TRL-TOC

Total Organic Carbon Analyzer for Solid Samples

Rev.3 / 20.03.2015

Read this manual carefully and keep it with the instrument for future reference

TERRALAB LABORATORY EQUIPMENT & WEAR MANUFACTURING & TRADING Co.

ANKARA, TURKEY

TRL Instruments is the registered trademark of Terralab laboratory Equipment & Wear Manufacturing & Trading Co.

TERRALAB Is a ISO9001:2008 certified company having service quality accreditation

according to EN12426 and EN13201

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1. DECLERATION OF CONFORMITY

Standards:

This product can do analysis according to the following standards:

EN13137: Characterization of waste. Determination of total organic carbon (TOC) in waste, sludges and

sediments

ISO 10694: Soil quality -- Determination of organic and total carbon after dry combustion (elementary

analysis)

NCEA-C 1282: Methods for the determination of total organic carbon (TOC) in soils and sediments

ISO 8245: Water quality – Guidelines for the determination of total organic carbon (TOC) and dissolved

organic carbon (DOC)

EN 1484: Guidelines for the determination of total organic carbon (TOC) and dissolved organic carbon

(DOC)

ASTM D2579: Standard test method for total organic carbon in water

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2. CONTENTS

1. DECLERATION OF CONFORMITY ........................................................................................................... 1

2. CONTENTS ............................................................................................................................................. 2

3. PRECATUTIONS ..................................................................................................................................... 4

4. UN PACKING .......................................................................................................................................... 7

4.1 Checking the packing list ............................................................................................................... 7

4.1.1 Standard List ......................................................................................................................... 7

4.1.2 Spares and Consumables List ................................................................................................ 7

4.2 Placing and handling the packing contents .................................................................................. 7

5. INSTALLATION ....................................................................................................................................... 8

5.1 Software Installatıon ..................................................................................................................... 8

5.2 Hardware Installation ................................................................................................................... 8

5.2.1 Selecting an Installation site ................................................................................................. 8

5.2.2 Loading the catalyst and installing the catalytic reactor ...................................................... 9

5.2.3 Installing the combustion tube ............................................................................................. 9

5.2.4 Installing the catalytic furnace .............................................................................................. 9

5.2.5 Making the tubing and flow equipment connections ........................................................... 9

5.2.6 Making the electrical connections ...................................................................................... 10

5.2.7 Unscrewing the IC handle ................................................................................................... 10

6. FIELD TESTS (INSTALLATION QUALIFICATION, OPERATION QUALIFICATION) .................................... 11

6.1 Installation Qualification ............................................................................................................. 11

7. OPERATION ......................................................................................................................................... 18

7.1 Sample Loading/Unloading ......................................................................................................... 18

7.2 Software ...................................................................................................................................... 18

7.2.1 Authorization ...................................................................................................................... 18

7.2.2 Setting up the connection ................................................................................................... 18

7.2.3 New Wizards: In this part, user can define new sample, method, task and calibration. ... 19

7.2.4 Displaying the created samples, methods, tasks ................................................................ 23

7.2.5 Running an analysis ............................................................................................................. 24

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7.2.6 Displaying, refining and reporting the results..................................................................... 26

8. MAINTENANCE .................................................................................................................................... 28

9. TROUBLESHOOTING ............................................................................................................................ 29

10. APPENDIX ............................................................................................................................................ 32

TERRALAB CONTACT INFORMATION .......................................................................................................... 33

4

3. PRECATUTIONS

The followings is the list of labels used for warning and to call for the attention of users in case of risks,

and remarks for safety, used on and in the instruments.

Corrosive Substance! Avoid contact with the skin and Use appropriate Personal

Protective Equipment (PPE)

Flammable materials are those which can catch fire readily!

Do not Touch!

Warning/Caution! A hazardous or potentially hazardous situation that, if not

avoided, will result in product and/or property damage and possible injury and/or

death.

Hot Surface Area!

Electrical Hazard!

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Risk of Eye Injury.

Proper eye protection must be worn.

Read the Appropriate Documentation!

Put on Safety Glasses and Protective Clothing before proceeding to the next step.

Working Safely:

Will destroy or irreversibly damage another substance with which it comes in

contact. The main hazards include damage to eyes, skin and tissue under the skin,

but inhalation or ingestion are also very risky. Avoid contact, and bear in mind that

these can (under some circumstances) rust chemical cupboards.

Never use hydrogen and other flammable gas with TRL-TOC instrument. Do not

place flammable materials near the furnace exhaust. Follow the manufacturer’s

directions for safe handling of gas and chemicals.

Since they might be extremely hot, use appropriate equipment to touch quartz

boat, loader mechanism and heat sink.

Be careful when instrument is being transported or replaced, instrument can be

damaged, broken and cracked! Maintain a consistent temperature environment. Do

not keep corrosive or combustible gas near the instrument.

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Do not place flammable materials near the furnace exhaust. Do not touch this area!

Voltages inside the instrument are line voltage and can cause injury or death. Turn

off and unplug beforing service.

7

4. UN PACKING

TRL-TOC is delivered within a crate and before opening it you should make sure that the crate is not

damaged or opened. If any of the mentioned problems is diagnosed please do not accept the delivery.

The crate is opened from the top lid by unscrewing the lid with a screwdriver.

4.1 Checking the packing list

Confirm that all of the items listed in section 4.1.1 and 4.1.2 are included.

4.1.1 Standard List

Table 1. List of the standard parts; make sure that all of the following contents are available within the packing

Part Number Part Name Standard Quantity Included

99-0348-2 Main assembly of TC 1 1

99-0349-2 Main assembly of TC-

IC 1 -

99-0353-2 Main assembly of TN 1 -

4.1.2 Spares and Consumables List

Please see the packing list and check with your purchase order. If there is a conflict between anyone of

packing list, the items delivered and your purchase order, please either let us or your local agent know

to resolve.

4.2 Placing and handling the packing contents

The package contains brittle materials such as quartz or pyrex and one should be careful during handling

of the contents.

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5. INSTALLATION

5.1 Software Installatıon

5.2 Hardware Installation

5.2.1 Selecting an Installation site

Instrument should be installed in a suitable site by considering the size and operation conditions. Lift the

instrument by the base plate. Do not lift it by the air gas separator window, valves window, top window

or any other spacing on the instrument, as this may cause instrument damage. The dimensions of the

instrument are height: 450mm, width: 800mm and depth: 450mm and the front panel should be

directed to user. This placement allows the user to load/unload sample, control flows and drain the air

gas separator easily.

Instrument should be installed within environmental conditions listed below:

- Organic gasses, flammable gasses and dust should not be present.

- Bench should be free of vibration or any other impact

- Temperature should be stable and at the level of room temperature.

- Electricity and gas connections are located at the back side of the instrument. In order to have

easy access to those connections, instrument should be located at least 200mm away from the

wall.

- Completely grounded and stable power should be supplied to the instrument.

Figure 1 TRL-TOC Front View

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5.2.2 Loading the catalyst and installing the catalytic reactor

Catalyst is in the form of beads and is sent within a 40ml bottle. In order to load catalyst to the reactor

the following procedure should be followed:

- Place 20mm quartz wool to one end of the tube (97-0273-01)

- Pour all of the catalyst from the other end

- Place 20mm quartz wool to the other end of the tube

- Place the reactor within the hole of the catalytic furnace

- Place the gaskets (05-0447-2) from the both ends of the catalytic tube

- Place the female part of the fitting (02-0277-01) and then place the o-ring (05-0248-01) to the

reactor

- Mount the male parts of fittings (02-0277-1) until the o-ring hold on to reactor.

5.2.3 Installing the combustion tube

The reactor of the larger furnace should be installed prior to catalytic furnace installation.

- Lubricate the o-rings 05-0181-1

- Place the reactor (97-0253-1) to the furnace

- Mount the 02-0266-1 with the supplied M3x10 screws

- Place the female part of the fitting (02-0276-1) and then place the o-ring (05-0246-1) to the

reactor

- Mount the male parts of fittings (02-0276-1) until the o-ring hold on to reactor.

5.2.4 Installing the catalytic furnace

- Place the catalytic furnace on the rack.

- Mount the furnace to the 02-0261-1 and 02-0262-1 with supplied M4x12 screws

5.2.5 Making the tubing and flow equipment connections

- Place the female part of the fitting (02-0278-1) and then place the o-ring (05-0247-1) to the

reactor

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- Mount the male parts of fittings (02-0278-1) until the o-ring hold on to probe.

- Place the sampling probe (97-0272-1) to the 97-0253-1

- Connect the probe outlet with the upper inlet of the catalytic furnace. Use supplied tubing(01-

0238-1) for this purpose.

- Connect the lower outlet of the catalytic reactor (01-0007-1) to the cooling unit inlet(07-0009-1)

5.2.6 Making the electrical connections

- Connect the coming electric line to the terminal of the catalytic furnace via suitable screwdriver.

5.2.7 Unscrewing the IC handle

Inorganic carbon mechanism is delivered in transport safe mode by simply tying with a cable tie. In order

to unlock the mechanism, cable tie is cut.

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6. INSTALLATION AND FIELD TESTS

6.1 Installation

TRL TOC software is delivered within a CD. Insert the CD to the CD rom and wait for the auto run

window appearance. With the approval of the user the installation will start and be completed

automatically.

After installation is completed a TRL Instruments icon will appear on your desktop, double-click it to run

the software. The TRL -TOC application will start and the Login screen will appear.

Figure 2 Login screen, from this screen Administrator and defined users can login the TRL TOC software

TRL-TOC has a default administrator account that is used when the application is run for the first time.

User must login using the administrator’s Username and Password and then, for security reasons,

change the password that we provide for user.

1. Type “Administrator” for the Username.

2. Type “22” for the password.

3. Click the Login button.

After that screen will appear that Administrator can do a few changes.

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Figure 3 Administrator Screen

1) ''Account Manager'' can be used to change administrator account information.

Figure 4 Admin Account information screen

a) Type “Administrator” for the Administrator Name.

b) Type ''22'' for the old password.

c) Choose a password that user wish to use in case user needs access to the default administrator’s

account in the future. User may choose to use “TRL Instrument”, for instance.

d) Using this new password type it into both the ''New Password'' and ''Confirm''

e) Click the ''Save'' button.

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Note: DO NOT FORGET THE NEW PASSWORD!!!

2) ''User Maneger'' can be used to define a new user, to change exisiting users’ properties. A new

user definition will be explained here.

Figure 5 User Maneger screen

Figure 6 New User screen

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Adminisitrator should fill in the blanks to add a new user. The blanks with the stars should be filled.

Administrator can also give permissions for each user. If administrator checks all the permission boxes,

the user can use all the properties of the programme like administrator. There are 11 functions that can

be permitted to user or not. Below the definitions of these functions are given.

Create Method: User can create a new method.

Create Sample: User can create to analyze a different sample.

Create Task: User can create a new task.

Create Schedule: User can create a new schedule and/or import a schedule file.

Create Calibration: User has access to create new calibration files.

Generate Report: User can open and edit reports.

Calculate Result: User can calculate result.

Calculate Blank: User can calculate the values of the blank parameters.

Maintenance Cleaning: User can run the Maintenance-Cleaning tasks.

Flow Adjustment: User can adjust gase flow.

User outlier function: User can refine and recalculate the obtained results

3) ''TRL TOC Software'' can be used to enter the software as an administrator, with the complete

authorization.

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Figure 7 TRL TOC Software screen

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Tools/Communication: The operating system treats USB devices like COM devices. It assigns them a

logical COM port number. In order to set the software configuration user need to know which logical

com port number the TRL-TOC has been assigned.

Figure 8 Communication Page screen

Checking of the operation of process equipments can also be done manually on communication page

screen.

Solenoid Valves: User check all valves by entering Tools/Communication in the software.

Pumps: There are two pumps; Peristaltic Pumps (PP1 and PP2) and Diaphragm Pump Compressor

(DPC1) in TRL TOC instrument. User can check the operations of these pumps. User should enter

Tools/Communication in the software to check the operations of these equipments.

When checking the PP1 pump, user have to use install the standard vial in to IC

chamber. If not, TRL TOC instrument can be damaged because of acid.

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There is also status panel selection part on communication page screen. By this part, user can select the

ststus of Trl-TOC device.

Status should be selected as shut down before the software is closed.

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7. OPERATION

7.1 Sample Loading/Unloading

7.1.1 Total Carbon Application (TC)

Sample is introduced within a quartz boat to the furnace. Sample loading should be done wearing

gloves and goggles. Quartz boat should be handled by using a forceps. Amount of the sample should

be weighed and noted down before placing it to the loader.

Be careful! Quartz boat will be extremely hot after the analysis. Do not Touch quartz

boat with bare hands, use supplied forceps (96-0446-1)!

7.1.2 Inorganic Carbon Application (IC)

Sample is introduced within a standard vials to the IC unit. Sample loading should be done wearing

gloves and goggles. Amount of the sample should be measured and noted down before placing it to

the IC unit.

It is important to be careful while inserting samples into the instrument. Needle

might be harmful.

7.2 Software

7.2.1 Authorization

Please see section 6.1 Installation qualification

7.2.2 Setting up the connection

- Attach USB cable on the right panel the TRL TOC instrument.

- Attach the other end of the USB cable to the appropriate port on the computer.

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7.2.3 New Wizards: In this part, user can define new sample, method, task and calibration.

7.2.3.1 New sample definition: New sample definition wizard appear by clicking the sample

under new menu.

Figure 9 New Sample Definition screen

User should select sample type (unknown sample, validation sample or calibration sample) according to

the purpose of the experiment. Also user should define measurement parameter of the sample (TC, TN,

IC or combination of these parameters).

If sample is unknown, user should fill Sample Name, Estimated Carbon Concentration of TC and IC(ppm,

% or mg/L), Estimated Nitrogen Concentration of TN(ppm, % or mg/L), Submitter and Description boxes.

If sample sample is validation sample or calibration sample, user should fill in the Known Carbon and

Nitrogen Concentration boxes. If the sample is define true, user can save sample by clicking the “finish”

button.

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7.2.3.2 New Method Definition: New method definition wizard appear by clicking the method

icon under new menu.

Figure 10 New Method Definition screen

User should select analysis mode (IC or TC/TN). Also user should select type of method by cliking high or

low carbon concentration.

If user select IC mode, user should fill in a method name, description boxes, enter the maximum run

time and select heater on/off. “Heater on” is applicable for IC determination at elevated temperatures

of 70ºC. This is an optional property for TrL-TOC, there is no Heater on option for standart device.

“Heater off” is applicable for IC determination at room temperature. In case of “heater on” user should

wait for 5 minutes after insertion of the sample cup into the IC chamber, before user start running the

analysis. If the Method is define true, user can save sample by clicking the “finish” button.

If user select TC/TN mode, user should fill in the method name and description boxes and assign Furnace

Temperature, Maximum Operation Time parameters. Furnace temperature is preset to 850ºC as default,

that is usually the best choice for most of the cabon applications. User may assign a higher temperature

if user know that the analysis takes long time (longer than 10 minutes), the analysis includes nitrogen

and peak tailing is considerable.If the sample is define true, user can save sample by clicking the “finish”

button. Total carbon concentration is equivalent to the total of inorganic plus organic carbon

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concentration (TC=TOC+IC). If user want to learn TOC concentration, user can find total of organic

carbon concentration by using this formula.

7.2.3.3 New Task Definition: New task definition wizard appear by clicking the task icon under

new menu.

Figure 11 New Task Definition screen

User should select sample type and method that will be used for analysis. If selected sample is a

calibration sample, select calibration part of the screen stays deactive. If selected sample is a validation

or unknown sample, select calibration part of the screen becomes active. When this part becomes

active, user should be selected a calibration to calculate concentration of carbon or nitrogen of their

sample. Task name and sample size should be filled and number of repeat should be assigned by user. If

the task is define true, user can save sample by clicking the “finish” button.

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7.2.3.4 New Calibration Definition: New calibration definition wizard appear by clicking the

calibration icon under new menu.

In New Calibration Wizard, user can select analysis mode, either IC, TC or TN. IC mode is for detecting

inorganic carbon concentration, TC mode is for detecting total carbon concentration and TN mode is for

detecting total nitrogen concentration. Also user should select method mode, either High or Low. The

method type should be selected according to known carbon concentration. “Low” is suitable for low

carbon concentrations up to 1500 µgC and “High” is suitable for high carbon concentrations from 1500

µgC to 50000 µgC.

Figure 12 Method and Analysis Mode screen

After user select ''Parameter'' and ''Method Mode'', user should select ''Method Name'' which wants to

create calibration file. After that, a page will open showing all analysis of calibration of selected method.

User should define range of calibration by selecting from result of calibration analysis.

User can see R2 and RSD values of the calibration file on the screen. According to results of calibration

user can dispose outlier point by entering number in ''Number of Outlier'' box and recalculate equation

and R2 values.

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Figure 13 Calibration Diagram screen

User can see R2 and RSD values of the calibration file on the screen. According to results of calibration

user can dispose outlier point by entering number in ''Number of Outlier'' box and recalculate equation

and R2 values.

7.2.4 Displaying the created samples, methods, tasks

7.2.4.1 Opening sample:

Defined samples can be viewed by clicking samples icon under open menu.

7.2.4.2 Opening Method:

Defined methods can be viewed by clicking methods icon under open menu.

7.2.4.3 Opening Task:

Defined tasks can be viewed by clicking tasks icon under open menu.

7.2.4.4 Opening Calibration:

Defined calibrations can be viewed by clicking calibrations icon under open menu.

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7.2.5 Running an analysis

Run Menu: This menu contains two tabs (Run Task and Run Sequence).

Figure 14 Run Page screen

Run/Run Tasks: User can run to predefined tasks. Press ''Task'' button and select the task that wanted

to be run. After double clicking on the selecting task, running task screen will be appeared. (figure 15).

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Figure 15 Running Task screen

Now user can start analysis. Press ''Initialize'' button activate run button. Software will ask for flow

adjustment. Flow adjustment is the key factor for an analysis, correct flows gives accurate results. If the

flow adjusted previously press ''Yes'' button ,if not, press ''No'' button and adjust flow.

If sample is prepared, user can put to analyze sample on loader mechanism and user can start task by

pressing ''Run'' button. In this part, user can check task properties, sample size and save results at the

end of the experiment. User can look RSD, mean, real time and maximum time of analysis.

User should enter sample weight to begin a new analysis at the end of each repeated analysis. If not,

''Run'' button will be inactive.

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7.2.6 Displaying, refining and reporting the results

Figure 16 Results Page screen

User can see calibration, unknown, validation results and take a report of these results.

If the obtained results wanted to be viewed results menu is opened. Obtained results can be refined and

recalculated by pressing “refine/recalculate” button. With the refine recalculate option calibration file

can be changed by selecting the calibrations in the “change calibration” drop down menu. Moreover

bad points can be excluded in the repeated analysis by using outlier function.

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Figure 17 Detail Page screen

Figure 18 Sample Report screen

User can print results of analysis from “Report” section in “Results” menu. User can add a header by

pushing “Load Header” button and upload a header image. User also can give a report name and

reference name/number from this screen. If user wants to take a detailed report, “Detailed Report” box

should be checked.

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8. MAINTENANCE

CONTINUOS MAINTENANCE CHECK

Detector Baseline: Check the detector baseline is maximum 0.06 before running every task.

Condensate separator: Check the liquid level in the separators for every 3-4 runs if liquid sample

is emptied.

DAILY MAINTENANCE CHECK

Perform continues maintenance check

Gas Supply: Check the gas supplier is supplying a pressure higher than 2 bar. If the supplier is a

gas cylinder, replace it when the pressure becomes less than 2 bar.

Regulator: Check the regulator is showing the inlet pressure as 2 bar.

Halogen Scrubber: Check color of the copper in scrubber. If the copper side is discolored,

replace copper and tin together.

Acid Supply: Check 20% phosphoric acid is available for IC analysis. (Minimum 50 mL) 20%

phosphoric acid should be made with DI water daily.

Waste: Check vent line is correctly connected to a drum.

WEEKLY MAINTENANCE CHECK

Perform daily maintenance check

System cleaning: Check the system is cleaned by making empty run and only DI water run every

week.

MONTHLY MAINTENANCE CHECK

Perform weekly maintenance check

Reactor: Check the reactor for any corrosion or destruction and replace it if necessary.

Catalyst: Inspect the catalyst for crashing or any kind of destruction and replace it if necessary.

Permeation Dryer: Inspect the dryer for water accumulation, damage or color change and

replace it if necessary.

Ball Screw: Check the lubricant on the ball screw and lubricate it if necessary.

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9. TROUBLESHOOTING

Table 2 Troubleshooting guide

Symptoms First thing to

look Possible Cause Solutions

Sample boat does not

exit from the furnace. Electronic failure.

Close the Trl-TOC device and

re-open it.

Sample boat does not

come to home position. Electronic failure.

Close the Trl-TOC device and

re-open it.

Sample boat does not

move.

Cable connection

failure.

Check the connection of 07-

0407-1

Failure to return to

baseline between

replicates.

Insufficient baseline

stabilization time.

Increase waiting time

between the replicates.

Low recovery for only

higher end.

Furnace is not at set

temperature.

Allow the furnace to heat to

set temperature.

Furnace does not heat.

Communication is

lost.

Or

Coil of the furnace

can be broken.

Check electronic

connections.

Or

Replace or fix the furnace.

Unit does not initialize.

Device is not plug in.

Or

Power switch is OFF.

Plug in the device.

Or

Switch on the device.

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There is no NDIR signal

change.

Check the

detector vent (if

there is a flow)

You make run in high

mode but your

sample is in low

mode.

Run the device in low mode.

You make run in low

mode but carbon

content of your

sample is lower than

LOD

Put more sample in device.

NDIR is out of order. Change NDIR.

Furnace is out of

order.

Check the furnace is hot or

cold.

Catalyst is

degenerated. Replace the catalyst.

Check the

detector vent (if

there is no

flow)

DPC is out of order or

electronic failure. Check DPC can work or not.

There can be a

leakage from the line

between FZ1 and

NDIR.

Check if there is a leakage or

not.

Sample boat cannot

press the furnace

correctly.

Correct the limit switch

lengths from the factory

settings.

If any problem is not considered above, contact Terralab Customer Support Center.

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RETURNING THE TRL-TOC

Do not return the Trl-TOC unless a Terralab representative authorizes you to do so. A

service representative may be able to help you solve the problem over the telephone. If the

instrument must be returned, the representative can tell you how to prevent damage

during shipment. The representative must give you a return authorization number. Write

this number on the return label.

UNIT AND PARTS DISPOSAL

Do not discard!

Please contact Terralab or your local distributor for instructions on returning the system for

proper disassembly and disposal.

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10. APPENDIX

Figure 19 Process and Instrumentation Diagram

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TERRALAB CONTACT INFORMATION Terralab Laboratuvar Malzemeleri Sanayi ve Ticaret A.Ş.

http://www.terralab.com.tr

e-mail: info@terralab.com.tr

Çetin Emeç Bulvarı 1328.Sokak No:14/9 06460 A.Öveçler/ANKARA

Tel: +90 312 472 73 96

Fax: +90 312 472 73 98

http://www.terralab.com.tr/