Organic Carbon, Total HR, 10128

Organic Carbon, Total

DOC316.53.01095

Direct Method1

Method 10128

HR (100 to 700 mg/L C)

Scope and Application: For wastewater and industrial water
1

U.S. Patent 6,368,870

Test preparation

How to use instrument-specific information

The Instrument-specific information table displays requirements that may vary between
instruments. To use this table, select an instrument then read across to find the corresponding
information required to perform this test.

Table 1 Instrument-specific information

Instrument

Light shield

Adapter

DR 5000

DR 2800

LZV646

DR 2700

LZV646

DR/2500

DR/2400

5945700

Before starting the test:

DR 2800 and DR 2700 only: Install the light shield in Cell Compartment #2 before performing this test.
A reagent blank is required for each series of samples.
To test for TOC levels below 100 mg/L C, use Method 10129.

Collect the following items:

Description

Quantity

Total Organic Carbon Direct Method High Range Test N Tube Reagent Set

Cylinder, graduated, 10-mL

DRB200 Reactor

Light Shield or Adapter (see Instrument-specific information)

pH Paper

Flask, Erlenmeyer, 50-mL

Magnetic Stirrer

Pipet, TenSette, 0.1 to 1.0 mL plus tips

Pipet, TenSette, 1.0 to 10.0 mL plus tips

Stir Bar, magnetic

Organic Carbon, Total

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Organic Carbon, Total

Collect the following items: (continued)
Description

Quantity

Test Tube Rack

Water, organic-free

0.3 mL
1

Wipes, disposable, Kimwipes

See Consumables and replacement items for reorder information.

Direct method

1. Turn on the DRB200

reactor. Select the TOC
program.

2. Use a graduated
cylinder to add 10 mL of
sample to a 50-mL
Erlenmeyer flask that
contains a stir bar.

3. Add 0.4 mL of Buffer

Solution, pH 2.0. Use pH
paper to make sure the
sample pH is 2.

4. Place the flask on a

stir plate and stir at a
moderate speed for
10 minutes.

5. Label two High Range

Acid Digestion vials
sample and reagent blank.

6. Use a funnel to add

the contents of one TOC
Persulfate Powder Pillow
to each Acid Digestion vial
(colorless liquid).

7. Use a TenSette Pipet

to add 0.3 mL of
organic-free water to the
reagent blank vial and
0.3 mL of prepared
sample to the sample vial.
Swirl to mix.

8. Rinse two blue MR/HR

Indicator Ampules with
deionized water and wipe
them with a soft, lint-free
wipe.

Organic Carbon, Total

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Do not touch the

ampules sides after
wiping. Pick them up by
the top.

Organic Carbon, Total

Direct method (continued)

Stored Programs
426 Organic Carbon HR
Start

9. Lower one unopened

ampule into each Acid
Digestion vial. When the
score mark on the ampule
is level with the top of the
Acid Digestion vial, break
the top off the ampule and
allow it to drop into the
Acid Digestion vial.

10. Cap the vial

assemblies tightly, insert
them in the COD reactor
and close the lid for 2
hours at
103105 C.

11. Carefully remove the

vial assemblies from the
reactor. Place them in a
test tube rack.
Allow the vials to cool for
one hour for accurate
results.

12. Select the test.

Insert a light shield or an
adapter if required (see
Instrument-specific
information).

The liquid in the reagent

blank vial should be dark
blue.

Do not invert or tilt the

vial after inserting the
ampule.

Zero

13. Wipe the reagent

blank with a damp towel,
followed by a dry one, to
remove fingerprints or
other marks.

14.

15. ZERO the instrument.

The display will show:
0 mg/L C

16. Wipe the sample vial

assembly with a damp
towel, followed by a dry
one, to remove fingerprints
or other marks.

Organic Carbon, Total

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Organic Carbon, Total

Direct method (continued)

Read

17. Insert the sample vial

assembly in the 16-mm
round cell.

18. READ the results in

mg/L C.
The display will show
Underrange when the
mg/L C value is below the
lower limit of the method.

Interferences
The Interfering substances table lists substances that have been tested for interference and found
not to interfere up to the levels indicated.
If the sample contains greater than 1000 mg/L CaCO3 alkalinity, lower the sample pH to less than
7 before testing by adding Sulfuric Acid Solution.
Most sample turbidity is either dissolved during the digestion stage or settled during the cooling
period. Sample turbidities up to 50 NTU have been tested without interference.

Table 2 Interfering substances

Interfering substance

Interference level

Aluminum

10 mg/L

Ammonia Nitrogen

1000 mg/L as N

ASTM Wastewater

No effect

Bromide

500 mg/L Br

Bromine

25 mg/L Br2

Calcium

2000 mg/L as CaCO3

Chloride

5000 mg/L

Chlorine

10 mg/L Cl2

Chlorine Dioxide

6 mg/L ClO2

Copper

10 mg/L

Cyanide

10 mg/L CN

Iodide

50 mg/L

Iron (II)

10 mg/L

Iron (III)

10 mg/L

Magnesium

2000 mg/L as CaCO3

Manganese (VII)

1 mg/L

Monochloramine

14 mg/L NH2Cl as Cl2

Organic Carbon, Total

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Organic Carbon, Total

Table 2 Interfering substances (continued)
Interfering substance

Interference level

Nitrite

500 mg/L NO2

Ozone

2 mg/L O3

Phosphate

3390 mg/L PO43

Silica

100 mg/L SiO2

Sulfate

5000 mg/L SO42

Sulfide

20 mg/L S2

Sulfite

50 mg/L SO32

Zinc

5 mg/L

Sample collection, preservation and storage

Collect samples in clean glass bottles.

Rinse the sample bottle several times with the sample to be collected.

Fill the bottle completely full before capping.

Test samples as soon as possible.

Acid preservation is not recommended.

Homogenize samples containing solids to assure representative samples.

Accuracy check
Standard additions method (sample spike)
Required for accuracy check:

Potassium Acid Phthalate, dry primary standard

Organic-free Reagent Water

1-L Class A volumetric flask

TenSette Pipet

Acid Digestion Vials (3)

TOC Persulfate Powder Pillow (1)

50 mL Class A Volumentric flask

1. After reading test results, leave the sample cell (unspiked sample) in the instrument.
2. Select standard additions from the instrument menu:
Instrument

Navigate to:

DR 5000

OPTIONS>MORE>STANDARD ADDITIONS

DR 2800

OPTIONS>MORE>STANDARD ADDITIONS

DR 2700

OPTIONS>MORE>STANDARD ADDITIONS

DR/2500

OPTIONS>STANDARD ADDITIONS

DR/2400

OPTIONS>STANDARD ADDITIONS

3. Accept the default values for standard concentration, sample volume and spike volumes. After
the values are accepted, the unspiked sample reading will appear in the top row. See the user
manual for more information.
Organic Carbon, Total
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Organic Carbon, Total

4. Prepare a 1000-mg/L organic carbon stock standard solution:
a. Dissolve 2.1254 g of dry primary standard Potassium Acid Phthalate in Organic-free
Reagent Water.
b. Dilute to 1000 mL. This stock standard is stable for about 1 month at room temperature.
5. Prepare a 300 mg/L C standard solution as follows:
a. Transfer 15.00 mL of the prepared 1000-mg/L organic carbon stock standard solution to a
50-mL volumetric flask.
b. Dilute to the mark with Organic-free Reagent water. Insert the stopper and mix thoroughly.
Prepare this solution daily.
6. Use the TenSette Pipet to prepare spiked samples: add 0.1 mL, 0.2 mL and 0.3 mL of the
prepared 300-mg/L standard to three Acid Digestion Vials.
7. Add the contents of one TOC Persulfate Powder Pillow to each vial.
8. Add 0.3 mL of sample to each vial. Swirl to mix.
9. Continue the test starting at step 8 of the Direct method test procedure for each of the spiked
samples, starting with the 0.1 mL sample spike. Measure each of the spiked samples in the
instrument.
10. Select GRAPH to view the results. Select IDEAL LINE (or best-fit) to compare the standard
addition results to the theoretical 100% recovery.
Standard solution method
Note: Refer to the instrument user manual for specific software navigation instructions.

Required for accuracy check:

Potassium Acid Phthalate, dry primary standard

Organic-free Reagent Water

1-L Class A volumetric flask

1. Prepare a 1000-mg/L organic carbon stock standard solution:

a. Dissolve 2.1254 g of dry primary standard Potassium Acid Phthalate in Organic-free
Reagent Water.
b. Dilute to 1000 mL. This stock standard is stable for about 1 month at room temperature.
2. Prepare a 300 mg/L C standard solution as follows:
a. Transfer 15.00 mL of the prepared 1000-mg/L organic carbon stock standard solution to a
50-mL volumetric flask.
b. Dilute to the mark with Organic-free Reagent water. Insert the stopper and mix thoroughly.
Prepare this solution daily.
3. Use this solution in place of the sample. Follow the Direct method test procedure.

Organic Carbon, Total

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Organic Carbon, Total

4. To adjust the calibration curve using the reading obtained with the standard solution, navigate
to Standard Adjust in the software.
Instrument

Navigate to:

DR 5000

OPTIONS>MORE>STANDARD ADJUST

DR 2800

OPTIONS>MORE>STANDARD ADJUST

DR 2700

OPTIONS>MORE>STANDARD ADJUST

DR/2500

OPTIONS>STANDARD ADJUST

DR/2400

OPTIONS>STANDARD ADJUST

5. Turn on the Standard Adjust feature and accept the displayed concentration. If an alternate
concentration is used, enter the concentration and adjust the curve to that value.

Method performance
To test for TOC levels below 100 mg/L C, use Method 10173 or Method 10129.
Program

Instrument

Standard

Precision95% Confidence
Limits of Distribution

SensitivityConcentration
per 0.010 Abs

426

DR 5000

350 mg/L C

337363 mg/L C

4 mg/L C

DR 2800

350 mg/L C

337363 mg/L C

4 mg/L C

DR 2700

350 mg/L C

337363 mg/L C

4 mg/L C

DR/2500
DR/2400

100 mg/L C

14 mg/L C

4 mg/L C

250 mg/L C

13 mg/L C

400 mg/L C

15 mg/L C

550 mg/L C

23 mg/L C

700 mg/L C

34 mg/L C

Summary of method
The total organic carbon (TOC) is determined by first sparging the sample under slightly acidic
conditions to remove the inorganic carbon. In the outside vial organic carbon in the sample is
digested by persulfate and acid to form carbon dioxide. During digestion, the carbon dioxide
diffuses into a pH indicator reagent in the inner ampule. The absorption of carbon dioxide into the
indicator forms carbonic acid. Carbonic acid changes the pH of the indicator solution which, in
turn, changes the color. The amount of color change is related to the original amount of carbon
present in the sample. Test results are measured at 598 and 430 nm.

Consumables and replacement items

Required reagents
Description
Total Organic Carbon Direct Method
High Range Test N Tube Reagent Set, includes:
Acid Digestion Solution Vials, High Range TOC1
Buffer Solution, Sulfate
Funnel, micro

Unit

Catalog number

50 vials

2760445

50/pkg

0.4 mL

25 mL

45233

each

2584335

TOC1

10/pkg

TOC Persulfate Powder Pillows1

50/pkg

5/pkg

39133

0.3 mL

500 mL

2641549

Indicator Ampules, MR/HR

pH Paper
Water, Organic-free
1

Quantity/Test

Not sold separately.

Organic Carbon, Total

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Organic Carbon, Total

Required apparatus
Description

Quantity/Test

Unit

Catalog number

Cylinder, graduated, 10-mL

each

50838

DRB200 Reactor, 110 V, 15 x 16 mm

each

LTV082.53.40001

DRB200 Reactor, 220 V, 15 x 16 mm

each

LTV082.52.40001

Flask, Erlenmeyer, 50-mL

each

50541

Magnetic Stirrer

each

2881200

each

1970001

50/pkg

2185696

each

1970010

Pipet Tips, for TenSette Pipet 1970010

50/pkg

2199796

Stir Bar, magnetic

each

4531500

13, 5.2 N

each

1864100

280/pkg

2097000

Description

Unit

Catalog number

Potassium Acid Phthalate

500 g

31534

TOC Standard Solution (KHP Standard, 1000-mg/L C)

5/pkg

2791505

Unit

Catalog number

Pipet,

TenSette,

0.1 to 1.0 mL

Pipet Tips, for TenSette Pipet 1970001

Pipet,

TenSette,

1.0 to 10.0 mL

Test Tube Rack

Wipes, Disposable,

Kimwipes

Recommended standards

Optional reagents and apparatus

Description

100 mL

244932

Pipet Tips, for TenSette Pipet 19700-10

Sulfuric Acid Solution, 5.2 N

1000/pkg

2185628

Pipet Tips, for TenSette Pipet 19700-10

250/pkg

2199725

Balance, analytical, 80 g capacity

115 VAC

2936701

Weighing Paper, 76 x 76 mm

500/pkg

1473800

Flask, volumetric class A

50 mL

1457441

Flask, volumetric class A

1000 mL

1457453

FOR TECHNICAL ASSISTANCE, PRICE INFORMATION AND ORDERING:

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Outside the U.S.A. Contact the HACH office or distributor serving you.
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Hach Company, 2007. All rights reserved. Printed in the U.S.A.

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Telephone: (970) 669-3050
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Updated February 2008, Edition 5