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8. Analytical Quality Assurance (AQA)

AQA check OK ...

...or error message

– Repeat the check

If the error is repeated, perform troubleshooting of 
the error. See "Analytical Quality Assurance" in part 
"General information".

The system

 

AQA2 check must be performed 

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.  

After approx. 
2 s:

Example: Report output (AQA moden weeks)

AQA check system

AQA2

26.08.97

11:02

operator:

AQA interval

4 weeks

method

meas. 
value

unit

theor. val.

tolerance

result

14554

1.95

mg/l

2.00

0.20

ok

Example: Report output (AQA moden measurements)

AQA check system

AQA2

26.08.97

11:02

operator:

AQA interval

100 measurements

method

meas. 
value

unit

theor. val.

tolerance

result

14554

1.95

mg/l

2.00

0.20

ok

Summary of Contents for PhotoLab S6

Page 1: ...ba75430e01 04 2004 Operating Instructions Part 1 Part 2 General Information Functional Description...

Page 2: ......

Page 3: ...reliminary Tests VII 3 3 Dilution VIII 3 4 Filtration VIII 3 5 Homogenization IX 3 6 Decomposition IX 4 Pipetting System XI 5 Analytical Quality Assurance AQA XI 5 1 Quality Control at the Manufacture...

Page 4: ...h the concentration of the absorbing sub stance The following connection exists between absorbance and transmittance A log T Experiments by BOUGUER 1698 1758 and LAMBERT 1728 1777 showed that the abso...

Page 5: ...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 reac...

Page 6: ...ment 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 correspo...

Page 7: ...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 fals...

Page 8: ...he zero position Place the tip of the syringe firmly on the leakproof attach ment of the bottle In some cases in which an exact dosage of gene rally small quantities of reagent is called for it is nec...

Page 9: ...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...

Page 10: ...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 DF 100 dilution number 1 99 Step 2 Take 5 ml...

Page 11: ...lly wetted free of air bubbles Filter the contents of the syringe into the intended glass vessel Procedure for microfiltration As a measure to ensure that a representative sample can be taken in the p...

Page 12: ...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 Append...

Page 13: ...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 err...

Page 14: ...erent quality mode The instrument or the whole system includ ing reagents and all accessories will be checked depending on which quality mode selected All of checking operations can thus be supported...

Page 15: ...cludes checking the working equipment and checking the handling operations The overall system can be checked using standard solutions of a known content preferably with the Spectroquant CombiCheck thi...

Page 16: ...ed 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 Were t...

Page 17: ...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 determin...

Page 18: ...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 T...

Page 19: ...hate 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 Ce...

Page 20: ...tr 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...

Page 21: ...l 19898 Potassium Cell Test 14562 K 25 0 mg l 4 0 mg l 70730 Potassium Cell Test 00615 K 150 mg l 15 mg l 70730 Residual Hardness Cell Test 14683 Ca 2 50 mg l 0 30 mg l 19778 Silicate Silicic Acid Te...

Page 22: ...ion 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 pipett...

Page 23: ...es 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 Standard solution...

Page 24: ...1000 Formaldehyde solution min 37 GR 1 09099 1000 Iodine solution 0 05 mol I2 l 0 1 N solution 1 09147 1000 Sodium thiosulfate solution 0 1 mol l 0 1 N solution 1 09137 1000 Sodium hydroxide solution...

Page 25: ...ive concentration for approximately one week to one month Reagents required 1 02400 0080 Potassium hydrogen phthalate GR volumetric standard 1 16754 9010 Water GR Instructions for the Preparation of S...

Page 26: ...ne standard solution Pipette 20 ml KlO3 Kl standard solution into a 100 ml volumetric flask add 2 0 ml of H2SO4 0 5 mol l art 1 09072 leave to stand for 1 min and then add NaOH 2 mol l art 1 09136 dro...

Page 27: ...ls of sodium sulfide hydrate approx 35 GR in a calibrated or conformity checked 1 l volumetric flask dissolve with DI water and make up to the mark The stock solution prepared according to this proced...

Page 28: ...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 acid 25 GR Titrate with a 0 02 mol l potassium permanganate solution u...

Page 29: ...Edition 03 2004 Order no BA41107d05 Functional description...

Page 30: ...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 clai...

Page 31: ...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 10 5 2 Measuring the absorba...

Page 32: ...ection functions 37 9 1 Blank value 37 9 1 1 Activating the blank value measurement 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 co...

Page 33: ...Recess for MemoChip e Absorbance measure ment key f Concentration measure ment key g Notch for cell alignment h Round cell shaft i Storage space for anal ysis regulations short form j Cover with inte...

Page 34: ...appears If the select method menu is displayed align the line mark of the round cell to the notch of the photometer The measured value appears on the display Measured values outside the specified meas...

Page 35: ...z Call up the meter setup submenu by pressing 1 The required menu item is selected using 3 called up using 1 Selection lists Changes to the settings are accepted after confir mation by pressing 1 Cur...

Page 36: ...ies l Observe the regulations when dealing with dangerous substances l Follow the operating instructions at the workplace l Use only original spare parts 2 2 1 Labeling of notes indicates notes that y...

Page 37: ...3 1 Preparing the photometer Place the photometer on a hard flat surface and protect it against intensive light and heat Line operation Plug the original power pack into the socket on the photometer...

Page 38: ...cks 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 The measured value appears on the dis...

Page 39: ...barcode the method must be selected manually The last method set up manually appears on the display Select the required method with 3 Confirm with 1 The measured value appears on the display 4 2 Measu...

Page 40: ...suring mode transmission The transmission measurement is not described separately in the following example as it operates in exactly the same way as the absor bance measurement However the result of t...

Page 41: ...ight appears This measured value is automat ically stored If necessary call up further wavelengths with 3 The measured value for the selected wavelength appears and can be stored and output to the int...

Page 42: ...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 1 The following display appears Call up the documenta...

Page 43: ...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 onl...

Page 44: ...ium l to display l to printer PC serial interface Select the menu item with 3 Confirm with 1to start the memory download Each data record appears individually on the display beginning with the data re...

Page 45: ...ed to the printer PC via the serial interface Call up the output methods submenu The following parameters can be set l all Download of all stored methods Select the menu item with 3 Start the download...

Page 46: ...arameters menu l citation l unit To switch on the photometer open the cover Press 1 The following display appears Call up the method parameters submenu Input the method number Confirm with 1 Select th...

Page 47: ...Example Change the citation form from NH4 N to NH4 Call up the citation submenu The current setting NH4 N S Using 3 scroll to NH4 Confirm with 1 Citation form NH4 is set S 7 1 Citation form 7 1 1 Chan...

Page 48: ...specifications Example Determination of iron II and iron III Enter method 106 Confirm with 1 Call up the citation menu item The current setting Fe Using 3scroll to Fe II Fe III Confirm with 1 Citatio...

Page 49: ...splay Fe Remove cell 1 Press 1 Start the 2nd measurement by inserting cell 2 The 2nd measured value appears on the display Iron II Continue to the display of both measured values using 1 Display of bo...

Page 50: ...Method Parameters The preset unit is mg l It can be changed to mmol l Call up the unit submenu The current setting mg l S Using 3scroll to mmol l Confirm with 1 Unit mmol l S is set 7 2 Selecting the...

Page 51: ...solu tions If this is performed successfully it also includes photometer monitoring AQA1 See also part General information for further information on Analytical Quality Assurance AQA The AQA mode must...

Page 52: ...was incorrect Repeat the input If you have forgotten the password contact the service department After the password has been successfully input the AQA configuration submenu appears Call up the AQA mo...

Page 53: ...tive values that were input remain stored even if they are not activated Additionally two separate intervals can be set up for both photometer monitoring AQA1 and system moni toring AQA2 For the total...

Page 54: ...ready 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...

Page 55: ...Select the menu item with 3 Confirm with 1 8 1 4 Locking the system The function system locked is effective if for a moni tored method l no AQA check was performed l the AQA check system has expired...

Page 56: ...0 with 3 Confirm with 1 Input the password once again Confirm with 1 If the Analytical Quality Assurance is to be switched off completely or reset to the delivery state this can be made via the reset...

Page 57: ...AQA functions submenu Input the password Call up the AQA standards submenu and the following display appears Call up the PhotoCheck submenu Select between l input Input the theoretical value absorban...

Page 58: ...ect with 3 Quit via the menu item return Confirm with 1 Input the theoretical value 445 1 Confirm with 1 If the standard is already stored this value appears on the display Input the tolerance with 3...

Page 59: ...till be stored to be able to perform the AQA check function meter monitoring In the PhotoCheck standards submenu call up the erase menu item Displays the stored PhotoCheck standards Select with 3 Quit...

Page 60: ...4 Performing Photometer monitoring Photometer monitoring AQA1 includes a check of the l Light barriers using the L1 L2 cells contained within the scope of delivery of the Spectroquant PhotoCheck l Ab...

Page 61: ...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 4 Use a new Spectroquant Photo Chec...

Page 62: ...the tolerances for finding it again i e it is then first stored no premature quitting Press 1to call up the setup menu Call up the meter setup submenu Call up the AQA functions submenu Input the passw...

Page 63: ...to theoretical value 8 mg l tolerance 0 7 mg l CombiCheck 20 Confirm with 1 Enter the new theoretical value e g 8 0 mg l with 3 Values in parentheses indicate the range in which the theoretical value...

Page 64: ...utput submenu Confirm with 1 Select the output medium l to display l to printer PC serial interface Select with 3 Confirm with 1to start the download 8 3 2 Output of standards Example Report output AQ...

Page 65: ...check can be performed after it has been activated see section 8 1 The following display appears For AQA2 with the setting n measurements we recommend to check and if necessary change the currently se...

Page 66: ...h the date and the specified interval The AQA2 interval system set up for the respective method begins again Afterapprox 2 s Example Report output AQA mode n weeks AQA check system AQA2 26 08 97 11 02...

Page 67: ...e 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 bla...

Page 68: ...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...

Page 69: ...ions for blank values are already occupied If the blank value of a method for which a blank value was already stored is measured again this error message does not appear and the new measured value rep...

Page 70: ...stored blank values l single Erase individual stored blank value Each stored blank value is displayed with the date of the blank value measurement and the relevant method designation Select the blank...

Page 71: ...ing 9 2 Turbidity correction Turbidity correction is used in sample solutions that contain finely distributed suspended particles The suspended particles cause a light absorption This leads to incorre...

Page 72: ...l on initial commissioning l if the photometer was mechanically stressed e g percussion transport l if the ambient temperature changed by more than 5 C since the last zero adjustment l at least every...

Page 73: ...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...

Page 74: ...ed value storage l setup Reset all settings to the delivery state Example Performing a total reset Select the reset menu item Confirm with 1 A meter reset is performed measured value memory and setup...

Page 75: ...45 11 Meter Setup Call up the system info menu item Sample display 11 4 System info...

Page 76: ...xxx nova60md xxx nova400md xxx xxx version Carry out the update as follows Switch on the photometer open the cover Switch on the PC Download from the Internet the software including the method data ex...

Page 77: ...lows In the setup menu call up the meter setup submenu Call up the system info menu item Sample display the software version is irrelevant here The method version here 19 00 has to agree with the meth...

Page 78: ...f the remote control String to meter Reply from meter Operating mode S CR CR Remote remote control Command xx see 15 2 command list Reply string command xx CR Remote remote control CLOC CR Concentrati...

Page 79: ...ement Character Meaning 3 consecutive number not required for interface commands CMES CEXT and CBLA 5 method designation 6 I D number 17 date and time 4 special characters 9 meas value 10 unit 12 cita...

Page 80: ...n Set up the photometer again and connect it to the power line Press and hold 3 Switch on the meter open the cover and after the following display appears release 3 Press 1 14 2 Actions to take if a c...

Page 81: ...ectronic measured value recording barcode recognition Time Date Real time clock in the photom eter Dimensions H 140 mm D 270 mm W 260 mm 15 Technical Data Weight approx 2 3 kg battery version 2 8 kg M...

Page 82: ...ea is likely to cause harmful interference in which case the user will be required to correct the interference at his own expense Software settings when delivered Measured value number 1 blank value i...

Page 83: ...e Switch on the printer or pull out the interface cable Error messages remove cell The message remove cell appears on the display although no cell is inserted Clean the cell shaft with a damp lint fre...

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