Chloramine (Mono) : Indophenol Method Method 10171 0.04 To 4.50 MG/L CL (LR) Powder Pillows

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Chloramine (Mono) DOC316.53.

01015

Indophenol Method1 Method 10171


0.04 to 4.50 mg/L Cl2 (LR) Powder Pillows
Scope and application: For chloraminated drinking water and chlorinated wastewater. This product has not been
evaluated to test for chlorine and chloramines in medical applications in the United States.
1 U.S. Patent 6,315,950

Test preparation

Instrument specific information


Table 1 shows all of the instruments that have the program for this test. The table also
shows requirements that may vary between instruments, such as adapter and sample cell
requirements. To use this table, select an instrument, then read across to find the
corresponding information for this test.
Table 1 Instrument-specific information
Instrument Adapter Sample cell orientation Sample cell
DR 6000 A23618 The orientation key is toward the user. 4864302
DR 5000 The orientation key is toward the user.
DR 3900 LZV846 (A) The orientation key is away from the user.
DR 900 — The orientation key is toward the user.
DR 3800 LZV585 (B) The 1-cm path is aligned with the arrow on the adapter. 5940506
DR 2800
DR 2700

Before starting
Samples must be analyzed immediately after collection and cannot be preserved for later analysis.
Install the instrument cap on the DR 900 cell holder before ZERO or READ is pushed.
In bright light conditions (e.g., direct sunlight), close the cell compartment on spectrophotometers, if applicable, with the
protective cover during measurements.
To measure chloramine (mono) and free ammonia on the same sample, use Method 10200 Nitrogen, Free Ammonia and
Chloramine (Mono).
For best results, measure the reagent blank value for each new lot of reagent. Replace the sample with deionized water in
the test procedure to get the reagent blank value. Subtract the reagent blank value from the sample results automatically
with the reagent blank adjust option.
Review the Safety Data Sheets (MSDS/SDS) for the chemicals that are used and use any recommended personal protective
equipment.
Dispose of reacted solutions according to local, state and federal regulations. Use the Safety Data Sheets for disposal
information for unused reagents. Consult the environmental, health and safety staff for your facility and/or local regulatory
agencies for further disposal information.

1
Items to collect
Description Quantity

Monochlor F reagent pillows 1


Sample cells (For information about sample cells, adapters or light shields, refer to Instrument
2
specific information on page 1.)

Refer to Consumables and replacement items on page 6 for reorder information.

Sample collection and storage


Collect samples in clean glass bottles. Open the sample valve or spigot and let the water
flow for a minimum of 5 minutes. Rinse the sample bottle several times with the sample
and let the sample overflow each time, then cap the container so that there is no head
space (air) above the sample. Analyze samples immediately after collection.
Color development time
Test results are strongly influenced by the sample temperature. The reaction period
indicated in the procedure is for a sample temperature of 18–20 ºC (64–68 ºF). Adjust the
reaction period according to Table 2. Samples can be read up to 15 minutes after the
listed development time.
Table 2 Color development time
Sample temperature (°C) Sample temperature (°F) Development time (mintues)
5 40 10
7 42 9
9 48 8
10 50 8
12 54 7
14 58 7
16 61 6
18 68 4
20 73 3
23 75 2.5
25 77 2
> 25 > 77 2

2 Chloramine (Mono), Indophenol Method (4.50 mg/L)


Indophenol method, powder pillows

Start

1. Start program 66, 2. Fill the sample cell with 3. Clean the prepared 4. Insert the blank into the
Monochloramine LR. For 10 mL of sample. sample. cell holder.
information about sample
cells, adapters or light
shields, refer to Instrument
specific information
on page 1.
Note: Although the program
name may vary between
instruments, the program
number does not change.

Zero

5. Push ZERO. The display 6. Remove the sample from 7. Add the contents of one 8. Close the sample cell.
shows 0.00 mg/L Cl2. the cell holder. Monochlor F powder pillow Shake the sample cell for
to the sample cell. about 20 seconds to
dissolve the reagent.

Read

9. Start the instrument 10. Clean the prepared 11. When the timer expires, 12. Push READ. Results
timer. A 5-minute reaction sample. insert the prepared sample show in mg/L Cl2.
time starts. into the cell holder.
For samples colder than
18 °C, refer to Table 2
on page 2.

Chloramine (Mono), Indophenol Method (4.50 mg/L) 3


Interferences
Table 3 shows the substances that have been tested for interference and do not interfere
at or below the indicated levels. Table 4 suggests treatments for interferences.
Table 3 Non-interfering substances
Interfering substance Interference level
Alanine 1 mg/L N
Aluminum 10 mg/L Al
Bromide 100 mg/L Br–
Bromine 15 mg/L Br2
Calcium 1000 mg/L as CaCO3
Chloride 18,000 mg/L Cl–
Chlorine Dioxide 5 mg/L ClO2
Chromium (III) 5 mg/L Cr3+
Copper 10 mg/L Cu
Cyanide 10 mg/L CN–
Dichloramine 10 mg/L as Cl2
Fluoride 5 mg/L F–
Free Chlorine 10 mg/L Cl2
Glycine 1 mg/L N
Iron (II) 10 mg/L Fe2+
Iron (III) 10 mg/L Fe3+
Lead 10 mg/L Pb
Nitrate 100 mg/L N
Nitrite 50 mg/L N
Phosphate 100 mg/L PO4
Silica 100 mg/L SiO2
Sulfate 2600 mg/L SO42+
Sulfite 50 mg/L SO32–
Tyrosine 1 mg/L N
Urea 10 mg/L N
Zinc 5 mg/L Zn

Table 4 Interfering substances


Substance Effect Interference level Recommended treatment
Magnesium + Above 400 mg/L CaCO3 Add 5 drops of Rochelle Salt Solution prior to testing. OR: use
the high range (HR) test.
Manganese (+7) – Above 3 mg/L Use the HR test; it will tolerate up to 10 mg/L.
Ozone – Above 1 mg/L Usually does not coexist with monochloramine.
Sulfide + A "rust" color develops if present. Usually does not coexist with monochloramine.
Thiocyanate – Above 0.5 mg/L This method will tolerate up to 2 mg/L.

4 Chloramine (Mono), Indophenol Method (4.50 mg/L)


Accuracy check
Standard solution method
Items to collect:
• Buffer Powder Pillow, pH 8.3
• Nitrogen, Ammonia Standard Solution, 100-mg/L as NH3–N
• Chlorine Solution Ampules, 50–70 mg/L
• 100-mL Class A volumetric flask
• 50-mL graduated cylinder
• Pipet, TenSette®, 0.1–1.0 mL and tips
• Pipets, Volumetric, 2-mL Class A and Mohr, 5-mL
• Pipet bulb
• Organic-free water

1. Prepare a 4.5-mg/L (as Cl2) monochloramine standard immediately before use as


follows.
a. Add the contents of one Buffer Powder Pillow, pH 8.3 to approximately 50 mL of
organic-free water in a clean 100-mL Class A volumetric flask. Swirl to dissolve
the powder.
b. Use a Class A volumetric pipet to add 2.00 mL of Nitrogen, Ammonia Standard
Solution, 100-mg/L as NH3–N into the flask.
c. Dilute to the mark with organic-free water. Mix well. This is a 2.00-mg/L buffered
ammonia standard.
d. Use a graduated cylinder to add 50.00 mL of the buffered ammonia standard into
a clean 100-mL beaker. Add a stir bar.
e. Find the exact concentration of the Chlorine Solution Ampules, 50–70 mg/L from
the label on the package.
f. Calculate the volume of the Chlorine Solution to add to the ammonia standard:
mL chlorine solution required = 455/(free chlorine concentration).
g. Open an ampule and use a glass Mohr pipet to add the calculated amount of
Chlorine Solution slowly to the ammonia standard in the beaker. Keep the beaker
on a stir-plate at medium speed during the chlorine addition.
h. Stir the monochloramine solution for 1 minute after the Chlorine Solution addition
is complete.
i. Quantitatively transfer the monochloramine solution to a clean 100-mL Class A
volumetric flask. Dilute to the mark with organic-free water and mix well. This is a
nominal 4.5-mg/L (as Cl2) monochloramine standard.
2. Use this standard within 1 hour of preparation. Use the test procedure to measure the
concentration of the monochloramine standard solution.
3. Compare the expected result to the actual result.
Note: The factory calibration can be adjusted slightly with the standard adjust option so that the
instrument shows the expected value of the standard solution. The adjusted calibration is then
used for all test results. This adjustment can increase the test accuracy when there are slight
variations in the reagents or instruments.

Method performance
The method performance data that follows was derived from laboratory tests that were
measured on a spectrophotometer during ideal test conditions. Users may get different
results under different test conditions.
Program Standard Precision (95% Confidence Interval) Sensitivity
Concentration change per 0.010 Abs change
66 2.60 mg/L Cl2 2.58–2.62 mg/L Cl2 0.04 mg/L Cl2

Chloramine (Mono), Indophenol Method (4.50 mg/L) 5


Summary of method
In the presence of a cyanoferrate catalyst, monochloramine (NH2Cl) in the sample reacts
with a substituted phenol to form an intermediate monoimine compound. The
intermediate couples with excess substituted phenol to form a green-colored indophenol,
which is proportional to the amount of monochloramine present in the sample. The
measurement wavelength is 655 nm for spectrophotometers or 610 nm for colorimeters.
Consumables and replacement items
Required reagents

Description Quantity/Test Unit Item no.

Monochlor F Reagent Pillows 1 50/pkg 2802246

Recommended standards

Description Unit Item no.

Buffer Powder Pillow, pH 8.3 25/pkg 89868


®
Chlorine Standard Solution, 10-mL Voluette Ampule, 50–75 mg/L 16/pkg 1426810
®
Chlorine Standard Solution, 2-mL PourRite Ampules, 50–75 mg/L 20/pkg 1426820
®
Chlorine Standard Solution, 2-mL PourRite Ampules, 25–30 mg/L 20/pkg 2630020
Nitrogen Ammonia Standard Solution, 100-mg/L as NH3–N 500 mL 2406549
Nitrogen, Ammonia Standard Solution, 1000-mg/L NH3-N 1L 2354153
Organic-free water 500 mL 2641549

Optional reagents and apparatus

Description Unit Item no.


®
Ampule Breaker, PourRite ampules each 2484600
®
Ampule Breaker, Voluette ampules each 2196800
Beaker, glass, 100-mL each 50042H
Flask, volumetric, Class A, 100-mL each 1457442
Monochlor F Reagent Powder Pillows 100/pkg 2802299
Monochloramine/Free Ammonia SpecCheck™ Kit each 2507500
Paper, pH, 0–14 pH range 100/pkg 2601300
Pipet, Mohr, glass, 5-mL each 2093437
®
Pipet, TenSette , 0.1–1.0 mL each 1970001
Pipet tips for TenSette Pipet 1970001 50/pkg 2185696
Pipet tips for TenSette Pipet 1970001 1000/pkg 2185628
Pipet, volumetric, Class A, 2-mL each 1451536
Pipet, volumetric, Class A, 50-mL each 1451541
Rochelle Salt Solution 29 mL 172533
Shears each 2369400
Stir bar, octagonal each 2095352
Stirrer, magnetic each 2881200
Thermometer, non-mercury, -10 to +225 °C each 2635700

6 Chloramine (Mono), Indophenol Method (4.50 mg/L)


Chloramine (Mono), Indophenol Method (4.50 mg/L) 7
FOR TECHNICAL ASSISTANCE, PRICE INFORMATION AND ORDERING: HACH COMPANY
In the U.S.A. – Call toll-free 800-227-4224 WORLD HEADQUARTERS
Outside the U.S.A. – Contact the HACH office or distributor serving you. Telephone: (970) 669-3050
On the Worldwide Web – www.hach.com; E-mail – techhelp@hach.com FAX: (970) 669-2932

© Hach Company/Hach Lange GmbH, 1989–2013. All rights reserved. 04/2013, Edition 8

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