TOC-L Series

Quick Reference Guide

Click to begin…
Table of Contents
Instrument Start-up and Shut-down Analysis:
• Instrument Start-Up • Principals of Analysis
• Instrument Shut-Down • Creating a Hardware Configuration
• Creating a Calibration Curve
Software Administration Functions • Creating a Method
• Creating Control Samples
Standards and Reagent Prep • Creating a Schedule
• Creating a Sample Table
• Starting a Sample Run
Periodic Maintenance For TOC • Editing a Sample Table
• Daily Checks • Viewing Sample Results
• Replacing catalyst • Viewing Calibration Curves
• Replacing the Halogen Scrubber • Creating a Sample Report
• Replacing the Syringe / Plunger tip
• Replacing the TC Slide Injection O-rings
• Replacing the IC Slide Injection O-rings (only for TOC-LC*H high
Special Analysis:
• Solid Sample Module (SSM)
sensitivity models)
• Total Nitrogen Module (TNM-L)
• Replacing the Rotor in the 8-port Valve
• Pharmaceutical Water Testing
• Replacing the CO2 scrubber
• Cleaning Validation with the SSM
• Replacing the IC Reaction Vessel Pump Head (only for TOC-LC*H high
sensitivity models)
• Replacing the TC Injection Tubing Troubleshooting Common Issues:
• Instrument Flow Diagrams
• No Peaks
Periodic Maintenance For ASI auto-sampler • High Baseline Position
• Replacing Rinse Pump Head • Poor Reproducibility
• Replacing ASI Sample Needle • Poor Recovery of Control Samples or Check Standards
• High Blank Values
Periodic Maintenance For TNM-L • ERROR: Syringe Pulse Count / Syringe Pump
• ERROR: 8port Valve Pulse Count / 8port Valve Position
• Replacing the detector gasket
• ERROR: TC / IC Slider Position
• Replacing the ozone killing catalyst
• ERROR: ASI Arm Vertical Pulse Count / ASI Arm Vertical Position
• ERROR: ASI Arm Horizontal Pulse Count / ASI Arm Horizontal Position
Periodic Maintenance For SSM • ERROR: ASI Tray Pulse Count / ASI Tray Position
• Removing the Covers • Mechanical Check
• Replacing the Catalyst • Troubleshooting TNM-L issues
• Replacing the O-rings • Troubleshooting SSM Issues 2
Instrument Start-Up
1. Turn on main power switch on
the right hand side of instrument
2. Push power button on the front
3. Turn on carrier gas

3
Instrument Start-Up

Click on the ‘TOC-Control L icon to open the

software

Click ‘Sample Table Editor’

Click the ‘Administration’ to open the TOC Software.
tab to view Software
Administration Functions

Click ‘H/W Settings’ to view or

create a hardware
configuration.

4
Instrument Start-Up

1. Open the TOC sample table editor and open a new sample table
2. Select the correct hardware configuration
3. Press ‘OK’

5
Instrument Start-Up
Press ‘Connect’ to start initializing the instrument

6
Instrument Start-Up

It Takes approximately 30-45 minutes for the instrument to stabilize and come to a ready status.

Push the ‘Monitor’ button to view the instrument status in real time. When all parameters are ok the
instrument is ready to start running samples.

Return to Table of Contents 7

Instrument Shutdown

It is always necessary to follow this procedure to

shutdown the instrument to prevent melting of the
injection block. This procedure shuts the furnace
off and allows the instrument fans to cool the
instrument for thirty minutes before the main power
shuts off.

Return to Table of Contents 8

Software Administration Functions
Select the ‘TOC-Control L’ icon to open the software. Select
‘Administration’ to view the administration settings.

9
Software Administration Functions

‘System Policy’ allows you

to view the policies enacted
when the software was ‘S/W Validation’ allows you
installed to perform software program
validation tests.

10
Software Administration Functions
If audit trail is enabled, log browser allows you to
search the audit trails.

‘Add a Log Event’ allows you

to manually add an event to
the audit trail.

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Software Administration Functions

Shows a list of registered users and is where

Administrators can add or delete user’s. Different
user levels can be assigned different rights within
the software.

12
Software Administration Features
Allows you to customize
LIMS Settings

13
Daily Checks

1. Verify there is enough water for

analysis in the dilution water
bottle. For low level analysis
replace daily
2. Verify there is enough acid for
analysis.
3. Check to make sure the drain
pot is full and fill if necessary.

14
Daily Checks

Check the level of water in the humidifier

Return to Table of Contents 15

Replacing Catalyst

16
Replacing Catalyst

After the combustion tube has been removed the catalyst can be removed and washed or if it is
consumed can be replaced with new. Quartz combustion tubes can be rinsed with DI water and reused
until they break.

17
Replacing Catalyst

18
Replacing Catalyst

19
Replacing Catalyst

20
Replacing Catalyst

TOC-LC*N TOC-LC*H

21
Replacing Catalyst

22
Replacing the Halogen Scrubber

23
Replacing the Syringe / Plunger Tip

24
Replacing the Syringe / Plunger Tip

25
Replacing the Syringe / Plunger Tip

26
Replacing the TC Slide Injection O-rings

Open the lid on the top of the TOC and locate the
TC injector block.

27
Replacing the TC Slide Injection O-rings

28
Replacing the TC Slide Injection O-rings

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Replacing the IC Slide Injection O-rings

Open the front door of the TOC and locate the 1. Remove the thumb screw connecting
sliding IC sample injector the PTFE slider to the motor drive.

2. Pull the PTFE slider forward and out of

the sliding injection block.

30
Replacing the IC Slide Injection O-rings

31
Replacing the Rotor in the 8-port Valve

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Replacing the Rotor in the 8-port Valve

33
Replacing the CO2 Scrubber

Disconnect the flexible tubing from the old CO2 scrubber and dispose of the scrubber per
your local waste disposal regulations. Follow instructions below for installing the new
scrubber.

34
Replacing the IC Vessel Pump Head

35
Replacing the ASI Rinse Pump Head

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Replacing the TC Injection Tubing

The TC injection tubing should be checked and replaced

periodically. This tubing connects from port 7 on the valve
to the slider on top of the injection block. If the tubing looks
pinched or kinked it should be replaced.

When replacing the tubing it is important to make sure it is

installed correctly in the slider and that it is injecting sample
straight down onto the catalyst bed. If the sample injection
sprays outward and hits the side of the combustion tube it
will result in poor reproducibility

37
Replacing the TC Injection Tubing

38
Replacing the TC Injection Tubing

39
Replacing the ASI Needle

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Replacing the Detector Gasket

1. Locate the TNM-L unit mounted to the top of the TOC.

2. Loosen the two screws on the back of the TNM-L that hold the cover on.

3. Lift the cover up and remove.

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 Replacing the Detector Gasket

1. Remove theses four screws and

pull the reactor forward and away
from the detector

2. Remove the old gasket and

replace with new making sure the
flat side is facing the detector
window

3. Clean the detector window with a

Kim Wipe and some alcohol

4. Reconnect the reactor to the

detector and replace the TNM-L
cover

42
Replacing the Ozone Killing Catalyst

43
Replacing the Ozone Killing Catalyst

44
Replacing the Ozone Killing Catalyst

45
Removing the Covers

Section 1 / 2 46
Removing the Covers
Remove the screws and carefully
remove the rear cover first.

CAUTION

Be careful as there is a wire harness connected to a fan

on the left hand side of the cover that needs to be
unclipped before the cover can be completely removed.

Next Remove the front cover:

• Move the sample pushrod knob to the

‘Measuring’ position
• With the sample port cover closed, slightly lift
the rear of the front cover, pull it forward about
8cm and lift off.

Section 2 / 2 47
Replacing the Catalyst

The following procedure describes

removal of the TC combustion
tube. This same procedure can
also be used to remove the IC
combustion tube. The only
difference is the IC combustion
tube is an empty quartz tube while
the TC combustion tube is filled
with catalyst.

Section 1 / 7 48
Replacing the Catalyst

1. Locate where the

combustion tube comes out
the back of the TC Furnace

2. Find the stainless steel

elbow fitting that connects
the combustion tube to the
glass shaped ‘L’ tube

3. Loosen the fitting on the side

of the combustion tube and
remove the fitting.

Section 2 / 7 49
Replacing the Catalyst

Unscrew the metal ring to

disconnect the sample port from
the quartz combustion tube

Section 3 / 7 50
Replacing the Catalyst

1. Loosen the four thumbscrews on

the sides of the sampling port

2. Remove the blue air line from the

left hand side of the sampling
port. To do this, push the blue
collar of the fitting toward the
sampling port while at the same
time pulling the blue tubing away
from the sampling port.

3. Loosen the two screws toward

the front that holds the push rod
to the frame.

Section 4 / 7 51
Replacing the Catalyst
1. Remove the sampling port

2. Remove the combustion tube by carefully

pulling the combustion tube forward until it
is completely out of the furnace.

CAUTION

Make sure to pull the combustion straight

forward until it is completely out of the furnace
otherwise you risk breaking the end of the
combustion tube.

Section 5 / 7 52
Replacing the Catalyst

Section 6 / 7 53
Replacing the Catalyst

Place the white PTFE o-ring around the

newly packed combustion tube. Then
place the metal sample port adapter around
the combustion tube.

Follow the instruction in reverse order to

install the combustion tube into the furnace
and attach the sample port to the
combustion tube.

CAUTION

When tightening the metal sample port

adapter to the new combustion tube only
hand tighten. Over tightening could cause
the combustion tube to break upon heating
the tube as the quartz expands.

Section 7 / 7 54
Replacing the O-rings

Remove the combustion tube and

sample port following the instructions
for replacing the catalyst.

Replace the white PTFE o-ring that is

around the combustion tube.

Replace the black viton o-ring the fits

on the end of the sample port and seals
to the combustion tube.

Section 1 / 3 55
Replacing the O-rings

Loosen the blue knob for TC or green knob for

IC and slide the sample port cover to the right.
Remove the old o-ring and replace with new.

Section 2 / 3 56
Replacing the O-rings

Section 3 / 3 57
Creating a Hardware Configuration

58
Creating a Hardware Configuration

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Creating a Hardware Configuration

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Creating a Hardware Configuration

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Creating a Calibration Curve
1. Push the calibration curve list button
2. Push the ‘New’ button
3. Select the correct hardware configuration

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Creating a Calibration Curve

Select the curve type

1. Select ‘Normal’ to create a curve with individually

prepped standard solutions.

2. Select ‘Use dilution from standard solution’ to

create a curve where the instrument will auto-
dilute a high standard to create a multi-point
calibration curve.

3. Select ‘USP/EP Support’ to create a curve using

the USP criteria.

4. Select ‘JP Support’ to create a curve using the

JP criteria.

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Creating a Calibration Curve

1. Select the type of analysis from the

drop down tab

2. Select ‘Zero Shift’ to shift the curve

down through the origin

3. Select ‘Multiple Injections’ to

perform multiple sample injection
from one syringe full of sample.

4. Give the curve a unique name

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Creating a Calibration Curve

Select the parameters for the

calibration curve.

Please note that in this example the

measurement type is NPOC so there
is an option for selecting a sparge
time and acid addition. When
performing TC analysis there will be
no option for selecting a sparge time.

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Creating a Calibration Curve

Creating a curve using the auto-

dilution function

1. Select ‘Add’ to add a new point

2. Insert here the concentration of the high

standard being used in the curve.

3. Insert here the actual concentration of the

standard point.

4. The dilution rate will automatically populate

here

5. The injection volume will be displayed

here. The software will automatically
select the most appropriate injection
volume based upon the concentrations of
points in the curve.
66
Creating a Calibration Curve

Creating a curve using individually

prepped standards for each point

1. Select ‘Add’ to add a new point.

2. Insert here the concentration of the standard

point.

3. The injection volume will be displayed here.

The software will automatically select the
most appropriate injection volume based
upon the concentrations of points in the
curve.

67
Creating a Calibration Curve

1. If integrations times need to be

adjusted parameters can be changed
here. Default settings a OK for 99% of
analysis.

2. A pass/fail criteria can be set here to

determine if a curve is OK based on a
desired correlation coefficient.

3. Push ‘Finish’ to save the curve.

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Creating a Method

1. Push the ‘Method’ button to show the 3. Select the correct hardware
list of saved methods. configuration.
2. Push the ‘New’ button. 4. Select ‘Next’

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Creating a Method

1. Select the type of measurement to be

performed. Note that multiple
measurements can be selected in a
method. In this example we will select
TOC which will prompt the instrument
to perform both TC and IC
measurement and then calculate TOC
by the difference in TC and IC
measurements. TOC = TC – IC.

2. Give the method a unique name.

3. Select ‘Next’.

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Creating a Method

1. Push the ‘…’ button to select the curve for TC analysis.

2. Select the TC curve to be used for analysis.

3. Push ‘Open’ to select the curve and insert in ‘Calibration Curve 1’

4. Push ‘Next’

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Creating a Method

Confirm the conditions for the TC analysis.

Note that these conditions were pulled in
from the calibration curve selected but can
be changed if needed.

Check the box next to ‘Correction of inj.

Vol’ or ‘Correction of dilution’ if you wish to
have the instrument auto-dilute or lower
injection volume for sample that are over
the range of the calibration curve.

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Creating a Method

Confirm the peak time parameters for

the TC analysis.

Note that defaults settings are OK for

99% of analysis.

Select ‘Next’ to move on and set the

parameters for the IC measurement.

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Creating a Method

1. Push the ‘…’ button to select the curve for IC analysis.

2. Select the IC curve to be used for analysis.

3. Push ‘Open’ to select the curve and insert in ‘Calibration Curve 1’

4. Push ‘Next’

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Creating a Method

Confirm the conditions for the IC

analysis. Note that these conditions
were pulled in from the calibration
curve selected but can be changed
if needed.

Check the box next to ‘Correction of

inj. Vol’ or ‘Correction of dilution’ if
you wish to have the instrument
auto-dilute or lower injection volume
for sample that are over the range of
the calibration curve.

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Creating a Method

Confirm the peak time parameters

for the IC analysis.

Note that the default parameters

are OK for 99% of analysis.

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Creating a Method

1. If this method is pharmaceutical testing select the appropriate test otherwise

select ‘None’

2. Push ‘Finish’ to save the method to the list of Methods.

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Creating Control Samples
1. Push the ‘Control Samples’ button to show the list of control samples
2. Push the ‘New’ button to create a new control sample
3. Select the correct hardware configuration from the drop down list
4. Press ‘Next’

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Creating Control Samples

1. Select ‘Control Sample’

2. Give the control sample a unique

name

3. Press ‘Next’

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Creating Control Samples

1. A control sample can be analyzed using either a

method file or calibration curve file. In This
example a calibration curve file will be used
2. Push the ‘…’ button to open the list of calibration
curves
3. Select the calibration curve to be used

4. Push ‘Open’ to select the calibration curve

5. Push ‘Next’

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Creating Control Samples

1. Confirm that the conditions on this

page are correct.

2. Give the control sample a unique

default sample name which will
appear when the control sample is
inserted into a sample table.

3. If there is a manual dilution being

performed on the samples select the
appropriate dilution rate.

4. Press ‘Next’

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Creating Control Samples

Confirm the condition for analysis.

note: the parameters that appear on

this page are the ones selected in the
calibration curve or method file being
used.

Press ‘Next’

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Creating Control Samples

Confirm the Peak Time Parameters

Note: the default parameters will be

OK for 99% of analysis.

Press ‘Next’

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Creating Control Samples

Control samples can be set-up many different ways

1. Percent recovery of the control sample or percent

recovery of a spiked sample
2. Mean value of the measured concentration of the
control sample
3. Blind value area counts of the measured control
sample
4. Spanwidth of the measured control sample
concentration

5. This is where the accepted criteria is entered for each

control checking type
6. This is where you have the option to ignore the zero
shift of the calibration curve when calculating the
controls. This should be selected if the control sample
is prepped in the same water as the calibration curve
standards. If the control sample is prepped in different
water than the calibration curve standards then do not
check this box
7. This is where you can select actions to be performed
upon the failure of a control sample
84
Creating Control Samples

Recovery %

Select this control checking type to calclulate the % recovery a

control sample or check ‘Spiked’ to calculate the % recovery of
the amount spiked into sample.

Enter the correct concentration of the control sample or the

amount spiked into the sample.

Enter the correct acceptance criteria for the analysis. In the

top example, a control sample that is measured between 90%-
110% of 5 ppm would pass. In the bottom example, a recovery
of 85%-115% of the 1 ppm spiked into the sample would pass.

Note: when ‘Spiked’ is selected when you insert the control into
the sample table, two lines in the table will be entered. The
first line is for the un-spiked sample and the second line is for
the spiked sample. The result of the sample spike is calculated
as the difference between these two values.

85
Creating Control Samples

Mean Value Concentration

Select this control checking type to

determine a passing control sample using a
measured concentration.

In this example, a 5 ppm control is used and

the acceptance criteria is a measured
concentration between 4 an 6 ppm.

86
Creating Control Samples

Blind Value of Area

Select this control checking type to

calculate the control sample based on area
count response of the sample.

In this example the acceptance criteria for

the control sample is an area count
response between 25 and 35 area counts.

87
Creating Control Samples

Spanwidth of Control Concentration

Use this control checking type to calculate

the control sample based on the maximum
deviation of replicate injections.

In this example the acceptance criteria is

replicate control sample injections that do
not deviate between 5%.

88
Creating Control Samples

Selecting actions for control failures

Select the desired actions for first time failure of a control

sample.

If applicable based on the action selected for the first failed

control sample, select the actions for a second failure of the
control sample.

89
Creating Control Samples

Select ‘Finish’ to save the control sample template to the list of control
samples.

90
Creating a Schedule

1. Push the ‘Schedule’

button to show the list
of saved schedules.

2. Push the ‘New’ button

to create a new
schedule.

3. Use the drop down list

to select the correct
hardware
configuration

91
Creating a Schedule

92
Creating a Schedule

1. To save the schedule, push

‘Save’.

2. Give the file a unique name.

3. Push ‘Save’

93
Creating a Schedule
A schedule file can then be inserted into a sample table. Schedule files are useful for labs where the
same samples are run often.

94
Creating a Sample Table
1. Push the ‘Sample Table’ button to show the list of saved sample tables.
2. Push the ‘New’ button to open a new table
3. Select the correct hardware configuration from the drop down list
4. Press ‘OK’

95
Creating a Sample Table

Push the ‘Calibration Curve’ button to display the saved calibration curves and drag
and drop the desired Calibration curve into the sample table

96
Creating a Sample Table

Highlight the next row in the table and right click on the mouse. From the drop
down list select ‘Insert – Sample’

97
Creating a Sample Table

1. Select to either run your sample using a method or a

calibration curve.
2. Push the ‘…’ button to open the list of methods or
calibration curves.
3. Select the desired method or calibration curve.

4. Push ‘Open’

5. Push ‘Next’

98
Creating a Sample Table

1. Give the sample a name

2. Give the sample an ID

3. If there was a manual dilution

performed to the sample prior to
running it on the TOC enter that
factor here.

4. If you wish to perform the sample

measurement more than once and
then average those results together,
enter that number here.

5. Press ‘Next’.

99
Creating a Sample Table

make sure the correct calibration curve is listed in

‘Calibration Curve 1’. Additional calibration curves can
be added to positions 2 or 3 if desired.

100
Creating a Sample Table

Confirm that conditions in this window are

correct.

Parameters in this window are pulled in

from either the calibration curve or
method file selected.

It is possible to have the instrument

correct for samples over the range of the
calibration curve. Select ‘Correction of
inj. Vol’ to have the instrument lower the
injection volume for over range samples
or ‘Correction of dilution’ to have the
instrument auto-dilute over range
samples.

101
Creating a Sample Table

Confirm the Peak Time Parameters

Note: the default parameters will be

OK for 99% of analysis.

Press ‘Next’

102
Creating a Sample Table

If the sample entered is following

pharmaceutical water testing
guidelines select the appropriate
protocol to follow. For all other
analysis check ‘None’

Press ‘Finish’ to save the sample to

the sample table.

103
Creating a Sample Table

The sample should now appear in the table.

104
Creating a Sample Table
Add as many sample to the table as needed. Note that multiple samples can be added to
the table at once by selecting ‘Insert-Multiple Samples’

105
Creating a Sample Table

Push the ‘Control Sample’ button to show the list of saved control samples.

Drag and drop the appropriate control sample into the sample table.

106
Creating a Sample Table

When finished entering all curves, samples, and

control standards are into the sample table,
push the “Birthday Cake” button.

1. Enter the correct the vial position on the

auto-sampler tray for each sample. You
can manually enter each number or double
click on the position in the diagram.
2. Use this to measure a sample ‘Off-Line’.
This refers to using the port 1 sampling line
for measurement instead of the auto-
sampler which is connected to port 2 of the
valve. Selecting ‘Off-Line’ will enter the vial
position as ‘0’. This can be useful for
samples like controls that may be run
multiple times throughout a run.
3. Press ‘OK’

107
Creating a Sample Table

1. Press the ‘Save’ button to save

the sample table.

2. By default the file name will be

entered with date and time
stamp but it can be changed to
another unique name.

3. Press ‘Save’ to save it to the list

of sample tables.

108
Starting a Sample Run

Open an existing sample table or create a new sample table.

Then press ‘Connect’ to establish a connection with the instrument.

109
Starting a Sample Run

1. Wait until the green

‘Ready’ status is displayed
in the top right corner.

2. Press ‘Start’. If you are

using the ASI auto-sampler
the window below will
appear.

3. Select the action to be performed upon completion of the sample

table. ‘Sleep’ function allows the user to put the instrument into a
sleep mode. A date and time can then be entered to wake the
instrument.

4. Push ‘Start’

110
Starting a Sample Run

When NOT using the ASI Auto-

sampler the window below will
appear when ‘Start’ is pushed.

111
Editing a Sample Table

112
Viewing Sample Results

Sample results can be found in the ‘Result’ column of the sample table. Note that samples that are
using a Method with multiple analysis types show results for all measurements in the ‘Result’ column.

To view more detailed information for each sample push

113
Viewing Sample Results

114
Viewing Sample Results

115
Viewing Sample Results

116
Viewing Sample Results

117
Viewing Sample Results

118
Viewing Sample Results

119
Viewing Calibration Curves

The TOC-L software will create two different types of calibration curve files.

1. Calibration curve template files. (calibration curve.cal)

• These files contain the calibration curve parameters
• They DO NOT contain any data
• Are NOT saved with a date and time stamp.

2. Calibration curve data files. (calibration curve.cal.date.time)

• These files contain the calibration curve parameters
• They DO contain data and resultant curves
• When a calibration curve template file is inserted into a sample table and ran, the software will save
a calibration curve file with a date and time stamp from when the curve was created.

It is important to understand this difference as it is designed as a simple way to ensure

that the most current calibration curve data file is being used to calculate results. The
calibration curve template file can be used to run samples or can be entered into a
method file. When the instrument runs the samples, the software will look for a
calibration curve data file of the same name and use the most current one to calculate
results.

120
Viewing Calibration Curves

To view a calibration curve template

file:

1. Press the ‘Cal….’ button to show

the list of saved curves.

2. Double click the mouse on the

desired curve to open the
‘Calibration Curve Properties
Window’

3. Use the tabs across the top of the

window to view the calibration
curve parameters.

NOTE: there is no data saved in this

file.

121
Viewing Calibration Curves

To open a calibration curve data file:

1. Press the ‘Cal…’ button to show

the list of saved calibration
curves.

2. Scroll to the bottom of the list and

use the ‘+’ button to expand the
list to see all files.

OR

3. Push ‘Open’

4. Use the drop down tab for ‘Files

of Type’ to select ‘All Cal. Curve
Files’

122
Viewing Calibration Curves

The calibration curve properties will now be

opened.

Use the tabs across the top to view the curve

parameters.

NOTE: there will be data in these files that

can be viewed.

123
Creating a Sample Report

There are two different ways to print sample reports.

The sample table can be printed. It will appear in the

report exactly as it does on the screen in the software.

A customized report can be created and printed. The

entire report can be printed or certain samples in the
table can be highlighted to only print those samples.

124
Creating a Sample Report
To customize a report select ‘File’ then ‘Page Setup’. In the page setup window select the items to be
displayed in the report.

125
Creating a Sample Report

126
Solid Sample Module Analysis

Section 1 / 8 127
Solid Sample Module Analysis

Section 2 / 8 128
Solid Sample Module Analysis

Section 3 / 8 129
Solid Sample Module Analysis

Section 4 / 8 130
Solid Sample Module Analysis

Section 5 / 8 131
Solid Sample Module Analysis
Once a calibration curve for solid samples has been
created, samples can be entered into the sample
table just like for liquid samples.

See Creating a Sample Table

Note that sample amount can either be entered by

weight or by volume.

Section 6 / 8 132
Solid Sample Module Analysis

Samples are then weighed or pipetted into the ceramic sample

boats. The ceramic boats are then placed on the sample boat
holder in the sampl
sample ports in preparation for measurement

After sealing the sample boat into the sample port chamber you need
to wait 3-5 minutes before starting analysis. This is the time it takes
for the air trapped in the system to work through the detector. Failure
to do so will result in false peaks from the CO2 in the air
compromising measurement of the sample.

Section 7 / 8 133
Solid Sample Module Analysis

Section 8 / 8 134
Total Nitrogen Module (TNM-L)

With the optional TNM-L total nitrogen module, the analysis of the
total nitrogen in a sample can be performed. Please note that it can
only measure TOTAL nitrogen and cannot speciate out the different
forms of nitrogen present.

It is possible to perform carbon and nitrogen measurements

simultaneously with one sample injection

135
Total Nitrogen Module (TNM-L)

136
Total Nitrogen Module (TNM-L)

To create a calibration curve for total nitrogen

analysis follow the instructions for creating a
calibration curve. On page 3 of the calibration
curve window make sure to select ‘TN’ form the
drop down tab for ‘Analysis’.

137
Total Nitrogen Module (TNM-L)

To measure carbon and nitrogen

simultaneously, a method will need to be
created. Follow the directions for creating a
method and on page2 of the Method Wizard,
use the drop down tab for ‘Analysis’ to select
either ‘TC/TN’ or ‘NPOC/TN’. Follow the
wizard and on the next pages select the
correct calibration curves and properties for
carbon analysis and nitrogen analysis.

138
Total Nitrogen Module (TNM-L)

When samples are measured using a method for both carbon and nitrogen, the instrument will
perform one injection and measure both carbon and nitrogen simultaneously. Results for both
analysis will be displayed in the ‘Result’ of the Sample Table.

139
Total Nitrogen Module (TNM-L)

To view detailed information for each analysis use the

tabs at the bottom of the sample window.

140
Pharmaceutical Water Testing

141
Pharmaceutical Water Testing

142
Pharmaceutical Water Testing

143
Pharmaceutical Water Testing

144
Pharmaceutical Water Testing

145
Pharmaceutical Water Testing

146
Pharmaceutical Water Testing

147
Pharmaceutical Water Testing

148
Pharmaceutical Water Testing

149
Pharmaceutical Water Testing

150
Pharmaceutical Water Testing

151
Pharmaceutical Water Testing

152
Pharmaceutical Water Testing

153
Pharmaceutical Water Testing

154
Pharmaceutical Water Testing

155
Pharmaceutical Water Testing

156
Pharmaceutical Water Testing

157
Pharmaceutical Water Testing

158
Cleaning Validation with the SSM

159
Cleaning Validation with the SSM

160
No Peaks

Probably the most common issue with the TOC-L is when user’s see no peaks
during analysis or no instrument response. This problem it almost always
caused by one of two things:

1. No sample being injected into the combustion tube

2. A Leak of carrier gas somewhere inside the instrument causing no sample

to be carried to the detector.

161
No Peaks

To check to make sure sample is being injected into the combustion tube, start a sample analysis and open the
front door of the TOC and watch what the instrument does.

Watch the 8-port valve and the syringe to make sure the instrument is pulling in sample and then injecting it into
the combustion tube via port-7 of the 8-port valve. You can tell which port the valve is on by watching the “O”
mark on the valve. Whichever port the “O” lines up with is the port it is currently on.

Open the lid on top and locate the top of the combustion tube that
sticks up out of the furnace. Make sure that when the slider moves
forward over the combustion tube you see sample being injected into
the combustion tube. If no sample is being pulled up and injected into
the combustion tube:

1. Check the auto-sampler tubing and make sure it is not clogged or

pinched
2. Replace the ASI auto-sampler needle if it is clogged
3. Check the 8-port valve and if necessary replace the 8-port valve
rotor.
4. Check the syringe and if needed replace the syringe, and/or
plunger tip.

162
No Peaks

To perform a leak check, pinch the “L” tubing going to the CO2 scrubber blocking any flow of gas that may be going
through that tube. While pinching the tube, check for bubbling in the drain pot on the left hand side of the instrument.

If there is NO bubbling in the drain pot then there is a gross leak of carrier gas somewhere in the system. If
there IS bubbling in the drain pot then there is no leak of carrier gas in the system.

163
No Peaks

The most common spots for leaks of carrier gas are in or around the combustion
tube. If it is determined there is a leak of carrier gas:
1. shut off the furnace and allow it to cool before proceeding.

1. Remove the combustion tube and check to make sure it is not cracked or broken and replace if necessary.

2. Replace the o-rings in the TC Injection block.

164
High Baseline Position

A high baseline is any baseline position above 200 mV. When the baseline is above 200 mV the instrument will give a
‘NOT READY’ status and will not allow a run to be started. At this point action needs to be taken to lower the baseline
below 200 mV. There are several things that can cause a high baseline including:

1. A leak of carrier gas. The TOC measures CO2 so if there is a leak of carrier gas, no clean gas is flowing through the
detector so it becomes filled with ambient air. The instrument will then measure the CO2 in ambient air resulting
in a high baseline position.

2. A dirty detector cell. The detector cell is gold lined for maximum transmission of light to the detector. Over time
the gold lining can become dirty, corroded, or even scratched, leading to a high baseline. In this scenario the
baseline will usually creep up over time and when it gets to 200 mV, will no longer give the ‘READY’ status. Please
contact Shimadzu for technical assistance.

3. Contaminated carrier gas. Carrier gas that contains high levels of CO2 or other hydrocarbons can lead to a high
baseline. If using compressed cylinders, it is possible to get the occasional bad cylinder of air. If using a TOC gas
generator, check the filters and scrubbers on the generator and replace if necessary.

4. A faulty detector or light source. This is the least common scenario as the detector and light source are quite
robust typically lasting for ten years or more. This scenario usually results in a baseline being so high or so low
that it cannot even be seen on the background monitor page. Please contact Shimadzu for technical assistance.

165
Poor Reproducibility

It is common in TOC analysis to perform multiple injections for each sample and then average those results together
for the final result. Replicate injections should have low CV (RSD) values, and low SD values. When these values
become large, action should be taken.

166
Poor Reproducibility

There are many things that can cause poor reproducibility including:
1. A worn out syringe and/or plunger tip

2. Clogged or leaking 8-port valve/rotor

3. Clogged or kinked injection line (port 7 tubing)

4. Worn out or leaking o-rings

5. Cracked or broken combustion tube

6. Poor injection into the combustion tube

167
Poor Recovery of Control Samples / Check Standards

Low Recovery of Control Samples or Check Standards could be caused by:

1. Bad or consumed catalyst. Remove the combustion tube and replace the catalyst.

2. Clogged ASI needle or ASI tubing. Check the needle and tubing and replace if necessary.

3. Worn out syringe or syringe plunger tip. Check and replace if necessary.

4. A leak of carrier gas. Check for a leak of carrier gas.

5. Worn out o-rings. Check and replace o-rings as needed.

6. Improperly prepped Calibration Standards. Check the calibration standards and re-prep if necessary.
Then re-run the calibration curve.

168
Poor Recovery of Control Samples / Check Standards

High recovery of Control Samples or Check Standards is much less common than low recovery however
High recovery could be caused by:

1. Instrument contamination. If instrument contamination is suspected, remove and clean these parts:
⚫ The ASI needle
⚫ The syringe
⚫ The 8-port valve rotor
⚫ The combustion tube
⚫ The TC injection tubing

2. Instrument Carry-over. If Carry-over between sample is suspected, increase the number of washes
and/or ASI needle rinses.

3. Improperly prepped Calibration Standards. Check the calibration standards and re-prep if necessary.
Then re-run the calibration curve.

169
High Blank Values

High blank values can be caused by many things, including:

1. Contamination in the instrument. If instrument contamination is suspected, remove and clean these
parts:
⚫ The ASI needle
⚫ The syringe
⚫ The 8-port valve rotor
⚫ The combustion tube
⚫ The TC injection tubing

2. Contaminated DI water. Replace the dilution water bottle and ASI rinse bottle with freshly collected
DI water.

3. Contaminated acid. Replace the acid with a new or freshly prepped acid.

4. Not enough ASI needle rinses or syringe /flow line washes. Click to the next pages for instructions on
where to increase these values.

170
High Blank Values

In the TOC-L software, ‘Washes’ refers to the number of times the instrument washes the syringe, valve, and flow lines with
SAMPLE prior to analysis. These values can be changed by opening either an existing calibration curve file or method file.

171
High Blank Values

In the Hardware Settings, the number of times the auto-sampler rinses the needle with DI
rinse water can be set. Increase this value for really dirty samples or if needle contamination
and carryover is suspected.

1. Open the list of saved sample

tables.

2. Expand the list of Hardware (H/W)

Settings and select the desired
configuration.

3. Select the ‘ASI’ tab to view the

auto-sampler settings.

4. Change the number of needle

washes to the desired amount.

172
ERROR: Syringe Pulse Count / Syringe Pump

Either of these error messages signifies an issue with the syringe

pump drive in the TOC.

1. Restart the instrument.

2. During the Instrument ‘Initialization’ open the front door and

watch what the syringe drive does.
▪ If the syringe never moves up or down and the same error
message is generated again, it is usually due to a faulty
syringe pump motor. Replace the motor.
▪ If the syringe moves up and down a few times and then
gives the same error message, it is usually due to a faulty
photo-sensor. Replace the photo-sensor.

3. Contact Shimadzu Tech Support for current part numbers and

prices for the motor an sensor.

173
ERROR: 8port Valve Pulse Count / 8port Valve Position

Either of these error messages signifies an issue with the 8-port Valve
drive in the TOC.

1. Restart the instrument.

2. During the Instrument ‘Initialization’ open the front door and

watch what the 8-port valve does.
▪ If the valve never rotates and the same error message is
generated again, it is usually due to a faulty 8-port valve
motor. Replace the motor.
▪ If the valve rotates a few times and then gives the same error
message, it is usually due to a faulty photo-sensor. Replace
the photo-sensor

3. Contact Shimadzu Tech Support for current part numbers and

prices for the motor an sensor.

174
ERROR: TC / IC Slider Position

Either of these error messages signifies an issue with

the TC or IC slider drive mechanism.

1. Restart the instrument.

2. During the Instrument ‘Initialization’ open the

front door and watch what the slider does.
▪ If the slider never moves forward or backward
and the same error message is generated
again, it is usually due to a faulty slider motor.
Replace the motor.
▪ If the slider moves forward and backward a
few times and then gives the same error
message, it is usually due to a faulty photo-
sensor. Replace the sensor.

3. Contact Shimadzu Tech Support for current part

numbers and prices for the motor an sensor.

175
ERROR: ASI Arm Vertical Pulse Count / ASI Arm Vertical
Position

Either of these error messages signifies an issue with the ASI arm in the auto-sampler in relation to the up
and down movement.

1. Restart the instrument

2. Start an analysis and watch the ASI auto-sampler arm.

▪ If the arm never moves up or down and the same error message is generated again, it is usually
due to a faulty ASI motor.
▪ If the arm moves up and down a few times and then gives the same error message, it is usually due
to a faulty photo-sensor.

3. Contact Shimadzu Service. Removing the covers to get down to the motor drives in the ASI is difficult
and requires a trained Shimadzu Service Engineer.

176
ERROR: ASI Arm Horizontal Pulse Count / ASI Arm
Horizontal Position

Either of these error messages signifies an issue with the ASI arm in the auto-sampler in relation to the forward and
backward movement.

1. Restart the instrument

2. Start an analysis and watch the ASI auto-sampler arm.

▪ If the arm never moves forward or backward and the same error message is generated again, it is usually
due to a faulty ASI motor.
▪ If the arm moves forward and backward a few times and then gives the same error message, it is usually due
to a faulty photo-sensor.

3. Contact Shimadzu Service. Removing the covers to get down to the motor drives in the ASI is difficult and
requires a trained Shimadzu Service Engineer.

177
ERROR: ASI Tray Pulse Count / ASI Tray Position

Either of these error messages signifies an issue with the sample tray in the auto-sampler.

1. Restart the instrument

2. Start an analysis and watch the ASI auto-sampler tray.

▪ If the tray never rotates and the same error message is generated again, it is usually due to a faulty ASI
motor.
▪ If the rotates around a few times and then gives the same error message, it is usually due to a faulty photo-
sensor.

3. Contact Shimadzu Service. Removing the covers to get down to the motor drives in the ASI is difficult and
requires a trained Shimadzu Service Engineer.

178
Mechanical Check
Mechanical check allows users to check all the mechanical functions of the TOC-L. It can be very useful
for troubleshooting and diagnosing mechanical issues. To access the mechanical check, select
‘Instrument’ > ‘Maintenance’ > ‘Mechanical Check’.

179
Mechanical Check

180
Mechanical Check

181
Troubleshooting TNM-L Issues

Section 1 / 5 182
Troubleshooting TNM-L Issues

Section 2 / 5 183
Troubleshooting TNM-L Issues

⚫ The TNM-L is downstream of the TOC-L. Sample passes through the TOC-L where carbon Is measured and then enters the TNM-
L where nitrogen is measured.

⚫ When troubles arise with nitrogen measurement such as no peaks or poor reproducibility it is first a good idea to check the
carbon measurement.

⚫ If carbon measurement is normal and looks good then the issue with the TNM-L measurement lies within the TNM-L so
troubleshoot the TNM-L

⚫ If carbon measurement is not good then the issue with TNM-L measurement is likely a result of something within the TOC-L
so troubleshoot the TOC-L

Section 3 / 5 184
Troubleshooting TNM-L Issues

⚫ No peaks during for nitrogen

⚫ Make sure air is being supplied to the TNM-L unit at 200 kPa

⚫ Make sure there is no leak of gas within the TNM-L

⚫ Check the hours on the Ozone Generator. The ozone generator does have a lifespan and if no ozone is being generated then
there will be no peaks for nitrogen measurement. Replacement of ozone generator is performed by Shimadzu Service
Engineer. Please contact your local Shimadzu Office.

Section 4 / 5 185
Troubleshooting TNM-L Issues

⚫ Poor reproducibility for nitrogen measurement

⚫ Check for a leak of carrier gas within the TNM-L unit

⚫ Check black tubing that connects the detector of the TOC-L to the reactor on the TNM-L and make sure the connection is
good at the TNM-L reactor.

⚫ Pull apart the TNM-L reactor assembly and inspect and/or replace the detector gasket.

⚫ See Replacing the TNM-L Detector Gasket

Section 5 / 5 186
Troubleshooting SSM Issues

Section 1 / 2 187
Troubleshooting SSM Issues

Section 2 / 2 188
Principles of Analysis

Section 1 / 4 189
Principles of Analysis

Section 2 / 4 190
Principles of Analysis

Section 3 / 4 191
Principles of Analysis

Section 4 / 4 192
TOC-LC*H

Section 1 / 4 193
TOC-LC*H + TNM-L + Ext. Sparge Kit

Section 2 / 4 194
TOC-LC*N

Section 3 / 4 195
TOC-LC*N + TNM-L + Ext. Sparge Kit

Section 4 / 4 196
Preparation of Standard Solutions

Section 1 / 8 197
Storage of Standards

Section 2 / 8 198
TC/NPOC Standard Prep

Section 3 / 8 199
IC Standard Prep

Section 4 / 8 200
TN Standard Prep

Section 5 / 8 201
TC/TN Mixed Standard Prep

Section 6 / 8 202
Hydrochloric Acid Solution

Section 7 / 8 203
IC Reagent (Phosphoric Acid Solution)

Only for TOC-LC*H High sensitivity model Instruments

Section 8 / 8 204