KEM MKC-710 Operation Manual Download Page 9

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MKC-710

7-1-1. Karl Fischer grease

.................................................................................................................84

7-1-2. Replacement of septum

.......................................................................................................85

7-1-3. Changing the desiccant

........................................................................................................85

7-1-4. Replacement of the anolyte (anode reagent)

..........................................................86

7-1-5. Replacement of the catholyte (cathode reagent)

..................................................86

7-1-6. Check the instrument

............................................................................................................87

7-1-7. Check the cable

........................................................................................................................87

7-1-8. Check the connectors

...........................................................................................................87

Other Maintenance

........................................................................................................... 88

7-2.

7-2-1. Storage of the instrument

..................................................................................................88

7-2-2. Cleaning the electrode

.........................................................................................................88

7-2-3. Cleaning the titration cell

....................................................................................................91

7-2-4. Distance adjustment between anode electrode and diaphragm

...................91

7-2-5. Replacement of pump tube

...............................................................................................92

7-2-6. Replacement of the filter

....................................................................................................93

7-2-7. Replacing the clock battery

................................................................................................94

8. Troubleshooting

Error messages and alarm messages

..................................................................... 95

8-1.

Stirrer does not work properly

.................................................................................... 97

8-2.

Drift level is too high

....................................................................................................... 98

8-3.

It runs into over-titration

............................................................................................... 99

8-4.

Poor repeatability or no EP found

......................................................................... 100

8-5.

Glass contact area jammed

...................................................................................... 101

8-6.

When the drain pump is clogged

........................................................................... 102

............................................................................................................................. 103

9-1.

Options

............................................................................................................................... 107

9-2.

Specification

..................................................................................................................... 112

9-3.

Principle of measurement

......................................................................................... 113

9-4.

Karl Fischer reagent

..................................................................................................... 114

9-5.

Parameter list

.................................................................................................................. 117

9-6.

9-6-1. Setup parameters

................................................................................................................. 117

9-6-2. Method parameters

............................................................................................................. 119

9-6-3. Selection of Method parameters and printout

...................................................... 120

International standards

.............................................................................................. 121

9-7.

10. Warranty and After-sales Service

122

Summary of Contents for MKC-710

Page 1: ...ance of the equipment Overseas Division Yamawaki Bldg 9F 4 8 21 Kudan Minami Chiyoda ku Tokyo 102 0074 JAPAN FAX 81 3 3237 0537 Phone 81 3 3239 7333 E mail overseas tokyo kyoto kem com URL http www kyoto kem com Factory 56 2 Ninodan cho Shinden Kisshoin Minami ku KYOTO 601 8317 JAPAN FAX 81 75 691 9961 Phone 81 75 691 4122 AN 59 00392 01 Ver 00 ...

Page 2: ......

Page 3: ...stored in USB flash drive and data can be managed as an electron record Moreover the measurement result can be stored as PDF file and the convenience of data has been improved A keyboard for the input of number a barcode reader for the sample setting and a foot switch that can start to measure without touching a device are installed as option The working efficiency of measurement improved for cust...

Page 4: ...tuated or near power source or magnetic field Excessive range of temperature other than specified Ambient humidity exceeding 85 RH Under vibration Location with large temperature difference Power Source Warning You must ground earth wire of power cable Danger of electric shock if not grounded to earth The power supply from AC adapter other than that are specific to the equipment we can not guarant...

Page 5: ...utionary statements of the reagent label Drained before the waste bottle is full the amount of waste Dispose of in accordance with laws and regulations If spilled reagent after measurement may corrode the tube connector causing the dispenser malfunction Other Cautions Caution Do not attempt overhaul or repair the unit by unauthorized person except authorized by KEM Danger of electric shock fire or...

Page 6: ...plained the sign each of PRE TITR and It is prohibited to duplicate any part or all of manual without prior consent This manual has been prepared to the best of our knowledge however if you should find any missing or ambiguous description please contact your nearest dealer or sale representative Maker will not be liable for any loss or damage caused by use of or the result of the product This manu...

Page 7: ...general 16 2 2 2 2 1 Basic key operation 17 2 2 2 Description of display messages 18 Setting Language 19 2 3 Setting date and time 20 2 4 3 Basic operation 21 Sequence of measurement 21 3 1 Assemble the Titration cell 22 3 2 Filling reagent and draining 23 3 3 3 3 1 Catholyte 23 3 3 2 Anolyte 24 Measure the sample 27 3 4 Re calculate titration data 29 3 5 Batch processing of titration data 31 3 6 ...

Page 8: ... Connecting to instrument 65 5 5 2 Starting app 66 5 5 3 Starting Pre titration 67 5 5 4 Starting measurement 68 5 5 5 Measurement 70 5 5 6 Entering weight 70 5 5 7 Uninstall Android apps 71 6 Setup 72 Interface 73 6 1 6 1 1 RS 232C setting 73 6 1 2 Date acquisition software SOFT CAP 74 6 1 3 Printer setting 74 6 1 4 Balance setting 76 6 1 5 USB setting 76 Operator 77 6 2 Date Time 78 6 3 Serial N...

Page 9: ...of pump tube 92 7 2 6 Replacement of the filter 93 7 2 7 Replacing the clock battery 94 8 Troubleshooting 95 Error messages and alarm messages 95 8 1 Stirrer does not work properly 97 8 2 Drift level is too high 98 8 3 It runs into over titration 99 8 4 Poor repeatability or no EP found 100 8 5 Glass contact area jammed 101 8 6 When the drain pump is clogged 102 8 7 9 Others 103 Parts list 103 9 1...

Page 10: ......

Page 11: ...on Cell Unit 65 00028 01 Clamp filter 1 64 00898 AC Adapter Type4 1 64 00633 64 00633 01 64 00633 02 64 00633 03 Power Cord EU KR with PlugC WS 010 Power Cord US TW with PlugB WS 001 Power Cord GB with PlugG WS 012A Power Cord CN with PlugI WS 015D 1 200 240 V 100 120 V 220 240 V 200 240 V 64 01386 Stirrer Cable 0 6m 1 12 04251 Washing Bottle 1 12 01394 10 Septum 10pcs set 1 12 04232 KF Grease 5g ...

Page 12: ...Cell Transparency 1 Components of Manual Solvent Change Unit 12 05685 Part Number Part Description Qty Remarks 12 05686 Bottle holder unit 1 with Desiccant Tube 69 00028 00 Polyethylene Bottle 1L 1 12 03926 Reagent Bottle Cap with Plug 1 12 03926 01 Reagent Bottle Cap for Injection 1 12 04875 Rubber Globe for Suction 1 12 04875 01 Rubber Globe for Drain 1 12 02020 11 Injection Tube 2 3 L 1180mm PF...

Page 13: ...e Bottle Cap 2 12 02020 11 Injection Tube 2 3 L 1180mm PFA 1 12 01260 Desiccant Tube φ18x120 with Silica Gel 1 12 04538 02 Drain Tube to Cell 2 3 L 0 69m PFA 1 12 04539 Drain Tube to Waste Bottle 2 3 L 1m PFA 1 20 02559 00 Plug for Titration Flask 1 60 00109 02 Tube 4x8 L 1m Silicone 2 12 06270 Suction Tube Bottle Cap Pump 1 20 06823 Bottle holder 1 1 20 06823 01 Bottle holder 2 1 20 06823 02 Bott...

Page 14: ...the port plug and syringe inlet Note Make sure to apply KF grease around glass sliding area Note The seal on desiccant tube A on titration flask must be removed before using Warning When handling the inner burette do not hold the housing black resin area and sliding area of desiccant tube in order to avoid breakage electrode port plug stirrer rotor desiccant tube inner burette syringe inlet ...

Page 15: ...lectrode Tighten the plug screws firmly 1 2 2 Installation of Clamp Filter Install the clamp filter to AC adapter as figure below Hold the clip of the clamp filter and open as figure below and wrap treble remaining the tip by about 30mm 30mm Clip Note Installation of the clamp filter to AC adaptor is needed to satisfy the condition of EMC standard ...

Page 16: ...re the power switch is in Off position as figure below 2 Connect the cables as shown below Install Power cord to AC adapter and plug in AC adapter on the back of main unit Stirrer Cable Power cord Power switch AC adapter 3 Connect Power cord to the power outlet ...

Page 17: ...he rubber globe 5 Connect the reagent bottle to a commercially sold KF reagent bottle filled with anolyte Drain side Discharge side Injection tube Reagent bottle cap Squeeze in Insert Insert to desiccant tube Rubber globe Rubber globe for drain Drain tube Polyethylene bottle Squeeze in Insert Reagent bottle cap with plug Squeeze in Note If loosely squeezed it in pressurized air may leak and it may...

Page 18: ... the holder use the bottle holder and bottle stand as shown below 8 Connect the tube for drain and injection to the Plug for titration flask as shown below respectively Plug for titration flask To rubber ball for reagent discharge Bottle stand Bottle holder 9 Insert the Plug for titration flask carefully into the titration cell At this point apply a small amount of KF grease on slide contact area ...

Page 19: ...r leak which would prevent the dispenser from working properly in suction and draining 2 Connect the silicone tubes on both ends of desiccant tube and put the tube in place as shown below 3 Put the above 1 bottle in reagent bottle holder If the outside diameter of solvent bottle does not match the holder use the bottle holder and stand as shown below 4 Connect the silicon tubes one to the top of s...

Page 20: ...e and the drain tube to Cell to magnetic stirrer back side pump 8 Connect the silicone tube connected 2 to SOLVENT port on the rear panel of magnetic stirrer 9 Attach a filter to INTAKE port on the rear panel of magnetic stirrer Note Please attach a filter to INTAKE by all means In other words it might break down in the electromagnetic valve in the flow when absorb dust Drain tube to waste bottle ...

Page 21: ...ransfer of solvent z INTAKE Inlet port of air 10 Insert the plug for titration cell carefully into the lid At this point apply a small amount of KF grease on slide contact area Caution When handling this chemical protect yourself with gloves and glasses If it touches your skin immediately rinse it with running water ...

Page 22: ... the Auto Solvent Change Unit as follows Installation in the negative pressure Connect the Drain tube to Cell to waste bottle Use Stopper and Long Male Union supplied to Drain tube to Waste Bottle Connect the Suction tube Bottle Cap Pump to waste bottle Connect the Suction tube Bottle Cap Pump to magnetic stirrer back side pump IN Note Please refer to a previous page for the connection of other pa...

Page 23: ...ration cell 5 Stirrer 1 Key panel Use for each setting 2 Liquid crystal display Display the measurement result or parameters 3 Desiccant tube The gas fume from titration cell is exhausted through this tube 4 Titration cell The iodine generated in electrolysis and water in sample reacts here 5 Stirrer Measuring unit for Karl Fischer titration with a magnetic stirrer 0 STOP 9 FAST ...

Page 24: ...de 9 Power switch 6 Inner burette The anode and cathode liquid reacts here for electrolysis 7 Titration cell holder This is the lid for titration cell 8 Twin platinum electrode This electrode detects the potential level of the anolyte inside the titration cell 9 Power switch This switch turns on or off the unit ...

Page 25: ... the key board for inputting letters the barcode reader for sample setting or the foot switch that can start to measure without touching the unit The control with PC and the data communication with PC are possible by connecting PC special data installation software SOFT CAP is necessary 12 STIRRER connecter to Stirrer This connects the stirrer to stir sample solution 13 Inner burette connector The...

Page 26: ...ey to move to menu screen from the main screen and to set the parameter Also key to return to the main screen from each input screen PRE TITR Key to start stop pretitration Cursor key and to change number Cursor key and to change number SAMPLE Cursor key and to move to the sample setting screen from the main screen Parameter regarding the sample such as number or size can be set on the sample sett...

Page 27: ...h and pressing ENTER or The movement of inside is operated with and confirmed with ENTER The character is changed with in order in the following tables and with to the opposite direction in the following tables Input only the number due to the position of are fixed when inputting the number ex To input C at the uninput cursor position press 3 times Moreover to input 2 at the uninput cursor positio...

Page 28: ...initial displays appear one after another as follows When the main screen displays it is the standby mode ready for titration Main screen Active method number Active method name Current sample number Measured value is displayed Drift Moisture Concentration Detected potential Guiding messages and mode of the system ...

Page 29: ... MKC 710 19 Setting Language 2 3 Set language displayed on the screen 1 Press MENU HOME 2 Press twice select 8 Setup and ENTER to confirm 3 Press 5 times select 6 Language and confirm with ENTER 4 Select language with and confirm with ENTER ...

Page 30: ...8 Setup and ENTER to confirm 3 Press 2 times select 3 Date Time and confirm with ENTER 4 Select Date Style with and confirm with ENTER Press ENTER at Date and Time set with each of and confirm with ENTER Move the cursor to Exit and with ENTER to escape from the screen The time of clock starts when Time is confirmed with ENTER ...

Page 31: ...on Here is the description on basic measurement sequence Sequence of measurement 3 1 When required Assemble the Titration cell Filling titration reagent Always Selection of the method Measure the sample Usage of titration data Use USB flash drive ...

Page 32: ...burette the electrode desiccant tube A the port plug and syringe inlet desiccant tube electrode syringe inlet port plug inner burette 2 Place the titration cell onto the titration holder and plug in the cable from the inner burette and the electrode Tighten the plug screws firmly Note Make sure to apply KF grease around glass sliding area ...

Page 33: ...nt life value set 0 Enter Drain 3 To drain out the liquid use the supplied washing bottle for draining Note When one component cell is used for inner burette catholyte is not needed injection 1 Inject 5mL catholyte into the inner burette using a syringe The lower line outside the cell shows approx 5mL 2 After changing catholyte to change the life value of catholyte to zero ...

Page 34: ...TER key Drain 1 To drain out the liquid use the supplied washing bottle for drainingct When do not use the Auto Solvent Change Unit injection 1 With Funnel pour a solvent into the titration cell 100mL it becomes 100mL when match it with the line Lower the titration cell 2 After changing anolyte change the life value of anolyte to zero ...

Page 35: ...Press MENU HOME key Select 1 Manual Operation and press ENTER key Select Pump Press Injection Pump On key to inject approx 100mL of anolyte into the titration cell The lower line of the titration cell is a 100mL mark Off On key automatically changes to On Off at this time Press Injection Pump again and injection will stop 2 After changing anolyte set the life value of anolyte to 0 ...

Page 36: ...to avoid clogging of drain tube Such waste liquids if spilled after measurement may corrode the tube connectors causing the Auto Solvent Change Unit malfunction Note Change the connecting of the Auto Solvent Change Unit for those samples which are oily in order to avoid damage of drain tube Drain 1 Press Drain Pump On key to drain waste liquid ...

Page 37: ...tly used Press PRE TITR key to start pretitration The display will show the message of pretitration going on 2 After pretitration is finished it will shift to Standby mode 3 Press START STOP key The message Inject sample on display 4 Weigh the syringe with sample in it and record the weight Wt1 5 Press SAMPLE key and enter the weight of 4 in Wt1 Sample name and sample ID can be entered in the same...

Page 38: ...eigh the syringe after sample is injected and record the weight Wt2 Press START STOP again when the measurement is discontinued on the way 8 When titration is finished by reaching an endpoint the results will be shown on the screen A setup of font size is Please refer to 6 9 Other ...

Page 39: ...HOME select 2 Data File with and press ENTER 2 Select the result with and press ENTER 3 Select Re Calculation and confirm with ENTER 4 Change the sample size unit print format with and move the cursor to Execute and press ENTER to re calculate ex Change the sample size Note Move the cursor to Exit and press ENTER if the change is not executed ...

Page 40: ...ion 30 5 Select Size with and press ENTER Change the sample size with and press ENTER 6 Move the cursor to Execute with and press ENTER to re calculate Move the cursor to Exit and with ENTER to escape from the screen ...

Page 41: ...ion RSD 1 Press MENU HOME select 2 Data File with and press ENTER 2 Move the cursor to Statistics with and press ENTER 3 Sort out the data for batch calculation Select High Sample No Method No and Date with and move the cursor to Execute and press ENTER to batch ex Sort out Method No and Date 4 Select Method No with and press ENTER Change On with and press ENTER 5 Set Method No with and press ENTE...

Page 42: ... of date with and press ENTER 8 Press ENTER to batch at Execute and the result is displayed Move the cursor to Exit and with ENTER to escape from the screen The result can be excluded from the batch calculation by pressing on the result list is displayed ahead of the exclude result ...

Page 43: ...ata in USB and can be used on PC 1 Press MENU HOME select 4 Data Copy with and press ENTER 2 Select 1 Result Data and press ENTER 3 Select the stored format which is CSV or PDF with and confirm with ENTER 4 Insert USB to the USB connecter 5 Move the cursor to Execute with and press ENTER ...

Page 44: ...Select this when saving a file in PDF format or when using data with Tview6 Use this format when sending measurement results to KEM or your nearest distributor x CSV Saved in CSV file Select this if you wish to perform your own analysis or to make a report with a commonly used application software product such as Microsoft Excel Microsoft Access Microsoft Word etc The same results as printout are ...

Page 45: ... are locked Follow the steps in 4 1 and unlock method first Select how you wish to save method conditions Item Description 1 Select Data Copies each method individually Select a method No of either MKC 710 or the USB flash drive and select the method No of MKC 710 or the USB flash drive to which you wish to copy Then execute copying 2 All Data Copies all data at a time Select MKC 710 USB or USB MK...

Page 46: ...an store standard methods No 01 through 20 Each method can be named individually A Method consists of Titration parameter Calculation parameter and Report parameter To edit a method press MENU HOME on the Main screen to display 3 Method and put the cursor on the method to be edited followed by pressing ENTER key Each parameter can be selected with corresponding Key on display Note For details of e...

Page 47: ...Method and press ENTER 3 Select Lock with and press ENTER 4 Enter your password in Password with m o and press ENTER 5 Move the cursor to Lock and press ENTER 6 Select Yes with and press ENTER 7 An icon of key will appear next to Method List and method contents are now protected ...

Page 48: ...ck with and press ENTER 4 Enter your password in Password with m o and press ENTER 5 Move the cursor to Unlock and press ENTER Method is now unlocked Note Once method is locked 2 Method Data on Menu 4 Data copy may not be used Once method is unlocked 2 Method Data on Menu 4 Data copy may be used ...

Page 49: ...10 Titration Mode Mode Titration mode is selective as follows H2O This mode is selected for measurement of water content for regular moisture titration Br2 This is for measurement of bromine number Cell type Selection of titration cell type 2 comp This cell is generally used for titration with anode cathode reagent using an electrolytic electrode with diaphragm 1 comp This cell is generally used f...

Page 50: ... for a measurement from start to end in case a plural number of inflection points exist or unexpected endpoint is detected due to fluctuating drift level 15 99999s t max Limit a time length for a titration electrolysis This means the total time length from start to end is t stir t wait t max The printing covers the measuring process t max 0 means titration will not terminate by time limit This is ...

Page 51: ...rift at time of start Relative drift This mode is typical for regular direct titration method x Abs Regardless of drift level at start end point is determined when the drift level during titration goes down below Absolute drift level In this mode titration will not end if the drift level at the end of titration goes up To prevent this select a t max to end the titration Rel Here you enter a relati...

Page 52: ...ndard Use this mode for regular type of measurement Fast Use this mode for a sample with water more than 5000ug H2O Note Measurement results may be deviated with Fast mode more than Standard Check on the expected precision with the sample you are going to measure Stable To display Stable status you need to enter the drift change rate down lower than preset level Select a larger amount for the rate...

Page 53: ...es with a small amount of water Auto Titration starts automatically by sensing water increase in the sample after discharged into the cell Data sampling time Select a time interval for data sampling Titration volume and accumulated amount will be automatically sampled at the interval of an input time 1 99999s ...

Page 54: ... measurement Blank Set up a Method for blank measurement Check Set up a Method for check measurement with standard substance Calculation No Here you select the numbered equation Choose Eq 1 for water content and Eq 2 for concentration For titration mode of H2O 1 6 For titration mode of Br2 7 8 Note For calculation units and numbers refer to 4 4 Calculation formula ...

Page 55: ...ion by individual sample weight at each time This setting is for Calc No 2 3 6 only and not available for Calc No 1 4 5 The weight is entered by Sample key Drift Comp Selection of drift compensation Off No compensation is made Select this to know total water content including drift Manual Enter offset value This is useful when there is much difference in drift level between start and the end of ti...

Page 56: ...alue Enter a standard value to make the evaluation in the following range 0 0000 99999 9999 Permit Error Enter permit error to determine if the calculation result is off the range against the standard value 0 0000 99999 9999 ...

Page 57: ... the volume of gas sample is measured k 273 Temp 1 18 V2 22 4 Moisture FA u u u u u Unit k 0 0001 ppm mg kg μg g k 1 6 Concentration of a weighed part of water in solid dissolved with solvent extraction Sample is not soluble ｋ u u u u X FA Wt0 B A 10 X Wt0 B Wt2 Wt1 Moisture X 6 Determine X from this equation Unit k 0 0001 ppm mg kg μg g k 1 7 Concentration when liquid or solid is weighed in bromi...

Page 58: ...ted from titrated water volume Wt1 g The total weight of sample and sampler before sample is discharged The sample actually discharged is Wt1 Wt2 Wt2 g The total weight of sampler and sample residue after sample is discharged The sample actually discharged is Wt1 Wt2 Wt0 g The amount of sample discharged into extracting solvent a part of which is taken out for measurement B g Weight of solvent ext...

Page 59: ...n of print out of the data list x Off No printout of data list x On Printout of data list Graph Selection of graphic print together with measurement results when they are printed out x Off No printout of graph x Form1 The accumulated titrated water is printed in graphic form The axis of accumulated amount is shown in percent and the evaporation rate against 100 water at EP is shown on display or p...

Page 60: ...LP Model Serial No Off On On Printed date On Method name On Sample No On LOT No On Titration date On Calculation No Off Drift compensation Off Moisture Off Result On Reagent life Off Titration time On Blank Off Sample size On Sample constant Off Operator On ...

Page 61: ... reset halfway or sample size is input after titration Operator when re calculated its person s name appears hereModel Model MKC 710 Serial No 10100001 Print 2014 01 01 00 00 Recalculation Method No Name 01 METHOD 01 Sample No 01 02 LOT No ABCDEFGHIJ Date 2014 01 01 00 00 Calc No 1 Drift 0 05 ug s Moisture 109 4 ug Result 122 36 ug A Capa 1 mg C Capa 1 mg Titr time 00 01 00 Blank 0 0000 ug Wt1 5 0...

Page 62: ...sing system Select this when injecting reagents or draining 2 Data File Shows and prints out titration results Also conducts recalculation and statistic calculation 3 Method Edits methods to be used in titration 4 Data Copy Saves measurement results in a USB flash drive Also transfers data to edit methods on PC 5 History Reviews check records or calibration records 6 Sample Sets up sample related ...

Page 63: ...ulate the result The results of recalculation are printed out with sample number Sample No headed with mark Note Up to 100 samples measurement results can be stored As for After Titr result 2 results are stored When it exceeds 100 note that data will be erased on the first in first out basis Re Calculation Move the cursor to Re Calculation and press ENTER to recalculate Sample size and unit of the...

Page 64: ...umber of Method particular to it x Titration Date The date of measurement when it was performed Execute The selected data under the conditions as above will appear as a list of results on display And the result can be excluded from a statistic calculation by pressing on a result display screen is displayed on the excluded result before displaying a result Statistics Press Statistics on Results lis...

Page 65: ...rint You can choose from Yes or No to print the statistical data x Off No printout x On Print the results list Note If the mean value is zero 0 RSD will appear on display and be printed out as symbols not as zero 0 In addition when the number of digits of statistical calculation results is greater all digits may not be displayed Refer to 3 6 Batch processing of titration data in the operation manu...

Page 66: ...od for check measurement 2 Reagent The exchange history of an anolyte and a catholyte is displayed Note Up to 10 data can be saved When exceeding data will be deleted from the oldest 5 1 6 Sample Sets up sample related parameters Select SAMPLE on main screen Or press MENU HOME select 6 Sample with and press ENTER Sample No Here you select sample number The sample number consists of a high order an...

Page 67: ...ecting the sample in Wt2 If a balance is connected you can follow its instructions Absolute values are entered with a balance connected x 0 9999 9999g FA Factor value that is coefficient related to the results x 0 99999 9999 Sample setting after titration has started If you press SAMPLE key during titration the following display will appear and you can enter sample setting Enter items you wish to ...

Page 68: ...last date when reagent was replaced are displayed If you have replaced reagents enter 0mg and press ENTER key Alarm Set Alarm by consumption of reagent can be set If you turn it on you can set up the life upper limit and the reagent replacement interval Name A reagent name can be set Up to ten 10 letters can be input Lot A lot No can be set Up to ten 10 letters can be input ...

Page 69: ...containing bromine ion 2Br Br2 2e 2 When generated bromine is consumed according to Eq 1 the electrode detects bromine consumption and continues generating bromine according to Eq 2 Such bromine is generated in proportion to the electricity determined by Faraday s Law From Eq 1 Bromine reacts with coupled C C evenly 1 1 Thus one mol of bromine 159 8g is equivalent to 2 u 96500 coulomb which means ...

Page 70: ...elow formula 1000 g e cyclohexen g toluene 100 mass molecular e cyclohexen 82 15 g e cyclohexen mass molecular bromine 159 83 100g Br mg value l Theoretica 2 u u u Prepare reagent Refer to the below chart for sample size Bromine index mg 100g Sample size g Below 10 10 15 10 50 5 10 50 100 3 5 100 200 1 3 More than 200 1 For bromine number a sample is diluted with toluene to Bromine number 0 2 g 10...

Page 71: ...dilution coefficient D Press MENU HOME to Main display 3 Press Start key and discharge the sample into the cell Again press Start key for titration to start 4 After titration is over the measurement results appear on display with printout when a printer is connected Note When discharged samples exceed 100mL in total change the anolyte Changing the anolyte may be required each time for those sample...

Page 72: ...alance Select the maker s name of your balance Select NONE if no balance is connected For details data format refer to the Table5 3 x NONE x KEM x Mettler x A D x Shimadzu x Sartorius x Mettler Old Note Make sure to contact your local dealer to see if any particular connecting cable may be required Table 5 3 Balance setting Balance KEM Mettler Mettler Old A D Shimadzu Sartorius Baud Rate 2400 9600...

Page 73: ... from the titrator x Print Press Print key of the balance to enter the weight from the balance Inputting sample size 1 Select Sample on main screen Sample screen will appear 2 Move the cursor to Wt1 and press Enter 3 Tare the balance and then place the sample Once the balance becomes stable press Enter to fix the sample size When Continuous is selected on output mode of the balance After tarring t...

Page 74: ...f Keys Key on MKC 710 Keyboard START STOP F5 MENU HOME Esc SAMPLE STIRRER ENTER Enter USB Printer The Thermal Printer DP 600 can be connected to print out parameters and measurement results USB Barcode Scanner A barcode scanner can be connected to import a sample ID If you use a barcode scanner on main screen a sample ID can be imported into the sample ID on current sample conditions USB Foot Swit...

Page 75: ...ty does not cover malfunction or breakdown of Android devices regardless of the cause Operation check was performed per ADK Protocol Ver 1 0 stipu lated in the Android specifications Some Android devices however may not be connected 5 5 1 Connecting to instrument 1 Connect an Android device and the MKC 710 with a USB cable 2 Some messages will appear on the display and press View 3 When you access...

Page 76: ...app management 5 5 2 Starting app 1 Connect an Android device and the MKC 710 with a USB cable 2 A confirmation message will appear when you start the TitrationViewer Press OK 3 If you wish to start the TitrationViewer every time you connect the Android device to the MKC 710 check Use by default for this USB accessory 4 The TitrationViewer will start This app cannot be started from the app list or...

Page 77: ...Press Titration start 3 Titration will start During titration a titration curve will appear on the display If you press Titration start or Reset or if titration starts display of titration results will be cleared 4 If pre titration is started a display will come pre titrating 5 After pre titration is completed a display will be the wait stable drift or drift stable state ...

Page 78: ...will be in the wait stable drift and a Drift stable an upside green button will change to Titration start Press Titration start 7 A message becomes Inject sample by setup of equipment Inject the sample into the cell and press Titration start 8 Titration will start ...

Page 79: ...send it 11 Press Entry completion button to complete after entry 12 Entering weight and pressing Entry completion button before sending the weight will show the right dialog box When sending entered weight to complete after entry Check sent weight box and press Send button When completing after entry without sending entered weight Press Don t send button When re entering weight Press Cancel button...

Page 80: ... starts display of titration results will be cleared 5 5 6 Entering weight 1 If you touch the edit box on the top of the display soft keys will appear Enter the weight 2 If the weight remains unsent transmission button will turn light blue 3 Once you have entered the weight press Wt1or Wt2 button to send the weight 4 Once the weight has been sent the transmission button will turn gray ...

Page 81: ... 5 5 7 Uninstall Android apps 1 Apps or Application manager this may differ depending on your device 2 Touch the app you d like to uninstall TitrationViewer 3 Select Uninstall The messages will appear on the display and press OK ...

Page 82: ...Serial No The connected device burette the version number of the auto sampler and software version number can be checked 5 LCD Contrast The contrast for LCD can be adjusted 6 Language Languages can be set 7 Beep Beep tone for alarm can be selected on this display 8 Parameter Clear It is necessary to initialize preset parameters and setting in order to reset the system to default value In this inst...

Page 83: ...ud Rate Select baud rate x 300 bps 600 bps 1200 bps 2400 bps 4800 bps 9600 bps Parity Select parity x NONE EVEN ODD Stop Bits Select stop bits x 1bit 2bits Data Bits Select data bits x 7bits 8bits Note When you want to transfer the output data to a personal computer you need to purchase our optional Data Acquisition Software SOFT CAP But you have to check the version of the Data Acquisition Softwa...

Page 84: ...iving date The SOFT CAP software can export the measurement results as follows 1 It transfers the data to Microsoft Excel workbook 2 It stores the data in CSV format so that spreadsheet can be used Sending date The personal computer can send commands including titration start and reset Note For details see the operation manual for Data Acquisition Software SOFT CAP 6 1 3 Printer setting IDP 100 Co...

Page 85: ...igurations for your printer refer to the operation manual for the printer Baud Rate If you use other printer as defined on Printer you have to select baud rate for your printer x 300 bps 600 bps 1200 bps 2400 bps 4800 bps 9600 bps Parity If you use Other printer as defined on Printer you have to select parity for your printer x NONE EVEN ODD Stop Bits If you use Other printer as defined on Printer...

Page 86: ... cursor to Print on wherever Print is shown Press ENTER to start printing 6 1 4 Balance setting For details on balance setting refer to 5 3 Balance setting 6 1 5 USB setting Select 4 USB with and press ENTER Mode Select USB mode Normally select Host Once setup is completed restart the titrator x Host Select this when connecting USB devices x MCU Select this when connecting MCU and the KF Win throu...

Page 87: ...haracters alphanumeric capital letters Select 2 Operator with and press ENTER Current No Select the number of the operator you wish to put on the measurement data Select with keys and press ENTER To enter an operator Move the cursor with keys to the number 01 to 10 you wish to enter Press ENTER Then enter a name with keys and press ENTER again Up to twenty 20 letters can be input ...

Page 88: ...MM DD Christian year month in number day of the month x MM DD YYYY month in number day of the month Christian year x DD MM YYYY day of the month month in number Christian year Date Input the present date 2001 1 1 2099 12 31 Input with keys and press ENTER Time Input the present time 00 00 23 59 Input with keys and press ENTER Note See 2 4 Setting date and time of this Operation Manual for how to s...

Page 89: ...ware version will also be shown Note Make sure to advise your distributor of the serial No and the software version should you require servicing Running Time Multiplication of the operation time for measuring equipment is displayed LCD Contrast 6 5 The contrast for LCD can be adjusted Select 5 LCD Contrast with and press ENTER LCD Contrast Adjust contrast of LCD with 14 steps by m o key and confir...

Page 90: ...e the cursor with keys to the language you wish to use and press ENTER x English Shows in English x Japanese Shows in Japanese x Mandarin Shows in Mandarin Chinese x Korean Shows in Korean x Russian Shows in Russian x Spanish Shows in Spanish Note See 2 3 Setting Language of this Operation Manual for how to set ...

Page 91: ...Type Select the beep from the five 5 types below Move the cursor with keys to the type you wish to use and press ENTER x Type1 Beep sound lasts for about two seconds pi pea pea pea pea x Type 2 Beep sound lasts for about four seconds pi pi pi pi pi pi x Type 3 Beep sound lasts for about ten seconds pi pea pea pea pea x Type 4 Beep sound lasts for about one second pi pi pi pi pi pi x Type 5 Beep so...

Page 92: ...n below Items Contents 1 Method Parameter Initialize Parameters Titration Control Result of each Method 2 Measure Data Erase all measurement results data stored in Data File 3 History Erase all the calibration records and the check records in History 4 All Parameter Initialize all of the above items once for all When initialization is chosen the confirming message appears Select Yes No by n p key ...

Page 93: ...On Header is printed Print Footer Make setting of footer printing The footer includes a printing operator Select with keys and press ENTER x Off No footer is printed x On Footer is printed Auto Set mean The average value of a plural number of blank levels that have been measured will be automatically set into the blank value to be used in sample setup to be used in reagent information respectively...

Page 94: ...y If not apply thin coating of grease Do not apply too much grease as it may penetrate the titration cell and increase the background owing to the water content of the grease Caution Check the glass joints from time to time so that applied grease will not solidifies If grease on the glass contact areas becomes hard and the respective parts are difficult to separate take the following steps 1 Disch...

Page 95: ... An old septum is easily broken and allows air into titration cell to increase the background Septum 7 1 3 Changing the desiccant The desiccant tube is removed from a titration cell like the clause of an application of KF grease And the desiccant tube is removed from a bottle holder Replace the desiccant with new one when its moisture absorption turns down to reddish color Be sure to apply KF grea...

Page 96: ...city see Instruction of the reagent you have purchased Please refer to 3 3 2 Anolyte 7 1 5 Replacement of the catholyte cathode reagent Exchange timing x When the accumulated moisture measurement reagent life has reached 300mgH2O after the last replacement with new one x When drift level goes up Note Negligence of replacing cathode reagent will cause higher drift level foreign objects generated ar...

Page 97: ...not use solvent but use water only 7 1 7 Check the cable Make sure by visual check all the cables including power cord various cables and electrode lead to see if any dent or bent is found Replace the cable if it is dent or bent 7 1 8 Check the connectors Make sure the connectors are not dusty or rusted If dusty clean it by a vacuum cleaner If rusted repair is necessary ...

Page 98: ...tuates cleanse it with nitric acid and after cleaning by methanol wipe off with clean gauze Inner burette Periodical cleaning of inner burette is recommended since if the inner burette is stained the electrolysis reaction will not run smoothly and may cause a longer time length in measuring process with measurement results higher than theoretical value Cleaning with alcohol general method 1 Turn o...

Page 99: ...sses If it touches your skin immediately rinse it with running water Caution Be careful not to burn yourself when using a hot stirrer Cleaning with chromic acid mixture When a dirt does not come off If foreign objects are observed on diaphragm and platinum surface use chromic acid mixture instead of methanol for cleaning Chromic acid mixture 1 5g approx potassium dichromate dissolved in 100mL of c...

Page 100: ...sold drying under reduced pressure Diagram of Decompression dryer Commercially available vacuum dryer 燥器 3 way vent cock Vacuum pump Oil trap Desiccator Inner burette Note Dry the inner burette itself only after removed from the titration cell in order to avoid possible breakage of inside ceramic diaphragm Use a hair dryer if a compression dryer is not available With a hair dryer dry the inner bur...

Page 101: ...rgent under running water 4 After drying the glassware in a heater either cool them in desiccator or dry them Note Insufficiently dried glassware may cause higher drift level 7 2 4 Distance adjustment between anode electrode and diaphragm If the anode electrode in the inner burette and the diaphragm are too close together electrolysis reaction will not run in normal condition Use the supplied anod...

Page 102: ...est which may be reduced when the tube is used for a long time This may result in leakage of samples at the time of measurement Follow the instructions below 1 Remove the tubes connected to cassette 2 Remove the pump tube cap as shown on the right 3 Remove the pump tube as shown on the right Nut Cap Tube ...

Page 103: ...sed samples you can use the 64 01473 pump tube option And you can use the 12 03961 01 extraordinary chemical resistance pump tube option 7 2 6 Replacement of the filter Place the filter for injection pump as a dustproof to the back of auto dispensing part Since the filter might be dirty when the flow of injection pump becomes lower change the filter Note With no filter dust may go into the tubing ...

Page 104: ...ide battery needs to be replaced with new one Ask your local dealer for its replacement Open the battery cover on the bottom of the main unit with a slotted screwdriver Replace the old battery with a new one CR2032 Caution Follow your national regional and local regulations for disposal of batteries ...

Page 105: ...rode Over Titr Over titration is underway Reagent with too much iodine is cell Add water to the cell The titration cell is under direct sunlight Refrain from direct sun s ray or use a brown cell The anode is stained with foreign objects Clean the inner burette and the electrode Meas Over When measurement exceeds the range Change the catholyte Also change the anolyte if necessary One time measureme...

Page 106: ... preset level A replace Day Because the date for changing the anolyte becomes due today Change the reagent and clear the due date setting C replace Day Because the date for changing the catholyte becomes due today A Replace now Because the date for changing the anolyte is past C Replace now Because the date for changing the catholyte is past A replace in xx days Because the preset due date to chan...

Page 107: ...rly 8 2 START Stir cable connected Stir motor running Repair by manufacturer END Connect stir cable Contact your dealer NO NO YES YES Stir rotor spinning Change with correct rotor 35mm NO YES Something in cell Remove foreign objects and clean the cell NO YES ...

Page 108: ...Change with new one NO NO YES Is reagent correct YES Use correct reagent NO YES Is reagent new Change with new one NO YES Is inner burette dry Dry the burette NO Is anode in contact with diaphragm Use anode adjuster to detach from each other 1 5 2 0mm NO YES YES Inner burette or Electrode good Change it if malfunctioning NO YES ...

Page 109: ...nufacturer END Keep away from sunlight Change with new one NO NO YES YES YES Is reagent correct Use correct reagent NO YES YES Is electrode working alright Clean the electrode NO Change with correct rotor 35mm Make stirrer speed increase Is the length of stirrer rotor normal Is stirrer speed appropriate YES NO NO ...

Page 110: ...er to the attached chart on sampling NO NO YES YES Start with stable drift Wait for stable drift NO YES Is drift 0 1ug s Wait until drift settle down NO YES Inner burette or Electrode good Is reagent correct Use correct reagent NO Side reaction YES YES Change reagent or use indirect method NO Rinse and clean them NO Measurement parameters correct Check on drift stop mode NO YES YES ...

Page 111: ...nd the respective parts are difficult to separate take the following steps 1 Discharge anolyte and catholyte 2 When using a glass port plug warm it up with a hair dryer or something similar to soften KF grease before removing When using a PTFE port plug remove it after cooling the titration flask in a freezer for about five 5 minutes Warning Do not try and open solidified jointed parts by force Gl...

Page 112: ...ease remove the clogging by the following steps when the drainage volume is lowered 1 Remove the tube 2 Insert the dropping pipette to the tip of the pump tubing or tube remove the clogging Caution When removing the tube please attach the eye protection and gloves Please be careful because there is a possibility that the drainage jump out Remove ...

Page 113: ...n obtain any of these parts at your dealer or from sales representative Parts AC Adapter Type4 64 00898 Plug Adapter AC3P 2P 12 02170 Cell Holder for Coulometric 20 09176 Pipette 10mL 66 00071 Funnel 66 00141 Washing Bottle 12 04251 Stirrer Cable 0 6m 64 01386 Anode Adjuster 20 06380 01 MKC 710 Operation Manual CD RO M 12 05186 Power Code 64 01107 ...

Page 114: ... Inlet with Septum 12 00661 11 Septum 10pcs set 12 01394 10 Stirrer Rotor 35mm 5pcs set 12 00661 12 KF Grease 5g 12 04232 KF Grease 50g 12 04232 01 Inner Burette 12 05195 2Component 12 05194 1Component Desiccant Tube φ18x120 with Silica Gel 12 01260 Silica Gel 500g 61 00249 Titration Cell Transparency 20 04042 00 ...

Page 115: ...lug 12 03926 Reagent Bottle Cap for Injection 12 03926 01 Tube 4x8 L 1m Silicone 20 09874 01 Rubber Globe for Suction 12 04875 Plug for Titration Flask 20 02559 00 Polyethylene Bottle 1L 69 00028 00 Rubber Globe for Drain 12 04875 01 Injection Tube 2 3 L 1180mm PFA 12 02020 11 1180 O ring P7 NBR 63 00131 05 Desiccant Tube No 1 L 160 12 01250 10 Silica Gel 500g 61 00249 ...

Page 116: ...ottle Cap12 02021 10 Tube 4x8 L 1m Silicone 20 09874 01 Plug for Titration Flask 20 02559 00 Desiccant Tube φ18 120 12 01260 10 Injection Tube 2 3 L 1180mm PFA 12 02020 11 1180 Desiccant Tube No 1 L 160 12 01250 10 Silica Gel 500g 61 00249 Drain Tube to Waste Bottle 2 3 L 1m PFA 12 04539 Pump Tube WPX1 P 3 2 3 with Grease 64 01473 01 Filter 10pcs set 12 05069 Suction Tube Bottle Cap Pump 12 06270 ...

Page 117: ...EM Contact your local dealer or sales representative MKC 710 Print out of measurement results Dot Matrix Printer IDP 100 Thermal Printer DP 600 Measure the moisture in the sample by Evaporator Evaporator Control from your PC データ収集ソフトウェア Title SOFT CAP KYOTO ELECTRON I CS SOFT CAP Date Acquisition Software Date capture into your PC ...

Page 118: ...ubber 5pcs set 12 04577 02 Syringe 2mL with Needle 12 04577 01 Syringe 20mL with Needle Printer Part code Part name Remarks Sketch 12 02028 01 12 02028 02 Dot Matrix Printer AC120V AC230V 12 02618 01 12 02618 02 12 02618 03 12 02618 04 Thermal Printer EU KR GB US TW CN ピンセット微量試料投入器カップ蓋５個カップ３０個 Consumables ...

Page 119: ...ell Unit with Cock Transparent cell with a drain cock Two component cell Twin platinum electrode KF and other attachment 12 00662 01 1Component Type Titration Cell Unit Transparent cell with a drain cock One component cell Twin platinum electrode KF and other attachment 12 00662 10 1Component Type Titration Cell Unit with Funnel Transparent cell One component cell Twin platinum electrode KF and ot...

Page 120: ...marks Sketch 12 03265 Data Acquisition Software Pump Tube Part code Part name Remarks Sketch 64 01473 Pump Tube WPX1 F 3 2 3 with Grease Fluorine tube 12 03961 01 Pump Tube ePTFE FKM WP1000 C3 2 4 K φ3with Grease Extraordinary chemical resistance ...

Page 121: ...s MKC 710 111 Evaporator Part code Part name Remarks Sketch ADP 611 Evaporator ADP 512 Evaporator for ores Non CE ADP 512S Evaporator for high temperature Non CE ADP 513 Evaporator for high temperature Non CE ...

Page 122: ...conditions Parameters Japanese English Mandarin Chinese Korean Russian Spanish Calculation Concentration Statistics mean SD RSD Auto input of blank Data memory 100 samples GLP support Registration of operator Record of calibration results Record of date for changing reagent External I O RS 232C 2 for dot matrix printer electronic balance Data Acquisition Software SOFT CAP USB 1 for USB flash drive...

Page 123: ...ording to 1 As soon as all the water reacts excess of iodine appears in the anolyte This iodine is detected by the platinum electrode and the iodine production is stopped According to Faraday s law the quantity of iodine produced is proportional to the current generated In equation 1 I2 and H2O react with each other in proportion 1 1 Therefore a mole of water 18 g is equivalent to 2 u 96500 coulom...

Page 124: ...vent Remarks General titration Alcohols Hydrocarbons Ethers Esters Gases Fats and Oils Amines Anolyte KEMAQUA Anolyte AGE KEMAQUA AGE CGE are non organic chlorines Amines To use KEMAQUA AGE add 10g salicylate acid to 100mL KEMAQUA AGE Catholyte KEMAQUA Catholyte CGE Fats and Oils Alcohols Hydrocarbons Ethers Esters Gases Anolyte KEMAQUA Anolyte AO Catholyte KEMAQUA Catholyte CGE Ketones Anolyte KE...

Page 125: ...lomat AG Catholyte Coulomat CG Ketones Anolyte Coulomat AK Formaldehyde can only be titrated among other aldehydes Coulomat CG K are non organic chlorines Catholyte Coulomat CG K Gases Anolyte Coulomat AG Oven Catholyte Coulomat CG Fats and Oils Anolyte Coulomat AG H Coulomat AG H CG are non organic chlorines Catholyte Coulomat CG General titration Alcohols Hydrocarbons Ethers Esters Amines Gases ...

Page 126: ...AX CXU are non organic chlorines Amines To use Aquamicron AX add 10g salicylate acid to 100mL Aquamicron AX Catholyte Aquamicron CXU Fats and Oils Alcohols Hydrocarbons Ethers Esters Gases Anolyte Aquamicron AS Catholyte Aquamicron CXU Ketones Anolyte Aquamicron AKX Formaldehyde can only be titrated among other aldehydes Aquamicron CXU are non organic chlorines Catholyte Aquamicron CXU ...

Page 127: ...ts As displayed Printer NONE NONE OTHER DP USB IDP Printer As displayed Balance NONE NONE KEM Mettler A D Shimadzu Sartorius Mettler Old Balance As displayed Interface COM1 COM1 COM2 Interface As displayed Mode Continuous Continuous Print Mode As displayed USB Host Host MCU Mode As displayed Beep Parameter and default Item Default Selection range Beep Set Set off Type Type1 Type1 Type2 Type3 Type4...

Page 128: ...00 00 00 23 59 Language English Japanese English Mandarin Korean Russian Spanish Other setup Parameter and default Printout Item Default Selection range Item Printing Character Disp lay Large Normal Large Character Disp As displayed Print Header On Off On Print Header As displayed Print Footer On Off On Print Footer As displayed Auto set mean On Off On AutoSet Mean As displayed ...

Page 129: ...d Standard Standard Standard Standard Standard Standard Stable 0 1ug min 0 1ug min 0 1ug min 0 1ug min 0 5ug min 0 1ug min 0 1ug min Start Mode Manual Manual Auto Auto Manual Manual Manual Data Sampling Time 5s 5s 5s 5s 5s 5s 5s Caluculation Parameter Caluculation Type Sample Sample Sample Sample Sample Check Sample Caluculation No 1 2 2 2 7 2 1 Unit ug ppm ppm ppm mg 100g ppm ug Weight Input Vari...

Page 130: ...0 99 99μg s Stable 0 0 99 9ug s Start Mode Manual Auto Start As displayed Data Sampling Time 1 99999s Samp Time As displayed Caluculation Parameter Displays Printout Item Selection Item Selection Caluculation Type Sample Blank Check Calc Type As displayed Caluculation No 1 6 7 8 Calc No As displayed Unit μg mg ppm mg kg μg g 100g mg 100g Unit ug mg ppm mg kg ug g 100g mg 100g Weight Input Variable...

Page 131: ...ican Society for Testing and Materials U S A ASTM D 1533 Standard Test Method for Water in Insulating Liquids by Coulometric Karl Fischer Titration U S A ASTM D 4928 Standard Test Method for Water in Crude Oils by Coulometric Karl Fischer Titration U S A ISO 760 Determination of water Karl Fischer method General method International ...

Page 132: ... applied to glassware or plastics z malfunction or leakage is caused by sample properties corrosively solid materials etc z malfunction is caused by any device part and or chemical other than those supplied by KEM z overuse has led to fatigue or wear of parts z items are consumables or wearing parts z this product has been moved or transported to another place once accepted and installed z breakag...

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