Total Organic

Carbon (TOC)
Analysis
Technique
Comparison
A Practical Guide
Rev: A, Sept - 2021
Copyright
Copyright © 2021 Teledyne Technologies Incorporated

All rights reserved. Reproduction, adaptation, or translation without permission is prohibited, except as allowed under copyright
laws. Printed in the U.S.A.

Updated Information
The information contained in this document is subject to change without notice. This document may be translated into languages
other than English. If the accuracy of any information is in doubt, always refer to the English version and/or contact Teledyne
Tekmar for clarity.

Trademarks
The companies indicated own the following trademarks:

Tekmar .......................................... Teledyne Instruments, Inc.

All other brands or product names are trademarks or registered trademarks of their respective owners.

Contact Information
Teledyne Tekmar
4736 Socialville Foster Road
Mason, OH 45040 U.S.A
www.teledynetekmar.com

Toll Free: 800-543-4461

Sales/Support: 800-874-2004
Main: 513-229-7000
Fax: 513-229-7050

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Table of Contents

About This Guide ...................................................................................................................... 1

TOC Analysis Overview............................................................................................................ 1
The History of TOC ................................................................................................................... 2
TOC Measurement Overview ................................................................................................... 2
TOC Definitions......................................................................................................................... 2
Oxidation Techniques For TOC ............................................................................................... 3
Catalytic Combustion ..........................................................................................................................................3
UV/Persulfate ......................................................................................................................................................3
Gas Flow Control Systems for TOC ........................................................................................ 3
Non-Dispersive Infrared (NDIR) Detection For TOC .............................................................. 4
Flow-Through NDIR Design ................................................................................................................................4
Static Pressure Concentration (SPC) NDIR Design............................................................................................4
NDIR Limitations .................................................................................................................................................5
Other Detection Methods For TOC.......................................................................................... 6
Conductivity.........................................................................................................................................................6
Membrane Conductivity ......................................................................................................................................6
Summary.................................................................................................................................... 6
About Teledyne Tekmar ........................................................................................................... 6
Fusion UV/Persulfate TOC Analyzer ....................................................................................... 7
Torch Catalytic Combustion TOC Analyzer ........................................................................... 7
Lotix Catalytic Combustion TOC Analyzer............................................................................. 8
Contact Us ................................................................................................................................. 8
References................................................................................................................................. 9

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 Total Organic Carbon (TOC) Analysis Technique Comparison

Total Organic Carbon (TOC) Analysis Technique

Comparison
ABOUT THIS GUIDE
This guide was designed to explain a variety of current TOC analysis technologies and assist in the selection of an
analyzer, according to sample type and application.

TOC ANALYSIS OVERVIEW

Total Organic Carbon (TOC) is a non-specific indicator of water
cleanliness and purity that grew from analysis of wastewater and
municipal water for organic matter. The need to protect water
quality and establish criteria for screening and measuring
contaminant levels was officially recognized when Congress
enacted the Resource Conservation and Recovery Act (RCRA) in
1976. This act required operators of waste disposal sites to
monitor their groundwater for organic carbon levels and organic
halide levels.1
Today, TOC analysis is used effectively in a variety of applications
including drinking water, wastewater and soils and is employed in
numerous fields and laboratories including:
 Environmental
 Contract Laboratories
 Municipalities
 Pharmaceutical
 Universities
 Petrochemical
Because TOC analysis is considered an effective indicator of organic contamination in drinking water, it can be used as a
quality control (QC) measure for water purification/disinfection. When high-organic content water is subjected to the
disinfection process during normal purification, carcinogenic by-products are created. Consequently, it is important to
ensure TOC levels are low in water entering and leaving water treatment facilities to ensure public safety.
For similar analytical reasons, TOC analysis has found wide acceptance in the biotechnology/pharmaceutical industry.
The United States Pharmacopoeia (USP), European Pharmacopoeia (EP) and Japanese Pharmacopoeia (JP) all mandate
TOC analysis as a required test. Specifically, United States Pharmacopoeia (USP) Method <643> Bulk and Sterile Water
Carbon Concentrations provides guidelines and requirements for Total Organic Carbon (TOC) analysis of water for
injection (WFI) and purified water (PW).
TOC analysis is also useful for pharmaceutical cleaning validation (CV) and clean in place (CIP) procedures. To ensure
public safety, TOC concentration levels are used to verify the success of manufacturing cleaning procedures and prevent
cross-contamination.

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 Total Organic Carbon (TOC) Analysis Technique Comparison

THE HISTORY OF TOC

The study of total organic carbon (TOC) has existed for hundreds of years, and continues to
be improved and refined. Carbon analysis began in the 1630s with Jan Baptist Van Helmont’s
discovery that as wood is burned, carbon dioxide is emitted.2 In 1756, Joseph Black also
identified carbon dioxide by observing the loss of mass of samples after heating. From this
difference in mass, the amount of carbon could be determined.3
In 1948 the infrared gas analyzer was invented by American Cyanamid, leading ultimately to
the use of the non-dispersive infrared (NDIR) detector for TOC analysis.4 Finally in 1967,
Dow Chemical patented, “Method and Apparatus for Determination of Total Carbon Content
in Aqueous Systems.” This system manually injected aqueous samples directly into a stream
of oxygen in a 700 to 900 °C furnace. The CO2 produced during this process was measured
with infrared absorbance. This was the first combustion TOC instrument produced. The
analytical range at that time was 2 to 500 ppmC with a 98% combustion efficiency rate.5
As mentioned earlier, TOC analysis grew in importance as a method to analyze wastewater and municipal water for
organic matter under the Resource Conservation and Recovery Act (RCRA) in 1976.1 This act established criteria for
screening and measuring contaminant levels. Today TOC instrumentation and analysis continues to evolve in
functionality, accuracy and precision to meet changing needs in a variety of industries.

TOC MEASUREMENT OVERVIEW

TOC analyzers can measure:
 Total Carbon (TC)
 Total Organic Carbon (TOC)
 Inorganic Carbon (IC)
 Non-Purgeable Organic Carbon (NPOC)
 Purgeable Organic Carbon (POC)
TOC measurement involves:
 Oxidizing organic carbon in a sample
 Detecting and quantifying the oxidized carbon (CO2)
 Presenting the results in units of mass of carbon per volume of sample

TOC DEFINITIONS
 Total Carbon (TC) - The measure of all the carbon in the sample, both inorganic and organic, as a single
parameter. Generally, the measurement is made by analyzing the sample directly, without pretreatment.
 Total Organic Carbon (TOC) - The sum of all the organic carbon in the sample.
 Direct TOC Measurement (NPOC) - In the direct approach, IC is first removed by acidification and sparging
and the remaining carbon is measured as TOC. IC and POC are not recovered for further analysis in this
approach. However, since POC generally represents 1% or less of total carbon in a sample, it is considered
negligible.
 TOC Measurement by Difference (TC-IC) - This approach requires two analyses: one to measure TC, and one
to measure IC. The difference between these two measurements is precisely TOC.
 TOC Measurement by Sum - This approach measures NPOC and POC. The sum of these measurements is
precisely TOC.
 Inorganic Carbon (IC) - Includes carbonate, bicarbonate, and dissolved carbon dioxide. IC is analyzed in liquid
samples by acidifying with an inorganic acid to pH 3 or lower, and then sparging with a stream of inert gas. The
acidification converts carbonates and bicarbonates to carbon dioxide, which is then removed along with
dissolved CO2 by the gas stream and measured to provide an IC value.

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 Total Organic Carbon (TOC) Analysis Technique Comparison

OXIDATION TECHNIQUES FOR TOC

There are two primary oxidation techniques employed by TOC analyzers today: catalytic combustion and
UV/persulfate. A description of each oxidation technique, along with the benefits and limitations of each, is discussed
briefly below.

Catalytic Combustion
Catalytic combustion systems are based on the injection of a sample into a catalyst-packed quartz tube
enclosed in a furnace. The catalyst tube is typically heated anywhere from 680 ˚C to 1000 ˚C. Through the
combination of catalyst, high temperature and an oxygen rich environment (generally ultra-zero air or
oxygen), the carbon in the sample is oxidized to CO2. The CO2 is then swept to the NDIR detector for
measurement.
Catalytic combustion is suited to wastewater applications with a 10 to 20,000 ppmC range, and is not
sensitive enough for accurate low-level analysis, such as drinking water or pharmaceutical water for
injection (WFI) samples. Ongoing consumable costs of this type of analyzer include phosphoric acid
reagent, periodic replacement of catalyst and halogen scrubber contents (tin and copper). Catalytic
combustion system limitations include the analysis of samples containing salt (halogens) which can be
successfully analyzed, but will decrease catalyst lifespan, as well as the longevity of other minor system
components. For samples containing salt, Teledyne Tekmar recommends the use of salt analysis kit that
includes a special catalyst and parts that require frequent replacement.

UV/Persulfate
UV/Persulfate systems transfer an aliquot of sparged sample to a “UV reactor” where a combination of
sodium persulfate (Na2S2O8) (chemical oxidizer) and UV light are used to oxidize the sample.
UV/Persulfate systems are good for low-level analysis and are well-suited to the pharmaceutical
industry, specifically for water for injection (WFI), ultra-pure water and clean in place (CIP)
applications. UV/Persulfate should only be used for samples less than 50 ppmC without dilution and
contain no particulates. Dilution may cause this range to reach to 1000 ppmC or above.
Limitations of the UV/persulfate technique include samples that are difficult to oxidize (those
containing particulates, high levels of carbon, oils or salts). For this reason, seawater samples should
not be run on a UV/persulfate system as the salt will prevent the sample from fully oxidizing and could
harm the detector.
It is also important to note, that while combustion analyzers use lab grade air, analysis using
UV/persulfate requires the use of nitrogen to prevent the creation of ozone, a health hazard (air or
oxygen will form ozone during the chemical oxidization process). Ongoing consumable costs include
phosphoric acid reagent, sodium persulfate reagent and halogen scrubber contents (tin and copper).
When making the reagents required for the oxidation process, extreme care must be used to not
contaminate the glassware with carbon from carbon containing cleaners.

GAS FLOW CONTROL SYSTEMS FOR TOC

The gas flow through a TOC analyzer is typically managed by a gas pressure regulator or mass flow controller (MFC). The
MFC provides highly-accurate, variable-flow conditions and features such as automated system leak checking and
reduced gas consumption. Pressure regulators primary advantage is their affordability, but have significant drawbacks
including limitation to one flow rate, and need for additional system gas pathway components, such as flow restrictors,
to vary flow rates.

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 Total Organic Carbon (TOC) Analysis Technique Comparison

NON-DISPERSIVE INFRARED (NDIR) DETECTION FOR TOC

Measurement of CO2 in the sample is accomplished by non-dispersive infrared (NDIR) detector. This detector type
employs an infrared (IR) beam that passes through a chamber filled with the sample CO2 gas. According to system
design, the measurement may be taken by allowing the gas to pass through the chamber (flow through) or allowing it to
reach equilibrium and then sealing the chamber (static pressure concentration [SPC]).
The CO2 measurement is a function of the absorption of IR energy as it travels through the optical path. Concentration
measurements are based on the difference ratio in the IR absorption between a reference and sample signal. Reference
and sample channels measure CO2 in a single path through the use of narrow band optical filters with appropriately
selected bands. The CO2 sample channel uses an optical filter centered at 4.24 micrometers. This filter corresponds to
the absorption band for CO2. Concentrations of CO2 present in the optical path will result in a reduction in IR energy as it
traverses the optical path. The reference channel is established using a filter with a center wavelength at 3.95
micrometers. Examples of two NDIR detector designs used in Teledyne Tekmar TOC analyzers are shown in Figure 1.

Figure 1 TOC NDIR Diagrams1

Fusion and Torch TOC Analyzer NDIR Detector Lotix TOC Analyzer NDIR Detector

Flow-Through NDIR Design

Traditional flow-through detection involves measuring the absorption of infrared light over time, as the CO2 is swept
through the detector. The resulting measurement correlates to a peak, which can be integrated and calculated to a
concentration. Flow-through detection may use an MFC or a pressure regulator. The Teledyne Tekmar Lotix Combustion
TOC analyzer design uses this detection scheme.

Static Pressure Concentration (SPC) NDIR Design

Static pressure concentration (SPC) allows for the specific carbon component to be oxidized and the resultant carbon
dioxide swept into the detector using a non-interfering, inert gas, which is measured by an MFC. Once the gases inside
the detector have reached equilibrium, the detector is sealed. A single reading is used to determine the amount of CO2 in
the detector cell. The reading correlates directly to the concentration of the carbon contribution from the sample. The
SPC is visually shown as a bar graph because it is a reading taken at one moment in time. The Teledyne Tekmar Torch
Combustion TOC analyzer and Fusion UV/Persulfate TOC analyzer both use this detection scheme. Click Here for more
information on NDIR pressurization.

1. Optical bench illustration copyright LI-COR, Inc; used by permission.

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 Total Organic Carbon (TOC) Analysis Technique Comparison

NDIR Limitations
NDIR detectors, often the most expensive system component, can be damaged by both halogens and moisture as
explained in the sections below:
 Because halogenated compounds are known to damage the NDIR detector, most TOC
analyzers include halogen scrubbers to remove the halogens prior to the sample gas
stream reaching the NDIR detector. In Teledyne Tekmar analyzers, a tin/copper halogen
scrubber protects the NDIR detector. As the tin collects the harmful halogen
compounds, the copper turns dull to act as an indicator. Replacement of halogen
scrubber contents is a typical preventative maintenance task.
The most common source of halogen issues in TOC analysis is salt in seawater samples.
When analyzing seawater samples, verify the amount of salinity the system was designed
to accept. Teledyne Tekmar suggests as little as possible, but realistically, samples under
4% salinity will generally not harm the NDIR detector. For this sample type, Teledyne
Tekmar offers a Salt Analysis Kit to aid in the analysis of salt containing samples. The kit
contains a special sample loop and catalyst, as well as replacement parts for
components whose lifespan is reduced when analyzing this sample type. Halogen Scrubber

Additional sources of halogens can be derived from halogenated acids such as hydrochloric. Care must be taken
when using HCl for sample preservation and glassware cleaning. Teledyne Tekmar recommends only using
phosphoric acid to preserve samples and nitric acid to clean the glassware.
 Like halogens, water is also harmful to the NDIR detector. Teledyne Tekmar analyzers employ a two-stage
moisture removal process, consisting of a mist trap and permeation dryer. After oxidation of the sample, carrier
gas sweeps CO2 and water vapor to the mist trap. During the transfer, some condensation will occur in the
system tubing, and in catalytic combustion systems, a condensing loop with fan cools the heated air to
encourage condensation. Once the sample carrier gas reaches the mist trap, a majority of the condensate is
removed. The sample gas then travels to the permeation dryer, which removes the remainder of the moisture
from the sample gas. The permeation dryer is a tube inside another tube. The inner tube is made of a special
membrane material that allows moisture to permeate. The outer tube has gas that sweeps in the opposite
direction to remove the permeated moisture. Once analysis is complete, the condensate is sent to the waste
container. All TOC analyzers should have some form of moisture removal to ensure the life of the detector.

Condensing Loop Mist Trap Permeation Dryer

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 Total Organic Carbon (TOC) Analysis Technique Comparison

OTHER DETECTION METHODS FOR TOC

Conductivity
The conductivity method measures the conductivity of the sample before and after oxidation; the difference yielding the
amount of TOC. The sample forms dissolved CO2 in the oxidation phase, which acts as a weak acid. This acid in turn
weakens the conductivity of the sample and is proportional to the amount of TOC. This simple method may, depending
on the chemical species of each individual sample and unique oxidation products, present a proportional positive or
negative interference to the calculated TOC value. Conductivity detection limits are under 50 ppmC. When carbon
content is greater than 50 ppmC, the conductivity is no longer proportional. This method is often used for on-line
applications in the pharmaceutical industry.

Membrane Conductivity
The use of hydrophobic gas permeation membrane has been used to improve the accuracy of conductivity and allow for
greater discrimination of dissolved CO2 over other chemical compounds. Although this membrane has the unique ability
to differentiate, it can become clogged with microbes and other particulates. Additionally, membranes can also develop
flow problems, dead spots and micro leaks, all of which will impact analytical performance. Once the membrane has
been overloaded, it may take hours before returning to working order. It should also be noted that some amines have the
ability to pass through the membranes and add conductivity, resulting in a false high concentration. This method is
often used for on-line applications in the pharmaceutical industry and like non-membrane conductivity, it is not
recommended for concentrations greater than 50 ppmC.
Determining the best TOC analyzer for pharmaceutical cleaning validation and purified water applications often results
in a comparison of the two commonly used detection techniques already briefly discussed in this guide: NDIR detection
and membrane conductivity. For an in-depth analytical comparison, refer to the Teledyne Tekmar White Paper: “An
Analytical Detector Comparison for TOC Analysis in Cleaning Validation and Water Purification Applications” by clicking
Here.

SUMMARY
When choosing a TOC analyzer for a particular application or sample type, consider the anticipated concentration range
of the samples, the sample type itself and any analytical issues associated with that sample type (particulates, salt, etc.).
By focusing on these attributes first, it can then be determined what oxidation technique and detection method will
work best. Once decided, address additional considerations including system flexibility, features and accessories.

ABOUT TELEDYNE TEKMAR

At Teledyne Tekmar, we design and manufacture industry leading environmental instrumentation including purge and
trap (P&T) sample preparation systems for VOCs and TOC analyzers. Dedicated to continual improvement, we strive to
understand our customer’s analytical needs and develop instrumentation that meets those requirements. Our product
support extends far beyond a customer’s initial investment with a team of highly-skilled technicians and chemists to
provide troubleshooting and application assistance. By working closely with our customers, we continue to improve our
products and the future of environmental analysis.

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 Total Organic Carbon (TOC) Analysis Technique Comparison

FUSION UV/PERSULFATE TOC ANALYZER

The Teledyne Tekmar Fusion UV/Persulfate TOC analyzer was designed for both drinking water
and pharmaceutical applications. With its extremely low detection limit of 0.2 ppbC and its
ability to handle certain levels of carbon, it is a very versatile analyzer for many sample
matrices. The pharmaceutical industry will find the Fusion to be an ideal solution for clean-in-
place (CIP), water-for-injection (WFI) and ultra-pure (UP) water applications.
The Fusion uses safe, proven UV/persulfate oxidation of carbonaceous material to CO 2 ,
followed by NDIR detection. UV/Persulfate contributes very little background carbon (lower
than TOC combustion systems), making it the better choice for drinking water and ultra-pure
water applications. The Fusion also does not suffer from an affinity to interferences, unlike
membrane conductivity systems. Membrane conductivity is very sensitive to interferences like
salt, acid, azide, halogenated organics and other compounds. The Fusion is the ideal TOC
analyzer for accurate, versatile and sensitive pharmaceutical applications.
Key features:
 Limit of detection (LOD) 0.2 ppbC with maximum measurable concentration of 4,000 ppmC
 NDIR Static pressure concentration (SPC) detection
 Automatic dilution of stock standards for calibration and unattended auto-calibration monitoring
 Intellidilution for automatically diluting a sample back into calibration range
 Automated self-diagnostic tools including leak check
 21 CFR 11 functionality - Electronic Records and Electronic Signatures (ERES), audit trails and user-accounts
 Mass flow controller (MFC) for reduced gas consumption and enhanced flow control
Methods:
 EPA 415.1- 415.3, 9060A
 Standard Method 5310C, ASTM D4779 and D4839
 Cleaning Validation / USP TOC Method <643> / EP 2.2.44 / JP
 Other additional Methods
For more information on the Fusion UV/Persulfate TOC Analyzer click Here. For information on using the Fusion
UV/Persulfate TOC analyzer in the pharmaceutical industry, click Here.

TORCH CATALYTIC COMBUSTION TOC ANALYZER

The Torch is Teledyne Tekmar’s premium TOC catalytic combustion analyzer that includes a
variety of useful features and automated analysis processes. Capable of stock standards serial
dilution to form a calibration curve as well as auto-dilution of samples with concentrations
above the calibration curve, the Torch was designed to simplify TOC analysis.
Key features:
 Limit of detection (LOD) 50 ppbC with maximum measurable concentration of
30,000 ppmC
 Automated self-diagnostic tools including leak check
 NDIR Static pressure concentration (SPC) detection
 Automatic dilution of stock standards for calibration and unattended auto-calibration
monitoring
 Intellidilution for automatically diluting a sample back into calibration range
 Auto-blanking
 Mass flow controller (MFC) for reduced gas consumption and enhanced flow control

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 Total Organic Carbon (TOC) Analysis Technique Comparison

Methods:
 EPA 415.1, 415.3 and 9060A
 Standard Method 5310B
 EP 2.2.44, ISO 8245
 Other additional methods
For more information on the Torch Combustion TOC analyzer click Here.

LOTIX CATALYTIC COMBUSTION TOC ANALYZER

The Lotix Catalytic Combustion TOC analyzer was designed as an economical option for
accurate carbon content measurement in aqueous matrices down to the ppbC level. With the
vast detection range and robustness of the Lotix, dilution and filtration is no longer required for
samples less than 20,000 ppmC and particles less than 0.8 mm in diameter. It uses proven high-
temperature combustion, oxidation of carbon material into carbon dioxide, and detection
using a Non- Dispersive Infrared (NDIR) detector. The Lotix is a reliable analytical solution for
wastewater, drinking and surface water, ground water, sea water and other hard to oxidize
matrices.

Key features:
 Limit of detection (LOD) 50 ppbC with ability to run from 0 to 20,000 ppmC concentration, without dilution,
using a single 0.5 mL sample injection. Higher concentrations are achievable with dilution prior to analysis.
 NDIR flow-through detection
 Cost-effective design without syringe drive or 7-port valve
 Ability to run 0-20,000 ppmC without dilution with a single 0.5 mL injection volume virtually eliminating the
need for multiple calibration curves
 Simple design ensures components can be accessed in minutes, and with the furnace located in the front,
combustion tube maintenance is fast and easy
 Pressurized 10 L deionized (DI) water reservoir to clean the sample pathway, sample loop and needle before
and after each sample, without using any autosampler positions
 Optional Lotix solids module (LSS) for soils, sludges, sediments, particulate-laden liquids and hard-to-oxidize
samples
Methods:
 Standard Method 5310B
 EPA 415.1 and 9060A
 ASTM D2579
 Other additional methods
For more information on the Lotix Combustion TOC analyzer click Here. For information on the optional Lotix Solids
Sampler (LSS) click Here.

CONTACT US
For additional information about Teledyne Tekmar TOC analyzers and special offers, visit our website at
www.teledynetekmar.com. To contact a regional sales representative, use the contact information located Here or email
us at [email protected]

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 Total Organic Carbon (TOC) Analysis Technique Comparison

References
1. United States Environmental Protection Agency (USEPA). [Online] https://www.epa.gov/rcra (accessed August 13,
2021).
2. Britannica. [Online] https://www.britannica.com/biography/Jan-Baptista-van-Helmont (accessed August 13,
2021).
3. Scottish Science Hall of Fame. [Online] https://digital.nls.uk/scientists/biographies/joseph-black/
discoveries.html (accessed August 13, 2021).
4. Kidder, R.E. Infrared Gas Analyzer. U.S. Patent 2,443,427, June 15, 1948. [Online]
https://patentimages.storage.googleapis.com/87/7f/d6/20783841808aed/US2443427.pdf (accessed August 13,
2021).
5. Stenger, V.A. Method and Apparatus for Determining the Inorganic Carbon Content in a Liquid. U.S. Patent
3,459,938, 1969. [Online] https://patentimages.storage.googleapis.com/2d/4b/70/c80095504f8a6e/US4095951.pdf
(accessed August 13, 2021).

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