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4

Calibration

This chapter describes the procedure for calibrating your

instrument. If you have questions or problems regarding the cal-

ibration procedure, please consult 

Chapter 5 —

Troubleshooting & Service

.

Calibration procedure

Aside from requiring manual sample introduction, calibration of

the 4250 is automatic. Following the procedure suggested

below, you simply select 

CALIB

and initiate six freezing-point

tests on each of two calibration standards, -422 m°H  (-408

m°C) and -621 m°H (-600 m°C), as prompted by the display. 

NOTE

If calibration information has been lost or bin numbers

have been changed, the results may not match the nomi-

nal value.

The calibration procedure follows:
1.  At 

“

Cryoscope Ready

”

(or the date and time standby dis-

play), press 

CALIB

. The 

CALIB

soft key will light and the

display will quickly change to 

“

Calibration

”

, then prompt

you for the first calibration standard.

     If the sample probe is replaced, the sample probe bin # must

be determined and set before the 4250 can be recalibrated.

2.  Load the standard sample prompted by the display into the

freezing chamber and press 

START

. The display will change

to 

“

Cooling Sample

”

, the operating head will lower, a cali-

bration test will be run, and the results will be displayed and

39

Содержание 4250

Страница 1: ...4255 Rev11 032317 The Advanced Cryoscope Model 4250 User s Guide...

Страница 2: ...not intended to be representa tions or warranties concerning the product described Microsoft and Windows are registered trademarks of Microsoft Corporation in the United States and other countries Int...

Страница 3: ...tional items 1 Step 3 Unpack the instrument 2 Step 4 Install the heat transfer fluid 2 Step 5 Load printer paper 5 Step 6 Power up the instrument 5 Step 7 Prime the heat transfer fluid pump 7 Step 8 R...

Страница 4: ...igure 6 Keypad Layout and Functions 14 Figure 7 Back Panel 15 Table 2 Barcode Port Connections 16 Table 3 Setup Menu Items 26 Chapter 3 Standards Quality Control 35 Repeatability and accuracy 35 Stand...

Страница 5: ...Figure 10 Operating Head 63 Figure 11 Mandrel Probe and Stir Freeze Wire Adjustment 65 Table 4 Test Menu Items 49 Appendices Appendix A Troubleshooting Table 67 Appendix B Product Specifications 75 A...

Страница 6: ...Notes vi Advanced Cryoscope Model 4250 User s Guide...

Страница 7: ...int within an equilateral triangle is intended to alert the user to the presence of important operat ing and maintenance servicing instructions in the literature accompanying this product The lightnin...

Страница 8: ...ct If the power cord provided is replaced for any reason or if an alter nate cord is used the cord must be approved for use in the local country The power cord must be approved for the product s liste...

Страница 9: ...o not operate this product with the covers removed or unsecured FCC Requirements WARNING Changes or modifications to this unit not expressly approved by Advanced Instruments could void the user s auth...

Страница 10: ...by one or more of the following measures Reorient or relocate the receiving antenna Increase the separation between the equipment and receiver Connect the equipment into an outlet on a circuit differe...

Страница 11: ...sor Keys Probe Stir Wire Alignment Tool Kit Mandrel Power Cord specify voltage and country One way Check Valve PART NO 70022 330016 3C2241 3DA811 4D3710 3D2340 FLA835 3D3185 3LA700 3LH500 4D3705 To or...

Страница 12: ...of Probe Bin Setting Fluid Stainless Steel Sample Tube Rack Sample Tubes marked at 2 mL and 2 5 mL RS 232 Cable 3 meters Service Manual 3250 4250 Stir Freeze Coil Stir Freeze Wire Advanced User Inform...

Страница 13: ...Reference Solution 512 m C PART NO 3LA023 3LA033 3LA030 NOTE Advanced Instruments cannot guarantee the stated instrument performance specifications and accuracy of test results unless Advanced Instru...

Страница 14: ...xiv Advanced Cryoscope Model 4250 User s Guide Notes...

Страница 15: ...re Most solutes impede the crystallization of water and depress its freezing point in proportion to their concentration Milk is a water based solution with various solids in suspen sion The solutes no...

Страница 16: ...storting the freezing plateau A sensitive probe monitors the sample temperature controls the degree of supercooling and freeze induction and measures the freezing point of the sample The tip of the sa...

Страница 17: ...wait for less repeatable peak readings In order to maintain agreement between dif ferent instruments milk cryoscope manufacturers traditionally have incorporated plateau timers set for a reasonable co...

Страница 18: ...gh varying slightly with breed and diet the freezing points of authentic samples of pure fresh milk from healthy cows in the U S and Canada average 540 4 m H 521 8 m C 2 The freezing point average was...

Страница 19: ...estigators often thought the solute concen tration of milk to be more constant than it actually is Contemporary milk cryoscopy literature often referred to a concept called added water which it was th...

Страница 20: ...percent deviation from base Using DFB in this manner can provide a guideline for estimating the quality of milk samples in respect to the base established All unknown samples of milk run against this...

Страница 21: ...o remain in the liquid state when cooled below its freezing point Crystallization Temperature Aqueous solutions can be induced to freeze i e crystallize most reliably when supercooled The crystalliza...

Страница 22: ...nation of the Freezing Point Depression of Milk BS3095 Part 1 1988 6 IDF 1S0 A0AC Method Water Added in Milk Thermistor Method Section 96LO7 AOAC METHODS Association of Official Analytical Chemists 15...

Страница 23: ...keep your workplace free of debris and allow 6 inches 15 cm of clear space on each side of the instrument for fan driven air circulation Electric outlet availability Your instrument will need to oper...

Страница 24: ...sing within 10 days of a shipment s arrival d If you receive any damaged items save the cartons and packing material those items came in for inspection by the insurer The carri er dealer and Advanced...

Страница 25: ...3LA030 530 m H Lactrol Reference Solution 512 m C 2 bottles 3DA811 Heat Transfer Fluid 1 3D3185 Operator Supervisor Keys set of 2 1 Power Cord as specified 1 3LA700 Probe Stir Alignment Tool Kit 1 3LA...

Страница 26: ...ainer to return the heat transfer fluid to the container for recirculation 7 Stand the container of heat transfer fluid in the plastic tray in the heat transfer fluid compartment making sure the filte...

Страница 27: ...uld be level If the paper roll is not level carefully reseat the roller between the roller guides 5 Hold the paper down onto the surface of the osmometer and center the paper on the printer tear bar W...

Страница 28: ...Advanced Cryoscope Model 4250 User s Guide 6 Figure 3 Load Printer Paper...

Страница 29: ...e TEST menu as follows 1 Insert sample tube in well and press the TEST key The display will change to Select Test Item 2 Press the key to step the display backward to Head Up Down Test 3 Press the STA...

Страница 30: ...spond with the display Running Diagnostics while it lowers the operating head cools the freezing chamber and com pletes a series of internal diagnostic checks If the diagnostic checks are not successf...

Страница 31: ...nglish If you would prefer to operate the instrument on one of the other languages you should change the language setting as described in Chapter 2 Step 11 Check initial factory calibration Your instr...

Страница 32: ...f you have followed the steps outlined in this chapter your instrument is ready for use To learn how to operate your instrument read the next chapter Instrument Operation We strongly recommend that yo...

Страница 33: ...these materials in a safe and acceptable manner that is in compli ance with all country state and local requirements CAUTION The heat transfer fluid contains hazardous chemicals Consult the material...

Страница 34: ...cate the probe and sample in the freezing chamber Freezing chamber Figure 5 Item 8 Sample cooling is performed by a thermoelectric cold stage The cham ber contains a small amount of heat transfer flui...

Страница 35: ...ication Board The application board contains the circuits for con trolling and interfacing with the other subsystems such as the keypad display head motor cooling assembly RS 232 printer and barcode p...

Страница 36: ...ic test menu Initiates calibration procedure Allows numeric input as required Steps through menu items Clears some data in setup mode and when using sample identification Confirms sample identificatio...

Страница 37: ...on allows access to the setup test and calibration functions as well as the sample and test func tions If the SETUP or CALIB key is pressed while the Supervisor Operator keyswitch is in the Operator p...

Страница 38: ...e 7 The RS 232 port allows you to output your instrument s data messages to an external device such as a computer For more detailed information dealing with the RS 232 port please read the section tit...

Страница 39: ...0 C for 5 minutes but note that for calibration accuracy the stan dards should be pre warmed as well Particulate matter can also cause premature crystallization Both particu late matter and congealed...

Страница 40: ...l methods of plateau determi nation These are grouped into two types TIMED and SEEKING Setup menu item 10 Select Plateau Mode is used along with the or keys to cycle through the choice of 30 60 or 90...

Страница 41: ...be stir freeze wire mandrel and the top of the freezing chamber in that order with a soft lint free non ionic paper tissue dampened with distilled water to remove anything that might contaminate the s...

Страница 42: ...rerun the same sample or use it for another procedure remove it from the freezing chamber as soon as possible and keep it covered between tests 6 Always use the same operating procedure as proper cons...

Страница 43: ...ing head will lower the sample probe into the sample tube in the freezing cham ber The fan will come up to full speed and the freezing chamber will cool The sample temperature will follow the freezing...

Страница 44: ...accuracy before running tests on unknown samples Follow the techniques recommended on page 20 Repeatability Tips When checking cali bration and repeatability with standards or reference solutions it i...

Страница 45: ...ything that might contaminate the sample to be tested Be careful not to bend the probe or stir freeze wire 3 Select a reference solution or NaCl standard with a freezing point close to that expected f...

Страница 46: ...r with a soft clean dry lint free paper tissue after each test to avoid contaminating the next sample Be careful not to bend the probe or stir freeze wire 10 Repeating steps 1 8 test two to four more...

Страница 47: ...ndividually set up at the factory for normal opera tion but SETUP may be required for changing the date and time or customizing the SETUP parameters for your own individual needs NOTE The Supervisor O...

Страница 48: ...is installed in your instrument or if the parameters have been lost Upon entering Set Block Bin the current setting will be displayed To change the setting enter your new block probe bin number by me...

Страница 49: ...u may also use the keys to step through the available choices Once you press ENTER you will be asked to confirm the change Press ENTER to confirm Changing the sample probe bin number forces recalibrat...

Страница 50: ...ses the stir amplitude pressing decreases the stir ampli tude 3 Press ENTER to store the new setting or STOP to restore the original setting 5 Set Date Time This menu item enables changing the date ti...

Страница 51: ...cated by the symbol 2 At on beeper off press or to toggle the keypad beeper on or off Neither selection will affect the invalid selec tion beeper except that when the keypad beeper is on an invalid se...

Страница 52: ...etup menu This number is set by the factory and cannot be changed by the operator 10 Select Plateau Mode This menu item enables changing the way the 4250 evaluates the plateau An idealized dimensionle...

Страница 53: ...dout temperature units see Foreword for a discussion of the units of measurement used for milk cryoscopy CAUTION Changing this setting requires changing the DFB set ting if not set at zero as well See...

Страница 54: ...gram for use in plotting freezing curves 16 Assistance Pressing START at this SETUP menu item will present you with infor mation on how to contact Advanced Instruments for supplies and ser vice Import...

Страница 55: ...data rate for communications is 9600 bps bits per second though you may alternatively select 1200 2400 4800 and 19200 bps The DB 9 RS 232 port on your instrument conforms to the DTE EIA 232C standard...

Страница 56: ...34 Advanced Cryoscope Model 4250 User s Guide Notes...

Страница 57: ...in the same result time after time on the same sample Repeatability or precision is usually quantified as the standard deviation S D of a set of measurements normally distributed about a mean 1 S D ab...

Страница 58: ...latory bodies for their guidelines and or control requirements Maintenance of standards Doubts about the accuracy of standards destroy confidence in the accu racy of the test Advanced cryoscope standa...

Страница 59: ...ggestions in the repeatability tips section 4 Instrument accuracy is determined by comparing your results on precisely known standards and or controls with their specified val ues The instrument accur...

Страница 60: ...Advanced Cryoscope Model 4250 User s Guide 38 Notes...

Страница 61: ...OTE If calibration information has been lost or bin numbers have been changed the results may not match the nomi nal value The calibration procedure follows 1 At Cryoscope Ready or the date and time s...

Страница 62: ...eadout and display Calibration Complete 3 At Calibration Complete one may press STOP to return to Cryoscope Ready CALIB to restart the calibration sequence or START to lower the operating head and sta...

Страница 63: ...nternally the 4250 accomplishes calibration in two steps First it records the raw means of the results of freezing point tests on standards at each of the two calibration levels Then it performs the n...

Страница 64: ...e If the repeatability problem recurs despite good operating technique please call or write immediately for Hot Line service NOTE If the instrument has lost all previous calibration data and you see t...

Страница 65: ...or mechanical hazards Performing service or maintenance not detailed in the User s Guide with or without a Service Manual should only be done by a qualified service technician Never restrict airflow...

Страница 66: ...second time it is probably caused by failure of a component part If this occurs refer service to qualified service personnel Always replace the fuse with one of the same rating voltage and type Never...

Страница 67: ...ng recommended diagnostic checks If you need to order parts or service a purchase order from your purchasing agent will be neces sary After Hot Line diagnosis your service technician may assist you in...

Страница 68: ...ent or accept the damage risk Routine maintenance Daily Checks you should perform to keep your instrument in peak con dition are 1 Calibration Repeatability Readings each day on separate aliquots of t...

Страница 69: ...If you are experiencing difficulties with your instrument first carefully review the operational requirements listed in the product specifications and the recommended setup and oper ating procedures...

Страница 70: ...following two ways At Select Test Item repeatedly press the key to step the display forward or to step the display backward through the list The list is cyclic pressing at the last item cycles the dis...

Страница 71: ...t results 5 Press the left key a second time to display the coefficient of variance of the selected number of last results 6 To return to the diagnostic menu press the STOP switchpad 7 To return to Cr...

Страница 72: ...will display and print the data of the most recent test result 4 Use the or keys to see the results stored in the recall buffer 5 Continue in this manner until you have recalled the necessary results...

Страница 73: ...e from off to 1 to 8 in steps of 1 C to off etc The sample head will rise when temperature is set to off and lower at any other setting Pressing the key sequentially changes the channel and readout un...

Страница 74: ...H2O may be used in place of probe bin setting fluid for this test The bin number thus determined will be acceptable for bin setting though the probe resistance displayed will be that at the freezing...

Страница 75: ...e procedure Set Sample Bin described in Chapter 2 to preset a random sample probe bin number such as 5 Then press TEST and rerun the probe bin test Finally as necessary press SETUP and use the Set Sam...

Страница 76: ...beeper 2 Press STOP to exit to the test menu 9 Keypad Test This test enables checking each key on the keypad as well as the lamps of each illuminated key As each key is pressed its name should be dis...

Страница 77: ...rd 2 Use a small flat bladed screwdriver or similar tool to remove the fuse holder door Remove the fuse holder 3 Double check the values marked on the fuses The Model 4250 will automatically adjust fo...

Страница 78: ...turn it off 3 Remove the head cover by removing the two top screws and pulling the cover straight up 4 Unplug the sample probe connector Figure 10 Item 1 The probe leads are electrically accessible t...

Страница 79: ...ting the mandrel Then raise the mandrel up around the stir wire Align the mandrel so the stir wire channel is perpendicular to the front edge of the chassis and so the flange is flush with no gaps bet...

Страница 80: ...easure a sample of probe bin setting fluid into a clean sample tube place the tube in the freezing chamber and press the START soft key The 4250 will run a special freezing point test to determine the...

Страница 81: ...and adjustment of the mandrel probe and stir freeze wire are of utmost importance to assure accuracy precision and proper operation of the instrument NOTE After making any probe and or stir freeze wi...

Страница 82: ...is tort the thin plastic wall of the mandrel Recheck the probe position 4 The bottom of the stir freeze wire should be even with the same level as the end of the probe As necessary remove the head cov...

Страница 83: ...he probe tip is necessary to center the black bead in the 2 mL sample volume loosen the probe setscrew Figure 10 Item 6 then manually raise or lower the probe within the man drel Retighten the setscre...

Страница 84: ...stir freeze wire and press If properly adjusted as recommended in Chapter 2 Set Buzz Amplitude the stir freeze wire should produce a loud buzz vibrate principally fore and aft and never strike the pr...

Страница 85: ...g the coil to clapper spacing probably will adversely affect the stir freeze wire tip location after bending the yoke realign the stir freeze wire according to the recommendations in the Mandrel Probe...

Страница 86: ...ess the START soft key The display will change to Amplitude xxx with xxx being a value of approximately 140 Looking from the side of the instrument you should be able to see a stir vibration blur at t...

Страница 87: ...robe and or stir freeze wire adjustments check the instrument calibration and re calibrate as necessary 65 Troubleshooting Service The flange of the mandrel must be flush with the head chassis The bla...

Страница 88: ...66 Advanced Cryoscope Model 4250 User s Guide Notes...

Страница 89: ...and change as necessary Error is self correcting If the error persists contact Advanced Instruments for Hot Line Service Reset baudrate If the error persists contact Advanced Instruments for Hot Line...

Страница 90: ...ent s cooling chamber contains enough heat trans fer fluid If the problem persists contact Advanced Instruments for Hot Line Service Turn unit off and on Custom settings and probe bin numbers may need...

Страница 91: ...t the fan is plugged in and that the fan isn t blocked Check the fan driver LED on the application board Try restarting your instrument If this does not solve your problem contact Advanced Instruments...

Страница 92: ...ent will function normal ly as long as the main power remains on Contact Advanced Instruments for Hot Line Service The heat transfer fluid pump may be malfunc tioning or there may be a leak or obstruc...

Страница 93: ...there is paper in the printer If there is not install paper per the instructions in Chapter 1 Installation and Setup If there is paper in the printer make sure that the printer cover is completely an...

Страница 94: ...lease call Hot Line Service for assistance Test another aliquot of that sample in a clean sample tube Try testing samples known to be within the range of the instrument This message can be displayed f...

Страница 95: ...Switch the instrument off then on Make sure the sample probe is plugged into the main board Check the sample probe by running the A D tests If the error message does not persist and other error messa...

Страница 96: ...b lem persists check your block probe number If you need more assistance contact Advanced Instruments for Hot Line Service This error message indicates a problem with your thermoelectrics Check the th...

Страница 97: ...1 m C or m H Communications On board printer DTE EIA 232 V 24 RS 232 serial port and optional barcode scanner Performance at Reference Conditions1 Linearity Less than 0 5 from a straight line Repeatab...

Страница 98: ...nd Level Measured at operator s position 45 dB A Typ 90 dB A max 2 sec Dimensions inches centimeters Width 13 0 33 0 Depth 18 0 45 7 Height 12 0 30 5 with Head Up 16 0 40 6 Weight pounds kilograms Net...

Страница 99: ...international approvals to this product Consult the distributor or dealer for more information and documentation Connections to this product must be made with shielded cables Use of non shielded cable...

Страница 100: ...roduct meets the intent of Directive 2014 30 EU Conformity EMC for Electromagnetic Compatibility Compliance was demonstrated using the following standards as listed in the Official Journal of the Euro...

Страница 101: ...a tion Canadian ICES 003 This Class B digital apparatus complies with Canadian ICES 003 Cet appareil num rique de la classe B est conforme la norme NMB 003 du Canada Japan VCCI This Class B digital ap...

Страница 102: ...80 Advanced Cryoscope Model 4250 User s Guide Notes...

Страница 103: ...nsibilities which constitute contractual warranties and conditions between the seller and the user for the maximum benefit and useful ness of the instrument ADVANCED INSTRUMENTS WARRANTS THAT IT 1 Has...

Страница 104: ...ithout written approval from Advanced Instruments 4 Advanced Instruments will be notified immediately if any injury occurs in any association with the instrument and will be allowed prompt and thoroug...

Страница 105: ...orrected repairs d Only for the purpose stated in the instructions provided with the instrument e In which the equipment has been maintained according to the instructions provided 3 Immediate notifica...

Страница 106: ...Advanced Cryoscope Model 4250 User s Guide 84 Notes...

Страница 107: ...s no protocol for talking to the instru ment This product s serial port output is based on ASCII code protocols No special codes are used to identify errors test results or normal oper ational message...

Страница 108: ...and cable are operating correctly 1 Create a Hyperterminal connection using the Hyperterminal pro gram 2 While working within that connection choose the Properties selec tion from the File menu 3 Sel...

Страница 109: ...87 Supplemental RS 232 Information Null Modem Cable Shield connects to metalized con nector housing at both ends...

Страница 110: ...88 Advanced Cryoscope Model 4250 User s Guide Notes...

Страница 111: ...ons Appendix F On Off Feed Interrupt Test Start Stop Record Review Setup Calibration Cancel Delete Functional Arrow Printer Enter RS232 Bar Code Attention Caution Hot Surface Dangerous Voltage Lifting...

Страница 112: ...gile Irritant Keep Dry Date Manufactured Sterile Non Sterile Serial Number Solution Do Not Open Top Handle With Care Toxic Use Blade To Open Do Not Re Use For In Vitro Diagnostic Use European Conformi...

Страница 113: ...tions Sufficient for x Tests Open Here Low Fluid Level Keep Hands Clear Manufacturer Latex Free Diluent See Instructions for Temperature Guidelines Potential Puncture Hazard Electronic Equipment Dispo...

Страница 114: ...92 Advanced Cryoscope Model 4250 User s Guide Notes...

Страница 115: ...ce regulations governing the disposal of your instrument and acces sories may vary depending upon your geographic location the following guidelines are provided to assist you in identifying the option...

Страница 116: ...cts can be sent Contact Advanced Instruments Hot Line Service 800 225 4034 toll free within the USA and Canada after nor mal business hours dial extension 2191 US 781 320 9000 elsewhere 781 320 0811 f...

Страница 117: ...95 Model 4250 Serial Number Software Revision Sample Probe Number Block Probe Number Service Log Appendix H Date Problem Symptom Action...

Страница 118: ...Advanced Cryoscope Model 4250 User s Guide 96 Date Problem Symptom Action...

Страница 119: ...calibration 39 procedure 39 notes 41 calibrators xiii control circuits 13 crystallization temperature xxi D data capture 32 date time 9 28 definitions xxi 82 89 diagnostic test 8 48 dis enable I D 27...

Страница 120: ...milk cryoscopy xv O operating head 12 63 operational requirements 47 obtaining service 44 P packing list 3 added water xxii DFB xix xxii 30 plateau mode 18 30 power cord connector 16 power module 16...

Страница 121: ...ting 25 date time 28 sample bin number 27 serial rate 29 stir amplitude 28 standards and controls 18 statistics 48 stir freeze test 52 stir freeze wire alignment 59 supercooling xxi supervisor operato...

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