DR 4000 Detergents-Surfactants Method 8028

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)

Page 1 of 6
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.

Page 2 of 6
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.
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.

Page 3 of 6

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.

Page 4 of 6

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.

Page 5 of 6

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 [email protected]
Hach Company, 1997-2003. All rights reserved. Printed in the U.S.A.
Page 6 of 6
HACH COMPANY
WORLD HEADQUARTERS
Telephone: (970) 669-3050
FAX: (970) 669-2932
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DR/4000

Crystal Violet Method*

Scope and Application: For water, wastewater and seawater.

1. Press the soft key

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

Select the stored program

HACH PROGRAM: 1850

The wavelength (),

graduated cylinder to the

DETERGENTS, Anionic (Surfactants)

DETERGENTS, Anionic (Surfactants), continued

5. Add the contents of

7. Place the separatory

Note: Spilled reagent will

Note: Use benzene only in

Note: Excessive agitation

8. After the timer beeps,

9. Drain the top

10. Fill another

11. Place the blank in

sample cell to the 25-mL

the cell holder and close

Note: The benzene

DETERGENTS, Anionic (Surfactants)

12. Press the soft key

DETERGENTS, Anionic (Surfactants), continued

13. Place the prepared

Interference Levels and Treatments

Interferes at all levels

Interferes at all levels

Sample Collection, Storage and Preservation

DETERGENTS, Anionic (Surfactants)

DETERGENTS, Anionic (Surfactants), continued

95% Confidence Limits

0.1470.153 mg/L LAS

0.005 mg/L LAS

0.0026 mg/L LAS

0.0038 mg/L LAS

0.0047 mg/L LAS

See Section 1.5.3 Sensitivity Explained for more information.

DETERGENTS, Anionic (Surfactants)

DETERGENTS, Anionic (Surfactants), continued

Pollution Prevention and Waste Management

DETERGENTS, Anionic (Surfactants)

DETERGENTS, Anionic (Surfactants), continued

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

REQUIRED EQUIPMENT AND SUPPLIES

OPTIONAL REAGENTS AND STANDARDS

OPTIONAL EQUIPMENT AND SUPPLIES

FOR TECHNICAL ASSISTANCE, PRICE INFORMATION AND ORDERING:

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

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