Index Instruments Limited PTR 2a and PTR 2a X High Accuracy Refractometers Operators Handbook © This handbook is copyright Index Instruments Ltd. 2005 INDEX INSTRUMENTS LIMITED Index Instruments Limited Bury Road Industrial Estate Ramsey, Huntingdon, Cambs., PE26 1NF England Tel No.: +44 (0)1487 814313 Fax No.: +44 (0)1487 812789 E-mail: [email protected] Website: www.indexinstruments.com PTR 2a Handbook – Issue 3 June 2009 OPERATOR'S HANDBOOK PTR 2a and PTR 2aX AUTOMATIC REFRACTOMETER Issue 3 June 2009 MODE D’EMPLOI REFRACTOMETRES AUTOMATIQUES A EFFET PELTIER Modèles PTR 2 et PTR 2 X Version 3 Juin 2009 BEDIENUNGSANLEITUNG für die AUTOMATISCHEN REFRAKTOMETER PTR 2 und 2 X Ausgabe 3 Juni 2008 MANUAL DEL OPERADOR REFRACTOMETROS AUTOMATICOS MODELOS PTR 2 y PTR 2 X Documento 3 Junio 2008 © Index Instruments Ltd. 2009 INDEX INSTRUMENTS Ltd. Industrial Estate, Bury Road, RAMSEY, Huntingdon, Cambridgeshire, PE26 1NF ENGLAND Tel: +44 (0)1487 814313 Fax: +44 (0)1487 812789 E-mail: [email protected] Web site: www.indexinstruments.com i PTR 2a Handbook – Issue 3 June 2009 ii PTR 2a Handbook – Issue 3 June 2009 CONTENTS INSTALLATION CHECK LIST 1 INTRODUCTION 2 WARNINGS 3.1 INSTALLATION, PTR Refractometer 3.2 PRINTER INSTALLATION 4.1 DIAGRAM OF INSTRUMENT 4.2 DISPLAY - BASIC 5 OPERATION 6 SAMPLE HANDLING 6.1 STANDARD HINGED SAMPLE COVER 6.2 SOLID SAMPLES 6.3 SAMPLING WITH FUNNEL CELL 6.4 SAMPLING WITH FLOW / INJECTION CELL 7 WATER REFERENCE POINT (ZERO CHECKING AND SETTING) 8 ADVICE ON TEMPERATURE CONTROL 9 OUTPUT / INPUT 9.1 CONNECTING A PRINTER 9.2 REMOTE PORT 9.3 BAR CODE READER 9.4 AUXILIARY PORT 10 FITTING / CHANGING SAMPLE CELLS 11 REMOTE CONTROL UNIT (Optional Accessory) 1 3 4 8 9 10 11 12 13 13 15 16 18 20 22 23 23 24 24 25 26 27 APPENDIX 1: Technical Specification APPENDIX 2: RI Water v Temperature APPENDIX 3: Use of Solid Test Pieces APPENDIX 4: Refractometer Reference Standards APPENDIX 5: Marginal Substances APPENDIX 6: Samples of Print Out APPENDIX 7: Error Messages APPENDIX 8: Brix Scale APPENDIX 9: FURTHER INFORMATION ON PROGRAMMABLE FUNCTIONS APPENDIX 10: Guarantee APPENDIX 11: Declaration of Conformity INDEX 29 31 32 33 34 35 36 37 38 43 45 47 iii PTR 2a Handbook – Issue 3 June 2009 iv PTR 2a Handbook – Issue 3 June 2009 INSTALLATION CHECK LIST For reference you may wish to complete the following check list for your particular installation. The information recorded will assist traceability records. Refractometer model no. PTR 2a / PTR 2a X * Serial number Date installed Location Service interval Recalibration interval Accessory check list: Power supply Mains lead Operator's Handbook Dust cover Cell type: Hinged sample cover (normally fitted yes as standard) /no* List other cells: OPTIONAL ACCESSORIES: Printer Bar code reader Remote control * Delete as appropriate 1 PTR 2a Handbook – Issue 3 June 2009 2 PTR 2a Handbook – Issue 3 June 2009 1 INTRODUCTION Thank you for choosing an INDEX INSTRUMENTS PTR 2a or 2aX automatic refractometer. The PTR refractometers have been designed to be accurate, reliable and simple to use. The temperature is controlled electronically using a Peltier cell to a high degree of stability, removing the need for an external thermocirculator. The PTR 2a and 2aX models are the simplest models within the range of PTRs and are ideal for routine measurements at a single fixed temperature on a single fixed scale. They are therefore extremely easy to set up and use. The reading can be output to a computer or printer at any time. Sample identification can be added using a bar code reader. Suitable printers and bar code readers are available as optional accessories from Index Instruments. By purchasing the optional remote control unit, access can be gained to additional facilities such as changing the scale, changing the sample temperature or altering the mode of operation. Use of the remote control also allows the addition of time, date, instrument serial number or sample number to the print out. Refractive index is measured by the "critical angle" method similar to the method used in a visual Abbe refractometer. Because back reflected light is used, very dark samples can be measured as easily as clear samples. The wavelength of light used is sodium yellow (589nm). The PTR refractometer has an almost indestructible sapphire prism, a sealed casing, no moving parts and a selection of optional sample cells making it both extremely reliable and versatile in use. Although we are sure you want to start making measurements immediately, to get the best out of your new PTR, please take a little time to read this handbook, especially the warning section and sections on sample handling. All PTRs are very carefully calibrated and inspected on an individual basis before being packed with equal care for dispatch to all parts of the world. Should you encounter any problems on initial installation, please contact your local agent or Index Instruments for advice. 3 PTR 2a Handbook – Issue 3 June 2009 2 WARNINGS MANUFACTURER'S STATEMENT ON CALIBRATION AND GUARANTEE Index Instruments Ltd apply modern computerized calibration methods using skilled staff working in temperature controlled calibration rooms. The calibration samples used on the PTR range from reference crystals to standard liquids covering the whole range of the instrument. In addition to the above, each individual instrument is tested on a range of known, difficult samples, many of which cannot be read on a visual refractometer. In common with manufacturers of similar equipment, we can only guarantee compliance with the quoted specification at the actual time of calibration and final testing. The reason for this is that, while we take meticulous care in calibrating, packing and shipping instruments, we have no control over how an instrument is handled or used once it leaves our premises. While our guarantee covers faulty parts and materials for one year, it is the responsibility of the purchaser/user to check that the calibration is of sufficient accuracy for their requirements. Index Instruments Ltd will not be held responsible for calibration errors, however caused, and absolutely excludes itself and its staff from any subsequent loss, even in the unlikely event of negligence on our part. Our responsibility is limited to the repair or replacement of the faulty equipment. Never attempt to open the sealed base unit of the PTR. Opening the sealed base unit invalidates the guarantee. There are no user adjustments inside this sealed unit. If a fault develops which you suspect is within the sealed unit, contact Index Instruments Ltd or your local distributor. CHEMICAL COMPATIBILITY AND AGGRESSIVE SAMPLES No instrument can be completely impervious to attack from all types of products and chemicals and you should therefore read the following warning before using the PTR refractometer. The materials that normally come into contact with the sample on a standard PTR are:- synthetic sapphire, stainless steel, silicone rubber, "Delrin" plastic (Acetal Homopolymer). Samples which attack these materials should not be used on the PTR. If your samples do attack any of the above, it may be possible to supply a specially modified instrument to suit your particular samples. Please contact Index Instruments Ltd. Samples that are NOT suitable include strong acids and strong alkalis and solvents such as heptane. It is best to avoid prolonged contact with any aggressive sample or solvent. ELECTRICAL SAFETY Always connect the instrument as instructed in this handbook. Disconnect power supply from mains before servicing. 4 PTR 2a Handbook – Issue 3 June 2009 (F) 2 MISE EN GARDE AVANT L’INSTALLATION CONSEILS ELEMENTAIRES DE SOIN D’UTILISATION Le prisme est en saphir synthétique et ne risque donc pas d'être endommagé par des échantillons corrosifs ou abrasifs. Par contre, aucune colle, ni joint d'étanchéité, n'étant complètement inerte à tous les produits chimiques, dans le cas d'utilisation d'échantillons ou de solvants de nettoyage particulièrement agressifs, consultez-nous et nous vous conseillerons pour l'application projetée. Le PTR est auto-thermostaté électroniquement par effet Peltier et un thermomètre incorporé contrôle en permanence la température de l'échantillon et l’affiche pendant tout le temps que dure la mesure. ETALONNAGE EN SORTIE D’USINE Index Instruments a étalonné votre PTR avec soin dans son laboratoire de métrologie qui est sous température contrôlée et régulée. La procédure utilisée comprend l’emploi d’étalons solides et liquides qui couvrent la totalité de la plage de mesure de l’appareil. En outre chaque appareil est ensuite testé avec des produits réputés difficiles à mesurer et dont l’indice de réfraction ne peut pas être mesuré avec un réfractomètre d’Abbe classique. Comme tous les fabricants d’appareils similaires, Index Instruments ne peut que garantir que l’appareil étalonné a satisfait aux tests de conformité au moment de l’étalonnage. En effet, malgré le soin que nous apportons ensuite aux conditions de stockage et à l’emballage de nos appareils, nous n’avons aucun moyen de contrôle ni sur les conditions réelles de transport, ni sur les conditions d’utilisation de nos appareils. Index Instruments ne peut donc être tenue pour responsable d’erreurs éventuelles d’étalonnage qui surviendraient soit à la livraison soit en cours d’utilisation de ses appareils, ni des conséquences qui pourraient en résulter. La seule responsabilité d’Index Instruments ou de son distributeur local ne peut être alors que la réparation de l’appareil ou son remplacement. COMPATIBILITE CHIMIQUE POUR ECHANTILLONS AGRESSIFS Certains échantillons peuvent être chimiquement agressifs. Aussi il vous appartient de vérifier la compatibilité chimique des matériaux qui sont ou peuvent être en contact avec vos échantillons. Ces matériaux sont : le saphir de synthèse, l’acier inox 316, le caoutchouc silicone, le Delrin (Acetal Homopolymère). Nous déconseillons formellement d’utiliser votre réfractomètre PTR avec des acides forts, des bases fortes et de l’heptane. D’autres échantillons peuvent s’avérer néfastes pour votre réfractomètre ; en cas de doute, n‘hésitez pas à nous contacter. SECURITE ELECTRIQUE Avant de brancher votre réfractomètre, lisez attentivement les recommandations du chapitre 3.1. Ayez toujours le réflexe de ne jamais ouvrir le boîtier de l’alimentation électrique sans l’avoir débranché au préalable. 5 PTR 2a Handbook – Issue 3 June 2009 (D) 2 Besondere Hinweise für den Anwender Herstellerzertifickat für Kalibrierung und Garantie Index Instruments hat sehr gut ausgebildetes Personal, um mit Hilfe des Computers moderne Kalibriermethoden in speziell hierfür eingerichteten Räumen durch zuführen. Die für das PTR zur Kalibrierung verwendeten Proben, von Referenzkristallen bis hin zu Flüssigen Standards, decken den ganzen Messbereich des Gerätes ab. Zusätzlich wird jedes Gerät noch von bekannten sehr schwierigen Proben getestet, die für ein visuelles Refraktometer nicht messbar sind. Ebenso wie Hersteller von ähnlichen Geräten, können wir nur die angegebenen Spezifikationen garantieren, die bei der Kalibrierung und dem Abschlusstest festgestellt worden sind. Wir verwenden äußerste Sorgfalt für die Kalibrierung, Verpackung und Versendung der Geräte, aber wir haben keine Kontrolle, wie ein Gerät behandelt oder benutzt wird, wenn es unsere Firma verlässt. Unsere Garantieleistung für 1 Jahr beinhaltet Ersatz von fehlerhaften Teilen und Material. Der Endbenutzer hat deshalb zu prüfen, ob die Kalibrierung für seine Anforderungen ausreichend ist. Index Instruments schließt jegliche Haftung für Kalibrierfehler aus und übernimmt die volle Verantwortung für die Reparatur oder den Ersatz von fehlerhaftem Material innerhalb der Garantiezeit. Das versiegelte Gehäuse darf vorn Anwender des PTR nicht geöffnet werden. Das Öffnen des versiegelten Gehäuses macht die Garantie ungültig. Für den Anwender gibt es keine Bedienelemente innerhalb des Gehäuses. Sollte der Anwender vermuten, dass ein Fehler innerhalb des Gehäuses ist, so solte er Index Instruments oder seinen zuständigen Lieferanten verständigen. Chemische Verträglichkeit und sehr stark aggressive Proben Kein Gerät kann vollständig von der Aggressivität von den verschiedensten Produkten und Chemikalien geschützt werden. Deshalb sind die folgenden Hinweise sorgfältig zu lesen, bevor das PTR-Refraktometer in Betrieb genommen wird. Die Materialien des PTR's welche in Kontakt mit der Probe kommen können sind: das synthetische Prisma, Edelstahl, Silikongummi, Delrinplastik (Acetat Homopolymer). Proben, die all diese Materialien angreifen, solten nicht mit dem PTR in Berührung kommen. Sollte jedoch Ihre Probe nur eine davon angreifen, so ist es möglich, ein modifiziertes Gerät zu liefern, welches speziell für Ihr produkt geeignet ist. Deshalb sollte man vorher den Hersteller oder seinen Vertreter befragen. Proben die nicht verwendet werden dürfen, sind sehr starke Säuren und Alkalien, sowie Lösungen wie z. B. Heptan. Es ist daher zu empfehlen, den längeren Kontakt mit jeglichen aggressiven Proben und Lösungen zu Vermeiden. Elektrische Sicherheit Alle elektrischen Leitungen sollen genau wie im Handbuch beschrieben verbunden werden. Die Stromversorgung ist vor dem öffnen vom Netz zu trennen. 6 PTR 2a Handbook – Issue 3 June 2009 (E) 2 ADVERTENCIAS DECLARACION DEL FABRICANTE SOBRE CALIBRACION Y GARANTIA Index Instruments Ltd. Aplica modernos métodos computarizados de Calibración utilizando personal capacitado, trabajando en cuartos de Calibración con Temperatura controlada. Las muestras de Calibración usadas en la Línea de los Refractómetros PTR abarca desde cristales de referencia hasta estándares líquidos cubriendo el rango total del Instrumento. En adición a lo anterior, cada instrumento individualmente sobre un rango de conocidas, muestras difíciles, muchas de las cuales no pueden ser leídas en un Refractómetro Visual. En común con los productores de equipos similares, nosotros podemos garantizar únicamente conformidad con las especificaciones cotizadas al momento actual de la calibración y prueba final. La razón para esto es que mientras que nosotros tenemos un meticuloso cuidado en la calibración, empaque y despacho de los instrumentos, nosotros no tenemos control sobre cómo un instrumento es manejado o usado una vez este sale de nuestras instalaciones. Mientras nuestra garantía cubre fallas en partas y materiales por un año, es la responsabilidad del comprador o usuario chequear que la calibración esté lo suficiente precisa para sus requerimientos. Index Instruments Ltd no se hace responsable de errores de calibración, sin embargo causados, y absolutamente se excluye el mismo y su personal de cualquier subsecuente pérdida, aún en el muy poco probable evento de negligencia de nuestra parte. Nuestra responsabilidad es limitada a la reparación o reemplazo del equipo que falle. Nunca intente abrir la base de la unidad sellada del PTR. Abriendo la base de la unidad sellada invalida la garantía. No hay ajustes que deba realizar el usuario dentro de la unidad sellada. Si una falla se presenta la cual usted sospecha que está dentro de la Unidad sellada, contacte a Index Instruments Ltd o a su distribuidor local. COMPATIBILIDAD QUIMICA Y MUESTRAS AGRESIVAS Ningún instrumento puede ser completamente insensible al ataque de todo tipo de productos y químicos y usted debería por consiguiente leer la siguiente advertencia antes de usar el Refractómetro PTR. Los materiales que normalmente están en contacto en un Refractómetro PTR estándar son: - zafiro sintético, acero inoxidable, silicona, plástico “Delrin” ( Acetal Homopolimero). Muestras que ataquen estos materiales no deben ser usadas sobre el Refractómetro PTR. Si sus muestras atacan cualquiera de estos materiales es posible suministrarle un instrumento especialmente modificado que sea apropiado a sus muestras particulares. Por favor contacte Index Instruments Ltd. Muestras que NO son apropiadas incluyen ácidos fuertes y bases fuertes y solventes tales como el Heptano. Es mejor evitar cualquier prolongado contacto con cualquier muestra agresiva o solvente. SEGURIDAD ELECTRICA Siempre conecte el instrumento como es indicado en este manual. Desconecte la fuente de poder del circuito principal antes de cualquier revisión o mantenimiento. 7 PTR 2a Handbook – Issue 3 June 2009 3.1 INSTALLATION PTR Refractometer FRANCAIS (F): INSTALLATION DEUTSCH (D): AUFSTELLUNG ESPANOL (E): INSTALACION FUSE: 1 A, 20mm anti surge FUSIBLE: 1 A, 20mm NETZSICHERUNG: 1 A, 20mm FUSIBLE: 1 A, 20mm anti-surtension trage contra sobrecargas AC 50/60Hz 95-265v * POWER SUPPLY Alimentation Stromversorgung Caja suministro de Energia * PTR BROWN - LIVE BLUE - NEUTRAL YELLOW/GREEN - EARTH (GROUND) BRUN BLEU JAUNE/VERT BRAUN BLAU GELB/GRUN MARRON AZUL AMARILLO/VERDE * HEAT SINK - DO NOT COVER Boîtier formant radiateur : ne pas couvrir Die Heizvorrichtung sollte - nicht abgedeckt sein DIFUSOR DE CALOR - NO CUBRA 8 - PHASE NEUTRE TERRE PHASE NEUTRAL ERDUNG FASE NEUTRO TIERRA PTR 2a Handbook – Issue 3 June 2009 3.2 PRINTER INSTALLATION BRANCHEMENT D'UNE IMPRIMANTE AUFSTELLUNG DRUCKER CONECTANDO UNA IMPRESORA AUXILLARY PRINTER REMOTE 25 way D 2 3 7 RS 232 2 9 3 7 25 way D PTR 2a Handbook – Issue 3 June 2009 4.1 DIAGRAM OF INSTRUMENT SCHEMA FONCTIONNEL DE L’APPAREIL Querschnitt des Gerätes DIAGRAMA DEL INSTRUMENTO SAMPLE PRESSER PRESSE-ENCHANTILLON .. PROBEN ANDRUCKSTEMPLE PRENSA MUESTRA PRISM PRISME PRISMA PRISMA SAMPLE COVER SAMPLE CUP COUVERCLE A CHARNIERE PROBEN DECKEL CUBRE MUESTRAS COUPELLE DE MESURE PROBENRAUM COPA PARA MUESTRAS HEAT SINK ECHANGEUR THERMIQUE DIE HEIZVORRICHTUNG SOLLTE DIFUSOR DE CALOR INPUT/OUTPUT SOCKETS PORTS ENTREE/SORTIES BUCHSEN FUR EIN UND AUSGANGE TOMA DE ENTRADA/SALIDA INFORMATION LABEL PLAQUE SIGNALETIQUE ETIKETT FUR WICHTIGE HINWEISE ETIQUETA DE IN FORMACION 10 PTR 2a Handbook – Issue 3 June 2009 4.2 DISPLAY - BASIC AFFICHAGE - INFORMATIONS DE BASE HAUPTANZEIGE PANTALLA - BASICA MODE OF OPERATION MODE DE MESURE BEDIENERMODUS MODO DE OPERATION READOUT SPEED F fast, M medium, S slow VITESSE - F rapide, M moyenne, S réduite GESCHWINDIGKEIT - F Schnelle, M Mittlere, S Langsame VELOCIDAD F rápida, M media, S reducida SCALE XXXXXXXXXXX ECHELLE SKALA ESCALA * (X) SAMPLE TYPE “E” EMULSION TYPE D’ECHANTILLON “E” EMULSION PROBEN VORWAHL E für dunkle Proben (Emulsionen) TIPO DE MUESTRA COLOCADA (X) XX XXXXXX SAMPLE XX.XX SET XX.X READING (or message) RESULTAT OU MESSAGE MESSERGEBNIS LECTURA (o mensaje) BLANK = NORMAL SAMPLE TEMPERATURE SET TEMPERATURE TEMPERATURE DE L’ECHANTILLON PROBEN TEMPERATUR TEMPERATURA DE LA MUESTRA TEMPERATURE DE CONSIGNE TEMPERATUR VORVAHL COLOCAR TEMPERATURA NOTE: emulsion scale is only available with remote control optional accessory 11 PTR 2a Handbook – Issue 3 June 2009 5 OPERATION SWITCH ON - mains switch on power supply box. Sample cover must be closed. Wait until stable - minimum 10 to 15 minutes. Apply sample (refer to section 6). Read result from display when sample temperature and reading are stable. If a printer is connected, press PRINT to print result. Remove sample / clean prism. (F) 5 UTILISATION DE L’APPAREIL “ON” : mise sous tension du réfractomètre. Pensez à fermer le couvercle de mesure pour permettre à l’appareil d’effectuer correctement ses auto-tests. Attendre au moins 10 à 15 minutes pour une stabilisation parfaite de la température de l’ensemble du réfractomètre, même si le prisme atteint la température de consigne beaucoup plus rapidement. Placer l’échantillon sur le prisme (voir §6). Le résultat s’affiche à chaque nouveau balayage optique (« scan ») environ toutes les 3 secondes (8 secondes pou les modèles "X") . Il vous appartient bien sûr de vérifier que la température et le résultat sont stables. Si vous voulez imprimer le résultat, appuyez sur : PRINT Retirez l’échantillon, rincez la coupelle, le presseur et le prisme avec le solvant adéquat. (D) 5 HAUPTBEDIENELEMENTE EIN-AUSSCHALTER an der Stromversorgung. Probenraumdeckel muß zugeklappt sein. Wartezeit mindestens 10 bis 15 Minuten für die Temperaturstabilisierung. Probe auf das Prisma auftragen (siehe Abschnitt 6). Lese das Ergebnis von der Anzeige ab, wenn Temperatur und die Anzeige stabil sind. Ist ein Drucker angeschlossen, so drücke die PRINT - Taste, um das Ergebnis auszudrucken. Entnehme Probe und reinige das Prisma. (E) 5 OPERACIÓN GENERAL ENCIENDA – El interruptor principal colocado en la Caja de suministro de Energía. El cubre muestras debe estar cerrado. Espere hasta que este estable – mínimo 10 a 15 minutos. Aplique la muestra ( Referirse a la sección 6 ). Lea los resultados desde la pantalla cuando la lectura y la temperatura de la muestra son estables. Si una impresora es conectada, presione PRINT para imprimir los resultados. Remueva la muestra / limpie el prisma. 12 PTR 2a Handbook – Issue 3 June 2009 6 SAMPLE HANDLING WARNING: Before using the PTR, read Section 2, "Chemical Compatibility and Aggressive Samples." 6.1 STANDARD HINGED SAMPLE COVER Ensure PRISM and SAMPLE PRESSER are CLEAN. LIQUIDS: Apply approximately 0.1ml to 0.3ml of sample to centre of prism. Thin liquids - use a disposable plastic pipette or similar. Thick, viscous liquids - use a plastic spatula or similar. Close sample cover. Read sample (See Section 5 Operating Instructions). CLEAN PRISM and SAMPLE PRESSER. Wipe sample from prism and presser with soft, absorbent tissue. Wash prism, sample cup and presser with a suitable solvent, water, alcohol, etc. Polish dry with soft tissue. If the sample is difficult to clean off, try flooding the prism area with about 1 to 1.5ml of solvent, leave for a few moments then mop out solvent and polish dry. Repeat until clean, checking that the whole prism surface is clean by looking at reflections from the prism surface. DO NOT LEAVE A SAMPLE ON THE PRISM AFTER MEASUREMENT. (F) 6 MANIPULATION DES ECHANTILLONS ATTENTION : avant toute utilisation du réfractomètre PTR, lisez attentivement le chapitre consacré à la compatibilité chimique des échantillons et des solvants de nettoyage avec les matériaux utilisés dans le PTR (§ 2). (F) 6.1 COUVERCLE STANDARD A CHARNIERE Assurez-vous d’abord que le prisme et le « presseur » sont parfaitement propres. LIQUIDES: Déposer environ 0.1ml à 0.3ml d’échantillon sur le prisme. Si besoin, étaler l’échantillon avec une spatule en bois ou en plastique ou l’embout d’une pipette plastique. Basculer le couvercle sur le prisme. Lire la mesure, selon le mode de mesure choisi (continu, discontinu, “en stabilité”), la lecture est immédiate ou différée (voir § 5). NETTOYAGE DU PRISME ET DU PRESSEUR. Essuyez l’échantillon sur le prisme et le presseur avec un tissu ou un papier doux et absorbant. Nettoyer le prisme et le presseur avec le solvant adapté à l’échantillon; généralement de l’eau ou de l’alcool ou éventuellement de l’acétone, mais vous pouvez en utiliser d’autres à condition de respecter les recommandations du § 2 sur les compatibilités chimiques des joints. Essuyer à nouveau pour bien sécher et recommencer l’opération si le nettoyage n’a pas été efficace. NE LAISSEZ PAS UN ÉCHANTILLON SUR LE PRISME OU SUR LE PRESSEUR CAR, EN SÉCHANT, IL POURRAIT SE FORMER UN FILM DIFFICILE À RETIRER OU A DISSOUDRE, CE QUI FAUSSERAIT LES MESURES ULTERIEURES. 13 PTR 2a Handbook – Issue 3 June 2009 (D) 6 Probenbeurteilung WICHTIG: Bevor Sie das PTR benutzen, verweisen wir auf Abschnitt 2 "Chemische Verträglichkeit und sehr aggressive Proben". (D) 6.1 Klappbarer Probenraumdeckel Es ist darauf zu achten, dass das Prisma und der Probenandrückstempel sauber ist. FLÜSSIGE PROBEN: Hierfür benötigt man ungefähr 0,1 bis 0,3 ml Probe auf die Mitte des Prismas. Bei dünnen Flüssigkeiten benutze man eine Einmalplastikpipette oder ähnliches. Bei dicken viskosen Proben benutze man einen Spatel oder ähnliches. Man schließe den Probenraumdeckel. Lese den Wert Probe ab (Siehe Abschnitt 5, des Bedienungshandbuches). REINIGEN DES PRISMAS UND DES ANDRUCKSTEMPELS Man wische die Probe vom Prisma und vom Anpresstempel mit einem saugfähigen Kleenextuch ab. Reinige das Prisma, Probenraum und Andrückstempel mit einer entsprechenden Reinigungsflüssigkeit. (Wasser, Alkohol oder ähnliches), und wische nochmals mit einem sauberen Kleenextuch nach. Solte die Probe sich sehr schwer entfernen lassen, so bedecke man den Probenraum mit ca 1 bis 1.5ml Lösung und lasse diese einen Augenblick darin, wische dann die Flüssigkeit wieder heraus und reibe das Prisma trocken. Dieser Vorgang ist zu wiederholen bis das Prisma sauber ist und man eine gute Reflexion erkennen kann. Nach dem Messvorgang muß die Probe wieder vom Prisma entfernt werden. (E) 6 MANEJO DE MUESTRAS ADVERTENCIA : Antes de usar el Refractómetro PTR, lea la sección 2, “COMPATIBILIDAD QUIMICA Y MUESTRAS AGRESIVAS ". (E) 6.1 DISPOSITIVO CUBRE MUESTRAS ESTÁNDAR CON BISAGRAS PARA LIQUIDOS Asegúrese que el PRISMA y la PRENSA MUESTRAS están LIMPIOS. LIQUIDOS: Aplique aproximadamente 0.1 ml a 0.3 ml de muestra al centro del prisma. Líquidos delgados – use una pipeta plástica desechable o similar. Líquidos viscosos o espesos – use una espátula plástica o similar. Cierre el Cubre Muestras. Lea la muestra ( Ver sección 5 Instrucciones de Operación ) LIMPIE EL PRISMA y la PRENSA MUESTRAS. Retire la muestra del prisma y prensa muestras con un paño de papel suave y absorbente. Lave el prisma, copa de Muestra y Prensa muestras con un solvente apropiado agua, alcohol, etc. Perfeccione el secado con un paño de papel suave. Si la muestra es difícil para limpiar, trate inundando el área del prisma con cerca de 1 a 1.5 ml de solvente, deje por unos pocos momentos luego retira el solvente y sécalo. Repita esta operación hasta que el prisma esté completamente limpio, chequee que toda la superficie del prisma esté limpia por medio de la observación de las reflexiones desde la superficie del prisma. NO DEJE UNA MUESTRA SOBRE LA SUPERFICIE DEL PRISMA DESPUES DE LA MEDICION. 14 PTR 2a Handbook – Issue 3 June 2009 6.2 SOLID SAMPLES Solid samples must be specially prepared with an optically flat surface between 3 and 11 mm diameter (not necessarily round). Use a contact fluid with RI greater than the sample RI. A non-contacting sample cover is available from Index Instruments for use when measuring solid samples. Flexible plastics or rubbers can sometimes be pressed onto the prism without using a contact fluid. Contact Index Instruments for advice. (F) 6.2 ECHANTILLONS SOLIDES Les échantillons solides doivent recevoir une préparation spéciale avant de pouvoir être mesurés car il faut qu’ils aient une face parfaitement plane pour un contact optimal avec la surface du prisme. Cette surface doit avoir une surface plane d’environ 3 à 11 mm de « diamètre » (bien qu’elle n’ait pas absolument besoin d’être ronde). Il faut en outre assurer un contact avec un liquide dit «liquide de contact » dont l’indice doit être supérieur à l’indice de l’échantillon (on utilise souvent du monobromonaphtalène d’indice élevé, mais d’odeur … désagréable). Les solides souples (caoutchoucs, matières plastiques, lentilles de contact etc…) peuvent parfois être mesurés sans avoir besoin de liquide de contact. Index Instruments commercialise un couvercle spécial pour la mesure des solides. Si vous devez mesurer des échantillons solides, nous vous conseillons de nous contacter pour recevoir nos conseils appropriés. (D) 6.2 FESTE PROBEN Feste Proben müssen zum Messen mit einer optisch flachen Oberfläche und einem Durchmesser von 3 bis 11 mm vorbereitet werden. Die Oberfläche muß nicht unbedingt rund sein. Es ist eine Kontaktflüssigkeit mit einem größeren RI als das der Probe zu verwenden. Für die Messung von festen Proben gibt es von Index Instruments einen extra Probenraumdeckel. Flexible Plastikteile oder Gummi kann man einfach auf das Prisma drücken, ohne eine Kontaktflüssigkeit zu verwenden. Sie können jederzeit Index Instruments oder dessen Vertreter um Rat kontaktieren. (E) 6.2 MUESTRAS SOLIDAS Las muestras sólidas deben ser especialmente preparadas con una superficie ópticamente plana con un diámetro entre 3 y 11 mm ( no necesariamente redondas ). Use un fluido de contacto con un Indice de Refracción mas grande que el Indice de Refracción de la muestras. Una cubierta par muestras sin contacto es disponible desde Index Instruments Ltd para usar cuando muestras sólidas van a ser medidas. Plásticos flexibles o cauchos pueden algunas veces ser presionados sobre el prisma sin usar un fluido de contacto. Contacte a Index Instruments Ltd para asesoría. 15 PTR 2a Handbook – Issue 3 June 2009 6.3 SAMPLING WITH FUNNEL CELL Check that the waste pipe has an uninterrupted run to a waste container at or below bench height. Pour approximately 50ml of sample through the funnel. To improve flushing, pour in half of the sample, pause, then pour in remainder. Read sample (See Section 5 Operating Instructions). Provided the solvent is the same, pour in the next sample and continue until you have measured the batch of samples. Pour approximately 250ml of solvent through the funnel to clean the cell. DO NOT LEAVE SAMPLES OR AGGRESSIVE SOLVENTS IN THE CELL. Occasionally lift the funnel cell and thoroughly clean the cell and prism surface. (F) 6.3 UTILISATION D’UNE CELLULE A ENTONNOIR Contrôler d’abord que le tube d’évacuation est bien libre et plonge dans un évier ou dans une bouteille de capacité suffisante pour recevoir les effluents des mesures (échantillons et solvants). Bien évidemment, l’écoulement de ce tube d’évacuation doit être à un niveau inférieur au réfractomètre. Verser environ 50ml de produit dans l’entonnoir en deux fois 25ml environ. Lire le résultat (voir § 5). Si les échantillons sont de même nature, vous pouvez éviter de rincer à l’eau entre chaque mesure : il vous suffit de rincer l’entonnoir et le circuit de mesure avec 2x20 ml de l’échantillon (N) de façon à bien purger toute trace d’échantillon (N-1) que vous venez de mesurer. Ensuite, quand vous avez terminé toute la série de mesures, verser en plusieurs fois 150ml à 250ml de solvant puis contrôlez éventuellement la propreté du système en effectuant une mesure sur l’eau. NE LAISSEZ PAS D’ÉCHANTILLON DANS LA CELLULE A ENTONNOIR CAR, EN SÉCHANT, IL POURRAIT SE FORMER UN FILM DIFFICILE À RETIRER OU A DISSOUDRE, CE QUI FAUSSERAIT LES MESURES ULTERIEURES. Nous vous conseillons aussi d’enlever la cellule à entonnoir de temps à autre et de nettoyer la surface du prisme. 16 PTR 2a Handbook – Issue 3 June 2009 (D) 6.3 Die Messung mit Hilfe eine Trichterzelle Überprüfe dass die Abflussröhre der Trichterzelle eien Schlauch zu einem Sammelbehälter in Tischhöhe oder darunter hat. Schütte ungefähr 50ml Probe in den Trichter. Um einen einwandfreien Durchfluß zu haben, gieße man nur die Hälfte in den Trichter. Um einen einwandfreien Durchfluß zu haben, gieße man nur die Hälfte in den Trichter und dann nach einer kleinen Pause den Rest. Lese dann den Wert der Probe ab. (Siehe Abschnitt 5 des Bedienungshandbuches) Vorrausgesetzt die Flüssigkeit ist die selbe, so gieße man die nexte Probe ein und fahre so fort, bis man alle Proben gemessen hat. Gieße anschließend 250ml Lösung durch den Trichter, um das Prisma zu reinigen. ES IST DARAUF ZU ACHTEN, DASS KEINE PROBEN ODER AGGRESSIVE MEDIEN FÜR LÄNGERE ZEIT IN DER ZELLE STEHEN DÜRFEN. Gelegentlich ist die Trichterzelle anzuheben, um die prismenoberfläche und die Zelle zu reinigen. (E) 6.3 MUESTRAS CON CELDA DE EMBUDO Chequee que la tubería de descartar o botar las muestras tenga una ininterrumpida salida a un recipiente para los desechos a / o más debajo de la altura de la mesa de trabajo. Vierta aproximadamente 50 ml de muestra a través del embudo. Para mejorar el lavado con la muestra, vierta la mitad de la muestra, haga una pausa, luego vierta el remanente. Lea la muestra ( Ver sección 5 Instrucciones de Operación) Si el solvente es la misma muestra, vierta la siguiente muestra y continue hasta que usted ha medido la tanda de muestras. Vierta aproximadamente 250 ml de solvente a través del embudo para limpiar la celda. NO DEJE MUESTRAS O SOLVENTES AGRESIVOS EN LA CELDA: Ocasionalmente levante la celda de embudo y limpie meticulosamente la celda y la superficie del prisma. 17 PTR 2a Handbook – Issue 3 June 2009 6.4 SAMPLING WITH FLOW / INJECTION CELL Method is similar to funnel cell (Section 6.3). INJECTION Inject approximately 1.5 to 2ml of sample using a syringe with standard luer taper. FLOW A peristaltic pump is suitable to draw sample through the cell. Pump minimum volume possible to flush cell but maintain stable temperature. Alternatively can be included in an automatic sampling system. FLOW CELL PUMP PTR SAMPLE WASTE (F) 6.4 MESURE AVEC UNE CELLULE A FLUX CONTINU La méthodologie est semblable à celle des mesures avec la cellule à entonnoir (voir § 6.3). INJECTION A LA SERINGUE Injecter environ 1.5 à 2ml d’échantillon avec une seringue à embout standardisé LUER. FLUX CONTINU L’échantillon est introduit généralement avec une pompe péristaltique, soit autonome soit incorporée à un passeur d’échantillons. Pensez à tenir compte du fait que le flux continu réel empêche le maintien de l’équilibre thermique et qu’il faut donc adapter le débit continu pour qu’il soit assez faible afin de maintenir cet équilibre thermique au niveau souhaitable. Débit Cellule Pompe PTR Echantillon Egout 18 PTR 2a Handbook – Issue 3 June 2009 (D) 6.4 Die Messung mit einer Durchfluß - oder Injektionszelle Die Messemethode ist ähnlich, wie bei der Trichterzelle (siehe Abschnitt 6.3). INJEKTION Injiziere ungefähr 1,5 bis 2ml Probe mit Hilfe einer Spritze mit Lueranschluß. DURCHFLUSS Mit Hilfe einer Schlauchpumpe kann man die Probe durch die Zelle pumpen. Anschließend ist mit dem geringst möglichen Volumen die Zelle zu spülen, um eine gleichmäßige Temperatur zu erreichen. Alternativ kann die Schlauchpumpe auch in ein automatisches Probenentnahmesystem integriert werden. DURCHFLUβZELLE PUMPE PTR PROBE ABFALL (E) 6.4 MUESTRAS CON CELDA DE FLUJO / INYECCIÓN El método es similar al de la celda de embudo ( Ver sección 6.3) INYECCION Inyecte aproximadamente 1.5 a 2 ml de muestra usando una jeringa con orificio de salida estándar. FLUJO Una bomba peristáltica es apropiada para aspirar la muestra a través de la celda. Bombee el mínimo volumen posible para lavar con la muestra la celda pero mantenga estable la temperatura. Alternativamente puede ser incluido un sistema de muestreo automático. CELDA DE FLUJO BOMBA PTR MUESTRA DESECHO 19 PTR 2a Handbook – Issue 3 June 2009 7 WATER REFERENCE POINT (ZERO CHECKING AND SETTING) Ensure prism and presser are clean. Apply a pure water sample (refer to section 6) and wait for sample to stabilise at instrument temperature. Read sample in normal way (refer to section 5). Is value for water correct? (Refer to Appendix 2.) If the reading is correct within the instrument's accuracy simply proceed to measure your samples. If the reading requires adjustment press ZERO . If a printer is connected, the message "Instrument zeroed" is automatically printed. DO NOT PRESS THE ZERO KEY UNLESS THE SAMPLE IS PURE WATER. (F) 7 MESURE DE REFERENCE AVEC DE L’EAU (Contrôle et reset du ZERO) Vérifiez que le prisme et le presseur sont propres. Mettre de l’eau sur le prisme (voir §6) et attendre l’équilibre thermique de l’appareil. Lire le résultat et contrôler que ce résultat est exact en fonction de la température (voir Annexe 2). Deux cas peuvent se présenter : OUI la valeur est exacte : votre appareil est parfaitement ajusté et vous pouvez effectuer les mesures sur vos échantillons NON la valeur n’est pas exacte : il est préférable de ré-ajuster la programmation de l’appareil. Pour cela appuyez sur ZERO . Lors de cette procédure, si une imprimante est reliée au PTR, l’impression “Instrument zeroed" sera automatiquement imprimée. NE LANCEZ PAS LA PROCEDURE DE <ZERO> SI VOUS N’AVEZ PAS MIS DE L’EAU SUR LE PRISME !!! 20 PTR 2a Handbook – Issue 3 June 2009 (D) 7 WASSERWERT (Nullpunktüberprüfung und Einstellung) Man überprüfe, dass das Prisma und der Andruckstempel sauber ist. Gebe eine Probe mit reinem Wasser auf das Prisma (siehe Abschnitt 6) und warte bis sich die Probe bei Gerätetemperatur stabilisiert hat. Lese den Wert der Probe ab. (siehe Abschnitt 5). Ist der Wasserwert korrekt? (siehe Anhang 2). Ist das Messergebnis innerhalt der für das Gerät vorgegebenen Genauigkeit in Ordnung, so kann man mit der Messung der Proben beginnen. Solte der angezeigte Wasserwer von der Tabelle abweichen, so drücke man die ZERO Nullabgleichtaste. Sollte ein Drucker angeschlossen sein, so wird automatisch die Meldung "Instrument zeroed" ausgedruckt. DER NULLABGLEICHKNOPF DARF NUR DANN GEDRÜCKT WERDEN, WENN DIE PROBE REINES WASSER IST. (E) 7 AGUA - PUNTO DE REFERENCIA ( CHEQUEO DEL CERO Y AJUSTE ) Asegúrese que el prisma y prensa muestra estén limpios. Aplique una muestra de agua pura ( referirse a la sección 6 ) y espere a que la muestra se estabilice a la temperatura del instrumento. Lea la muestra en forma normal ( referirse a la sección 5 ). Es el valor correcto para el agua ? ( referirse al Apéndice 2 ) Si la lectura es correcta dentro de la precisión del instrumento simplemente proceda a medir sus muestras. Si la lectura requiere ajustes presiones ZERO. Si una impresora esta conectada, el mensaje “ Instrument Zeroed “ es automáticamente impreso. NO PRESIONE EL BOTON ZERO A MENOS QUE LA MUESTRA SEA AGUA PURA. (ASEGÚRESE QUE LA MUESTRA SEA AGUA PURA ANTES DE PRESIONAR EL BOTON ZERO). 21 PTR 2a Handbook – Issue 3 June 2009 8 ADVICE ON TEMPERATURE CONTROL The temperature of the PTR 2a or 2a X is electronically controlled to the factory preset temperature by means of an internal Peltier cell which heats or cools the prism and sample cup as required. The prism and sample cup are insulated from the stainless steel top plate of the instrument and an insulating sample cover is provided. The Peltier temperature control system on the PTR refractometer is capable of maintaining a temperature stability of ±0.015°C. To achieve optimum performance the following precautions should be noted. Leave the sample cover closed even when not in use to improve temperature maintenance. To ensure proper cooling, the PTR should be located so that the heat sink at the rear of the instrument can conduct and radiate heat away from the instrument. It should therefore NOT be situated near a radiator, in direct sunlight or near other heat sources and should NOT be positioned such that the natural circulation of air around the heat sink is obstructed. Do not place the PTR's own power supply too close to the instrument. If the temperature of the surroundings is more than about 10°C above the required temperature, it will be necessary to provide additional cooling assistance by means of flowing water. For this you require the water jacket available as an optional accessory from Index Instruments Ltd. (part number 82-045). Refer to Figure 8.1 for the location of the water jacket and water connection details. This cooling water need not be at a controlled temperature and quite a low flow rate will provide the additional cooling necessary. For example, flowing water at about 25°C at less than 1 litre per minute is sufficient to reduce the sample temperature to 20°C or below from a room temperature of 35°C. Note that it is undesirable to keep the prism at a very low temperature when the ambient conditions are hot and humid. As the prism is open to the atmosphere, condensation will prevent sensible readings being made. In these conditions, control the prism at a higher temperature and correct the sample readings mathematically. If water is difficult to provide, an additional STEADY air flow from a fan across the heat sink will assist. (To ensure stable conditions, do NOT site the PTR in the direct draught of a FLUCTUATING air flow such as an air conditioner.) Similarly a flow of warm water will assist in heating the PTR if the required sample temperature is more than 20°C above ambient temperature. HEAT SINK Figure 8.1 CONNECTIONS FOR WATER ASSISTED COOLING 22 PTR 2a Handbook – Issue 3 June 2009 9 OUTPUT / INPUT 9.1 CONNECTING A PRINTER A suitable printer complete with cable ready to plug into the PTR may be purchased from Index Instruments Ltd. Otherwise use any standard RS232 printer, width 24 columns or more, with preferably at least an 8K buffer. Connect the printer to the 25 way D "Printer" port (centre connector) on the rear of the PTR. The pin connections are to normal RS232 standards: Pin 2 TX (data output from PTR) Pin 3 RX (data input to PTR) Pin 7 0 volts (ground) DO NOT CONNECT TO ANY OTHER PINS For a printer with a standard 25 way D RS232 connector the cable should be wired as follows: pin 2 to pin 3 pin 3 to pin 2 pin 7 to pin 7 The printer must be set for RS232 parameters as follows:Baud rate Length Parity Stop bits 9600 8 None 2 23 PTR 2a Handbook – Issue 3 June 2009 9.2 REMOTE PORT The remote port (9-way D) can be used for the following:a) input of a simple contact closure to remotely operate the PTR. b) input of bar code reader data. a) This contact closure mimics the action of the PRINT key. Short pins 6 and 8 for approximately 0.1 seconds. b) Bar code scanners are available from Index Instruments Ltd. (See below) Summary of Remote Port Pin Connections PIN FUNCTION 6 Remote print 7 0 v (ground) 8 Remote print DO NOT USE ANY OTHER PINS 9.3 BAR CODE READER A hand held laser bar code scanner is available from Index Instruments which plugs directly into the 9 way D "remote" socket on the rear of the PTR. (Alternatively, if you wish to use a different type of bar code scanner, you must select an RS232 type bar code reader, preferably with a 9 way D connector, but a scanner with a 25 way D plug can be connected to the "printer" RS232 port of the PTR using a 2 way adapter available from Index Instruments.) Scanning a bar code causes a print out frrom the PTR with the bar code data preceding the usual print-out (see Appendix 6). 24 PTR 2a Handbook – Issue 3 June 2009 9.4 AUXILIARY PORT The auxiliary port is used for communication with a computer. It is also used to connect other auxiliary equipment. The pin connections and cable requirements are the same as for the "printer" RS232 port (refer to section 4.1). The computer must be set for RS232 parameters as follows:Baud rate Length Parity Stop bits 9600 8 None 2 Alternatively, if you have the remote control optional accessory, you can change the RS 232 input parameters of the PTR 2a or PTR 2a X to match the auxiliary equipment. Software for collecting readings from or sending instructions to the PTR requires the following commands: NOTE: All commands should consist of two bytes of data. The first byte should always be ESC (1BH). The second byte may be any letter in the table below. Any other letter will cause a response of '?' followed by carriage return (CR). Any other sequence will be ignored. ESC R or r ESC B or b ESC C or c ESC D or d ESC P or p ESC T or t ESC X or x Return RI data Return Brix data Return corrected Brix data Return displayed scale data Mimics PRINT key - returns P Data is output via RS232 printer port Returns sample temperature Same data that would have been output by "print" is returned via RS232 auxiliary port. Each data string is terminated CRLF; the last data string is terminated CRLFLF All data returned is terminated with a single Carriage Return character (1BH). Returns 'E' CR if unable to read sample. 25 PTR 2a Handbook – Issue 3 June 2009 10 FITTING / CHANGING SAMPLE CELLS Optional accessories which may be purchased for the PTR refractometer include funnel, flow or injection cells. These may be fitted by the user, however it is very important to ensure that any new cell fitted lines up centrally over the prism of the PTR and sits down flat to ensure both correct screening from stray ambient light and a firm seal on the O-ring of funnel, flow or injection cells. Details of how to fit and adjust any particular type of cell will be supplied along with the cell at time of purchase. 26 PTR 2a Handbook – Issue 3 June 2009 11 Remote Control Unit (Optional Accessory) The standard PTR 2a or PTR 2a X models of refractometers are fixed scale instruments which are factory set to operate at a fixed temperature. If you purchase the remote control optional accessory, this allows the user access to other scales and other functions as detailed below. Further instructions for programming using the remote controller are given in Appendix 9. ENTER key enters and stores changes (QUIT key exits any function without making a change) Numeric, minus and decimal point keys are used to enter numeric data Use CONTRAST keys to optimise readability by adjusting contrast of liquid crystal display panel Use scroll arrow keys to move up or down, backwards and forwards when entering data in setup or calibrate Press CALIB. to enter "calibrate" mode - protected by security code SETUP KEYS (Use ENTER key to store change; use QUIT key to exit without making a change) Press TIME to set time and date Press TEMP to set temperature you want for sample Press PORT to set printout and RS232 output parameters SCALE SELECTION KEYS Press RI to select refractive index (and again for temperature corrected refractive index if set) Press BRIX to select Brix (% sucrose) Press BRIX again to select temperature corrected Brix scale (this is a mathematical correction to 20°C for use when the sample temperature is set to other than 20°C) 27 Press PRINT to choose what to print or to select autoprint Press DELAY to select operating mode (continuous or single scan/stability mode), to set delay time, stabilisation parameters or autoprint time, to select sample type (Normal or Emulsion) or to display archived data PTR 2a Handbook – Issue 3 June 2009 SECURITY ACCESS CODES for use with REMOTE CONTROL Optional Accessory Lockout code (required to unlock remote control) 1901 To access the following features, press CALIB and then type in the appropriate code. Set parameters for temperature corrected RI scale 3245 Select averaging/readout time 2468 (F = fast/no averaging, M = medium speed/averaging, S = slow/maximum averaging) Select display resolution - RI/Brix 4545 Select display resolution for thermometer (0.1 or 0.01°C) 1212 Optimise thermometers 9323 (Use only if sample temperature does not reach set temperature after 1 hour) Remove thermometer optimization 0932 Calibrate sample temperature thermometer 1001 (Use only if external temperature measurement of prism temperature with, for example an accurate thermocouple thermometer probe, indicates prism not at temperature indicated by PTR) Clear zero offset 0000 (Removes any zero adjustment made by the user and returns to factory set zero) Erase archived data 9070 28 PTR 2a Handbook – Issue 3 June 2009 APPENDIX 1 TECHNICAL SPECIFICATION PTR 2a SCALES RANGE READABILITY ACCURACY WAVELENGTH READOUT TIME TEMPERATURE CONTROL TEMPERATURE STABILITY TEMPERATURE ACCURACY SAMPLE TEMPERATURE WORKING AMBIENT TEMPERATURE RANGE Single scale: Refractive Index (RI) OR Brix OR Temperature corrected Brix depending on model selected OR all three scales with remote control RI 1.32 to 1.68, Brix 0 to 100% 0.0001 RI, 0.1 Brix +/-0.0001 RI, +/-0.1 Brix Sodium yellow 589nm Approximately 2 seconds, continuous update Internal electronic control by Peltier cell +/-0.015oC +/-0.1oC, thermometer resolution +/-0.1oC Preset to customer specification between 15°C and 50°C Or from 15°C to 50°C with remote control 10oC to 35oC PTR will control without assistance 10oC below ambient to 20oC above ambient Available as an option for control assistance by flowing water (need not be temperature controlled) 2 key membrane, PRINT, ZERO Back lit liquid crystal display LED Synthetic Sapphire 2 x RS232, 1 x remote Scale, reading, temperature, Bar Code TEMPERATURE CONTROL ASSISTANCE CONTROLS DISPLAY LIGHT SOURCE PRISM MATERIAL OUTPUTS / INPUTS DATA OUTPUT AVAILABLE POWER REQUIREMENTS 86 to 265 v ac, 47 to 63 Hz, less than 30 watts DIMENSIONS: Refractometer: w 258 x d 290 x h 160 mm Power Supply: w 80 x d 180 x h 60 mm WEIGHT Refractometer: 5.7kg Power Supply: 0.8kg PACKED WEIGHT Approximately 10kg 29 PTR 2a Handbook – Issue 3 June 2009 TECHNICAL SPECIFICATION PTR 2a X SCALES RANGE READABILITY ACCURACY WAVELENGTH READOUT TIME TEMPERATURE CONTROL TEMPERATURE STABILITY TEMPERATURE ACCURACY SAMPLE TEMPERATURE WORKING AMBIENT TEMPERATURE RANGE Single scale: Refractive Index (RI) OR Brix OR Temperature corrected Brix depending on model selected OR all three scales with remote control RI 1.32 to 1.68, Brix 0 to 100% 0.00001 RI, 0.01 Brix +/-0.00005 RI, 1.32 - 1.45 RI +/-0.05 Brix, 0 - 65 Brix +/-0.0001 RI, 1.45 - 1.68 RI +/-0.1 Brix, 65 - 100 Brix Sodium yellow 589nm Approximately 3 seconds, continuous update Internal electronic control by Peltier cell +/-0.015oC +/-0.05oC at 20oC, thermometer resolution 0.01oC Preset to customer specification between 15°C and 50°C Or from 15°C to 50°C with remote control 10oC to 35oC PTR will control without assistance 10oC below ambient to 20oC above ambient Available as an option for control assistance by flowing water (need not be temperature controlled) 2 key membrane, PRINT, ZERO Back lit liquid crystal display with contrast control LED Synthetic Sapphire 2 x RS232, 1 x remote Scale, reading, temperature, Bar Code TEMPERATURE CONTROL ASSISTANCE CONTROLS DISPLAY LIGHT SOURCE PRISM MATERIAL OUTPUTS / INPUTS DATA OUTPUT AVAILABLE POWER REQUIREMENTS 86 to 265 v ac, 47 to 63 Hz, less than 30 watts DIMENSIONS: Refractometer: w 258 x d 290 x h 160 mm Power Supply: w 80 x d 180 x h 60 mm WEIGHT Refractometer: 5.7kg Power Supply: 0.8kg PACKED WEIGHT Approximately 10kg 30 PTR 2a Handbook – Issue 3 June 2009 APPENDIX 2 RI WATER v TEMPERATURE (F) ANNEXE 2 TABLE D'INDICE DE REFRACTION DE L'EAU EN FONCTION DE LA TEMPERATURE (D) ANHANG 2 RI von Wasser in Abhängkeit von der Temperatur (E) APENDICE 2 INDICE DE REFRACCION DEL AGUA PURA COMO UNA FUNCION DE LA TEMPERATURA Temp (oC) RI (4 place) RI (5 place) 14 16 18 20 22 24 26 28 30 32 34 36 38 40 42 44 46 48 50 1.3335 1.3333 1.3332 1.3330 1.3328 1.3326 1.3324 1.3322 1.3319 1.3316 1.3314 1.3311 1.3308 1.3305 1.3302 1.3299 1.3296 1.3293 1.3289 1.33348 1.33333 1.33317 1.33299 1.33281 1.33262 1.33241 1.33219 1.33192 1.33164 1.33136 1.33107 1.33079 1.33051 1.33023 1.32992 1.32959 1.32927 1.32894 th 31 th PTR 2a Handbook – Issue 3 June 2009 APPENDIX 3 Instructions for the use of solid standard test pieces on the PTR range of refractometers Test pieces manufactured from glass, crystals and plastics can be successfully measured on the PTR range of automatic refractometers. Solid samples should be 9 to 11 mm in diameter, 4 to 6 mm thick and polished on one face to two fringes or better. Index Instruments can supply test pieces of this type and we will be pleased to quote for your requirements. To check the calibration of the instrument using a test piece, proceed as follows: 1. Carefully zero the refractometer using pure water according to the instructions given in the operator’s handbook. 2. Remove all traces of water and clean the prism face thoroughly with industrial alcohol (methylated spirits) and/or acetone using a soft lint-free cloth or small piece of chamois leather. Clean the polished face of the test piece in a similar way. It is essential that both the prism and the test piece are absolutely clean with no trace of dust. A single speck of dust will prevent an accurate reading. If necessary dust both the face of the prism and the test piece with a clean soft lens brush. 3. There are two alternative ways to apply the test piece: a) Carefully place the clean dry test piece in the centre of the prism. When the test piece is correctly applied, you will see one or two coloured fringes when viewing the test piece (through its rear face) from a slightly oblique angle. If the test piece does not go down into colour contact first time, do not be tempted to slide it around as this could damage the test piece; simply remove the test piece, clean both faces as previously described and try again. Then apply a small drop (approx. 1mm) of contact fluid NOTE 1 to the bottom edge of the test piece using a suitable dropper NOTE 2; the fluid should flow under the test piece, spreading to completely fill the gap between prism and test piece. b) Alternatively, place a drop (about 1mm) of contact fluid NOTE 1 on the centre of the prism and then carefully place the test piece over the contact fluid in the centrally on the prism. The fluid should spread out in a very thin layer to just fill the gap between prism and test piece. If too much contact fluid is used, the test piece will tend to “float” and give inaccurate readings; if too little fluid is used, the gap will not be completely filled. 4. Exclude light from the prism/test piece by using the non-contacting cover suitable for the refractometer. If a non-contacting cover is not available, a clean black screw cap from an ordinary laboratory chemical jar is a suitable alternative. 5. Check that you have a stable reading on the refractometer and note the displayed value as you would do for any liquid sample. If it is found that the instrument gives a value which is different from the expected value for the test piece, thoroughly clean and remount the test piece several times (3 or 5 times) to obtain a good average value. 6. REMOVAL of the TEST PIECE: The test piece can be difficult to remove, especially if it was in very good contact with the prism surface. DO NOT attempt to prise it off; this can cause damage to both test piece and prism. Instead flood the prism with industrial alcohol (methylated spirits) and, in a short time, you will find that the test piece can be lifted off easily. Always thoroughly clean both the test piece and the prism before attempting to measure any further samples. NOTE 1 CONTACT FLUIDS: The contact fluid must have a refractive index higher than that of the test piece being measured. Suitable contact fluids are 1-bromonaphthelene, suitable for test pieces up to about 1.6 RI, or di-iodomethane for test pieces up to 1.7 RI. These two fluids are both classified as not dangerous according to EC Directives but are labelled as Harmful/Irritant and therefore must be handled with care and used only in a well ventilated area. Both contact fluids mentioned above can be obtained from a normal laboratory chemical supplier and are not available from Index Instruments Ltd. An alternative, non-hazardous contact fluid is clove oil, suitable for silica and other test pieces up to about 1.51 RI. NOTE 2 DROPPER: A suitable small plastic applicator is supplied with Index Instruments test pieces. Alternative applicators include, for example, the end of a straightened paper clip. If you use a metal applicator, be careful not to scratch or damage the test piece. 32 PTR 2a Handbook – Issue 3 June 2009 APPENDIX 4 REFRACTOMETER REFERENCE STANDARDS A variety of reference standards for checking refractometer calibration are available, ranging from liquid standards with values traceable to internationally recognised certification bodies to solid test pieces of pure crystalline material of well researched and published refractive index. Secondary standards are also available for routine use. When purchasing refractometer reference standards, always ask what is the accuracy of the certified value and check that this is satisfactory for your purpose. Typical accuracies vary from 0.0002 RI to 0.00005 RI for liquid standards. Data on solid crystalline standards is available to the 5th decimal place of RI. Refractometer reference standards may be purchased from Index Instruments Ltd. Contact Index Instruments or your local agent for full details of standards currently available. SOLID TEST PIECES Of the substances listed below, we recommend silica. This is a tough, well researched, reasonably priced material, readily obtainable in optical quality. Lithium and calcium fluoride are expensive materials and are difficult to obtain in optical quality. They are also soft, leading to rapid surface erosion and are easily broken along the crystal cleavage planes. They are however available if you require a standard with a lower RI than silica. Crystalline substances of known RI at 589.3nm, 20°C: Lithium fluoride 1.39207 Calcium fluoride 1.43385 Silica 1.45840 (Reference: Tables of Physical and Chemical Constants, Kaye & Laby, 16th edition 1995, Longman) Average accuracy when used with PTR: +/-0.0001 taking all precautions listed in Appendix 3. SECONDARY SOLID STANDARDS Glass test pieces can be made for RI's between about 1.50 and 1.68. LIQUID STANDARDS Liquid standards with traceable values are available from Index Instruments at intervals over the whole range of the PTR refractometer, choice of accuracy +/0.0002 to 0.00005. SECONDARY LIQUID STANDARDS Make up as required from pure sucrose and pure water to cover RI range from water (1.3330) up to 1.5. 33 PTR 2a Handbook – Issue 3 June 2009 APPENDIX 5 MARGINAL SUBSTANCES The PTR is a modern, technically advanced instrument. It has made possible the measurement of substances that it was not possible to measure in the past either with visual or automatic refractometers . Usually these difficult substances reflect and scatter light which substantially degrades the demarcation between light and dark (the borderline). Because we apply reasonable criteria to the specification of all our instruments, program controls are inserted at various points. For example, a degraded borderline will only be allowed to deteriorate to some finite level before the instrument recognises that SENSIBLE accurate measurement is no longer possible; it then indicates unable to read sample. It will be realised that if you try to measure a sample that degrades the borderline to a level which almost causes the control to operate "no reading", then even stirring the sample or opening and closing the cover could be enough to cause the sample to read or not read, just depending on the amount of scattered light at any particular moment. Indeed the control levels inserted in the program turn out to be far more reliable than the human eye and make the use of a visual back-up unnecessary. Program control levels are not normally set on an individual instrument but are determined statistically over a whole batch. This could easily mean that with an average production spread, coupled to a marginal sample, individual instruments may differ on exact rejection levels. It does not mean that there is anything wrong with the instrument - far from it - it means that the control is doing exactly what it was designed to do. Control levels can often be set in the factory on an individual instrument to suit a particular range of samples being measured and usually without any loss of accuracy or stability. To carry out this work (for which we make a nominal charge) Index Instruments needs a small quantity of your sample for test purposes. 34 PTR 2a Handbook – Issue 3 June 2009 APPENDIX 6 SAMPLES OF TYPICAL PRINT OUT FROM THE PTR REFRACTOMETER a) PTR 2, using Refractive Index scale. RI 1.3416 @ 25.0 C b) PTR 2 X, using Brix scale. Brix 12.21 @ 20.0 C c) PTR 2, Bar code scanner in use, using temperature corrected Brix scale. F3674528976541 Brix 3.2 Corrected to 20 C 35 PTR 2a Handbook – Issue 3 June 2009 APPENDIX 7 ERROR MESSAGES NO READING ERROR No sample on prism or Sample cannot be read, possible reasons: bubbles in sample particles in sample which scatter too much light Result cannot be displayed e.g. Brix scale, result outside Brix range 0 to 100% Temperature corrected Brix scale, temperature outside correction range 15 to 40°C (see Appendix 8) 36 PTR 2a Handbook – Issue 3 June 2009 APPENDIX 8 BRIX SCALE A refractometer basically measures the refractive index (RI) of light in a sample. Refractive index is a measure of how much a light beam is bent when passing from air into a denser material and is proportional to the speed of light in the material. The refractive index of a solution varies with the concentration of dissolved solids and is very closely related to (although not the same as) the density of the solution. In the sugar industry the refractometer scale commonly used is called the "BRIX" scale (or "degrees Brix"). The term "Brix" comes from the "Brix Hydrometer" or "Spindle" which was the original instrument used to measure the density of sugar solutions. The "Brix" hydrometer was a standard hydrometer for measuring density but had a scale reading directly in g/100g of sucrose, these scale divisions being called "degrees Brix". The term "Brix" has been carried through to refractometers whose scales are also calibrated in g/100g of sucrose. Thus BRIX means: per cent by weight of sucrose i.e. grams of pure sucrose per 100 grams of pure sucrose solution in pure water. A great deal of work has been done over many years by the International Commission for Uniform Methods of Sugar Analysis (I.C.U.M.S.A.) in relating Brix to refractive index (RI) as a function of sucrose concentration, temperature and wavelength of light. In 1974 I.C.U.M.S.A. published a definitive recommendation relating Brix to RI and, for practical purposes, publish tables based on this work. References: I.C.U.M.S.A. Proceedings, 16th Session 1974 and 17th Session 1978. I.C.U.M.S.A. Methods, Specifications and Standards 1994, including subsequent revisions. The BRIX scale programmed into all Index Instruments refractometers is based on these I.C.U.M.S.A. recommendations. If your refractometer has a TEMPERATURE CORRECTED BRIX SCALE this gives the reading that would have been obtained at 20°C for readings where the actual sample temperature is between 15°C and 40°C. The correction applied is that officially recommended by I.C.U.M.S.A. whose tables cover the temperature range 15°C to 40°C. As refractometers have been calibrated in Brix for many years, other industries besides the sugar industry have, for convenience, also used the Brix scale, but remember that the Brix scale is only strictly accurate for sucrose solutions in water. In particular, the temperature correction is for sucrose in water. It may give a reasonable approximation for samples other than sucrose, but, for greatest accuracy, you are advised to calculate your own temperature correction when not measuring sucrose. 37 PTR 2a Handbook – Issue 3 June 2009 taken to stabilise at the new temperature will depend on the temperature difference. A small change will stabilise in a few minutes, but a large change may take up to 20 or 30 minutes to fully stabilise. Appendix 9 FURTHER INFORMATION ON PROGRAMMABLE FUNCTIONS The remote control unit is required to program the PTR 2a or 2aX models CONTENTS Section Title A9.1 Lock/unlock A9.2 SETUP keys A9.2.1 Set clock (Time and Date) A9.2.2 Set temperature A9.2.3 Serial port parameters A9.2.4 Set Print Options A9.2.5 Select mode A9.2.6 Set parameters A9.2.7 Set sample type A9.3 Calibrate (CALIB key) A9.3.1 Temperature Corrected RI Scale A9.3.2 Select averaging/readout time A9.3.3 Select display resolution A9.3.4 Calibrate thermometer The PTR refractometer is factory calibrated to optimise the temperature control in normal ambient conditions. If, after waiting for a sufficiently long time for the PTR to fully stabilise, the "sample temperature" never reaches exactly the "set temperature" it may be necessary to make an adjustment. Any required adjustment is likely to very small and the instrument is programmed to reject an adjustment greater than 0.5°C. To carry out this automatic optimisation on the PTR, press the CALIB key and type in Security Code for "Optimise thermometers" (Section 11). If you want to remove this adjustment, for example if the setting had been made before the instrument was fully stabilised, use the Security Code for "Remove thermometer optimisation." If for any reason you think that the actual sample temperature setting is not accurate you may recalibrate the thermometer as described in section A9.3.4. A9.1 LOCK / UNLOCK To prevent accidental or unauthorised changes to the PTR settings, the remote controller can be “locked”. When you press the LOCK key you are asked for an access code (refer to Section 11). This is the same code you require to unlock the remote controller when you press the UNLOCK key. A9.2.3 SERIAL PORT PARAMETERS Press the PORT key. This allows you to check or set the parameters for the printer, auxiliary and remote serial RS232 output ports. Type the number of the port you want to check or change. You can also set the number of printer line feeds after each reading when you select the PRINTER port. A9.2 SETUP KEYS A9.2.1 SET CLOCK (TIME AND DATE) Press the TIME key. The time must be entered in the format xx.xx.xx (hours, minutes, seconds) using the 24 hour clock, e.g. for 9am type 09.00.00 or for 2.30pm type 14.30.00. The date must be entered in the format dd.mm.yyyy (day, month, year), e.g. for 1st June 2009 type 01.06.2009. Press ENTER to save changes. To select whether or not to print time and date refer to section A9.2.4. Simply press ENTER to leave the parameters unchanged, or use U or V keys to change each parameter in turn to match the device to be connected and then press ENTER to save. The factory settings for both the printer and auxiliary output ports are: Options A9.2.2 SET TEMPERATURE The temperature of the prism of the PTR refractometer is controlled electronically by means of a Peltier cell. To set the operating temperature, press the TEMP key. available Baud rate Parity Stop bits Bits/char Paper feeds The instrument will not allow you to enter a temperature outside the range 10°C to 50°C. (You may need temperature control assistance (refer to section 8) if the set temperature is more than 10°C below or 20°C above room temperature.) 9600 None 2 8 2 4800, 2400 Odd, Even 1 7 Max 98, min 1 (Printer port only) A9.2.4 SET PRINT OPTIONS Press the SETUP key labeled PRINT. This allows you to set what additional information will be output to a printer (or other data collection device) along with each sample After changing the set temperature, the time 38 PTR 2a Handbook – Issue 3 June 2009 In "SINGLE SCAN" mode, the operator applies a sample and then presses the PRINT key to read. The PTR refractometer waits a preset time then scans, displays and holds the result. (Subsequent changes in the sample will not be seen.) To set the delay time, refer to section A9.2.6. Printout is automatic at the end of the scan. reading. The sample temperature, scale name and sample reading are always printed. You may select whether to print 1) Time and date yes/no 2) Instrument serial number yes/no 3) Sample number no/manual/automatic (see below) Press the number of the option you want to change and use the U or V keys to select YES print or NO print then press ENTER to save. Operation of the PTR refractometer in "STABILITY" mode is similar to "single scan" mode, but the instrument detects when a stable reading has been obtained and then displays the result. The level of stability that is acceptable can be set by the user; refer to section A9.2.6. For sample numbering you can choose automatic or manual numbering; if sample numbering is set to "manual", in normal use, when the operator presses the PRINT key, the instrument will ask for a sample number. Any number up to 9 digits may be typed in. The operator then presses ENTER to proceed. Obviously the operator must have access to the remote controller to use manual sample numbering. PTRs (V6.8+) store, in internal memory, the last 100 readings taken. A reading is stored when the PRINT key is pressed (only valid readings are stored); in single scan modes, this means the reading is stored for every scan; in continuous mode, pressing the PRINT key (whether or not a printer is connected) puts the displayed reading into store. To retrieve readings, select “DISPLAY ARCHIVE” mode. The last reading taken, along with the scale name, temperature and the time and date of the reading is displayed. To scroll through previous readings, use the U or V keys. Press QUIT to return to normal operation. If sample numbering is set to "automatic", you will be asked to enter a starting number. Each subsequent press of the PRINT key will increment the sample number by 1 automatically. If automatic sample numbering is set, the instrument will also ask for a starting number at power up. You may enter a number up to 9 digits long. To change the start number during operation, re-select auto sample numbering and, when requested, type in the new number. If a printer is connected to the PTR, press PRINT to print the displayed reading; pressing PRINT again will output the single displayed reading; pressing ENTER will output all stored readings (remember, there could be up to 100). Alternatively, the stored data can be downloaded to a computer with suitable communications software; connect the computer to the RS232 “printer” port. A9.2.5 SELECT MODE To select the operating mode, press DELAY key and type “1” for SET OPERATING MODE the mode in use is indicated by the arrow. To change mode, type the number of the option required. The mode in use is displayed at the top of the normal display screen, except for “Display Archive” mode, which simply displays the scale name, reading and temperature along with the time and date the reading was taken. To erase all stored data, press the CALIB key and enter the access code for “Erase archive data” (refer to Section 11). If you change your mind after entering the code, pressing QUIT will return to normal operation without erasing the data. When operating in "CONTINUOUS" mode, the PTR refractometer is reading all the time; simply apply a sample and read from the display when the reading is stable. To print the result, press the PRINT key. A9.2.6 SET PARAMETERS To select the operating parameters, press DELAY key and type “2” for SET PARAMETERS. Type the number for the parameter you wish to check or alter. "AUTOPRINT" mode is similar to "continuous" mode except that the instrument automatically outputs the reading to a printer or other data collection device. This is useful for monitoring changing samples. You can choose to print every scan, print on data change or print at preset intervals. To set the time intervals, refer to section A9.2.6. Autoprint Time Interval Key sequence DELAY 2) Set PARAMETERS 1) Autoprint Type in the time interval you require between automatic print-outs (if you make a typing error, 39 PTR 2a Handbook – Issue 3 June 2009 prevent the instrument trying for ever to read a sample that is unsuitable. For example, if you expect most of your samples to stabilise in about 30 seconds, we suggest you set a default time of 60 or 120 seconds to allow for samples which take a little longer to settle. simply overtype) and then press the ENTER key. The time is entered in seconds. You can set any time from 1 to 999 seconds. A scan takes from 1 to 9 seconds depending on model; any time less than the scan time of the model in use is probably not useful. When operating in timed "autoprint" mode, the time to the next print counts down at the top of the display. If a stable reading is not obtained within the default time, the reading is displayed with the error message "Reading at default time". Single Scan time Key sequence DELAY, 2) Set PARAMETERS, 2) Single scan Type in the required time and press ENTER. This time is the delay time between pressing PRINT/START and reading in "single scan" mode. Any delay time from 1 to 999 seconds can be set. For example, if the instrument is set for medium averaging/readout time, a delay of 1 second will give a reading in approximately 3.5 seconds (1 second plus 2.5 seconds for a scan). You should set a delay which allows sufficient time for the sample to come to thermal stability with the prism of the PTR before the reading is taken. A sample which is very hot or very cold compared to the set temperature of the prism will require a longer delay time. Alternatively you should consider using the "stability" mode which reads only when a stable result is obtained. The default time MUST be longer than the number of scans set for the "duration" plus one multiplied by the scan time, which is between 1.5 and 5 seconds depending on whether the averaging/readout time is set to slow, medium or fast, HOWEVER we suggest entering for the default time at least double this calculated minimum time, or longer for particurly hot or cold samples; the instrument will always output the result as soon as possible whatever default time is set. You can set a default time up to 999 seconds. Factory pre-set parameters are normally:Window Duration Default time +/-2 4 scans 60 secs A9.2.7 SET SAMPLE TYPE Key sequence: DELAY, 3) SET SAMPLE TYPE, U or V keys to amend Use the "normal" setting for the majority of samples whether clear, coloured, turbid or dark. Use the "emulsion" setting for the few samples, in particular emulsions, which scatter light from relatively large particles in the liquid. To find out the appropriate single scan delay time for your particular samples, operate the PTR in "continuous" mode first to find out how long the reading takes to stabilise. Stability Parameters Key sequence DELAY 2) Set PARAMETERS 3) Stability This allows you to set how stable you want a reading to be before the PTR, in stability operating mode, will accept it as "stable" and output the result. Type the number of the parameter you want to change and then type in the required value and press ENTER to save, QUIT to exit when all parameters set. When using the emulsion scale, the accuracy is reduced by a factor of about 2. The emulsion scale usually allows the PTR to measure samples which are extremely difficult or impossible to measure on a visual or other automatic refractometer, however it is neither possible nor useful to measure ALL emulsions on a refractometer. The PTR detects when the borderline is too diffuse to make a sensibly accurate measurement and displays "No Reading" rather than giving a meaningless number. You can set a stability "window", minimum +/-1, maximum +/-99. EXAMPLE: a window of +/-2 means that the reading must not move by more than +/-2 in the least significant digit of the scale and resolution selected. A letter "E" to the left of the display indicates that emulsion scale has been selected. The "duration" specifies the number of scans for which the reading must remain within the stability window, minimum 2, maximum 99. A9.3 CALIBRATE (CALIB Key) The options under "Calibrate" are protected by security access codes. These codes are listed in Section 11. Some of these options are discussed elsewhere in this manual. The other settings that are available are listed below: The "default" time sets the length of time in seconds that the instrument will wait for a stable reading. The purpose of the "default" time is to 40 PTR 2a Handbook – Issue 3 June 2009 programmed temperature coefficient. Press the RI key again to see the normal RI scale which still displays the actual RI measured at the actual temperature. Set temperature corrected RI scale Select averaging/readout time Select display resolution for RI, Brix and temperature Calibrate thermometer TO REMOVE the temperature corrected RI scale, repeat as above but set the temperature coefficient to zero. A9.3.1 TEMPERATURE CORRECTED RI SCALE The way the refractive index of a sample changes with temperature is entirely dependent on the particular sample in question, and also varies with sample concentration and temperature. For example: Per degree C change in temperature, the RI of pure water changes by approximately 1 in the 4th decimal place of RI around 20°C, and by approximately 1.5 in the 4th decimal place around 50°C. In the region of 20°C, the RI of a 20% concentration sugar solution changes by just over 1 in the 4th decimal place of RI per degree C, and a 60% concentration sugar solution by nearly 2 in the 4th. For carbon tetrachloride, the change in RI per degree C change in temperature is about 6 in the 4th decimal place of RI. A9.3.2 SELECT AVERAGING / READOUT TIME You may select the number of readings averaged. The larger the number of readings averaged the slower the readout time. The fastest readout time, with no averaging, is about 1 to 1.5 seconds but the readings may appear unstable, especially if the sample is not clear. A medium setting gives about a 2.5 second reading time, or slow,about 5 seconds. The optimum speed depends on the type of samples being measured. Choose the slower speeds if the sample is not clear. To select of averaging / readout time press the CALIB key and enter the appropriate security access code (Section 11); type the number of the option you want and press ENTER to save the setting. This is why it is impossible to have a generally applicable temperature corrected RI scale. However, many users are normally measuring similar samples and so it is useful for these users to be able to program the refractometer to automatically correct the RI scale for the samples normally being measured. In normal use, the speed selected is indicated to the left of the display by the letter "F" for fast, "M" for medium or "S" for slow. A9.3.3 SELECT DISPLAY RESOLUTION RI and Brix PTR 2a You may alter the display to show 5 decimal places of RI or 2 decimal places of Brix. The last decimal place may not be stable and the accuracy of reading is not improved, but showing the extra decimal place may be useful if you are watching a trend in changing readings. If showing 5 decimal places of RI, each reading may take longer than normal. To a first approximation, the variation of RI of a particular sample with temperature can be represented by the linear equation: RI(T) = RI(Tref)[1 + α(T - Tref)] where T = measurement temperature Tref = reference temperature α = temperature coefficient You may set the "reference" temperature, i.e. the temperature the instrument will correct to, and also the temperature coefficient. PTR 2 X You may alter the display to show 4 decimal places of RI or 1 decimal place of Brix. Reducing the resolution may speed up the reading time. Also, if a particular batch of samples only requires readings to 4 decimal places of RI, the result is rounded for you and is easier to read and less prone to copying errors. If the RI of your sample DECREASES with INCREASING temperature, the coefficient should be NEGATIVE, If the RI INCREASES with INCREASING temperature, the coefficient should be positive. To set-up the temperature correction press the CALIB key and enter the appropriate security access code. Type in the values and press ENTER to store. On returning to the normal display, press the RI key to view the temperature corrected RI scale identified as RI(T). RI(T) is the RI reading that would have been obtained at the reference temperature, calculated from the instrument reading and taking into account the user To change the display resolution press the CALIB key, enter the appropriate access code and type 1 for 4 decimal places of RI (1 decimal place of Brix), 2 for 5 decimal places of RI (2 decimal places of Brix) and press ENTER to save. Temperature display (all models) You may also choose whether to display the 41 PTR 2a Handbook – Issue 3 June 2009 temperature. sample temperature to 1 or 2 decimal places. Proceed as above, but type in the Access Code for "Select display resolution - thermometer". If you want to REMOVE any user temperature calibration and return to the Index factory calibration, proceed as above but, instead of entering the temperature, type the value 0. A9.3.4 CALIBRATE TEMPERATURE The thermometers in the PTR refractometer have been calibrated against standard thermometers prior to dispatch over the full range of the instrument (15 to 50°C). The specified maximum temperature error across the entire range of the instrument is +/-0.5°C, but the typical deviation from absolute accuracy across the range is of the order of 0.05°C to 0.2°C. If for any reason you think the thermometer calibration is not correct (see also section 8), you may recalibrate the thermometer as follows. BEFORE ENTERING THIS ROUTINE IT IS ESSENTIAL THAT YOU HAVE A SUITABLE INDEPENDENT CALIBRATED THERMOMETETER WITH WHICH TO MEASURE THE SAMPLE TEMPERATURE. A suitable thermometer is one with a flexible wire thermocouple type probe which can be placed in the sample and the sample cover closed on the probe. The calibration of the thermometer should be carried out with a sample on the prism and the end of the thermocouple probe of the independent calibrated thermometer in the sample. DO NOT ENTER THIS PROGRAMME unless you are certain you need to alter the temperature calibration, the instrument and sample are stable in temperature and you are sure that you know the actual sample temperature: Press the CALIB key and type in the security access code for "Calibrate temperature." Type in the actual temperature of your sample and press ENTER. As any thermometer calibration adjustment required is likely to be extremely small, no more than a fraction of a degree, the instrument is programmed to reject any thermometer adjustment greater than 1°C. (If you think a larger adjustment is required, this suggests that a fault has occurred and the refractometer should be returned to the manufacturer for service/repair.) The newly entered sample temperature will initially appear on the display, but as the "set" temperature in unchanged, the cooling/heating control will immediately operate to adjust the sample to that set temperature and your sample temperature will be seen to increase or decrease as necessary to reach the "set" 42 PTR 2a Handbook – Issue 3 June 2009 APPENDIX 10 GUARANTEE INDEX INSTRUMENTS equipment is guaranteed against faulty materials and workmanship for one year from the date of delivery. During the guarantee period, Index Instruments will repair or replace at their discretion any faulty part and cover the labour costs thus incurred. This guarantee excludes fair wear and tear and accidental damage. If, in our opinion, damage has resulted from mishandling or interference with parts or settings (except with instructions and permission from Index Instruments) our normal service charges will apply. Index Instruments Ltd will charge normal service rates where instruments are damaged due to the use of aggressive samples, i.e. samples that are able to attack 316 stainless steel, silicone based materials, "Delrin" plastic (Acetal Homopolymer) or sapphire, unless Index Instruments Ltd. have agreed otherwise in advance of purchase. This guarantee is invalidated if the base unit seal of the PTR is broken. In the event of a breakdown, contact either your agent or Index Instruments Ltd at the address given below. We will either: a) Advise you how to correct the fault yourself. b) Send an engineer to carry out the work. c) Ask you to return the faulty instrument to our works. Whenever possible, pack in the original packing box and always return the power supply along with the instrument. If you do not have the original packing box, a new one can often be sent on request. Returned items must be sent carriage paid and fully insured by you for both the outward and return journeys. If you are not using the original packing, mechanically isolate the power supply box from the instrument to prevent mutual damage. Note that if you are returning the instrument for repair, please enclose WITH THE INSTRUMENT a written description of the fault. INDEX INSTRUMENTS Ltd. Industrial Estate, Bury Road, RAMSEY, Huntingdon, Cambridgeshire, PE26 1NF ENGLAND In the U.S.A. contact INDEX INSTRUMENTS US INC. 3305 Commerce Boulevard Kissimmee, FL 34741 U.S.A. Tel: +44 (0) 1487 814313 Fax: +44 (0) 1487 812789 E-Mail: [email protected] Tel: 407 932 3688 Fax: 407 932 3686 E-mail: [email protected] 43 PTR 2a Handbook – Issue 3 June 2009 (F) ANNEXE 10 GARANTIE INDEX INSTRUMENTS garanti ses appareils contre tout vice de fabrication pendant un an date de livraison. La garantie s’entend pièces et main d’œuvre, matériel retourné en nos ateliers aux frais du client. Pendant la période de garantie, INDEX INSTRUMENTS se réserve le droit de réparer ou de purement et simplement échanger un appareil qui serait déficient. Sont exclus de la garantie les dommages dus à une mauvaise utilisation de nos appareils ou tout dommage consécutif à un choc ou encore toute intervention d’un tiers non autorisé par Index Instruments. La garantie cesse également s’il s’avère que l’appareil a été ouvert pendant la période de garantie. Il en est de même si l’appareil a été utilisé avec des échantillons ou des solvants incompatibles avec les matériaux en contact avec les échantillons ou susceptibles de l’être (inox 316, joints silicone, saphir de synthèse), sauf si vous avez obtenu notre accord écrit avant l’achat de l’appareil. En cas de doute sur la compatibilité de vos produits et solvants, reportez-vous au paragraphe ou n’hésitez pas à nous contacter. En cas de panne, ne retournez pas votre appareil a notre service technique sans avoir au préalable contacté soit notre importateur local soit notre société afin de connaître la marche à suivre. Selon la nature du problème, nous vous conseillerons soit de : a) Corriger vous-même l’anomalie de fonctionnement (pseudo pannes). b) Nous retourner l’appareil parfaitement emballé s’il s’agit vraiment d’une panne. Dans ce cas, n’oubliez pas de joindre un descriptif précis du problème rencontré. Nous vous rappelons que dans tous les cas, les appareils voyagent sous la seule responsabilité de nos clients : il vous appartient donc de payer les frais de port aller/retour ainsi que l’assurance pour le transport. Pour nous contacter : INDEX INSTRUMENTS Ltd. Industrial Estate, Bury Road, RAMSEY, Huntingdon, Cambridgeshire, PE26 1NF ENGLAND Telephone +44 (0) 1487 814313 Fax +44 (0) 1487 812789 E Mail [email protected] 44 PTR 2a Handbook – Issue 3 June 2009 APPENDIX 11 DECLARATION OF CONFORMITY (F) ANNEXE 11 DECLARATION DE CONFORMITE (D) ANHANG 11 Konformitätsbescheinigung (E) APENDICE 11 DECLARACION DE CONFORMIDAD EC Declaration of Conformity We of Index Instruments Ltd. Industrial estate, Bury Road, RAMSEY, Huntingdon, Cambridgeshire, ENGLAND PE26 1NF in accordance with the following Directives: 2004/108/EC The Electromagnetic Compatibility Directive 2006/95/EC The Low Voltage Directive hereby declare that: Product: Refractometer Models: PTR 2a, 2aX, 46, 46X, 46XP, 46DL is in conformity with the applicable requirements of the following standard: BS EN 61326:2006 Electrical equipment for measurement, control and laboratory use. EMC requirements. I hereby declare that the equipment named above has been designed to comply with the relevant sections of the above referenced specification. The unit complies with all applicable Essential Requirements of the Directives. Signed by: Name: J. L. Horn PhD BSc MInstP Position: Director At: Ramsey On: 4 September 2008 Document Ref. No. PTRCE2, Issue1 45 PTR 2a Handbook – Issue 3 June 2009 46 PTR 2a Handbook – Issue 3 June 2009 INDEX Aggressive samples, 4 Archive data, 27 Averaging 28, 41 Autoprint, 39 Auxiliary port, 25 Bar code, 24 Baud rate, 23, 25 Brix, 37 Calcium fluoride, 33 CE Certificate, 45 Cleaning, 13 Computer, 25 Contact fluid, 32 Continuous mode, 39 Date, 27, 38 Diagram of PTR, 10 Display, 11 Error message, 36 Fuse, 8 Glass test pieces, 32, 33 Guarantee, 43 Input, 24 Installation, 1, 8 Installation, printer, 9 Introduction, 3 Liquid standards, 33 Lithium fluoride, 33 Location, 22 Lock, 27 Mode of operation 27, 39 No reading, 34, 36 Operation, 12 Plastics, 15 Print options, 27, 38 Printer, 9, 23, 35 Remote Control Unit 27 Remote port, 24, 25 Resolution, 28,29,30,41 RS232, 9, 23, 38 Sample type (N or E), 40 Sampling, 13 Scales 27 Security access codes 28 Silica, 32, 33 Single Scan Mode, 39,40 Software, 25 Solid samples, 15, 32 Stability mode, 39 Standards, 33 Temperature, 22, 27, 38 Temperature corrected Brix scale, 27, 37 Temperature corrected RI scale 28, 41 Test pieces, 30, 36 Time 27,38 Time to read, 27,41 Warnings, 4 Zero, 20 47
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