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DR/4000

PROCEDURE

DETERGENTS, Anionic
(Surfactants)

Method 8028

Crystal Violet Method*


(0 to 0.275 mg/L)

Scope and Application: For water, wastewater and seawater.


The estimated detection limit for program number 1850 is 0.005 mg/L LAS.
* Analytical Chemistry, 38, 791 (1966)

HACH
PROGRAM

HACH PROGRAM:1850
Detergents, Anion.

ENTER

1. Press the soft key


under HACH PROGRAM.

2. The display will show: 3. Fill a clean 500-mL

Select the stored program


for anionic detergents
(surfactants) by pressing
1850 with the numeric keys.

Detergents, Anion.

HACH PROGRAM: 1850

The wavelength (),


605 nm, is automatically
selected.

graduated cylinder to the


300-mL mark with
sample. Pour the sample
into a clean 500-mL
separatory funnel.

4. Add 10 mL of Sulfate
Buffer Solution. Stopper
the funnel. Shake the
funnel for 5 seconds.

Press: ENTER
Note: If samples cannot be
analyzed immediately, see
Sample Collection, Storage
and Preservation
following these steps.
Note: The Flow Cell and
Sipper Modules cannot be
used for this procedure.

DetergentsAni_None_Other_CVI_Eng_4000.fm

DETERGENTS, Anionic (Surfactants)


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DETERGENTS, Anionic (Surfactants), continued

START
TIMER

5. Add the contents of


one Detergents Reagent
Powder Pillow to the
funnel. Stopper the
funnel and shake to
dissolve the powder.

6. Add 30 mL benzene
to the funnel. Stopper the
funnel. Gently shake the
funnel for one minute.

7. Place the separatory


funnel in a support stand,
and press the soft key
under START TIMER.

Note: Spilled reagent will


affect test accuracy and is
hazardous to the skin and
other materials.

A 30-minute reaction
period will begin.

Note: Use benzene only in


well-ventilated areas.

Note: Excessive agitation


may cause an emulsion to
form, requiring a longer time
for phase separation. For
these samples, remove most
of the water layer, then
gently agitate the funnel with
a clean inert object in the
funnel such as a Tefloncoated magnetic stirring bar.

8. After the timer beeps,


remove the stopper and
drain the bottom water
layer. Discard this layer
into an appropriate waste
collection container.
Note: Benzene solutions
are a regulated waste and
cannot be poured down
the drain. See Pollution
Prevention and Waste
Management following
these steps.

ZERO

9. Drain the top


benzene layer into a clean
25-mL sample cell
(the prepared sample).

10. Fill another

11. Place the blank in

sample cell to the 25-mL


mark with pure benzene
(the blank).

the cell holder and close


the light shield.

Note: The benzene


layer cannot be filtered
before color measurement.
Filtration removes the
blue color.

DETERGENTS, Anionic (Surfactants)


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12. Press the soft key


under ZERO.
The display will show:
0.000 mg/L LAS
Note: For alternate
concentration units,
press the soft key under
OPTIONS. Then press the
soft key under UNITS to scroll
through the available
options. Press ENTER to
return to the read screen.

DetergentsAni_None_Other_CVI_Eng_4000.fm

DETERGENTS, Anionic (Surfactants), continued

13. Place the prepared


sample into the cell
holder. Close the light
shield. The result in mg/L
anionic detergents as
LAS (or chosen units) will
be displayed.
Note: Acetone may be
used to clean benzene
from glassware.

Interferences
Table 1 Interfering Substances and Suggested Treatments for Powder Pillows
Interfering Substance

Interference Levels and Treatments

Chloride

High amounts of chloride, such as those levels found in brines and seawater, will cause low
results.

Perchlorate ions

Interferes at all levels

Periodate ions

Interferes at all levels

Sample Collection, Storage and Preservation


Collect samples in clean plastic or glass bottles. Analyze samples as soon as
possible, but they may be stored at least 24 hours by cooling to 4 C (39 F).
Warm to room temperature before testing.

Accuracy Check
Standard Additions Method
a. Leave the unspiked sample in the sample cell compartment. Verify that the
units displayed are in mg/L. Select standard additions mode by pressing
the soft keys under OPTIONS, (MORE) and then STD ADD.
b. Press ENTER to accept the default sample volume (mL), 300.
c. Press ENTER to accept the default standard concentration
(mg/L LAS), 60.000.
d. Press the soft key under ENTRY DONE.
e. Snap the neck off a Detergent Voluette Ampule Standard, 60 mg/L LAS.

DetergentsAni_None_Other_CVI_Eng_4000.fm

DETERGENTS, Anionic (Surfactants)


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DETERGENTS, Anionic (Surfactants), continued


f.

Use the TenSette Pipet to add 0.1 mL, 0.2 mL and 0.3 mL of standard,
respectively to three 300-mL samples and mix each thoroughly.

g. Analyze each standard addition sample and as described above. Accept the
standard additions readings by pressing the soft key under READ each
time. Each addition should reflect approximately 100% recovery.
h. After completing the sequence, the display will show the extrapolated
concentration value and the best-fit line through the standard additions
data points, accounting for matrix interferences.
See Section 1.4.1 Standard Additions for more information.

Method Performance
Precision
Standard: 0.150 mg/L LAS
Program

95% Confidence Limits

1850

0.1470.153 mg/L LAS

For more information on determining precision data and method detection limits,
refer to Section 1.5.
Estimated Detection Limit
Program

EDL

1850

0.005 mg/L LAS

For more information on derivation and use of Hachs estimated detection limit,
see Section 1.5.2. To determine a method detection limit (MDL) as defined by the
40 CFR part 136, appendix B, see Section 1.5.1.
Sensitivity
Program Number: 1850
Portion of Curve:

Abs

Concentration

0.010 Abs

0.010

0.0026 mg/L LAS

0.16 mg/L

0.010

0.0038 mg/L LAS

0.288 mg/L

0.010

0.0047 mg/L LAS

See Section 1.5.3 Sensitivity Explained for more information.

DETERGENTS, Anionic (Surfactants)


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DETERGENTS, Anionic (Surfactants), continued


Calibration Standard Preparation
To perform a surfactant calibration using the crystal violet method, use a Detergent
Voluette Ampule Standard, 60-mg/L LAS (Cat. No. 14271-10).
Prepare calibration standards containing 0.012, 0.06, 0.096, 0.12, 0.18, and a
0.24 mg/L LAS as follows:
a. Into six different Class A 500 mL volumetric flasks, pipet 0.1, 0.5,
0.8, 1.0, 1.5 and 2.0 mL of the 60-mg/L LAS stock solution using a
TenSette Pipet.
b. Dilute to the mark with deionized water. Mix thoroughly.
c. Using the crystal violet method and the calibration procedure described in
the User-Entered Programs section of the DR/4000 Spectrophotometer
Instrument Manual, generate a calibration curve from the standards
prepared above.

Summary of Method
Detergents, ABS (alkyl benzene sulfonate) or LAS (linear alkylate sulfonate) are
determined by association with crystal violet dye and extraction of the ion-pair
complex into benzene.

Safety
Good safety habits and laboratory techniques should be used throughout the
procedure. Consult the Material Safety Data Sheet for information specific to the
reagents used. For additional information, refer to Section 1.

Pollution Prevention and Waste Management


Benzene (D018) solutions are regulated as hazardous waste by the Federal RCRA.
Do not pour these materials down the drain. Collect water saturated with benzene
and benzene solutions for disposal with laboratory solvent wastes. See Section 1
for more information on proper disposal of these materials.

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DETERGENTS, Anionic (Surfactants)


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DETERGENTS, Anionic (Surfactants), continued


REQUIRED REAGENTS AND STANDARDS
Detergents Reagent Set ...........................................................................................................................24468-00
Includes: (2) 452-49, (3) 1008-68, (1) 14440-17
Quantity Required
per test

Description

Unit

Cat. No.

Benzene, ACS ................................................................................. 55 mL .....................4 L.................14440-17


Buffer Solution, sulfate-type ........................................................... 10 mL ..............500 mL.....................452-49
Detergent Reagent Powder Pillows ................................................ 1 pillow.............. 25/pkg...................1008-68

REQUIRED EQUIPMENT AND SUPPLIES


Clippers, for opening powder pillows ..................................................1 ....................... each.....................968-00
Cylinder, graduated, 25-mL .................................................................1 ....................... each.....................508-40
Cylinder, graduated, 50-mL .................................................................1 ....................... each.....................508-41
Cylinder, graduated, 500-mL ...............................................................1 ....................... each.....................508-49
DR/4000 1-Inch Cell Adapter ..............................................................1 ....................... each.................48190-00
Funnel, separatory, 500-mL .................................................................1 ....................... each.....................520-49
Support Ring, 4-inch ............................................................................1 ....................... each.....................580-01
Support, Ring Stand, 5 x 8 in. base ......................................................1 ....................... each.....................563-00

OPTIONAL REAGENTS AND STANDARDS


Acetone, ACS............................................................................................................500 mL.................14429-49
Benzene, ACS ...........................................................................................................500 mL.................14440-49
Detergent Standard Solution, 10-mL Voluette Ampule, 60-mg/L LAS..................... 16/pkg.................14271-10

OPTIONAL EQUIPMENT AND SUPPLIES


Ampule Breaker Kit ....................................................................................................... each.................21968-00
DR/4000 Carousel Module Kit ...................................................................................... each.................48070-02
Pipet, TenSette, 0.1 to 1.0 mL ........................................................................................ each.................19700-01
Pipet Tips, for 19700-01 Pipet ................................................................................... 50/pkg.................21856-96

FOR TECHNICAL ASSISTANCE, PRICE INFORMATION AND ORDERING:


In the U.S.A. Call toll-free 800-227-4224
Outside the U.S.A. Contact the HACH office or distributor serving you.
On the Worldwide Web www.hach.com; E-mail techhelp@hach.com

Hach Company, 1997-2003. All rights reserved. Printed in the U.S.A.

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HACH COMPANY
WORLD HEADQUARTERS
Telephone: (970) 669-3050
FAX: (970) 669-2932

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DetergentsAni_None_Other_CVI_Eng_4000.fm