SC400 Colorimeter. Silica. Photometer-System. Instruction Manual. SiO 2. Bedienungsanleitung Seite Instruction Manual Page 19 33

Transcription

1 Photometer-System SC400 Colorimeter SiO 2 Silica DE GB FR IT ES Bedienungsanleitung Seite 3 17 Instruction Manual Page d'emploi Page Instruction Manual Istruzioni d'uso Pagina Instrucciones Página 67 81

2 Requirements Method: Silicomolybdate Method Description: Under acidic conditions, silica and phosphate in the sample react with molydate ions in the reagent to form yellow colored chemical complexes. The addition of the citric acid reagent removes phosphate interferences. The level of the silica is then determined by measuring the remaining yellow color of the sample. Required Instrument: SC400 Colorimeter for Silica (P/N: SC400-90) Required Accessories: Sample Cell, Round Glass (Ø 24 mm) (P/N: L197620) Required Reagents: Range: Reagent Description: Reagent P/N: mg/l SiO 2 Silica No. 1 Tablet RT313-0 Silica No. 2 Tablet Silica PR Tablet RT314-0 RT mg/l SiO 2 Molybdate 3 Reagent Solution L Silica Citric Acid Powder Pack Silica Amino Acid Powder Pack RP171-0 RP mg/l SiO 2 Silica HR Molybdate Powder Pack RP172-0 Silica HR Acid Reagent Powder Pack Silica Citric Acid Powder Pack RP170-0 RP

3 Contents General notes...20 Guidelines for photometric measurements Method notes...20 Battery change Functional description...22 Operation...22 Backlight...23 Measuring the absorbance Methods Silicon dioxide, with tablet Silicon dioxide LR with Powder Reagent and Liquid Reagent Silicon dioxide HR with Powder Reagent Menu options...30 Menu selections Recall of stored data...30 Setting date and time Calibration...31 User calibration...31 Recommended calibration values Factory calibration reset Technical data...33 Operating messages Error codes CAUTION The accuracy of the instrument is only valid if the instrument is used in an environment with controlled electromagnetic disturbances according to DIN Wireless devices, e.g. wireless phones, must not be used near the instrument. 3

4 General notes Guidelines for photometric measurements 1. Vials, caps and stirring rods should be cleaned thoroughly after each analysis to prevent interferences. Even minor reagent residues can cause errors in the test result. 2. The outside of the vial must be clean and dry before starting the analysis. Clean the outside of the vials with a cleaning cloth to remove fingerprints and other marks. 3. calibration and the testing itself must be carried out with the same vial as there may be slight differences in optical performance between vials. 4. The vials must be positioned in the sample chamber for zeroing and test with the mark on the vial aligned with the mark on the instrument. 5. Always perform zeroing and test with the vial cap tightly closed. Only use the cap with a sealing ring. 6. Bubbles on the inside wall of the vial leads to incorrect measurements. To prevent this, remove the bubbles by swirling the vial before performing the test. 7. Avoid spilling water into the sample chamber because this can lead to incorrect test results. 8. Contamination of the lens in the sample chamber can result in errors. Check at regular intervals and if necessary clean the light entry surfaces of the sample chamber using a moist cloth or cotton buds. 9. Large temperature differences between the instrument and the environment can lead to errors due to the formation of condensation in the area of the lens or on the vial. 10. To avoid errors caused by stray light do not use the instrument in bright sunlight. 11. Always add the reagent tablets to the water sample straight from the foil without touching them with your fingers. 12. The reagents must be added in the correct sequence. Method notes Prior to measurement ensure that the sample is suitable for analysis (no major interferences) and does not require any preparation i.e. ph adjustment, filtration etc. Reagents are designed for use in chemical analysis only and should be kept out of the reach of children. Ensure proper disposal of reagent solutions. Material Safety Data Sheets: available on our web site, or upon request. 4

5 General notes Correct position of the vial (Ø 24 mm) Correct filling of the vial: Opening powder packs 1 2 B A 3 4 Battery change NOTE : If the battery is removed for more than one minute, the date and time menu starts automatically when the colorimeter is next turned on. 5

6 Functional description Operation On Off SIt Turn the unit on using the [ON/OFF] key. The display shows the following: Note: The unit is designed to measure Silica (SiO 2 ) either with tablet reagents or with powder packs. Please select the required method as described below. METHOD METHOD METHOD RESULT Select the required test using the [MODE] key: SIt (Silica tablet) SILr (Silica Low range) SIHr (Silica High range) AbS1 (Absorbance1) AbS2 (Absorbance2) SIt (Silica tablet)... (Scroll) The display shows the following: Fill a clean vial with the water sample up to the 10 ml mark, screw the cap on and place the vial in the sample chamber making sure that the marks are aligned. Press the [ZERO/TEST] key. The "Method" symbol flashes for approx. 8 seconds. The display shows the following: After zero calibration is completed, remove the vial from the sample chamber. When reagents are added, a color will develop if silica is present. Close the vial again and place in the sample chamber making sure that the marks are aligned. Press the [ZERO/TEST] key. The "Method" symbol flashes for approx. 3 seconds. The result appears in the display. The result is saved automatically. Repeating the test: Press the [ZERO/TEST] key again. New zero calibration: Press the [MODE] key until the desired "Method" symbol appears in the display again. 6

7 Functional description Display backlight! Press the [!] key to turn the display backlight on or off. The backlight turns off automatically during the measurement. Recall of stored data! If the instrument is turned on, press the [!] key for more than 4 seconds to access the recall menu. Measuring the absorbance AbS This function allows measurement of the absorbance at the specified wavelength. The result appears in the display in mabs (1000 mabs = 1 A (Absorbance unit)). Abs1: = 430 nm Abs2: = 660 nm 7

8 Methods Silicon dioxide with Tablet mg/l SiO SIt RESULT 1. Fill a clean vial (24 mm Ø) with 10 ml of the water sample and perform zero calibration (see Operation ). 2. Add one SILICA No. 1 tablet (P/N: RT313-0) straight from the foil to the water sample and crush the tablet using a clean stirring rod. 3. Close the vial tightly with the cap and swirl several times until the tablet is dissolved. Wait for a reaction period of 5 minutes. After the reaction period is finished proceed as follows: 4. Add one SILICA PR tablet (P/N: RT315-0) straight from the foil to the same water sample and crush the tablet using a clean stirring rod. 5. Add one SILICA No. 2 tablet (P/N: RT314-0) straight from the foil to the same water sample and crush the tablet using a clean stirring rod. 6. Close the vial tightly with the cap and swirl several times until the tablet is dissolved. 7. Place the vial in the sample chamber making sure that the marks are aligned. Wait for a reaction period of 1 minute. 8. Press the [ZERO/TEST] key. The method symbol flashes for approx. 3 seconds. The result is shown in the display in mg/l SiO 2. Accuracy: ± 0.1 mg/l 8

9 Methods Notes: 1. The tablets must be added in the correct sequence. 2. Phosphate ions do not interfere under the given reaction conditions. 3. If Phosphate is known to be absent, the addition of the SILICA PR tablet may be omitted. 9

10 Methods Silicon dioxide LR with Powder Reagent and Liquid Reagent mg/l SiO 2 SILr Use two clean vials (24 mm Ø) and mark one as blank for zeroing. 1. Fill each vial with 10 ml of water sample. 2. Fill the vial with drops of the same size by holding the bottle vertical and squeeze slowly (Note 5): 3. Add 14 drops of Molybdate 3 Reagent Solution (P/N: L531730) into each vial. 4. Close the vials tightly with the caps and swirl the vials several times to mix the contents (Note 1). Wait for a reaction period of 4 minutes (Note 2). After the reaction period is finished proceed as follows: 5. Add the contents of one Silica Citric Acid F10 Powder Pack (P/N: RP171-0) straight from the foil into each vial. 6. Close the vials tightly with the caps and swirl the vials several times to mix the contents. Wait for a reaction period of 1 minute (Note 3). After the reaction period is finished proceed as follows: 7. Add the contents of one LR Silica Amino Acid F10 Powder Pack (P/N: RP160-0) straight from the foil into the sample vial. Wait for a reaction period of 2 minutes. 8. Place the vial (the blank) in the sample chamber making sure that the marks are aligned. SILr SILr RESULT 9. Press the [ZERO/TEST] key. The method symbol flashes for approx. 8 seconds. 10. Remove the vial from the sample chamber. 11. Place the vial (the sample) in the sample chamber making sure that the marks are aligned. 12. Press the [ZERO/TEST] key. The method symbol flashes for approx. 3 seconds. The result is shown in the display in mg/l SiO 2. Accuracy: ± 0.1 mg/l 10

11 Methods Notes: 1. Close the vials with the cap immediately after adding the Molybdate 3 Reagent Solution; otherwise low readings may result. 2. The given reaction time of 4 minutes refers to a water sample temperature of 68 F (20 C). At 86 F (30 C) a reaction time of 2 minutes, at 50 F (10 C) a reaction time of 8 minutes are required. 3. The given reaction time of 1 minute refers to a water sample temperature of 68 F 20 C. At 86 F (30 C) a reaction time of 30 seconds, at 50 F (10 C) a reaction time of 2 minutes are required. 4. Interferences: Substance Iron Phosphate Sulfide Interference large amounts interfere does not interfere at concentrations less than 50 mg/l PO 4 at 60 mg/l PO 4 the interference is approx. 2% at 75 mg/l PO 4 the interference is approx. 1% interferes at all levels Occasionally water samples contain forms of silica which react very slowly with Molybdate. A pre-treatment with Sodium hydrogencarbonate and then with Sulfuric Acid will make these forms reactive to Molybdate (pretreatment is given in Standard Methods for the Examination of Water and Wastewater under Silica Digestion with Sodium Bicarbonate ). 5. Differing drop size results can interfere with the stated accuracy. This can be minimized by using a pipette. (14 drops is equivalent to 0.5 ml). 11

12 Methods Silicon dioxide HR with Powder Reagent mg/l SiO SIHr RESULT 1. Fill a clean vial (24 mm Ø) with 10 ml of the water sample and perform zero calibration (see Operation ). 2. Add the contents of one Silica HR Molybdate F10 Powder Pack (P/N: RP172-0) straight from the foil to the water sample. 3. Close the vial tightly with the cap and swirl several times to mix the contents. 4. Add the contents of one Silica HR Acid Rgt. F10 Powder Pack (P/N: RP170-0) straight from the foil to the same water sample. (Note 2) 5. Close the vial with the caps tightly and swirl the vials several times to mix the contents. Wait for a reaction period of 10 minutes. After the reaction period is finished proceed as follows: 6. Add the contents of one Silica Citric Acid F10 Powder Pack (P/N: RP171-0) straight from the foil to the water sample. (Note 3) 7. Close the vial tightly with the cap and swirl several times to mix the contents. 8. Place the vial in the zero chamber making sure that the marks are aligned. Wait for a reaction period of 2 minutes. 9. Place the vial in the sample chamber making sure that the marks are aligned. 10.Press the [ZERO/TEST] key. The method symbol flashes for approx. 3 seconds. The result is shown in the display in mg/l SiO 2. Accuracy: 0 20 mg/l: ± 1 mg/l > mg/l: ± 2 mg/l > mg/l: ± 3 mg/l > mg/l: ± 5 mg/l 12

13 Methods Notes: 1. Temperature of the sample should be 59 F 77 F (15 C 25 C). 2. If Silica or Phosphate is present a yellow color is developed. 3. In this step any yellow color due to Phosphate is removed. 4. Interferences: Substance Iron Phosphate Sulfide Interference large amounts interfere does not interfere at concentrations less than 50 mg/l PO 4 at 60 mg/l PO 4 the interference is approx. 2% at 75 mg/l PO 4 the interference is approx. 1% interferes at all levels Occasionally water samples contain forms of silica which reacts very slowly with Molybdate. A pre-treatment with Sodium hydrogencarbonate and then with Sulfuric Acid will make these forms reactive to Molybdate (pretreatment is given in Standard Methods for the Examination of Water and Wastewater under Silica Digestion with Sodium Bicarbonate ). 13

14 Menu options Store Time On Off! Date Cal Menu selections 1. Press the [MODE] key and hold. 2. Turn the unit on using the [ON/OFF] key. Hold (or depress) the [] key until the 3 decimal points are displayed. The [!] key allows for selection of the following menu points: 1 recall stored data 2 3 setting the date and time 4 user calibration The selected menu is indicated by an arrow in the display. Confirm the selection with the [MODE] key. 1 Recall of stored data! The photometer shows the last 16 data sets in the following format (automatically proceeds every 3 seconds until result is displayed): Number n xx (xx: ) Year YYYY (i.e. 2008) Date mm.dd (monthmonth:dayday) Time hh:mm (hourhour:minuteminute) Method Result x,xx The [ZERO/TEST] key repeats the current data set. The [MODE] key scrolls through all stored data sets. Quit the menu by pressing [!] key. SET DATE YYYY (2 sec.)! 2 3 Setting date and time (24-hour-format) After confirming the selection with the [MODE] key the value to be edited will be shown for 2 sec. The setting starts with the year (YYYY) followed by the actual value to be edited. Same applies for month (mm), day (dd), hour (hh) and minutes (mm). Set the minutes first in steps of 10, press the [!] key to continue setting the minutes in steps of 1. Increase the value by pressing the [MODE] key. Decrease the value by pressing [ZERO/TEST] key. Proceed to the next value to be edited by pressing [!] key. After setting the minutes and pressing the [!] key the display will show IS SET and instrument returns to the measurement mode. 14

15 Calibration 4 User calibration cal CAL CAL SIt METHOD CAL METHOD RESULT CAL CAL RESULT + x On Off : : Note: user calibration (Display in calibration mode) factory calibration (Display in calibration mode) After confirming the selection with the [MODE] key the instrument will show CAL/SIt. Scroll through methods using the [MODE] key. Fill a clean vial with the standard up to the 10 ml mark, screw the cap on and place the vial in the sample chamber making sure that the marks are aligned. Press the [ZERO/TEST] key. The method symbol flashes for approx. 8 seconds. The display shows the following in alternating mode: Perform calibration with a standard of known concentration (see "Operation"). Press the [ZERO/TEST] key. The method symbol flashes for approx. 3 seconds. The result is shown in the display, alternating with CAL. If the reading corresponds with the value of the calibration standard (within the specified tolerance), exit calibration mode by pressing the [ON/OFF] key. Changing the displayed value: Pressing the [MODE] key once increases the displayed value by 1 digit. Pressing the [ZERO/TEST] key once decreases the displayed value by 1 digit. Press the corresponding key until the reading equals the value of the calibration standard. By pressing the [ON/OFF] key, the new correction factor is calculated and stored in the user calibration software. Confirmation of calibration (3 seconds). Recommended calibration values Tablet: between 0.5 and 1.5 mg/l SiO 2 Powderpack LR: 1mg/L SiO 2 Powderpack HR: 50mg/L SiO 2 15

16 Calibration Factory calibration reset Resetting the user calibration to the original factory calibration will reset all methods and ranges. Store Time RESULT On Off Date Cal A user calibrated method is indicated by an arrow while the test result is displayed. To reset the calibration press both the [MODE] and [ZERO/TEST] key and hold. Turn the unit on using the [ON/OFF] key. Release the [MODE] and [ZERO/TEST] keys after approx. 1 second. The following messages will appear in turn on the display: SEL CAL The factory setting is active. (SEL stands for Select) or: SEL cal Calibration has been set by the user. (If the user calibration is to be retained, turn the unit off using the [ON/OFF] key). SEL CAL On Off Calibration is reset to the factory setting by pressing the [MODE] key. The following messages will appear in turn on the display: Turn the unit off using the [ON/OFF] key. 16

17 Technical data Operating messages Light source: Battery: Auto-OFF: Technical Data LED, Filter ( = 430 nm) LED ( = 660 nm) 9 V-block battery (Life approx. 600 tests), without display light. Automatic turn off 20 minutes after last keypress Ambient conditions: 41 F 104 F (5 40 C) 30 90% rel. humidity (non-condensing) CE: Certificate for Declaration of CE-Conformity at To ensure maximum accuracy of test results, always use the reagent systems supplied by the instrument manufacturer. Operating messages Hı Lo Measuring range exceeded or excessive turbidity. Result below the lowest limit of the measuring range. Replace battery. Error codes E 01 E 10 / E 11 E 20 /E 21 E 22 Light absorption too great. Reasons: e.g. dirty optics. Calibration factor "out of range" Too much light reaching the detector. Battery capacity was too low during measurement. Change battery. E 70 E 71 E 72 E 73 E 74 E 75 SIt: SIt: SILr: SILr: SIHr: SIHr: Factory calibration incorrect / erase User calibration incorrect / erase Factory calibration incorrect / erase User calibration incorrect / erase Factory calibration incorrect / erase User calibration incorrect / erase For assistance with Error Codes or other technical issues, please contact Customer Service. (Phone: or Toll-free U.S ) 17

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19 Technical changes without notice FOR TECHNICAL ASSISTANCE, PRICE AND ORDERING INFORMATION: In the USA - Call or the distributor serving you Outside the USA: Call or the distributor serving you. Web: service@orbeco.com Fax: Orbeco-Hellige, Inc, All rights reserved. Printed in Germany. Updated March 2009, Edition 1