Automatic Distillation Tester Model AD-6

Maintenance Manual Ver 3.01 100105

Read this manual thoroughly before maintenance. Store this manual in a safe place for future reference.

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Preface Thank you for purchasing the Tanaka Scientific Limited Model AD-6.

This instruction manual describes the procedures for readjustment, troubleshooting, and component

replacement for the Model AD-6.

Read and be sure that you thoroughly understand this manual in its entirety.

Intended Reader This manual is written for all users of Model AD-6.

The reader is assumed to have knowledge of JIS related standards and of the handling of hazardous

materials.

Note The contents of this manual are subject to change without notice.

For Safe Use Always follow the safety precautions presented in this manual and in the maintenance manual.

Tanaka Scientific Ltd. will take no responsibility for damage or accidents caused by failure to follow

the precautions herein.

In order to ensure the safe use of the instrument, this manual uses the following notation:

！ Warning: Failure to properly follow this procedure may result in fire or cause burns or a poisoning danger to the operator.

！ Caution: Failure to properly follow this procedure may damage the equipment or cause injury to the operator.

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C o n t e n ts

1 Periodic Inspection............................................................................................................................7 1.1 Internal Circulating Water Check................................................................................................7 1.2 Temperature Correction Value Check ........................................................................................7 1.3 Displayed Temperature Check ...................................................................................................7 1.4 Fire-Containment Shutter Operation Check ...............................................................................7

2 Adjustment ........................................................................................................................................8 2.1 Adjustment from the Menu Screen.............................................................................................8

2.1.1 Temperature Correction ......................................................................................................8 2.1.2 Correcting the Condenser Bath and Receiver Chamber Temperatures ............................12 2.1.3 Setting the Clock and the Barometric Sensor ...................................................................13 2.1.4 Meniscus Calibration and Verification ...............................................................................14 2.1.5 Setting the External Connection........................................................................................19 2.1.6 Distillation Rate Adjustment. .............................................................................................20 2.1.7 Temperature Circuit Check by Reference Resistance (Temp Check) ...............................22 2.1.8 Inspecting the Peltier Element ..........................................................................................23

2.2 Setting the Initial Heating Temperatures (1 and 2) ...................................................................24 2.3 Setting the Final Heating Voltage (8) ........................................................................................25

3 Troubleshooting...............................................................................................................................26 3.1 Trouble Display ........................................................................................................................26 3.2 Countermeasures by Error.......................................................................................................30

4 Component Replacement................................................................................................................31 4.1 Controller .................................................................................................................................31 4.2 Receiver Chamber ...................................................................................................................33 4.3 Condenser Bath .......................................................................................................................35 4.4 Heater Section .........................................................................................................................36

Appended Figure 1 Sample Print in Reference Mode

Appended Table 1 Specification for Standard Sample Composition (JIS K 2254)

Appended Table 2 Standard Recovered Temperature and allowance of Standard Sample A and B

Appended Figure 2 Front View of the Main Unit

Appended Figure 3 Component Arrangement in the Controller

Appended Figure 4 Top View of the Receiver Chamber

Appended Figure 5 Component Arrangement in the Receiver Chamber

Appended Figure 6 Component Arrangement on the Right Side of the Main Unit

Appended Figure 7 Component Arrangement on the Left Side of the Main Unit

Control Section Wiring Diagram

Mechanical Section Wiring Diagram

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1 Periodic Inspection

！ Caution: Failure to properly follow this procedure may damage the equipment or cause injury to the operator.

Inspect the instrument periodically for stable equipment performance and safety.

1.1 Internal Circulating Water Check

(1) The circulating water level can be checked through the internal circulating water viewing window on the right side of the unit. If the level is low, replenish the internal circulating water supply.

(2) Replace the internal circulation water periodically. (About once a year)

1.2 Temperature Correction Value Check

Referencing Section 2.1.1 (page 8), check that the pre-input temperature correction value is

stored correctly. (About once a month)

1.3 Displayed Temperature Check

Referencing Section 2.1.1 (page 8), check the displayed temperature semi-automatically.

(About once every six months)

1.4 Fire-Containment Shutter Operation Check

Press the manual switch of the fire-containment shutter (red button located at the upper-right

of the main unit). See Figure 1 on page 10 of the instruction manual. (About once every six

months)

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2 Adjustment

2.1 Adjustment from the Menu Screen For temperature correction, setting the clock, or other adjustments, select the appropriate item

from the Menu screen.

While holding down the FUNCTION key in the control panel, press and then release the RESET

key.

After checking that the Menu screen appears on the display unit, as shown in Figure 1, release

the FUNCTION key.

Fig.1 Menu screen

<Menu>

Dist. Temp. Corr ←Cursor Other Temp Corr Reference Data Time / Barometer Meniscus Corr Ext Out Dist Rate Adj Temp Chek

Peltier Check

Move the cursor to a setting or adjustment item using the ↑ and ↓ keys and press the ENTER

key.

The display panel will show the screen of the item indicted by the cursor position.

Press the RESET key to return from the Menu screen to the Standby screen.

2.1.1 Temperature Correction Before temperature correction, check that the temperature displayed on the tester matches the

prescribed glass thermometer temperature or the standard sample test result.

This instrument has reference mode for easy operation. (1) Operation in reference mode

By entering a temperature collation number from $1 to $6 at the beginning of a mode name, the instrument is changed to the temperature collation mode. If a test is executed with a temperature collation number of $1 to $4, differences from the readings of the prescribed glass thermometer (preset in the temperature collation data according to (3) on page 11) can be printed. Selecting temperature collation number $5 prints differences from the reference temperatures (set at shipping) of standard sample A(1). Selecting temperature collation number $6 prints differences from those of standard sample B(1). (See Appended Figure 1, "Sample Print in Reference Mode" on page 33.)

Note (1) Standard sample A and B are prescribed in JIS K 2254. fro the detail, see appended

Table 1.

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(Mode Select) (Mode Contents)

<1> The test method is identical to that of an ordinary test. For a temperature check, prepare a

sample (the distillation temperature of which was measured by either the manual method or the semi-automatic method(2) or the standard sample).

Note (2) In the semi-automatic method, a sample is distilled via a prescribed glass thermometer rather than by a temperature sensor (PT-100) and the distillation temperature is measured using an automated tester. The operation method is as follows:

• The mode selection and contents are the same as in the automatic method. • Attach a glass thermometer, rather than a temperature sensor, to the flask. • While holding down the key, press and release the RESET key. • The Standby screen changes from Standby 1 or 2 to Semi-automatic Measurement 1 or 2.

(The RUN screen displays Semi-automatic.) • After checking the above screen, execute the test in the same way as in the automatic

method. • The buzzer sounds at IBP, 5, 10, • • • 90, 95, and 97%. Read and record the distillation

temperature from the glass thermometer at each point. • After checking the end point, press the MANUAL CUT key. The test will end in five minutes. • To release the semi-automatic measurement mode, press the RESET key.

<2> Select a temperature collation number from $1 to $4 and enter the selected number at the beginning of the mode name. Set test conditions according to the temperature check sample and the distillation temperature measured by the manual method or the semi-automatic method in the temperature collation data. (See “(3) Setting temperature collation data" on page 11.) This is not necessary when using standard samples and temperature collation numbers $5 or $6 (set at shipping).

<3> After <2>, execute an ordinary automatic test on a sample from the same lot. Like the print sample shown in Appended Figure 1, differences between the distillation temperatures set in the temperature collation and the measured temperatures (after loss correction and barometric correction) are displayed. If there is a difference, correct the temperature. (See "(2) Correcting the displayed temperature.")

<Standby 2> BARO 1013 hPa 14 INIT TEMP 1 250.0 °C 15 INIT TEMP 2 450.0 °C 16 H./FREEZE 95.0 % 17 Mode name FINAL H (AUTO) +00 V 18 Cursor TEMP RANGE 300 19 RESIDUE 1.0 % 20 DIST RATE 4.5 % 21* $1 GASOLIN 300 SET BATH 1.0 °C 22 $2 KAROSIN 300 SET REC 15.0 °C 23 $3 KAROSIN 400 24 $4 GAS-OIL 400 Test Start Temp. 25.0 °C 25 $5 STD-A Bath Temp. 1.0 °C 26 $6 STD-B Receiver Temp. 15.0 °C

Fig.2 Standby Screen

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-0.5°C Added temperature

Fig.4 Mechanism of Temperature Correction

Correction point

-1.0°C

-0.5°C

(2) Correcting the displayed temperature

<1> Select "Distillation temperature correction" on the Menu screen. The following screen will

appear:

<2> Selecting a range

Position the cursor to "Range (300)" and select the range used for the temperature check. <3> Adjusting the zero point "Posi"

Enter a numeric value at "Posi" above to correct all temperature ranges including zero by parallel translation. The adjustment range is up to ±9.9°C in increments of 0.1°C.

<4> Adjusting the intermediate point To adjust a displayed temperature to the prescribed glass thermometer, values measured using the temperature sensor (platinum resistance thermometer sensor) require detailed corrections throughout the temperature range. The Model AD6 has an intermediate point at every 20°C in each range of (300), (400), (P200), and (P400) to correct and display a measured temperature at each intermediate point. For example, if the intermediate point of 80°C is added to the current correction value (-1°C), the current temperature range is expanded by 20°C above and below (60°C to 100°C), as shown in Figure 4.

For the print sample in Appended Figure 1 (standard sample A), 1.0°C is subtracted from the intermediate point of 80°C because the IBP and 5% are not within tolerance (IBP: 76°C±2°C, 5%: 88.5°C±1.5°C). The values at the points are subtracted from the IBP (-1.0), 5% (-0.5°C), 10% (-0.3°C), and 20% (-0.1°C) to obtain an IBP of (77.7°C), 5% (89.9°C), 10% (93.0°C), and 20% (97.6°C), which is within tolerance.

60°C 70°C 80°C 90°C 100°C Current temperature

Range( 300) Posi (+0.0) 0 (+0.0) 20 (+0.0) 40 (+0.0) 60 (+0.0) 80 (+0.0) 100 (+0.0) 120 (+0.0) 140 (+0.0) 160 (+0.0) 180(+0.0) 200 (+0.0) 220 (+0.0) 240 (+0.0) 260(+0.0) 280 (+0.0) 300 (+0.0) 320 (+0.0) 340(+0.0) 360 (+0.0) 380 (+0.0) 400 (+0.0) 420(+0.0) 440 (+0.0)

Fig.3 Distillation Temperature Correction

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Since the initial heating temperature and the final heating voltage affect the corrections of

IBP and EP, see the setting methods for the initial heating temperature (Section 2.2, page

17) and the final heating voltage (Section 2.3, page 18).

<5> To change a numeric value, position the cursor using the ← and → keys and increment or

decrement the value with the ↑ or ↓ key. You can also use the FUNCTION key to move the

cursor vertically.

Press the ENTER key to display the Menu screen.

(3) Setting temperature collation data

<1> Select "Temperature Collation Data" on the Menu screen. The following screen appears:

IBP $1 • • • • • $2 • • • • • $3 • • • • • $4 • • • • • 5 → • • • • • → • • • • • → • • • • • → • • • • • 10 • • • • • • • • • • • • • • • • • • • • 20 • • • • • • • • • • • • • • • • • • • • 30 • • • • • • • • • • • • • • • • • • • • 40 • • • • • • • • • • • • • • • • • • • • 50 • • • • • • • • • • • • • • • • • • • • 60 • • • • • • • • • • • • • • • • • • • • 70 • • • • • • • • • • • • • • • • • • • • 80 • • • • • • • • • • • • • • • • • • • • 90 • • • • • • • • • • • • • • • • • • • • 95 • • • • • • • • • • • • • • • • • • • • 97 • • • • • • • • • • • • • • • • • • • •

E.P • • • • • • • • • • • • • • • • • • • •

Fig.5 Temperature Collation Data Setting Screen

<2> Set a distillation temperature at the temperature collation mark ($1 to $4) that was set at the

beginning of the mode name. For "• • • • •", position the cursor to select a temperature

collation mark and press the ↑ or ↓ key to display a numeric value. If there is no data for

97%, display "• • • • •" for no printing.

To change a numeric value to "• • • • •", set "000.0" for automatic change to "• • • • •".

<3> To change a numeric value, position the cursor using the ← and → keys and increment or

decrement the value using the ↑ and ↓ keys. The FUNCTION key can also be used to

move the cursor between the temperature collation marks.

Press the ENTER key to display the Menu screen.

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2.1.2 Correcting the Condenser Bath and Receiver Chamber Temperatures

Select "Other Temperature Correction" on the Menu screen. The following screen will appear:

Rec Temp +0.0 °C ( 15.0 °C )

Bath Temp +0.0 °C ( 1.0 °C )

Fig.6 Other Temperature Correction

(1) Correcting the condenser bath temperature

To correct the condenser bath temperature, change the numeric value at <A> "Bath Temp" shown in Figure 6. When the condenser bath temperature is displayed at <B>, compare the value with the calibration thermometer(3) reading and enter the difference if any exists.

Note (3) Insert the calibration thermometer into the condensation tube of the heater to measure the temperature. To keep the bulb of the thermometer about 80 mm deep in the condensation tube (thus avoiding the effect of external temperature), the thermometer should be 80 mm or longer from the bulb to the temperature scale. Tanaka Scientific Ltd. uses a ASTM 57C thermometer (option) for this purpose.

(2) Correcting the receiver chamber temperature

To correct the receiver chamber temperature, change the numeric value at <C> "Rec Temp" shown in Figure 6. When the receiver chamber temperature is displayed at <D>, compare the value with the calibration thermometer(4) reading and enter the difference if any exists.

Note (4) Attach a wire to the top of the calibration thermometer and hook the thermometer at the center of the IBP sensor to measure the receiver chamber temperature. For correction, a 150-mm alcohol thermometer (0-50°C) is used.

(3) To change a numeric value, position the cursor using the ← and → keys and increment or

decrement the value using the ↑ and ↓ keys. You can also use the FUNCTION key to move the cursor vertically. Press the ENTER key to display the Menu screen.

<A>

<B>

<C>

<D>

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2.1.3 Setting the Clock and the Barometric Sensor (1) Select "Date/Barometer Setting" on the Menu screen. The following screen will appear:

Time --------------------------------- 02/08/08 12:00:00:00 Set Time -------------- 02/08/08 12:00:00:00 Enter Time Barometer Data – 1013 hPa Set Barameter – 1013 hPa Enter Barameter 04 <--Barometric sensor correction value Return Menu

Fig.7 Date and Time/Barometer Setting

Position the cursor to "Return Menu" and press the ENTER key to return to the Menu screen.

(2) Setting the clock Set the current date and time (hh:mm:ss) at "Set Time" using the ←, →, ↑, and ↓ keys. Position the cursor to "Enter Time" and press the ENTER key at the set time. The Set Time data is ported to "Time" and the time incrementation begins.

(3) Setting the barometric sensor

Set the current barometric pressure at "Set Barometer." Position the cursor to "Enter Barometer" and press the ENTER key. The Set Barometer data is ported to "Barometer Data."

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2.1.4 Meniscus Calibration and Verification 2.1.4.1. Meniscus Calibration

Pour kerosene to 100ml filling mark of Tanaka cylinder. Do not measure exactly 100ml by calibrated pipette or another cylinder. The height of 100ml filling mark is used for meniscus calibration.

(1) Select "Meniscus Correction" on the Menu screen. The following screen will appear.

Fig.8 Correction/Verification Selection

(2) Select “Ms_Correction” and then push ENTER key. The following screen will appear.

Fig.9 Photo Adjustment

<PHOTO ADJUSTMENT>

IBP OUT 80 IN 3800 MS OUT 80 IN 3800

Set Receiver(With 100% Sample) Ms_Correction Ms_Verification Push Enter Key

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After photo adjustment is done, the following screen will appear.

Fig.10 Correction Ready

(3) Fill a sample (kerosene preferable) in a Tanaka 100ml Cylinder (= receiver) to filling mark, set

the receiver in the receiver chamber, and press the START key. The follower sensor begins

to descend, starts correction, and sets the distillation correction value automatically. Do not

measure 100ml sample with pipette or another cylinder.

The following screen appears and the buzzer sounds when measurement is complete.

Fig.11 Correction Complete

Press the ENTER key to return to the Menu screen.

Note: If the difference between the sample and the receiver chamber temperatures is great, the sample capacity changes. Be sure to match the temperatures.

Note: Be careful not to jar the instrument during meniscus correction. If the liquid surface in the receiver is not stable, an error may occur.

Set Receiver (with 100% Sample)

Finish Push Enter Key

MS Bias 162

Set Receiver (with 100% Sample)

Push Start Key

MS Bias 158

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2.1.4.2 Meniscus Verification Verification of follower sensor can be done using Tanaka 100ml Cylinder. Calibration must be done before verification.

(1) Select "Meniscus Correction" on the Menu screen. The following screen will appear.

Fig.12 Correction/Verification Selection

(2) Select “Ms_Verification” by ↓ key and then push ENTER key. The following screen will appear.

Fig.13 Photo Adjustment

<PHOTO ADJUSTMENT>

IBP OUT 80 IN 3800 MS OUT 80 IN 3800

Set Receiver(With 100% Sample) Ms_Correction Ms_Verification Push Enter Key

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After photo adjustment is done, the following screen will appear.

Fig.14 100ml Verification Ready

(4) Fill a sample (kerosene preferable) in a Tanaka 100ml Cylinder (= receiver) to filling mark, set

the receiver in the receiver chamber, and push the START key.

Fig.15 100ml Verification in progress

The follower sensor descends until lower end and then go up to meniscus position and

shows detected volume in ( ) column next to 100ml. Do not measure 100ml sample with

pipette or another cylinder.

The following screen appears and the buzzer sounds when measurement is complete.

Fig.16 100ml Verificatn Complete

Ms_Verification

Set Receiver (With 100ml Sample)

Push Start Key

100ml Volume ( 0 .0ml ) 5ml Volume ( 0 .0ml )

Ms_Verification

Set Receiver (With 5ml Sample)

Push Start Key

100ml Volume ( 100.1ml ) 5ml Volume ( 0 .0ml )

Ms_Verification

100ml Sample Verification

100ml Volume ( 0 .0ml ) 5ml Volume ( 0 .0ml )

Ms_Verification

Set Receiver (with 100ml Sample) Push Start Key

100ml Volume ( 0 .0ml ) 5ml Volume ( 0 .0ml )

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(5) Measure 5ml of sample (kerosene preferable) by pipette and then transfer to a Tanaka 100ml

Cylinder, set the receiver in the receiver chamber, and push the START key.

Fig. 17 5ml Verification in progress The follower sensor descends until lower end and then go up to meniscus position, and

shows detected volume in ( ) column next to 5ml Volume.

Fig. 18 5ml Verification Complete

(6) This is the end of verification. Push ENTER key to return MENU screen or push RESET to

return STAND-BY screen. If detected volume is out of 0.3ml range, contact local dealer or

Tanaka Scientific Limited.

Ms_Verification

5ml Sample Verification

100ml Volume ( 100 .1ml ) 5ml Volume ( 0 .0ml )

Ms_Verification

Finish Push ENTER Key

100ml Volume ( 100 .1ml ) 5ml Volume ( 5 .0ml )

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2.1.5 Setting the External Connection (1) Select "External Connection" on the Menu screen. The following screen will appear:

Machine No 01

RS-232C Bandrate Set Printer (Ach) 9600 Communication (Bch) 9600

ADmanager OFF

Fig.19 External Connection

(2) Setting the machine number

Set a number from 00 to 99 at "Machine No."

This number is unique for each machine and is printed in the first line of the results (see

Appended Figure 1, "Sample Print in Reference Mode). Since this number is used as an ID

number by ADManager, be sure to set different numbers when using several instruments of

the same type.

(3) Setting the RS-232C communication speed

Do not change the communication speed at "Printer" because this speed is used by the

printer that is built in to the instrument (baud rate: 9600 bps).

"Communication" is for external communication. The baud rate is set to 9600 bps at

shipment.

(4) Setting ADManager

When ADmanager is OFF, send the test results to the computer [Communication method:

Non-protocol (LIMS)].

When ADmanager is ON, the AD-6 is in ADManager mode, in which test progress and results

can be obtained by real-time communication with the computer and distillation curves can be

drawn.

For details, refer to the ADManager Instruction Manual.

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2.1.6 Distillation Rate Adjustment. (1) Select "Dist Rate Adj" on the Menu screen. The following screen will appear:

Fig. 20 Distillation Rate Adjustment Screen

(2) “Mode No” means the mode number of the Menu Screen. So, select the number which you

want to adjust the distillation rate. (3) “Proportional Const” means controlled variable of the distillation rate. The default setting is

“20”. When a sample has low boiling point (like a gasoline), set big amount (20-50), and a sample has high boiling point (like a gas oil), set small amount (10-20). Change this amount only when distillation rate is not well controlled by the amount of “20”.

(4) “0-10% Rate Set” means distillation rate offset value between 5 to 10% recovery. AD-6 controls distillation rate to 4.0 to 5.0% automatically, but not perfect for all samples. Set “-0.5%” when distillation rate between 5 to 10% is higher than 5.0%, set “0.5%” when distillation rate between 5 to 10% is lower than 4.0%.

(5) “Init Temp1 Time” means the applicable time for the mode condition “INIT TEMP1”. The default value is “4.0” min. Change this value only when the time from a start to IBP cannot follows test condition of ASTM D86.

(6) Distillation rate adjustment by the heater voltage setting The distillation rate of the most of samples (petroleum) can be adjusted by above settings, but it is difficult for bio-fuels. AD-6 has the function that can control heater output automatically based on the preset value of each distillation interval. When running special sample like bio-fuel, if required, please use this function by following procedure.

<Dist Rate Adj> Mode No 04 KEROSIN(400) Proportional Const 20 0 – 10% Rate Set 0.0% Init Temp1 Time 4.0min Manual Heater Set OFF

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Fig.21 Distillation Rate Adjustment (Manual Heater Set) Screen (6-1) Change “Manual Heater Set from “OFF” to “SET”, and then push RESET key to return to

the STANDBY Screen. (6-2) Following IT&Rate Auto Setting in the Instruction Manual 9.1 (19), obtain appropriate IT1

and IT2 temperature and heating rate. - If good distillation condition is found, Change “Manual Heater Set from “SET” to “OFF”, and then push RESET key to complete the setting. - If distillation rate is still out of specified range, go to next step.

(6-3) Recall Distillation Rate Adjustment (Manual Heater Set) Screen after complete above operation, Display shows controlled average voltage (%) of each distillation intervals.

(6-4) Adjust voltage (%) of each interval which is out of specified distillation rate. - Add some when distillation rate is specified. - Deduct some when distillation rate is higher than specified. Set “Proportional Const” to “10” after changing voltage (%). (6-5) Change “Manual Heater Set” from “SET” to “RUN”, then push RESET key to return the

STANDBY screen, and then run a test with the same sample. AD-6 controls heater output with “10” of proportional constant. If distillation rate is still out of range, change “Proportional Const” value bigger (6), and then try again. This operation may be repeated several times to find good condition.

Note(6): There is a threat that distillation temperature changes up/down in the case of the

sample of the high boiling point when ”Proportional Const” value is too big. In that case, it is necessary to set it down below “20”, and change voltage of each interval. AD-6 regulates heater output as set voltage when “Proportional Const” value is “00”.

<Dist Rate Adj> Mode No 04 KEROSIN(400) Proportional Const 20 0 – 10% Rate Set 0.0% Init Temp1 Time 4.0min Manual Heater Set SET 0 - 5% 50% 40 - 50% 55% 5 - 10% 50% 50 - 60% 57% 10 - 20% 52% 60 - 70% 58% 20 - 30% 52% 70 - 80% 60% 30 - 40% 54% 80 - 90% 62%

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2.1.7 Temperature Circuit Check by Reference Resistance (Temp Check)

This screen is for checking of temperature circuit of the AD-6. To perform temperature circuit, Resistance Decade Box (Range: 100Ω to 300Ω with 0.01Ω unit) or Reference Resister Connector (available as optional accessories, for 0oC, 200oC, 400oC) is required. If you use Resistance Decade Box, purchase the connector for temperature sensor from us, and then connects leads with 0.5 squares less than 1.5m length. The procedure for the circuit check is as follows. (1) Select “Temp Check” on the Menu screen. The following screen appears.

Fig.22 Temp Check Screen (2) Connect the resistance decade box to the AD-6 temperature sensor connector, and then

set it to 100.00Ω. Or connect Reference Resister Connector 0 oC to the AD-6 temperature sensor connector.

(3) Select “Range” to “Dist”. The temperature corresponding to the value of resistance is shown below “Temp”. Confirm that display shows 0 oC ± 0.2 oC. In the same way, select “Range” to “P200”, and then confirm that display shows 0 oC ± 0.2 oC.

(4) Stay “P200”, set resistance decade box to175.84Ω or connect Reference Resister Connector 200 oC to the AD-6 temperature sensor connector, and then confirm that display shows 200 oC ± 0.3 oC.

(5) Select “Range” to “Dist”, and then set resistance decade box to 247.04Ω or connect Reference Resister Connector 400 oC to the AD-6 temperature sensor connector, and then confirm that display shows 400 oC ± 0.3 oC.

(6) If each temperature is out of range, MAIN Board may be defective. Please contact Tanaka Scientific or local distributor.

<Temp Check> Range Dist (OHM) Temp Dist P 0oC 100.00 400.0 S 400 oC 247.04 P200 P 0 oC 100.00 S 200 oC 175.84

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2.1.8 Inspecting the Peltier Element If the condenser bath or receiver chamber cannot be controlled at each temperature, inspect

the bath or chamber as follows:

(1) Select "Peltier Element Inspection" on the menu screen. The following screen will appear:

Peltir Supply Volt

Bath (U) 12V Bath (M) 12V Bath (L) 12V

Rec 12V

Fig.23 Peltier Element Inspection

(2) The bath and chamber are normal if the Bath (U), Bath (M), Bath (L), and Rec voltages are within 12 ± 2 V. "Rec" is used to check the receiver chamber. "Bath (U)," "Bath (M)," and "Bath (L)" are used to check the Peltier elements at the top, middle, and bottom stages of the condenser bath. Note that a pair of Peltier elements is installed at each position.

(3) A voltage within the range of 12 ± 2 V indicates that the Peltier element has deteriorated. The

Peltier element does not require immediate replacement, but replacement should be performed at the earliest convenient time. If a voltage is 0 or 24 V, then the Peltier element has an open circuit or the thermo module control board (TEM-CTL) is faulty. Replace the Peltier element or the thermo module control board (TEM-CTL). For replacement, contact Tanaka Scientific Ltd.

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2.2 Setting the Initial Heating Temperatures (1 and 2) This instrument has a function that allows a distillation test to be executed automatically without the initial heating temperatures (1 and 2) being set. This function allows the heater temperatures (1 and 2) to be known easily for initial heating.

(1) After determining a mode number and setting conditions(6) other than the initial heating temperatures (1and 2), display the test condition screen of the mode number and set the “IT&Rate Auto Set” to “INIT”.

Note (6) If you cannot tell which group from 1 to 4 the sample belongs to, execute the test under the conditions for Group 4. Based on the obtained distillation temperature, identify the correct group. If the sample belongs to from Group 1 to Group 3, execute the test under the conditions of Groups 1 to 3. Since the sample may become solid at room temperature, it is recommended to set the condenser bath and receiver chamber temperatures slightly higher (30°C to 40°C) for safety when setting the conditions for Group 4. For representative sample conditions, see Table 2-1 on page 38 and Table 2-2 on page 39.

(2) After the settings in (1), load the sample and start the test. By raising the initial heating temperatures gradually, this instrument starts boiling smoothly (about 20 to 30 minutes from start until IBP for a test on a sample having a high boiling point). After the test, this instrument sets the appropriate initial heating temperatures (1 and 2) automatically.

(3) After the test, distill the sample again with the initial heating temperatures (1 and 2) obtained in (2). Then check the time from start until IBP and that from IBP until 5% and adjust the initial heating temperatures (1 and 2) more precisely(7).

Note (7) Basically, adjust both initial heating temperatures 1 and 2 by setting the same temperature. For a sample of a great loss, such as gasoline, adjust the time from start until IBP as initial heating temperature 1 and that from IBP to 5% as initial heating temperature 2 with the initial heating temperatures as criteria. More specifically, see "Gasoline" and LOW Naphtha" in Table 2-1 on page 38 and Table 2-2 on page 39.

(4) The initial heating temperatures may require not only the above time adjustments, but also adjustments to eliminate differences from readings of the prescribed glass thermometer. For reference, setting the time from start until IBP in the prescribed time range to be longer tends to raise the IBP temperature. Make adjustments as required.

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2.3 Setting the Final Heating Voltage (8) This instrument allows you to preset the final heating voltage ((MANU)XXV) according to a sample, or sets the final heating voltage automatically ((AUTO)±00 V) from the distillation control voltage by analogical reasoning without a sample. Use the automatic setting function except in the case of special samples (vapor temperature rises quickly or decomposed at 80% to 95%). The usual setting is "(AUTO)+00 V". When necessary, however, increase "(AUTO)+XXV" or decrease "(AUTO)-XXV" the automatically set final heating voltage. In general, adjust the final heating voltage as explained below.

(1) Decrease the automatically set final heating voltage when the time from the final heating start

point until EP is shorter than the standard or increase the automatically set final heating voltage if the time from the heat freeze point until EP is longer than the standard.

(2) To adjust the EP temperature difference between the displayed temperature of AD-6 and the

reading of the prescribed glass thermometer, increase the final heating voltage if the difference is lower than the glass thermometer reading or decrease the final heating voltage if the difference is higher than the glass thermometer reading.

Note (8) Set the final heating voltage to be an even number of volts. Odd values are discarded.

26

3 Troubleshooting

3.1 Trouble Display If a test condition error, an operational error, or an equipment abnormality occurs, a description of

the error is displayed on the screen and printed. The buzzer sounds for 10 seconds to indicate that

the test has been suspended or cannot be started. If an error occurs during testing, the data

collected up until the error is printed.

To return to the Standby screen, press the RESET key during the error display.

TROUBLE

NO RECEIVER!! <- Contents of trouble

REC 0.0% DIST 25.0°C

ROOM 25.0°C BATH 0.0°C

HEAT 25.0°C D.P 0.0

Fig.24 Example of Error Display

TROUBLE

DATE

2/ 8/20 11:30:00

NO RECEIVER!! <- Trouble

VOL 0.0% DIST 25.0°C

REC 25.0°C BATH 0.0°C

HEAT 25.0°C DP 0.0

Fig.25 Sample Trouble Printout

(1) Test condition or operational error <1> NO RECEIVER !!

Indicates that the cylinder is not loaded at test start. Load the cylinder before starting the test.

<2> BATH TEMP? Indicates that the condenser bath temperature is not within the set temperature range ±6°C at test start. Before starting the test, wait until the condenser bath temperature reaches the set temperature ±6°C. If the instrument does not reach the set temperature even after a

27

sufficiently long period of time, the Peltier element may be faulty. Inspect the Peltier element according to Section 2.1.8 (page 23).

<3> M.S FLWR POSITION Indicates that the test was started with the meniscus sensor in a position other than the upper fixed position. Before starting the test, check that the meniscus sensor is in the upper fixed position.

<4> HF POINT? Indicates that the heat freez point is not set correctly. The setting range of the heat freeze point is from 80% to 95%. Setting the heat freeze point outside this range will result in an error after starting the test.

(2) Other equipment abnormality <1> DETECTED IBP BEFORE START

Indicates that IBP has already been detected at the start. The IBP sensor is faulty. Replace the IBP sensor.

<2> REPLACE BATTERY Indicates that the memory backup battery has deteriorated. For memory backup battery replacement, see (4) of Section 4.1 on page 31.

<3> DIST TEMP FULL SCALE Indicates that the distillation temperature has exceeded the test temperature range. The upper limit of the test temperature range is 200°C for P200, 300°C for 300, and 400°C for 400/P400.(extended version is 450°C for 450/P450)

<4> DIST RATE ABNORMAL Indicates that the follower has stopped (for 4 min or longer) during testing. The cylinder is bent excessively or distillation is abnormal due to impacting the instrument. Before testing, check the cylinder position and also check for the presence of the bubble stone.

<5> MS FLWR UP LIMIT Indicates that the follower went up during testing, irrespective of the liquid level, and activated the upper limit switch. The cylinder is dirty or cloudy (especially when the receiver chamber is switched from cooling for Groups 1 to 3 to heating for Group 4.

If a temperature sensor is disconnected, one of the following messages is displayed. Reconnect the corresponding temperature sensor.

<6> "TEMP SENSOR (DIST)" (Distillation temperature sensor) "TEMP SENSOR (RECEIVER)" (Receiver chamber temperature sensor) "TEMP SENSOR (BATH)" (Condenser bath temperature sensor) "TEMP SENSOR (HEATER)" (Heater temperature sensor) "DP SENSOR" (Dry-point sensor)

<7> LIMIT SWITCH Indicates that the upper or lower limit switch of the follower sensor is faulty. When the follower sensor is at the lower end, the lower limit switch is faulty. When the follower sensor is at the upper end, the upper limit switch is faulty. Replace the proper switch.

28

<8> 12C COM ERROR Indicates that the main board is faulty. In the case of an IC error (I2C), "I2C (error IC number)" is displayed on the screen and printer common display and printed. When replacing the main board, contact Tanaka Scientific Ltd.

<9> RECVD < 5% (25 min) Indicates that the initial boiling point did not appear within 25 minutes after the start of the test. The initial heating temperatures is set too low or the heater has an open circuit. Check the heater wiring. If an open circuit is found, replace the heater.

<10> BATH TEMP OVER Indicates that the condenser bath temperature has exceeded 70°C. Check the temperature at "Condenser bath Setting." If the set temperature is over 70°C, lower the set temperature. If the temperature setting at "Condenser bath Setting" is normal, the thermo module control board (TEM-CTL) for condensation block may be faulty or the cooling system may be faulty (low on cooling water, faulty circulation pump, or faulty cooling fan). Contact Tanaka Scientific Ltd.

<11> REC TEMP OVER Indicates that the receiver chamber temperature has exceeded 70°C. Check the temperature set at "Receiver Chamber Setting." If the temperature setting is normal, then the trouble may be attributable to the same causes as described for the BATH TEMP OVER error. Contact Tanaka Scientific Ltd.

<12> EEPROM DATA ERROR Indicates that data was lost from the memory device (EEPROM: IC6 on the main board) that stores the distillation temperature, condensation block temperature, receiver chamber temperature, and position and span data of the heater temperature amplifier. Once this data has been lost, this instrument cannot display temperatures correctly. Contact Tanaka Scientific Ltd. immediately to order a new EEPROM for replacement.

<13> IBP SENSOR Indicates that the IBP sensor is faulty. Replace the IBP sensor.

<14> MS SENSOR Indicates that the meniscus sensor is faulty. Replace the meniscus sensor.

<15> SAFETY SSR BLAZE Indicates that the SSR for safety relays (circulation pump, cooling fan, and heater-cut relays) has an open circuit or that the thermo module (TEM-CTL) is faulty. Carefully disconnect the power lines (CN3) from the thermo module control boards (for the condenser bath and the receiver chamber) so as not to cause a short circuit between. Turn the main switch to ON. If the same trouble reoccurs, then the SSR is faulty. Replace the SSR (SSR1) on the main board. If the trouble no longer occurs, the thermo module control board (TEM-CTL) is faulty. Connect the power lines one at a time and replace the faulty thermo module control board.

29

<16> SAFETY SSR SHORT Indicates that the SSR for safety relays (circulation pump, cooling fan, and heater-cut relays) has a short circuit. Replace the SSR (SSR1) on the main board.

<17> HEATER BLAZE Indicates that the heater has an open circuit. If the heater has an open circuit, replace the heater. If the heater does not have an open circuit, the heater SSR (SSR1 for AC line) has an open circuit. Replace the heater SSR.

<18> COM ERROR Indicates that communication with the computer is not possible. The CPU board on the main board is faulty. Replace the CPU board.

<19> HEATER SSR SHORT Indicates that the heater was activated at a time other than during testing. The heater SSR (SSR1 for AC line) has a short circuit. Replace the heater SSR.

<20> COOLANT TEMP The temperature of the hot side of the Peltier Cooler has exceeded 70°C or floating switch in the water tank detects low coolant circulation. Replace the radiator fan motor or the circulation pump if they are not working. There is insufficient coolant circulation. Add coolant.

* In the cases of <8>, <10>, <11>, or <15>, the printer does not output error information.

(3) Printer trouble The following errors occur if there is no more paper in the printer or if the printer is faulty. If the printer is faulty, the corresponding message is displayed (but no error information is printed). If the printer is out of paper, the PAPER lamp on the printer will light. Load new printer paper. In other cases, the printer is faulty. Replace the printer. <1> PRINTER ERROR

Indicates that the printer is disabled. <2> SIO ERROR

Indicates that a communication error has disabled the printer. * If an error occurs but the above component replacement does not fix the problem, the main board is

faulty. For component replacement, see Section 4, "Component Replacement."

30

3.2 Countermeasures by Error

Table 1 Troubleshooting Errors Problem Inspection Item and Cause Solution

Nothing is displayed on the display panel.

Circuit protector open-circuit Circuit protector good Display panel backlight lit Display panel faulty Display panel not lit Control power supply faulty

Replace the main fuse. Replace the display panel. Replace the control power supply.

The display on the display panel is not normal.

All switches disabled CPU board faulty Switches not disabled Display panel faulty

Replace the CPU board. Replace the display panel.

The display panel backlight does not come on.

Backlight inverter faulty Inverter not faulty Display panel faulty

Replace the inverter. Replace the display panel.

Displayed Character is flickering

LCD contrast trimmer is misaligned See appended Fig.2

Adjust contrast trimmer by screwdriver

The buzzer continues to sound after the main switch is turned ON.

CPU board faulty (Runaway) Replace the CPU board.

The panel switches do not work (disabled).

Panel sheet switch faulty Switch faulty AD6-PNL not faulty AD6-PNL faulty

Replace the panel switch sheet. Replace AD6-PNL. Replace the main board.

Printing by the printer does not work.

Printer faulty Printer not faulty

Replace the printer. Replace the main board.

The cooling fan does not rotate.

Cooling fan connector (CN17) voltage 24 V output Cooling fan faulty 24 V not output Main board faulty

Replace the cooling fan.Replace the main board.

The condensate and receiver chamber temperatures do not reach the set temperatures.

Radiator cooling fane disabled Cooling fan faulty Cooling water level low Low on cooling waterCooling water not circulated Circulation pump faulty Cooling fan disabled Drive power supply faulty Cooling fan not disabled Thermo module control board or Peltier element faulty

Replace the cooling fan. Replenish supply of cooling water. Replace the cooling water circulation pump. Replace the drive power supply. See 2.1.8, "Inspecting the Peltier element."

The receiver chamber alone does not reach the set temperature.

Receiver chamber fan disabled Receiver chamber fan faulty Receiver chamber fan not disabled Thermo module control board or Peltier element faulty

Replace the receiver chamber fan. See 2.1.8, "Inspecting the Peltier element."

The condenser bath alone does not reach the set temperature.

Thermo module control board or Peltier element faulty See 2.1.8, "Inspecting the Peltier element."

The fire buzzer sounds. Fire fuse blown by a fire on the sample Open circuit due to deterioration of the fire fuse

Replace the fire fuse following the procedure described in the instruction manual.

* For component replacement, see Section 4, "Component Replacement."

31

4 Component Replacement

！ Warning: For component replacement, turn the main switch OFF, disconnect the power plug, and wait for one minute. Failure to follow this procedure may result in electric shock or damage the instrument.

For component positions, see the figures at the end of this manual. When installing new components, be sure to make note of the connections before disconnecting the components that are to be replaced.

4.1 Controller When replacing controller component, undo the screws on both sides of the controller cover at the upper part of this instrument and remove the cover. (1) Main board

The main board contains a digital circuit, an analog circuit, and an SSR circuit, including the CPU board.

Fig.26 Main board

Digital circuit

Analog circuit

CPU board

ROM notch

ROM

EEPROM Internal battery for clock

SSR circuit

Internal battery for data memory

Front Side

32

(2) CPU board The CPU board is attached to the main board via a socket. When the CPU board is replaced, all data must be reentered. Enter the data according to the adjustment procedure. The default data at shipment from Tanaka Scientific Ltd. can been entered.

(3) ROM(10) Insert the ROM device with the notch facing toward CN2, as shown in Figure 14. When the ROM device is replaced, all data must be reentered. Enter the data according to the adjustment procedure. Turn No2 in the SW1 on the MAIN board ON, and then turn MAIN switch ON. Once error message appeared, push RESET key and then turn No2 in the SW1 on the MAIN board OFF to clear barometric pressure constant. Note- If both No.1 and No.2 in the SW1 on the MAIN board ON, and then turn on the unit, all setting data includes temperature offset values and new mode which customer created are all cleared.

(4) Internal battery for data memory(10)

The internal battery is soldered. After replacement, set DIP switches (SW1) 1 and 2 to ON and press the RESET key to initialize the data. Then set DIP switches 1 and 2 to OFF and enter all data again according to the adjustment procedure. Remark: At CPU board replacement, the default data at shipping from Tanaka Scientific Ltd. can be entered.

(5) Internal battery for clock

As in (4), this internal battery is also soldered. After replacement, set the time by referencing Section 2.1.3, "Setting the clock and the barometric sensor" on page 13.

(6) EEPROM(9)

Replace IC6 (24C02) on the main board shown in Figure 26. To prevent mounting the EEPROM backwards, orient the EEPROM notch in the correct direction as described with the ROM notch.

Note (9) When the power switch is turned on after the internal battery for data memory, ROM and

EEPROM are replaced, an error message is displayed. Press the RESET key to clear the error state.

33

4.2 Receiver Chamber For component positions, see Appended Figure 5 "Component Arrangement in the Receiver Chamber."

(1) Follower sensor [DMB(MS) board] <1> Extract the connector and undo the two mounting screws. <2> Undo the lamp and the photo transistor board mounting screws and mount a new follower

sensor. Check that the lamp lights(10) as shown in Figure 27.

Fig.27 Follower Sensor Optical-axis Adjustment

Receiving surface

Adjust the board mount to align the optical axis of the lamp with the receiving surface.

Photo transistor board mount

Note(10) Power-on does not light the lamp. The lamp lights when the meniscus correction screen

is displayed.

<3> After replacing the follower sensor, execute a meniscus correction, as described in Section

2.1.4 (page 14).

(2) IBP sensor [DMB(IBP) board] <1> Extract the connector and undo the two mounting screws. <2> Remove the lamp and phototransistor board mounting screws, and mount a new IBP sensor.

Adjust the light emission board mounting so that the driver shadow reaches the center of the IBP sensor.

<3> After replacing the IBP sensor, measure a sample to see that the initial distillate is detected.

Condensate pipe

IBP sensor receiver

Thin screwdriver

Fig.28 IBP Sensor Adjustment

34

(3) Replacing the receiver chamber Peltier unit <1> Remove the right side cover toward this instrument to expose the back of the receiver

chamber (see Figure 29). Referencing Figure 30, pinch the internal water circulation hoses connected to the Peltier units using pinch cocks in order to prevent water leakage.

<2> Cut the typing band securing the hose to the Peltier unit and extract the band from the Peltier unit. Soak up the circulated water from the Peltier unit using a waste cloth.

<3> Undo the screws securing the Peltier units (four screws per unit) on the receiver chamber and disconnect the connectors to remove the Peltier units.

<4> Apply a thermally conductive grease thinly to the contact surface of each new Peltier unit (see Figure 31) and attach the receiver chamber by following the removal procedure in reverse. When attaching a new Peltier unit, note the direction of the arrow. (See the red arrow in Figure 30.)

<5> Replenish the circulated water supply if the supply is low.

Circulated water hose

Receiver chamber

Pinchcock

Contact surfaceFig.29

Fig.30

Fig.31

Pinchcock

Peltier unit

35

4.3 Condenser Bath For component positions, see Appended Figures 6 and 7. (1) Condenser bath block

Contact Tanaka Scientific Ltd. (2) Condenser bath Peltier unit

Before performing repairs, contact Tanaka Scientific Ltd. as field repair may not be possible under certain circumstances. For the replacement of one Peltier unit, follow the receiver chamber replacement procedure.

36

<A>

Terminal strip

<A>

<B>

Heater temperature sensor

Wire (red)

Red marking

4.4 Heater Section

(1) Heater coil <1> Turn the heater vertical adjustment knob to lift the heater to the top position. <2> Undo the two mounting screws and remove the heater terminal cover. (See Figure 32) <3> From the heater terminal strip (see Figure 33), undo the two screws at <A> in the figure.

Remove the heater coil and replace it with a new one.

(2) Heater temperature sensor <1> Turn the heater vertical adjustment knob to lift the heater to the top position. <2> Undo the two mounting screws and remove the heater terminal cover. (See Figure 32) <3> From the heater terminal strip (see Figure 33), undo the two screws at <B> in the figure.

Remove and replace the heater temperature sensor.

* Connect the temperature sensor with the red marking to the red wire. (See Figure 33)

Heater terminal cover

Fig.32 Heater Unit

Heater terminal cover mounting screws

Fig.33 Heater Connector

37

Fig.35 Rear view of the printer

<A>

(3) Printer (Option) <1> Undo the four screws <A> securing the printer cover on both sides. (See Figure 34) <2> Pull the printer cover to the printer side to expose the back of the printer.

Be careful not to pull the cable too hard because the cable is still connected.

<3> Once the printer has been pulled out as shown in Figure 35, disconnect the two connectors

and undo the two screws securing the printer. Remove and replace the printer.

Printer

Printer cover

Fig.34 Printer installation status

<A> <A>

Connector

Printer securing screws

Connector

38

Table 2-1 Model Test Conditions (without Heater Protecting Net)

Sample LOW

Naptha Gasoline

Kero sene

Gas oilKero sene

Gas oil Fuel oil Benzene Toluene Xylene

Initial Heat 1 (°C)

300 250 650 650 540 800 850 580 630 620

Initial Heat 2 (°C)

450 450 650 650 540 800 850 580 630 620

Final Heating Start Point

(%) 93 93 93 95 95 88 88 95 95 95

Final Heating (V)

(AUTO) +0

(AUTO) +0

(AUTO) +6

(AUTO)+0

(AUTO)+0

(AUTO)+0

(AUTO)+0

(AUTO) +20

(AUTO) +20

(AUTO)+30

Temperature Range

(°C) 300 300 300 400 400 400 400 P200 P200 P200

Residue (%)

1.0 1.0 1.0 1.5 1.0 0.0 0.0 1.5 1.5 1.5

Distillation Rate

(%/min) 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5

Condenser Bath

Temperature Setting

(°C)

0.5 0.5 2.0 30.0 25.0 30.0 30.0 25.0 25.0 25.0

Receiver Chamber

Temperature Setting (°C)

15.0 15.0 15.0 25.0 25.0 30.0 30.0 25.0 25.0 25.0

Distillation Volume or

Temperature Cut

88.8% 88.8%

Flask Support Hole

Diameter (mm)

38φ 38φ 38φ 50φ 50φ 50φ 50φ 25φ 25φ 38φ

IBP Temperature

Range (°C)

25 - 35 30 - 40 150 - 160

160 - 180

150 - 160

70 - 80 100 - 110

130 - 140

EP Temperature

Range (°C)

140 - 160

190 - 210

230 - 250

360 - 380

250 - 270

70 - 80 100 - 110

130 - 140

Remarks Groups 1 to 3 Group 4 For 10% residue,

use 250 ml flask and 200 ml cylinder.

BTX distillation. Use 200 ml flask.

39

Table 2-2 Model Test Conditions (with Heater Protecting Net)

Sample LOW

Naptha Gasoline

Kero sene

Gas oilKero sene

Gas oil Fuel oil Benzene Toluene Xylene

Initial Heat 1 (°C)

400 350 750 750 640 900 950 680 730 720

Initial Heat 2 (°C)

550 550 750 750 640 900 950 680 730 720

Final Heating Start Point

(%) 93 93 93 95 95 88 88 95 95 95

Final Heating (V)

(AUTO) +0

(AUTO) +0

(AUTO) +6

(AUTO)+0

(AUTO)+0

(AUTO)+0

(AUTO)+0

(AUTO) +20

(AUTO) +20

(AUTO)+30

Temperature Range

(°C) 300 300 300 400 400 400 400 P200 P200 P200

Oil Level (%)

1.0 1.0 1.0 1.5 1.0 0.0 0.0 1.5 1.5 1.5

Distillation Speed

(%/min) 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5

Condenser Bath

Temperature Setting

(°C)

0.5 0.5 2.0 30.0 25.0 30.0 30.0 25.0 25.0 25.0

Receiver Chamber

Temperature Setting (°C)

15.0 15.0 15.0 25.0 25.0 30.0 30.0 25.0 25.0 25.0

Distillation Volume or

Temperature Cut

88.8% 88.8%

Flask Support Hole

Diameter (mm)

38φ 38φ 38φ 50φ 50φ 50φ 50φ 25φ 25φ 38φ

IBP Temperature

Range (°C)

25 - 35 30 - 40 150 - 160

160 - 180

150 - 160

70 - 80 100 - 110

130 - 140

EP Temperature

Range (°C)

140 - 160

190 - 210

230 - 250

360 - 380

250 - 270

70 - 80 100 - 110

130 - 140

Remarks Groups 1 to 3 Group 4 For 10% residue,

use 250 ml flask and 200 ml cylinder.

BTX distillation. Use 200 ml flask.

- - 41

Appended Figure 1 Sample Print in Reference

AD-6 ( NO 1 ) OPERATOR SAMPLE DATE

4/ 4/ 13 10 : 32 : 14 MODE NO 15

STD A INIT TEMP 1 - 500.0(°C) INIT TEMP 2 - 500.0(°C) H./FREEZE -- 93.0(°C) FINAL H(AUTO)+ 0(%) TEMP RANGE - 300 RESIDUE --------- 1.0(%) DIST RATE ------- 4.5(%) SET BATH ------- 2.0(°C) SET REC -------- 15.0(°C) LOSS COR ---- GRAPH DISTILLATION DATA BATH TEMP --- 2.0(°C) REC TEMP ----- 15.0(°C) FINAL HEAT ---- 54(%) RECOVERY ---- 98.8(%) RESIDUE ------- 1.0(%) LOSS ------------- 0.2(%) RAW BARO LOSS TIME REC TEMP CORR CORR & (%) (°C) (°C) (°C) RATE IBP 76.0 78.7 519 S 5 90.8 90.4 73 S

10 93.4 93.3 4.3 % 20 97.7 97.7 4.4 % 30 103.0 102.9 4.5 % 40 109.2 109.1 4.4 % 50 116.8 116.7 4.4 % 60 125.9 125.8 4.4 % 70 138.8 138.6 4.5 % 80 157.3 157.0 4.4 % 90 184.1 183.6 4.3 % 95 194.1 193.7 97 199.4 198.9 E.P CUT ( 97.6% ) 202.0 202.0 188 S

REF DIFFERENCE DATA REF CORR DIFF REC TEMP TEMP TEMP (%) (°C) (°C) (°C) IBP 76.0 78.7 2.7 5 88.5 90.4 1.9

10 92.5 93.5 0.8 20 97.5 97.7 0.2 30 102.5 102.9 0.4 40 109.0 109.1 0.1 50 116.5 116.7 0.2 60 126.0 125.8 -0.2 70 139.5 138.6 -0.9 80 158.0 157.0 -1.0 90 184.0 183.6 -0.4 95 194.0 193.7 -0.3 E.P CUT ( 97.8% ) 203.5 202.0 -1.5

- - 42

Appended Table 1 Specifications for Standard Sample Composition (JIS K 2254)

Vol. % Ingredient (1) Standard Sample A Standard Sample B

Hexane 20 - Heptane 20 - Toluene 20 - Xylene 20 20

2-ethylhexanol 10 20 Tetrahydronaphthalene 10 20

Alpha-methylnaphthalene - 20 Hexadecane - 20

Note (1) Use guaranteed reagent. Appended Table 2 Standard Recovered Temperature(2) and allowance of Standard

Sample A and B (JIS K 2254) Unit:oC

Collected, % Standard Sample A Standard Sample B IBP (3) 76.0±2.0 148.5±2.0 5%*(3) 88.5±1.5 160.5±1.5 10% 92.5±1.5 166.0±1.5 20% 97.5±1.0 175.0±1.5 30% 102.5±1.0 184.5±1.5 40% 109.0±1.5 196.5±1.5 50% 116.5±1.5 208.0±1.5 60% 126.0±1.5 221.5±1.5 70% 139.5±1.5 234.0±1.5 80% 158.0±2.0 245.0±1.5 90% 184.0±2.0 261.0±1.5 95% 194.0±2.0 272.5±2.0

EP (3) 203.5±1.5 279.5±1.0 Note (2) Recovered temperature is against percent evaporated. Note (3) The temperature and allowance of IBP, 5% and EP are a reference.

- - 43

Appended Figure 3 Component Arrangement in the Controller

Appended Figure 2 Front View of the Main Unit

Operation switches

Fire-Containment Shutter

Temperature sensor

Thermo fuse

Heater

Printer

LCD Display Panel

Operation switch panel

Receiver chamber

Dry-point sensor connector

Main board

Peltier control board for condenser bath

LCD display panel

Drive power supply

Control power supply

Shutter solenoid

Peltier control board for receiver chamber

Temperature sensor connector

Display contrast adjuster hole

- - 44

Blank page

- - 45

Appended Figure 4 Top View of the Receiver Chamber

Appended Figure 5 Component Arrangement in the Receiver

Follower sensor mounting screw

Receiver chamber circulation fan

Pulse motor for follower sensor

Follower sensor

IBP sensor mounting screw

IBP sensor

IBP sensor connector

Follower sensor connector

Receiver chamber temperature sensor

- - 46

Blank page

- - 47

Appended Figure 6 Component Arrangement on the Right Side of the Main Unit

Appended Figure 7 Component Arrangement on the Left Side of the Main

Motor-cut relay (1R)

Heater-cut relay (2Ｒ)

Bottom-stage Peltier units for condenser bath

Main fuse

Main switch Power cable

connection port

Receiver Peltier units

Receiver chamber condensate drain

Heater SSR

Temperature sensor for condenser bath

Middle-stage Peltier units for condenser bath

Internal circulated water radiator

Circulated water reserve tank

Fan motor for internal circulated water radiator

Fan for internal circulated water radiator

Top-stage Peltier units for condenser bath

Heater cooling fan

Internal circulated water pump