Organic Carbon, Total MR, 10173

Organic Carbon, Total DOC316.53.01094

Direct Method1 Method 10173

MR (15 to 150 mg/L C)
Scope and Application: For water, drinking water and wastewater
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 higher ranges of TOC use Method 100173 or method 10128. To test lower ranges of TOC use method 10129.

Collect the following items:

Description Quantity

Total Organic Carbon Direct Method Mid Range Test N Tube Reagent Set 1

Cylinder, graduated, 10-mL 1

DRB200 Reactor 1

Light Shield or Adapter (see Instrument-specific information) 1

pH Paper 1

Flask, Erlenmeyer, 50-mL 1

Magnetic Stirrer 1

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Collect the following items: (continued)

Description Quantity

Pipet, TenSette, 0.1 to 1.0 mL plus tips 1

Pipet, TenSette, 1.0 to 10.0 mL plus tips 1

Stir Bar, magnetic 1

Test Tube Rack 1

Water, organic-free 3.0 mL

Wipes, disposable, Kimwipes 1

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 4. Place the flask on a
Solution, pH 2.0. Use pH stir plate and stir at a
paper to make sure the moderate speed for
sample pH is 2. 10 minutes.

5. Label two Mid 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 8. Rinse two blue MR/HR
to add 1.0 mL of Indicator Ampules with
organic-free water to the deionized water and wipe
reagent blank vial and them with a soft, lint-free
1.0 mL of prepared wipe.
sample to the sample vial. Do not touch the
Swirl to mix. ampules sides after
wiping. Pick them up by
the top.

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Direct method (continued)
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, snap
the top off the ampule and
allow it to drop into the
Acid Digestion vial.
Do not invert or tilt the
vial after inserting the
ampule.
13. Wipe the reagent
blank with a damp towel,
followed by a dry one, to
remove fingerprints or
other marks.
17. Insert the sample vial
assembly in the 16-mm
round cell.
10. Cap the vial 11. Carefully remove the
assemblies tightly, insert vial assemblies from the
them in the COD reactor reactor. Place them in a
and close the lid for 2 test tube rack.
hours at Allow the vials to cool for
103105 C. one hour for accurate
results.
The liquid in the reagent
blank vial should be dark
blue.
Zero
14. 15. ZERO the instrument.
The display will show:
0.0 mg/L C
Read
18. READ the results in
mg/L C.
Organic Carbon, Total
Stored Programs
425 Organic Carbon MR
Start
12. Select the test.
Insert a light shield or an
adapter if required (see
Instrument-specific
information).
16. Wipe the sample vial
assembly with a damp
towel, followed by a dry
one, to remove fingerprints
or other marks.
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Interferences
The Interfering substances table lists substance 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 1500 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
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.

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Homogenize samples containing solids to assure representative samples.

Accuracy check
Standard additions method (sample spike)
Required for accuracy check:
1000-mg/L C stock solution
50-mL Class A volumetric flask
Organic-free water
TenSette Pipet
Acid Digestion Vials (3)
TOC Persulfate Powder Pillow (1)

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.

4. Prepare a 300-mg/L C standard:

a. Transfer 15.00 mL of 1000-mg/L C stock solution to a 50-mL Class A volumetric flask.

b. Dilute to volume with organic-free water. Insert the stopper and mix thoroughly.

5. Use the TenSette Pipet to prepare spiked samples: add 0.1 mL, 0.2 mL and 0.3 mL of the 300-
mg/L standard to three Acid Digestion Vials.

6. Add the contents of one TOC Persulfate Powder Pillow to each vial.

7. Add 1.0 mL of sample to each vial. Swirl to mix.

8. 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.

9. Select GRAPH to view the results. Select IDEAL LINE (or best-fit) to compare the standard
addition results to the theoretical 100% recovery.

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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
50-mL 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 100 mg/L C standard solution as follows:

a. Transfer 5.00 mL of the prepared 1000-mg/L organic carbon stock standard solution to a
50-mL volumetric flask.
b. Dilute to volume 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.

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

Precision95% Confidence SensitivityConcentration

Program Instrument Standard
Limits of Distribution per 0.010 Abs
425 DR 5000 70 mg/L C 6872 mg/L C 1.2 mg/L C
DR 2800 70 mg/L C 6872 mg/L C 1.2 mg/L C
DR 2700 70 mg/L C 6872 mg/L C 1.2 mg/L C
DR/2500 15mg/L C 6 mg/L C 1.4 mg/L C
DR/2400 50 mg/L C 3 mg/L C
75 mg/L C 2 mg/L C
115 mg/L C 5 mg/L C
150 mg/L C 6 mg/L C

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 Organic Carbon, Total

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 Quantity/Test Unit Catalog number
Reagent Set, Total Organic Carbon Direct Method 50 vials 2815945
Mid Range Test N Tube, includes:
Acid Digestion Solution Vials, High Range TOC1 1 50/pkg
Buffer Solution, Sulfate 0.4 mL 25 mL 45233
Funnel, micro 1 each 2584335
Indicator Ampules, MR/HR TOC1 1 10/pkg
TOC Persulfate Powder Pillows1 1 50/pkg
pH Paper 1 5/pkg 39133
Water, Organic-free 1.0 mL 500 mL 2641549
1 Not sold separately.

Required apparatus
Description Quantity/Test Unit Catalog number
Cylinder, graduated, 10-mL 1 each 50838
DRB200 Reactor, 110 V, 15 x 16 mm 1 each LTV082.53.40001
DRB200 Reactor, 220 V, 15 x 16 mm 1 each LTV082.52.40001
Flask, Erlenmeyer, 50-mL 1 each 50541
Magnetic Stirrer 1 each 2881200
Pipet, TenSette, 0.1 to 1.0 mL 1 each 1970001
Pipet Tips, for TenSette Pipet 1970001 2 50/pkg 2185696
Pipet, TenSette, 1.0 to 10.0 mL 1 each 1970010
Pipet Tips, for TenSette Pipet 1970010 2 50/pkg 2199796
Stir Bar, magnetic 1 each 4531500
Test Tube Rack 1 each 1864100
Wipes, Disposable, Kimwipes 1 280/pkg 2097000

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Recommended standards
Description Unit Catalog number
Potassium Acid Phthalate 500 g 31534
TOC Standard Solution, 20 mL (KHP Standard, 1000-mg/L C) 5/pkg 2791505

Optional reagents and apparatus

Description Unit Catalog number
Sulfuric Acid Solution, 5.2 N 100 mL-MDB 244932
Pipet Tips, for TenSette Pipet 1970010 1000/pkg 2185628
Pipet Tips, for TenSette Pipet 1970010 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

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Hach Company, 2007. All rights reserved. Printed in the U.S.A. Updated February 2008, Edition 5