Instrument Description
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1 A Instrument Description A1 General LCM plus is a universal colorimeter for liquids suitable for manifold industrial applications. It is easy to handle and has a sturdy design. But what is really the reason why objective colour measurement of liquids is so important? The human eye is able to perceive about 100 spectral colours in approximately 100 degrees of brightness and saturation, which results in about 1 million perceptible shades. Therefore, hues are difficult to describe by subjective visual comparison. The specific colour of a product is often regarded as a sign of purity and quality, although that is not necessarily true. Clients often interpret deviations from the shade of an earlier production as defective product or supply and reject it preventively. In order to avoid such trouble, objective colour assessment, a uniform colorimetric system and reliable instrument are required for production and quality control of transparent coloured liquids. New Standard EN 1557 EN 1557 (Colorimetric characterization of transparent coloured liquids) now also defines colour measurement of liquids on the basis of the time-tested colorimetric standards of DIN The principle is to measure the X-, Y- and Z-transmissions. The sample is illuminated with a halogen lamp corresponding to standard illuminant C. On this basis, the LCM plus was developped for exact and reproducible measurements of transparent yellow-cast liquids. 30
2 A2 Instrument Design LCM plus measures transmissions of all transparent media. It operates with a halogen lamp producing standard illuminant C and uses the 2 standard observer as defined by DIN-standard A reference beam path compensates measuring values modified by driftings of lamps and temperatures during operation. Therefore, LCM plus provides an excellent long-term constancy and reproducible measuring results. The universal cuvette compartment suitable for 50 x 10mm square cuvettes and 11mm round glass cuvettes permits an optimum adaptation of LCM plus to the measurement tasks. In just one measurement, LCM plus evaluates by to the latest ISO-standards giving e.g. Iodine, Hazen or Gardner values. The basical instrument includes one optional colour number with the possibility of adding-on a random combination of colour numbers later or at once. These colour systems are available: Iodine number, Hazen number, Gardner number, Saybolt number and ASTM D number. To add-on more colour systems later, a program-module-box (bit-box) is supplied. The description of this bit-box is given in chapter D6. Fig. 9: Measuring principle of LCM plus 31
3 A3 Instrument Set-Up Unwrap the instrument carefully and check it for missing parts (delivery note). Please keep the packing box to pack the instrument safely in case it has to be transported again later. LCM plus should be placed on a level desk surface. The instrument comes with a power supply unit and adapter for the socket ( Volt / Hz) and is turned on by either pressing the OK-key or the grey menu key. Do not turn on and off too fast. Wait for 20 seconds before turning on again not to damage the electronic or mechanic system of the instrument. The blue lamp protection cover on the upper left part of the instrument serves to carry the heat off the lamp and must not be covered. As LCM plus is a sophisticated optical instrument, avoid the following at any rate: Do not use the instrument in direct sunlight. Do not allow water, inflammable or metallic objects to enter the instrument. Do not put filled cuvettes or heavy objects on the housing. Do not use the instrument in excessively moist, dusty or vibrating surroundings. Do not open the instrument. There are no parts in the housing for the user to check. If you have any questions of problems, please contact with our offices in Düsseldorf or one of our service stations (see page Fehler! Textmarke nicht definiert.). A4 Reference Standards In general, an absolutely transparent medium similar to the sample serves as a calibration or reference standard for coloriemtry on the transmission principle. To measure the colour of liquids, distilled water is filled into a cuvette similar to the measuring cuvette and used as a reference standards. In some exceptional cases where the density of the substance to be emasured differs from that of the distilled water, calibration is made against a colourless measuring medium. Calibration assigns the reference standard a transmission of 100% (or Iodine number = 0, Hazen = 0, etc.). As this assignment never changes, 100 no calibration value needs to be set for LCM. Instead, just fill a cuvette with the reference standard and put it into the cuvette compartment to perform calibration. 32
4 B Operation B1 Control And Functional Elements Figures Abb. 2 and Abb. 3 show the control and functional elements of LCM plus. Display Cuvette compartment Lamp cover Cursor keys Fig. 10: Front view OK-key Menu key Cal- and Measure key Battery cover Printer Mains socket Bit-Box compartment port Fig. 11: Back view 33
5 LCM plus is operated with 8 keys. The following table shows the keys and displays in the operating instructions. Cursor keys Calibration and Measure key Menu key OK-Key Display and input area Definition Press left, right, upper or lower cursor key Press blue key (Calibration) Press green key (Measurement) Turn instrument on Quit submenu option Turn instrument on Confirm or call the selected action Display of current values, data, submenus and input areas of the single options. The input area is marked by a window inviting inputs. Representation CAL calibration key (blue) Meas measure key (green) Menu key (grey) OK Aut.shut off: 30 min Menu selection Selecting an option with the cursor keys or key OK e.g..:_config, another window opens offering more options: Switch Off Config Printer Error messages It is necessary to acknowledge every error message by pressing the grey menu key, or the instrument stops operating. Min. limit: 10 34
6 B2 Initial Start-Up of the Instrument For start-up plug-in the mains plug and press the OK-key or grey menu key. The port for the power supply unit is at the rear of the instrument (page 7, Abb. 3, Items 10 and 8). When the instrument is on, the display indicates instrument type and number of EPROM-version while the self-check is running. When self-check and zero measurement are over (approx. 20 sec.) you are prompted to insert a calibration or sample cuvette. LCM plus V1.00 Pleas ins. cuv. for sample LCM plus V : B3 Printer Start-Up The supply voltage for the printer is turned on and off with the green toggle switch 1 on the right of the printer s front. The printer is on when the black key 2 is in neutral position (1) and off when key 2 is at (0). Paper feed is done pressing the ' ' part of key 2 next to the printing unit. B3.1 Connection to LCM plus The printer is connected by plugging the supplied connection cable to the RS232-port on the rear side of LCM plus. B3.2 Change paper Turn the printer on and open the flap 3 behind the printing unit. Put a new reel of paper into the paper container and unroll approx. 10cm of it. Then lead the free beginning of the paper into the slot until perceiving a slight resistance. Press the paper feed key and push the paper on carefully. Hold the key down until the paper passes the tear bar. Finally close the flap again. Fig. 12: Printer LD
7 B4 Battery Mode LCM plus can be used with power supply unit or rechargeable batteries. For the latter mode, open the cover of the battery compartment and insert the batteries as follows: 4. Insert the battery with the switch to the right into the holder until only one contact remains visible. 5. Shift the battery from the left side over the contacts, passing a slight resistance. 6. A beep indicates that the batteries are placed and ready for operation (only when the instrument is not connected to the mains). Battery switch Battery Fig. 13: Insertion of rechargeable batteries Contact Attention: The contacts must not get into contact with metal or greasy parts. To recharge the batteries, insert them into the compartment and connect LCM plus to the mains with the power supply unit. We recommend a continuous loading time of 14 hours before the first use. To exploit the battery capacity best, charge and discharge it always entirely. The display of LCM plus informs about the current discharge degree of the battery when the instrument is turned on. When the battery is discharged, a beep and a display message are given. The message must be acknowledged with the grey menu key to go on working for a short while. The display message battery empty means that the battery is definitely discharged and needs recharging. 36
8 B5 Turning-Off LCM plus turns off automatically by a timer function. Manual turning-off is possible, too. Manual Turning-Off Press Cursor-Key in the measuring menu and select option Switch Off with the OK-key. Then the instrument turns off. Turning-Off Via Timer On delivery, the timer of LCM plus is set to automatical turningoff time of 30 minutes. The automatical turning-off is only active if no measurement was made within the given period and no cuvette is in the compartment. The setting can be modified within the tolerances of 10 to 60 minutes (cp. C8.2). LCM Switch Offplus Config Printer V1.05 B6 Photometric Preparation The photometric preparation requires utmost care, because careless sample preparation is the major source of trouble, and not the handling of the instrument itself. Cleanliness is of vital importance in photometry. Therefore, clean the glass cuvettes immediately after use. Employ only optically perfect samples for measuring. They must be clean and not show any signs of opaqueness. Air bubbles in the sample or at the cuvette sides influence the measuring result. They can be avoided by filling the liquid slowly into the cuvette. Pasty or solid products should be melted and filled-in without bubbles, if they cannot be measured as they are. B6.1 Sampling And Sample Preparation Take a sample from the product you want to measure in accordance with DIN part 1. Eliminate turbidities by heating or filtration. Heat partly solid samples before measuring in order to dissolve the solid share in the liquid one. The preparation must not cause any chemical changes in the sample. During the measurement there should be no bubbles in the sample. 6 There are several cuvette types available for colour measurement with LCM plus, differing by material (glass, polystyrene or PMMA 7 ) and path length (11mm and 50mm). The program calculates automatically Iodine, Hazen, Gardner, Saybolt and ASTM D numbers under consideration of the cuvette type employed. For the 11mm disposable round glass cuvettes, a dry thermostat is available to warm up to 15 cuvettes to 100 C or 148 C. 6 7 Acc- to DIN 6162, ed , para. 5 a. 6 Polymethylmethacrylate 37
9 C Colour Measurement Whenever the instrument is turned on, a zero measurement is made, taking the empty value (i.e. the pure transmission values without cuvette inserted) of the optical beam path and comparing it with the empty value obtained in the previous zero measurement. If the difference between both empty values is near zero, you can start measuring without calibration. Calibration is only required in case of considerable deviations of the empty value due to e.g. fluctuations of temperature. The calibration remains valid until the next recalibration. LCM plus features a calibration memory for both path lengths employed (50mm square cuvette and 11mm round cuvette). If you have to use two different path lengths, owing to the nature of your samples (e.g. bright samples with Hazen values below 50 or strongly coloured samples with greater Gardner values), it is possible to calibrate both path lengths and then toggle between them. LCM plus uses the corresponding set of calibration data automatically. C1 Calibration LCM plus features a calibration memory for 11mm Dr. Lange round cuvettes and 50mm square cuvettes. To be on the safe side, calibrate LCM plus at least every day. In the calibration, the employed medium is assigned a transmission of 100% over the whole spectral range. Observe the following rules for calibration: The cuvette type selected for calibration must be identical to the one used for measurement, otherwise wrong Iodine, Hazen and Gardner values are given. Use always clean cuvettes and fresh distilled water for calibration. Instrument calibration for colour measurement 2. Turn-on instrument and printer, if desired. After self-check and zero measurement, LCM plus might ask for calibration. If LCM plus is already on, make sure the cuvette compartment is empty and press the blue CAL - key. The display reads: Zero meas.m. Please wait Pleas ins. cuv. for calibration 2. Fill a clean cuvette (material and path length to suit your samples) with distilled water and put it into the measuring compartment. Calibration Please wait 4. LCM plus detects the cuvette type automatically. 4. Now press the blue CAL - key again to trigger calibration. 5. When the calibration is over and the printer is on, date, time and selected cuvette type are printed, e.g. : 38
10 Calibration with 11 mm circular cuv. ok! 12: Then LCM plus prompts Please insert sample cuvette. Now you can insert your sample cuvette directly. As soon as you have done so, LICO starts measuring automatically. To calibrate one more path length, remove the cuvette and press the blue CAL -key again. iodine color value Please calibrate carefully to avoid mismeasurements caused by faulty calibration _DIM Conf 11 39
11 C2 Colour Measurement The colours of all transparent liquids can be measured, using 50mm square cuvettes or 11mm round glass cuvettes, depending on their transmittances. If required, select another colour system for printer output in the configuration menu (cp. page 19). Instrument preparation 3. Turn instrument and printer on. 4. Calibrate the instrument as described in chapter. C1. Measuring procedure 1. Fill the sample liquid into a cuvette and insert it into the corresponding compartment. Measurement starts automatically. 2. After measuring, the colour values of the sample will appear on the display and be printed, e.g. iodine color value 2.6 _DIM Conf Iodine color value 507 Hazen color value 3. Now press the -key (DIM) until the desired colour system appears on the display. 4. The colour system will be displayed during the measurements to follow. Hazen color value 507 _DIM Conf 11 40
12 C3 Iodine Number DIN 6162 defines the Iodine colour number as mg of iodine per 100ml of potassium iodide solution. Colour matching by the Iodine number serves to judge the shade depth of clear liquids like e.g. tensides, plasticizers, resins, oils and fatty acids, whose colours resemble that of an equally layered solution of potassium iodide. For Iodine numbers less than or about 1, the Hazen number according to DIN-ISO 6271 should be preferred. 8 Sampling and preparation are described in chapter B6. A satisfactory precision of the Iodine value is achieved with a 11mm round glass cuvette. Measuring procedure 2. Fill the sample liquid into a cuvette and insert it into the corresponding compartment. Measurement starts automatically. 4. After the measurement, the colour value is indicated on the display. iodine color value 70.5 _DIM Conf Now press the -key (DIM) until the Iodine number appears on the display. C4 Hazen Colour Number (APHA-Method) The Hazen colour number (DIN-ISO 6271, also known as "APHA-Method or Platinum-Cobaltscale ) is defined as mg of platinum per 1l of solution. The Hazen parent solution is composed of 1.246g potassium-hexachloroplatinate (IV) and 1.00g cobaltous (II)-chloride dissolved in 100ml of hydrochloric acid and filled up with distilled water until reaching 1000ml. The Hazen colour scale serves to determine the colours of nearly water-clear products. It has a narrower gradation in the light yellow range than the Iodine scale and reaches even water-clear casts. Attention: Samples with Hazen values between 50 and 1000 can be measured with sufficient accuracy in 11mm round cuvettes. Hazen values < 50 should be mesured in 50mm cuvettes, Hazen values < 10 should be measured with the cuvette which was used for calibration, because nearly water-clear products are susceptible to giving faulty measuring results due to cuvette tolerances. 8 acc. to DIN 6162, Edition 12.81, para. 1 41
13 Measuring procedure 1. Fill the sample liquid into a cuvette and insert it into the corresponding compartment. Measurement starts automatically. 2. After the measurement, the colour value is indicated on the display. Hazen color value 20 _DIM Conf Now press the -key (DIM) until the Hazen number appears on the display. C5 Gardner Colour Number The Gardner colour number is defined in DIN ISO The lighter Gardner colour standards (1 to 8) are based on potassium-chloroplatinate solutions, colour numbers 9 to 18 on ferric(iii)-chloride, cobaltous(ii)-chloride and hydrochloric acid solutions. LCM plus determines the Gardner number at all cuvette path lengths (in 50mm cuvettes only values between 0 and 4), with 11mm cuvettes providing sufficient accuracy. Measuring procedure 1. Fill the sample liquid into a cuvette and insert it into the corresponding compartment. 2. After the measurement, the colour value is indicated on the display. 3. Now press the -key (DIM) until the Gardner number appears on the display. Gardner value 6.5 _DIM Conf 11 color C6 Mineral Oil Colour Number ASTM D 1500 And ISO 2049 The Mineral Oil Colour Scale is used for matching the colours of mineral oil products like lubricating oil, fuel oil, diesel oil and paraffins. The colour scale begins at 0 for water-clear, colourless oils and ends at 8 for very dark brown oils. Visual matching is in steps of 0.5 ( ). LCM displays the results in steps of 0.1. For samples of stronger hue than colour glass 8, colour value D8 is displayed. Owing to the intensive colour gradation of the ASTM 9 D 1500 colour number, this is only determined for the 11mm round cuvette. There is no determination of path length 50mm American Society for Testing and Materials
14 Measuring procedure 1. Fill the sample liquid into a cuvette and insert it into the corresponding compartment. 2. After the measurement, the colour value is indicated on the display. 3. Now press the -key (DIM) until the ASTM- number appears on the display. ASTM D _DIM Conf 11 C7 Saybolt Colour Number (ASTM D 156) The Saybolt colour scale is used to match colours of refined oil products like fuel and kerosene or also petroleum waxes and pharmaceutical white oils. Its colorimetric characteristics are comparable with those of the Hazen scale (APHA). The Saybolt scale begins at +30 (brightest coloration, corresponding to approx Hazen) and ends at -16 (stongest coloration, corresponding to approx. 350 Hazen). Measurements can be made with cuvettes of 11mm or 50mm path lengths. The greater the path length, the better the measuring accuracy (50mm recommended). 1. Fill the sample liquid into a cuvette and insert it into the corresponding compartment. 2. After the measurement, the colour value is indicated in the configured colour system on the display. 3. Now press the -key (DIM) until the Saybolt number appears on the display. Saybolt value 24 _DIM Conf 50 color 43
15 C8 Configuration The configuration serves to select the colour systems for the print-out and general instrument settings like e.g. date/time, language, etc. Press cursor-key for configuration. The selection menu shown at the right opens. Move the bar to the menu options with cursor-key or. The option in reverse presentation can be selected by pressing key OK. C8.1 Turning-off After selecting option Turn-off and pressing key OK, LCM plus is turned off. LCM Switch Off plus Config Printer V1.05 LCM Switch Offplus Config Printer V1.05 C8.2 Configure After selecting option Config. and pressing key OK, another menu window opens. The small arrow in the frame window at the right indicates that there are more options to follow. Langue selection These languages are at choice: German (D), English (GB), French (F), Swedish (S), Spanish (E), Dutch (NL), Italian (I), Polish (PL) and Danish (DK). Move the bar to the desired language and select it with key OK. Date and time After selecting option Date and pressing key OK, a window opens to set date and time. Move the blinking cursor to the digit you want to change by cursor-key or. Cursor-keys or increase or decrease the blinking digit by one. Finish the setting with the OK -key. LCM Switch Offplus Config Printerer V1.05 Language Date Timer Display LCM Turn-offplus Language select: D Config. GB FPrinter S E LCM Turn-off Date Time plus Config V1.05 Printer 44
16 Timer Selecting option Timer and pressing key OK opens a window to set timer functions "Aut.shut off" and "delay meas.". Set the desired value with cursor-keys and. Auto shut off time Selecting option "Aut.shut off" and pressing key OK opens a window to set the turn-off time. Move the blinking cursor to the digit you want to change by cursor-key or Cursor-keys or increase or decrease the blinking digit by one. Finish the setting with the OK -key. Measurement delay Selecting option "delay meas." and pressing key OK opens a window to set the Measurement delay. Move the blinking cursor to the digit you want to change by cursor-key or. Cursor-keys or increase or decrease the blinking digit by one. Finish the setting with the OK -key. Turn-off LICO 100 Adjust timer: Config Aut.shut off Printer delay. meas. LICO Aut.shut off: min V1.00 LICO delay. meas sec V1.00 Display Selecting option "Display and pressing key OK opens a window for display settings of "Contrast" and "Lighting". Make your choice with the cursor-keys and and confirm it with key OK. Printer At this option, you can set more colour systems for printer output. The system selected at display is marked and will be printed in the first line. To add more colour systems, move the bar to the desired system with cursor-keys and and confirm your choice with the OK - key. When the cursor passes the upper or lower margin of the menu, it pages on and shows more options. Here you can add date and time to the measurement. To finish the configuration of the printer output, select "back" and press key OK. Turn-off LICO 100 Adjust display: Contrast... Config V1.00 Lighting Printer LICO Turn-off Iodine number 100 Config Hazen number V1.00 Gardner no. Printer Saybolt no. LICO Turn-off ASTM D Config Date / Time V1.00 back Printer The program returns to the beginning of the configuration. 45
17 C8.3 Instrument check LCM plus can be checked with a certified test solution set addista -color in compliance with ISO 9000ff. D Technical Notes D1 Error Messages The following display messages indicate errors of operator or instrument. *** Result outside the measuring range. Please remove cuvette! There is a cuvette left in the cuvette compartment. Insert paper Error! Calibration No Signal Lamp? Put new reel of paper into LD 500. The lamp is probably broken. Exchange it as described in chapter D3. If one of these error messages appears, please check whether e.g. the printer is connected properly, calibration is correct and the sample cuvette at its place. If you still cannot eliminate the error, contact our service department or field service. 46
18 D2 Maintenande and Test Media Control Even a perfected product like LCM plus requires careful handling. Use a dry cloth or a mild household cleaner for the housing, but never solvents like naphta, acetone or the like. The optical elements should be cleaned by our maintenance staff. A certified set of test solutions is available for test media control according to ISO 9000ff with order no The test set comprises six bottles containing 50ml of test solution each, a quality control certificate according to DIN part 18, and a test protocol for the documentation of reference, actual and tolerance values. LCM plus is tested as described in enclosed test instruction. The instrument should be tested in regular intervals of 1 to 2 weeks, depending on its application and frequency of use. Fig. 14: Test solution addista-color 47
19 D3 Lamp Exchange The lamp compartment is left of the display and covered with a slotted cap on the upper side of the housing. If the lamp is broken, it should be exchanged by Dr. Lange service staff, because w e recommend a general instrument check-up after an operating period of 1-2 years. If you insist on doing it yourself, proceed as follows: R e m o v e p o w e r s u p p l y u n i t o r b a t t e r y! Remove the grey cover of the bit-box. Loosen the fixture of the bit-box by pushing the locking clamp 1 and put it apart. Unplug contact 2 from the lamp. Loosen the metal clamps 3 at the upper end one be one from their stay and hinge them away. Take the lamp 4 off and put in a new one with the marking pointing to the left. Attention: Do not touch the glass bulb of the lamp. Fig. 15: Removing the fixture of the bit-box Hinge the metal clamps back to their places and fix them to their stay. Connect the new lamp with the plug-in contact 2 and do the same steps as for dismantling, but in reverse sense. Only when the instrument is mounted completely, turn it on and test it. Fig. 16: Lamp exchange D4 RS232C-Interface of LCM plus LCM plus has a serial interface at its rear side (page 7, Abb. 3) corresponding to RS 232 C and V24-standard. 48
20 D5 Technical Data Viewing geometry: 0 /180 (transmission) Display/operation: Backlit LC-display (128 x 64 Pixels) Reference standard: Distilled water Spectral range: 8 spectral wavelengths ranged from 400nm to 700nm Wavelength accuracy: ± 2 nm Diffuse light: < 1 % Light source: Krypton lamp Warming-up: approx. 2 minutes Reproducibility: ± 2 Hazen at 50mm path width Documentation: External printer LD 500 Control: Integated microprocessor Measuring time: approx. 10 sec. Program functions: Iodine number Hazen-(APHA) numberl Gardner colour scale ASTM D 1500 number Saybolt-number Cuvettes compartment: 50mm x 10mm square cuvette 11 mm round cuvette with automatic detection Control elements: 8 Foil keys Data interfaces: RS 232 C for LD 500-Printer Mains connection: power supply unit V, 47/63 Hz Dimensions: 260mm x 90mm x 200mm (WxHxD) Weight: approx. 1350g Subject to technical modifications. 49
21 E Annex E1 Spares and Accessories Identification: Quantity/Pcs. Order number: Square plastic cuvettes 10mm * 50mm Square glass cuvette 10mm * 50mm Round glass cuvettes 11mm Cuvette holder for 16 round cuvettes Printer paper 4 reels 6388 Exchange lamp Test solutions addista-color Rechargeable battery 1.4Ah E2 Regulations 10 and Standards EN 1557 Colorimetric characterization of optically clear coloured liquids (products) as X, Y, Z - tristimulus values in transmission, 10.'92 (DIN 53995) DIN 5033 Colour measurement (ASTM E 179, ISO 7724) DIN 6174 Colorimetric evaluation of colour differences (ASTM E 308) DIN 6162 ISO 6271 ISO 4630 ASTM D1500 Determination of iodine colour number Clear liquids;estimation of colour by the platinum-cobalt-scale (Hazen colour number, APHA colour number, also ASTM D , ASTM D , ASTM D , BS 2690:1956.) Estimation of colour of clear liquids by the Gardner colour scale, also ASTM D Standard Test Method for ASTM Color of Petroleum Products (ASTM Color Scale), also DIN/ISO ASTM D156 Standard Test Method for Saybolt Color of Petroleum Products (DIN 51411). ASTM D1925 ASTM D 6045 Yellowness-Index Standard Test Method for Color of Petroleum Products by the Automatic Tristimulus Method Standards can be ordered at: Beuth Verlag GmbH, Burggrafenstraße 6, D Berlin, /2601-0
22 Notizen/Notes: 51
23 52
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