted to Latin characters according to GOST Call up the select language menu item Select a language e g English Confirm with Press the key again Return to the meter setup submenu The displays appear in English 43 11 Meter Setup 11 2 Setting the date time Call up the set date time menu item Input the date using amp Confirm with Input the time with amp Confirm with amp lt is possible to reset the photometer to its factory e All AQA functions are retained when meter settings delivery state in single steps The reset total 2 setup is used function resets all settings and blank values at once See section 8 1 6 for AQA reset Call up the reset menu item Select between total Erase the measured value storage and reset the settings to the delivery state meas storage Erase the measured value storage setup Reset all settings to the delivery state Example Performing a total reset Select the reset menu item Confirm with e A meter reset is performed measured value memory and setup
66. loride Test 14897 CombiCheck 60 14696 Cl 125 mg l 13 mg l 19897 12 5 mg l 0 13 mg l 19897 Chromate Cell Test 14552 CombiCheck 40 14692 Cr 1 00 mg l 0 10 mg l 19780 Chromate Test 14758 CombiCheck 40 14692 Cr 1 00 mg l 0 10 mg l 19780 COD 160 C1 25 CombiCheck 10 14676 COD 80 mg l 12 mg l see prep instr COD 1500 C2 25 CombiCheck 20 14675 COD 750 mg l 75 mg l see prep instr COD Cell Test 14560 CombiCheck 50 14695 COD 20 0 mg l 4 0 mg l see prep instr COD Cell Test 14540 CombiCheck 10 14676 COD 80 mg l 12 mg l see prep instr COD Cell Test 14895 CombiCheck 60 14696 COD 250 mg l 20 mg l see prep instr COD Cell Test 14690 CombiCheck 60 14696 COD 250 mg l 25 mg l see prep instr COD Cell Test 14541 CombiCheck 20 14675 COD 750 mg l 75 mg l see prep instr COD Cell Test 14691 CombiCheck 80 14738 COD 1500 mg l 150 mg l see prep instr COD Cell Test 14555 CombiCheck 70 14689 COD 5000 mg l 400 mg l see prep instr COD Cell Test 09772 CombiCheck 10 14676 CSB 80 mg l 12 mg l see prep instr COD Cell Test 09773 CombiCheck 20 14675 CSB 750 mg l 75 mg l see prep instr Copper Cell Test 14553 CombiCheck 30 14677 Cu 2 00 mg l 0 20 mg l 19786 Copper Test 14767 CombiCheck 30 14677 Cu 2 00 mg l 0 20 mg l 19786 Cyanide Cell Test 14561 CN 0 250 mg I 0 030 mg l 19533 Cyanide Test 09701 CN 0 250 mg I 0 030 mg l 19533 Fluoride Cell Test 14557 _ F 0 75 mg I 0 08 mg l 19814 Fluoride Test
67. lorine Test 14732 no 10 10 10 Chlorine dioxide Test 00608 no 10 10 10 Chlorine dioxide 14732 no 10 10 10 Chloride Cell Test 14730 yes 20 1 Chloride Test 14897 yes 10 0 1 Chromate Cell Test 14552 yes 10 10 10 Chromium total Cell Test 14552 no 5 10 10 Chromate Test 14758 yes 10 10 10 COD C1 25 no 0 4 10 10 COD C2 25 no 0 4 10 10 COD Cell Test 14560 no 0 4 10 10 COD Cell Test 14540 no 0 4 10 10 COD Cell Test 14895 no 0 4 10 10 COD Cell Test 14690 no 0 4 20 20 COD Cell Test 14541 no 0 4 10 10 COD Cell Test 14691 no 0 4 20 20 COD Cell Test 14555 no 1 0 10 10 COD Cell Test Hg free 09772 no 0 10 10 COD Cell Test Hg free 09773 no 0 10 10 Copper Cell Test 14553 yes 15 15 15 Copper Test 14767 yes 15 15 15 Cyanide Cell Test 14561 no 10 10 10 Cyanide Test 09701 no 10 10 10 Fluoride Cell Test 14557 no 10 10 10 Fluoride Test 14598 yes 20 20 20 Formaldehyde Cell Test 14500 no 5 0 10 Formaldehyde Test 14678 no 5 0 10 Gold Test 14821 yes 10 20 5 Hardness see Total Hardness Cell Test Hydrazine Test 09711 no 20 5 2 Hydrogenperoxide Cell Test 14731 yes 20 20 20 lodine Test 00606 no 10 10 10 lron Cell Test 14549 yes 20 20 20 Iron Cell Test 14896 no 5 5 5 Iron Test 14761 yes 20 20 20 Iron Test 00796 yes 20 20 20 Lead Cell Test 14833 no 20 20 1 Lead Cell Test 09717 no 20 5 15 Magnesium Cell Test 00815 yes 2 2 1 Manganese Cell Test 00816 no 20 20 20 Manganese Test 14770 no 20 20 20 Molybdenum Cell Test 00860 no 20 20 5 Monochloramine Test 01632 no
68. ls according to chapter 15 TECHNICAL DATA Any other use is considered unauthorized 2 2 General instructions The photometer is constructed and tested according to the EN 61010 1 safety regulations for electronic measuring instruments It left the factory in a safe and secure technical condition The smooth functioning and operational safety of the photometer can only be guaranteed under the climatic conditions specified in chapter 15 TECHNICAL DATA of this operating manual Opening the photometer or adjustment maintenance and repair work must only be performed by personnel authorized by the manufacturer The only exceptions to this are the activities described in chapter 14 MAINTENANCE Non compliance results 2 2 1 Labeling of notes indicates notes that you must read for N your own safety the safety of others and to protect your meter from being damaged in the loss of warranty claims Follow the points listed below when operating the photometer Follow local safety and accident prevention regula tions Observe the enclosed instructions concerning reagents and accessories Observe the regulations when dealing with dangerous substances Follow the operating instructions at the workplace Use only original spare parts e indicates notes that draw your attention to 2 special features 2 2 2 Dangers of disregarding the safety instructions Disregarding the safety instructions can adversely affe
69. ments 3 1 2 Identifying the connectors 3 1 3 Short manual 0 000 4 1 3 1 Measuring the concentration 4 1 3 2 Activating AQA2 00 4 1 4 Selecting and calling up the menu items 5 2 Safety 0 0 6 2 1 Authorized use 0 ce ee 6 2 2 Generalinstructions 005 6 2 2 1 Labeling of notes 6 2 2 2 Dangers of disregarding the safety INStrUCTIONS 2 0 ee ee 6 2 2 3 Qualification of the personnel 6 2 2 4 Technical state of the meter 6 3 Commissioning 7 3 1 Preparing the photometer 7 3 2 Switching on the photometer 7 4 Measuring the Concentration 8 4 1 Measuring using cell tests 8 4 2 Measuring using tests without barcode manual method selection 9 5 Measuring the Absorbance Transmission _ 10 5 1 Switching to the Absorbance Transmission measuring mode 000 eee ae 10 5 2 Measuring the absorbance or transmission 10 5 3 Measuring using cell tests 11 5 4 Measuring using tests without barcode 11 6 Documentation 12 6 1 Resetting the number of the measured value 13 6 2 Download memory 22 22222 nern 13 6 3 Download of the methods list 15 7 Method Parameters 16 71 Citation form 22 2
70. n exactly the same way as the absor bance measurement However the result of the measurement is displayed as Transmission instead of A for Absorbance A measured reference absorbance is also effec tive in the measuring mode transmission It is displayed as reference absorbance 10 5 Measuring the Absorbance Transmission 3 3 Measuring using cell tests Insert the round cell with barcode into the round cell shaft until it clicks into place Align the line mark to the notch of the photometer The measured value for the wavelength displayed at the top right appears This measured value is automat ically stored If necessary call up further wavelengths with The measured value for the selected wavelength appears and can be stored and output to the interface with Sample display for transmission measurement The last wavelength measured appears on the display Select the wavelength with Start the measurement Press amp 11 p 6 Documentation The measured values can be documented as follows Storage in the measured value memory Output to a connected printer via the serial interface automatic when a printer is connected Transmission to a PC for further processing by using the relevant software e g Multi ACHATII or less conveniently by means of a terminal program To switch on the photometer open the cover Press amp Th
71. n is displayed 9 1 1 Activating the blank value measurement Inthe correction funct menu call up the blank value submenu The following display appears The blank value meas function appears Select the on menu item with amp Confirm with e e he stored blank values determined from blank 2 solutions prepared by the user can be deacti vated by switching off the blank value measure ment When doing so the blank values remain stored in the memory and can be reactivated later Activating or deactivating the blank value func tion applies to all measurements using methods a blank value was stored for in the memory The blank value function is active and appears in the setup menu To measure the blank value call up the blank value submenu in the setup menu 38 I 9 Correction functions 9 1 2 Measuring the blank value Call up the meas blank value menu item The menu items erase blank value and recall 2 blank values first appear after at least one blank value has been measured Insert a cell with blank solution to start a measure ment The message measuring appears on the display Afterapprox 2 S Or if all 10 storage locations for blank values are already occupied e fthe blank value of a method for which a blank 2 value was already stored is measured again this error message does not appear and the new measured value replaces the old measured value
72. nce AQA xI 5 1 Quality Control at the Manufacturer Xl 5 2 Quality Control for the User XII 5 2 1 Checking the Photometer XIII 5 2 2 Checking the Overall System XIII 5 2 3 Checking the Pipettes XIV 5 2 4 Checking Thermoreactors XIV 5 2 5 Testing for Handling Errors XIV 5 3 Determination of Sample Influences XIV 5 4 Definition OF Errors 14 ves ec ewex scene cecauees vs XV Table Suitability of Test Kits for Testing Salt Water XVI Table Spectroquant CombiCheck and Standard Solutions XVIII Appendix Instructions for the Preparation of Standard Solutions XIX ba75430e01 The Spectroquant Analysis System consists of the following components Photometric test kits Sets for sample preparation photo meters The individual components are optimally coordi nated to be fully compatible with each other and make it possible to conduct state of the art analysis without any further accessories being required according to GLP and AQA requirements 1 Photometers Documen tation Dp Analytical Quality Assurance Pipetting system 1 1 Photometry When a beam of light is transmitted through a coloured solution then this beam loses its intensity in other words a part of the light is absorbed by the solution Depending on th
73. ngsprotokoll Record of final inspection Photometer photometer SQ NOVA 60 Serien Nr Serial No 999999 Transponderfunktion fanction of transponder Korrektes Einlesen eines Testdatensatzes correct reading of test data set Selbsttest Self Check Signalabgleich ohne K vette signal adjustment without cell LS Check LS Check Korrekte Erkennung von Test Barcodes correct identification of test barcodes Nullabgleich Zero adjustment Bei allen Filterpositionen Abgleich auf E 0 mit entionisiertem Wasser als Messl sung at all filter positions adjustment to A 0 using deionised water as measurement solution Rundkilvette round cell o k Rechteckk vetten rectangular cells 10mm o k 20mm o k 50mm o k Photometrische Richtigkeit photometrical accuracy Extinktion einer Testl sung in Rundk vette absorbance of test solution in round cell Wellenl nge wavelength nm 605 Toleranz tolerance A 0 020 Sollwert nominal value A Messwert measured value A Linearitat linearity Extinktionsdaten von 2 Planfiitem in separater E1 E2 und kombinierter Anordnung E12 absorbance data of 2 plane filters in separate E1 E2 and combined configuration E12 Messwerte Measured values A 445nm El E2 El Anforderung requirement 0 020 lt El E2 E12 lt 0 020 Sicherhelt nach IEC 1910 safety according to IEC 1010 Elektrische Sicherh
74. number e g 086 for method 14729 CEXT LLL Measurement and transmission of the absorbance value for the wavelength LLL wavelength CBLA MMM Measurement and transmission of the sample blank value MMM method number CCLB MMM Erase measured sample blank values MMM method number e The error message Invalid command appears if 2 commands are unknown or cannot be carried out e g if optional parameters do not agree with the cell coding Optional parameters MMM and LLL need only be input for uncoded cells 48 b 13 RS 232 C interface f 13 3 Output format of measured values Character Meaning Notes 3 consecutive number not required for Data fields a separated by spaces interface commands CMES CEXT and Character set IBM code page 437 CBLA 5 method designation Meaning of the special characters 6 I D number I Measuring with blank value concentration or 17 AE reference absorbance absorbance 4 special characters tT Measurement with turbidity correction with high 9 meas value ren l l 10 unit Measured value outside the measuring range 42 Arena Q AQA measurement 4 AQA ID AQA2 AQA1 13 4 Data transmission Baud rate 4800 Data bits 8 Stop bits 1 Parity none Handshake Hardware Max cable length 15m 13 5 Pin assignment EI T T TE Deal Photometer Computer Printer 9 pin socket 9 pin socket 25 pin plug with RS 232 C interface 2 3 2 TXD 3 2 3 RXD 4 1 and 6
75. of four cells for a given wavelength tests in addition to the wavelength accuracy also the linearity of the absor bance over the effective range The verification of the instrument as it is required by DIN ISO 9000 or GLP can be easily performed by using the PhotoCheck The PhotoCheck allows you to check the linearity of the filters hence offering the possibility to check the instrument All of the corres ponding documentation required by these certifi cation guidelines is done by the photometer auto matically We guarantee for the Spectroquant PhotoCheck a 2 year warrantee In addition to the CombiCheck it is also possible to use ready to use single element standard solutions for this checking procedure These contain 1000 mg of the respective analyte per liter of solution They can be diluted to different final concentrations which should preferably lie approximately in the middle of the measuring range of the respective test kit The table on page XVIII provides an overview of the available CombiCheck and ready to use standard solutions Due to limited shelf life characteristics there are no CombiCheck or ready to use standard solutions for certain parameters Attached to the table are the instructions describing the reagents and working steps necessary to make your own solutions of a defined concentration This allows the control of parameters where there are no simple to prepare solutions available The individ
76. of others and to protect your meter from being damaged e indicates notes that draw your attention to 2 special features Scope of delivery Photometer Power pack AQA MemoChip Product documentation Warranty The designated meter is covered by a warranty of 2 years from the date of purchase The meter warranty extends to manufacturing faults that are determined within the period of warranty The warranty excludes components that are replaced during maintenance such as batteries accumulators lamps etc The warranty claim extends to restoring the meter to readiness for use but not however to any further claim for damages Improper handling or unauthorized opening of the instrument invalidates any warranty claim To ascertain the warranty liability return the meter and proof of purchase together with the date of purchase freight paid or prepaid Accuracy when going to press The use of advanced technology and the high quality standard of our instruments are the result of continuous development This may result in differences between this operating manual and your meter We cannot guar antee thatthere are absolutely no errors in this manual We are sure you will understand that we cannot accept any legal claims resulting from the data figures or descriptions The information in this manual is subject to change without notice gt Contents 1 Overview 2 2 2222er 3 1 1 Description of the operating ele
77. olume of Dilution Dilution dilution sample dist water factor number in mi in mi 2 1 1 1 3 1 2 1 4 1 3 1 5 1 4 1 10 1 9 3 4 Filtration Strongly turbid samples require pretreatment before they can determined in a photometer since the effect of turbidity can result in considerable variations in the measurement values and in false high readings Care must be taken here to ensure that the sub stance to be determined is not contained in the sus pended material in which case a sample decompo sition must be carried out Compounds that always occur in dissolved form for example ammonium nitrate nitrite chlorine chlo ride cyanide fluoride orthophosphate and sulfate permit a previous filtration even when the sample solution is strongly turbid Weak turbidity is eliminated by the automatic turbi dity correction feature built into the photometer see Function description Device set up Correction function in such cases it is not necessary to filter the sample before analysis Release 07 03 VIII 3 Sample Preparation As a measure to distinguish between dissolved and Following the recommendations stated in the refe undissolved water borne substances the water rence methods membrane filters with a pore size of sample can be filtered through a simple paper filter 0 45 um are required for fine filtration Procedure for microfiltration Jt za m LCA t Draw out the liquid to be Screw th
78. on converts the substance to be deter mined into an analyzable form In most cases de composition agents take the form of acids in com bination with oxidizing agents in exceptional cases e g in the determination of total nitrogen an alkaline decomposition is more effective The type of decom position procedure used depends on the analyte to be determined and the sample matrix The ready to use sample decomposition products Spectroquant Crack Set 10 and 20 are suited for the preparation of the sample materials for the deter minations stated in the table below Determination of Sample preparation with Crack Set 10 10 C Crack Set 10 10C Phosphorus total Chromium total sum of chromate and chromium lll Metal total sum of free and complex bound metal Crack Set 10 10C Nitrogen total Crack Set 20 The decomposition reagents are already contained in the packs of the respective cell tests Decomposition cells are included in the pack empty cells are required for the decomposition for Crack Sets 10 and 20 The decomposition processes are carried out in the thermoreactor capacity 8 12 decomposition cells at 120 C or respectively 100 C Details regarding the heating times and further treatment can be found in the package inserts contained in the Spectroquant Crack Set packs In the event that the sample to be analyzed is a high ly contaminated material high proportion of organic subst
79. quently add to this solu tion 5 ml of hydrochloric acid 25 GR and 3g of potassium iodide Close the conical flask with the ground glass stopper mix thoroughly and leave to stand for 5 min Titrate the eliminated iodine with sodium thiosul fate solution 0 1 mol l until a weakly yellow colour emerges Add 2 ml of zinc iodide starch solution and titrate from blue to colourless y Calculation 1l mli sodium thiosulfate solution 3 55 mg free chlorine Further investigational concentrations may be pre pared from the stock solution prepared according to the procedure described above by diluting accordingly vy Stability When stored in a cool place refrigerator the stock solution remains stable for approximately one week Further dilutions investigational con centrations are stable for approximately 2 hours v Reagents required 1 00316 1000 Hydrochloric acid 25 GR 1 05614 9025 Sodium hypochlor solution techn approx 13 active chlorine 1 09147 1000 Sodium thiosulfate solution 0 1 mol l 0 1 N solution 1 05043 0250 Potassium iodide GR 1 05445 0500 Zinc iodide starch solution GR 1 16754 9010 Water GR Release 07 03 gt Instructions for the Preparation of Standard Solutions Standard solution of free chlorine acc to DIN EN ISO 7393 Preparation of a KIO stock solution In a 1000 ml volumetric flask dissolve 1 005 g of KIO art 1 02404 in 250 ml of distilled water Subsequently make up to the mark wi
80. red in the photometer Confidence interval Maximum deviation from the desired value over the entire mea suring range every measurement value can be affected by this deviation this parameter is a measure for the accuracy Standard deviation for the procedure Measurement for the dispersion of the measurement values over the entire measuring range expressed in mg l Coefficient of variation for the procedure ne Measurement for the dispersion of the measurement values over the entire measuring range expressed in The smaller the stan O kimak dard deviation coefficient of variation for the procedure the more Da ee pronounced the linearity of the calibration curve 5 2 Quality Control for the User A complete check comprises the entire system i e checking operations can thus be supported by the the working equipment and the mode of operation photometer and the check values accordingly docu The photometer offers an optimum degree of support mented as per GLP Good Laboratory Practice in this regard in the form of the different quality recommendations see Function description Analy mode The instrument or the whole system includ tical Quality Assurance ing reagents and all accessories will be checked depending on which quality mode selected All of Checking the N working ay equipment ly V Pipette Test kit Photometer The following diagr
81. rs After approx 2 S 42 When performing the zero adjustment observe the following points Only use a clean scratch free round cell with distilled water A prepared zero cell is provided with your photometer In addition a prepared zero cell is contained in the scope of delivery of the Photo Check article 14693 f the round cell is visibly contaminated or at least every 24 months clean and refill it minimum filling level 20 mm Then check the cell for scratches Call up the zero adjustment submenu with Insert a cell with distilled water The message measuring appears on the display Successful zero adjustment 11 Meter Setup f To switch on the photometer open the cover Press ER In the setup menu call up the meter setup submenu The following display appears 11 1 Selecting the language The following languages are stored in the photometer Deutsch German English Francais French Italiano Italian Portugu amp s Portuguese Polski Polish Dansk Danish Svenska Swedish Espanol Spanish Nederlands Dutch Indonesia Indonesian Cestina Czech Magyar Hungarian Russkij Russian T rkce Turkish Brasil Brasilian m This chapter describes four functions of the meter setup menu select language set date time Performing a meter reset system info This is the order in which the available languages appear in the select
82. s are exceeded the instructions given in the section Pipetting system must be followed accordingly the instructions for use After the control lamp has gone out the temperature in the cell is measured using a calibrated thermometer The following desired temperatures must be achieved Block temperature 100 C desired temp 100 3 C Block temperature 120 C desired temp 120 3 C Block temperature 148 C desired temp 148 3 C Were the operating instructions for the test followed Was the sample volume correct Was the pipette handled properly Was a new pipette tip used Is the pH correct Was the reaction time adhered to Does the sample and reagent temperature lie within the correct range Is the cell clean Has the expiry date for the test kit been exceeded 5 3 Determination of Sample Influences The influence of other substances contained in the sample may under certain circumstances be so great that their recovery rates lie in the region of several percent It is recommended to check for any influence by using the addition solution contained in the Spectroquant CombiCheck pack A defined quantity of the addition solution R 2 which contains a known concentration of the respec tive analyte is added to the sample and the recovery rate is determined The following difference is then calculated Result sample addition solution Result sample If the calculate
83. set Settings after reset meas storage Meas value number 1 Measured values none Settings after reset setup Measured value 1 number blank value Off reference absorbance Off turbidity correct Off Language unchanged Settings after reset AQA Date of the last valid invalid not yet measured AQAI check AQA1 interval 12 weeks AQA2 interval 4 weeks AQA password 0000 AQA mode Off Lock measurement if AQA2 expired Off Checks to be measured none with AQA1 Input theoretical values and tolerances are not erased and are offered again with the next input AQA2 values none theoretical values and tolerances of all methods are set to default values according to the Se CombiCheck and standard solutions table in the part General information p 16 What to do if The display remains blank when switched on appears Date time is lost when switched off MemoChip is not recogni zed Password forgotten Photometer does not react Error messages remove cell lamp defective no zero adjustment method invalid wrong method E 0 E 1 E 2orE 3 Connect the photometer to the line power via the power pack In the case of battery operation Battery empty charging required approx 5h line operation is possible without restrictions during charging time Battery nearly empty Charging required see chapter 3 COMMISSIONING The backup battery of the real time
84. solution 1 09137 1000 Sodium hydroxide solution 1 mol l 1 N solution 1 00716 1000 Sulfuric acid 25 GR 1 05445 0500 Zinc iodide starch solution GR 1 16754 9010 Water GR Release 07 03 gt Instructions for the Preparation of Standard Solutions Standard solution of COD Preparation of a standard solution In a calibrated or conformity checked 1 1 volu metric flask make up 0 850 g of potassium hydrogen phthalate GR volumetric standard to the mark with DI water The stock solution prepared according to this procedure has a concentration of 1000 mg l COD Further investigational concentrations may be prepared from this stock solution by diluting accordingly v Stability When stored in a cool place refrigerator the stock solution remains stable for one month When stored under appropriate cool conditions refrigerator further investigational concentration dilutions remain stable depending on the respec tive concentration for approximately one week to one month Vv Reagents required 1 02400 0080 Potassium hydrogen phthalate GR volumetric standard 1 16754 9010 Water GR Standard solution of hydrazine Preparation of a standard solution Dissolve 4 07 g of hydrazinium sulfate GR with oxygen low boil previously DI water in a cali brated or conformity checked 1 I volumetric flask and make up to the mark The stock solution pre pared according to this procedure has a concen tration of
85. solution remains stable for one week The diluted investigational solutions must be used immediately v Reagents required 1 00206 0250 Phenol GR 1 16754 9010 Water GR Release 07 03 gt Instructions for the Preparation of Standard Solutions Standard solution of sulfide Preparation of a stock solution Place 7 2 g of glass clear if necessary washed crystals of sodium sulfide hydrate approx 35 GR in a calibrated or conformity checked 1 I volumetric flask dissolve with DI water and make up to the mark The stock solution prepared according to this procedure has a concentration of approx 1000 mg l sulfide vy Precise assay of the standard solution stock solution for sulfide Place 100 ml of DI water and 5 ml full pipette of sulfuric acid 25 GR in a 500 ml ground glass conical flask To this solution add 25 0 ml full pipette of the sulfide stock solution of approx 1000 mg l and 25 0 ml full pipette of iodine solu tion 0 05 mol l Shake the contents of the flask thoroughly for about one minute subsequently titrate with sodium thiosulfate solution 0 1 mol l until the yellow iodine colour has disappeared add 1 ml of zinc iodide starch solution and con tinue to titrate until a milky pure white colour emerges Vv Calculation of the exact content of the sulfide solution C1 consumption of sodium thiosulfate 0 1 mol l C2 quantity of iodine solution 0 05 mol l 25 0 ml mg l sulfide C2 C1 x
86. solution to be investigated can display varying concentrations in different places at different times In sampling a distinction is made between manual and automatic methods In many cases a true picture of the average composition of the sample can be obtained only once several individual samples have been collected this can be done manually or with an automatic sampler Clean plastic containers with a volume of 500 or 1000 ml are suitable for collecting samples They should be rinsed several times under vigorously sha ken with the water to be investigated and then filled free of air bubbles and immediately closed tightly The containers must be protected against the effects of air and heat and then be forwarded for the further analytical steps as soon as possible In exceptional cases preservation measures in the form of short term refrigeration at 2 to 5 C and chemical conservation can be taken Preservation 2 to 5 C max 24h or 18 C max 14 days Parameter COD N compounds NH N NO3 N NO gt N analyze immediately only in exceptional cases 2 to 5 C max 6h P compounds PO P P total short term storage no preservation with nitric acid to ph 1 max 4 weeks Heavy metals short term storage no preservation with nitric acid to ph 1 max 4 weeks 3 2 Preliminary Tests Correct measurement results can be obtained only within the measuring range specified for each indivi dual param
87. standard solution Dissolve 1 00 g of sodium 1 dodecanesulfonate with DI water in a calibrated or conformity checked 1 I volumetric flask and make up to the mark The stock solution prepared according to this procedure has a concentration of 1000 mg l anionic surfactants Further investigational concentrations may be prepared from this stock solution by diluting accordingly vy Stability When stored in a cool place refrigerator the stock solution remains stable for one month The diluted investigational solutions must be used immediately vy Reagents required 1 12146 0005 Sodium 1 dodecanesulfonate 1 16754 9010 Water GR XXV Instructions for the Preparation of Standard Solutions Standard solution of hydrogen peroxide Preparation of a stock solution Place 10 ml of Perhydrol 30 H20 GR ina calibrated or conformity checked 100 ml volumetric flask and make up to the mark with DI water Transfer 30 ml full pipette of this solution to a Calibrated or conformity checked 1 1 volumetric flask and make up to the mark with DI water The stock solution prepared according to this proce dure has a concentration of approximately 1000 mg l hydrogen peroxide v Precise assay of the standard solution stock solution for hydrogen peroxide Pipette 50 0 ml full pipette of the hydrogen per oxide stock solution of approx 1000 mg l into a 500 ml conical flask dilute with 200 ml of DI water and add 30 ml of sulfuric ac
88. t one with amp Input all PhotoCheck standards in this way 8 Analytical Quality Assurance AQA 8 2 2 Download of PhotoCheck standards Example Report output Inthe PhotoCheck standards submenu call up the output menu item Select the output medium jo display jo printer PC serial interface Select with amp Confirm with to start the download AQA check meter AQA1 26 08 97 13 19 AQA interval 12 weeks test sol unit theor val tolerance AQA date 445 1 A 0 200 0 020 26 08 97 8 2 3 Erasing PhotoCheck standards At least 1 standard must still be stored to be able to perform the AQA check function meter monitoring Inthe PhotoCheck standards submenu call up the erase menu item Displays the stored PhotoCheck standards Select with amp Quit via return Erase with 29 8 Analytical Quality Assurance AQA 8 2 4 Performing Photometer monitoring Photometer monitoring AQA1 includes a check of standards the l P Eg I h Light barriers using the L1 L2 cells contained me a men within the scope of delivery of the Spectroquant Call up the AQA check submenu PhotoCheck Call up the meter submenu Absorbance measurement using PhotoCheck The following display appears Insert the L1 cell um Afterapprox e Ifthe error message appears clean the cell 1s 2 shaft with a damp lint free cloth and repeat the check
89. th distilled water v Preparation of a KlO Kl standard solution Transfer 10 0 ml of the KIO stock solution to a 1000 ml volumetric flask add approx 1g of KI art 1 05043 and make up to the mark with distilled water this solution must be prepared freshly 1 ml of this solution is equivalent to 0 010 mg of chlorine vy Preparation of the chlorine standard solution Pipette 20 ml KIO KI standard solution into a 100 ml volumetric flask add 2 0 ml of H SO 0 5 mol l art 1 09072 leave to stand for 1 min and then add NaOH 2 mol l art 1 09136 dropwise approx 1 ml until the solution just loses its colour Subsequently make up the solution to the mark with distilled water The concentration of the solution is 2 00 mg l chlorine y Stability The KIO stock solution remains stable for 4 weeks when stored in a cool place The KIO3 KI standard solution can be used for 5 hours when stored in a cool place The dilute chlorine standard solution remains stable for a maximum of 5 minutes y Reagents required 1 05043 0250 Potassium iodide GR 1 09072 1000 Sulfuric acid 0 5 mol l 1 09136 1000 Sodium hydroxide solution 2 mol l Release 07 03 Standard solution of free chlorine Preparation of a standard solution Dissolve 1 85 g of dichloroisocyanuric acid sodium salt GR with DI water in a calibrated or conformity checked 1 I volumetric flask and make up to the mark The stock solution prepared according to
90. the handling operations The overall system can be checked using standard solutions of aknown content preferably with the Spectroquant CombiCheck this corresponds with the AQA 2 mode in the photometer Spectroquant CombiCheck are ready to use standard solutions that in terms of the analyte concentration are finely adjusted to the individual test kits They contain a mixture of several analytes that do not interfere with each other The standard solution R 1 is used in the same way as a sample A double determination is recommended as a measure to diagnose any random errors The desired values with the permissible tolerances are already electronically stored with the method in the photometer The AQA check mode is selected for the measurement which can be prompted using the MemoChip AQA The cells containing the standard solution are then identified as test solutions by the photometer and the measured concentration is then compared with the desired value When the result agrees with desired value within the permissible tole rance range the display shows the measurement value and the OK sign the photometer via the bar code and the measured absorbance is compared with the desired value The absorbance is shown in the display and can be entered into the corresponding control chart The measurement of at least one cell preferably cell 2 or 3 per wavelength is recommended when checking the photometer The measurement
91. this procedure has a concentration of 1000 mg l free chlorine Further investigational concentrations may be prepared from this stock solution by diluting accordingly vy Stability When stored in a cool place refrigerator the stock solution and the diluted investigational solutions remain stable for one day vy Reagents required 1 02426 0250 Dichloroisocyanuric acid sodium salt GR 1 16754 9010 Water GR Standard solution of total chlorine Preparation of a standard solution Dissolve 4 00 g of chloramine T GR with DI water in a calibrated or conformity checked 1 I volu metric flask and make up to the mark The stock solution prepared according to this procedure has a concentration of 1000 mg l total chlorine Further investigational concentrations may be prepared from this stock solution by diluting accordingly v Stability When stored in a cool place refrigerator the stock solution and the diluted investigational solutions remain stable for one day vy Reagents required 1 02426 0250 Chloramine T GR 1 16754 9010 Water GR Instructions for the Preparation of Standard Solutions Standard solution of chlorine dioxide acc to DIN EN ISO 7393 Preparation of a KIO stock solution Ina 1000 ml volumetric flask dissolve 1 005 g of KIO art 1 02404 in 250 ml of distilled water Subsequently make up to the mark with distilled water v Preparation of a KIO KI standard sol
92. tweezers Carefully clean the cell shaft with a damp lint free cloth 50 15 Technical Data Optical measuring principle Light source Receiver Optical filters Photometric reproducibility Photometric resolution Warm up time Measuring time Types of measurement Measuring range absorbance Measuring range transmission Balancing Drift correction Retrofitting of new methods Bar code recog nition Cell recognition Self Check Time Date Dimensions Filter photometer with reference beam absorption measurement simultaneous recording of all wavelengths Tungsten halogen lamp preset 6 x photo diode array 340 nm 445 nm 525 nm 550 nm 605 nm 690 nm Accuracy 2 nm Half width 340 nm 30 nm 2 nm all others 10 nm 2 nm 0 001 A at 1 000 A 0 001 A none approx 2 s Concentration method depen dent selectable display form absorbance transmission 0 300 A to 3 200 A 0 1 to 1000 Permanently stored Automatic on each Self Check via the Internet automatic selection of the method automatic recognition of the reagents lot automatic Test Memory optics electronic measured value recording barcode recognition cell recogni tion Automatic calibration Optics electronic measured value recording barcode recognition Real time clock in the photom eter H 140 mm D 270 mm W 260 mm Weight Meter safety Safety class Power pac
93. ual results are flagged as AQA2 if the AQA Check of the entire system has passed If not an error message is given and the individual compo nents of the instrument have to be checked in detail Release 07 03 XIII gt 5 Analytical Quality Assurance AQA 5 2 3 Checking the Pipettes The Spectroquant PipeCheck is used to check the pipettes The pack contains cells filled with colour dye concentrates After the addition of a predefined volume of water using the pipette in question the cell is measured against a corresponding reference cell also contained in the pack The difference in the absorbance values 9 2 4 Checking Thermoreactors The thermoreactors are checked at 100 120 and 148 C Here around cell filled to one half with gly cerol is place in any one of the compartments of the thermoreactor and the thermoreactor is heated as described in 9 2 5 Testing for Handling Errors The user s own mode of opera tion must also be subjected to an exact analysis The following questions may serve as a guide in this regard Is the test kit optimal for the measurement assignment in question Is the test kit s measuring range suitable Carefully pipette 3 ml of the sample into a reaction cell close tightly with the screw cap and mix vigorously Caution the cell becomes very hot of the measurement cell and reference cell may not exceed the tolerances given in the package insert If the tolerance
94. ution Transfer 10 5 ml of the KIO stock solution to a 1000 ml volumetric flask add approx 1g of KI art 1 05043 and make up to the mark with distilled water 1 ml of this solution is equivalent to 0 020 mg of chlorine dioxide v Preparation of the chlorine dioxide standard solution Pipette 10 ml KIO KI standard solution into a 100 ml volumetric flask add 2 0 ml of H SO 0 5 mol l art 1 09072 leave to stand for 1 min and then add NaOH 2 mol l art 1 09136 dropwise approx 1 ml until the solution just loses its colour Subsequently make up the solution to the mark with distilled water The concentration of the solution is 2 00 mg l chlorine dioxide y Stability The KIO stock solution remains stable for 4 weeks when stored in a cool place The KIO3 KI standard solution can be used for 5 hours when stored in a cool place The dilute chlorine dioxide standard solution remains stable for a maximum of 5 minutes y Reagents required 1 02404 0100 Potassium iodate volum standard 1 05043 0250 Potassium iodide GR 1 09072 1000 Sulfuric acid 0 5 mol l 1 09136 1000 Sodium hydroxide solution 2 mol l XXII Standard solution of formaldehyde Preparation of a stock solution In a calibrated or conformity checked 1 1 volu metric flask make up 2 50 ml of formaldehyde solution min 37 GR to the mark with DI water The stock solution prepared according to this procedure has a concentration of approximately 1000 m

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