Titration Application Note
Sulfate Content in Sodium Lauryl Ether Sulfate
Note
by Precipitation Titration
Titration Application
Introduction
The sample:
Sodium lauryl ether sulfate (SLES), also called
sodium laureth sulfate, is one of the most
important anionic surfactants that has found
broad use in detergents and cosmetics [1, 2].
Depending on the chain length of the ethoxy (EO)
unit i.e. CH3-CH2-O- in its molecular structure,
SLES may be a more or less viscous liquid:
Motivation:
On an industrial scale, SLES is mainly produced
by ethoxylation of the long alkyl chain alcohol n-
dodecanol. This step is first followed by the
sulfation of the ethoxylate product, and then by the
final neutralization to obtain the corresponding
T5 Titration Excellence with InMotion Flex – This fully automated system allows for automated sulfate content determination of multiple samples.
The whole system is controlled by the LabX software.
METTLER TOLEDO
M768 v1.0
sodium salt [1]:
2-
Thus, sulfate content SO4 is monitored at the end
of production for quality control.
Titration:
Sulfate content is determined by precipitation
titration using lead nitrate Pb(NO3)2 as a titrant to
form insoluble PbSO4 in a non-aqueous solution.
The titration is monitored with a lead selective
electrode with solid state membrane [3].
Sample preparation and procedures
 2.5 g of sodium lauryl ether sulfate is added in
a titration beaker.
 30 mL deionized water is added to the beaker.
 Subsequently, 30 mL ethanol is added to the
same beaker
 A small magnetic stirrer bar is added, and the
beaker is placed on the internal stirrer of
Titration Excellence, where it is stirred until
complete dissolution – i.e. the mixture is clear,
colorless, and transparent (see picture on the
next page)
Page 1 of 4
 Instruments and Accessories
Titration Application Note

 Titration Excellence T7/T9 or

T5 Package (30252672)
 T7/T9:
- 1 x 10 mL DV1010 burette (51107501),
- 1 x Compact Stirrer (51109150)
 InMotion Flex Base (30094121)
 InMotion Flex Rack Kit 100 mL (30094126)
 Titration beakers PP 100 mL (101974)
 PerfectION LEMO combined Pb-ISE
 The magnetic stirrer bar is removed. (51344830)
 The pH value is adjusted to pH 3 with 0.1 M  LabX software
HCl using a Pasteur pipette (ca. 2-3 mL).  XPE205 Analytical balance (30087653)
 Spatula
 The beaker is connected to the manual titration
 Pasteur pipette
stand of Titration Excellence – In this way, the
next sample can already be prepared by
Results
dissolving it on the internal stand while the
current sample is titrated (Note: change Sample size R1: Sulfate content
2-
[g] [mg SO4 /g]
titration stand).
1 2.7998 10.494
 At the end, the electrode, the stirrer and the 2 2.8391 11.021
tubes are first rinsed with water using a splash 3 2.9822 8.936 *
bottle, and then conditioned 2-3 times in a 4 2.6326 10.088
beaker with deionized water during some time 5 2.4544 9.919
e.g. 30 s. In addition, it may be necessary to 6 2.3670 9.589
gently remove with a paper tissue precipitated 7 2.4576 9.376
lead sulfate. 8 2.3637 12.451*
 Suitable rinsing and cleaning are crucial to Mean 10.081 (1.01%)
achieve correct results. s 0.603
srel 5.984%
Chemistry *) Outliers – excluded from statistics
2-
Sulfate, SO4 ,
M(SO4) = 96.06 g/mol , z = 1 Waste disposal and safety measures
2- 2+
SO4 + Pb → PbSO4 Lead is toxic. Dispose as heavy metal waste.

Solutions and Reagents References

 Titrant: [1] "Tech Profile - Sodium Lauryl Ether Sulfate
Lead nitrate, Pb(NO3)2,
Production", by Intratec Solutions,
c(Pb(NO3)2) = 0.05 mol/L th
Chemical Engineering, 1 of June 2018,
 Sample: https://www.chemengonline.com/sodium-lauryl-ether-
Sodium lauryl ether sulfate (SLES), 2-3 g sulfate-production-2/?printmode=1 , (recalled: 17.10.18).

 Chemicals: [2] "Sodium Laureth Sulfate", Wikipedia

- Ethanol, CH3CH2OH, https://en.wikipedia.org/wiki/Sodium_laureth_sulfate (17.10.18).
- Deionized water, H2O [3] Customer procedure:
- Hydrochloric acid, HCl, c(HCl)=0.1 M
Min Liu, “Inorganic Sulfate/Titration",
 Standard: UMA-HPC Method of Analysis, UMA -5591
Sodium sulfate, Na2SO4, M=142.04 g/mol, November 2014.
50 mg

METTLER TOLEDO Page 2 of 4

M768 v1.0
 Measured values
Titration Application Note

Time Volume Measured value dV Temperature dE 1st deriv. EQP

[s] [mL] [mV] [mL] [°C] [mV] [mV/mL]
0 0.0000 -275.5 25.0
3 0.1145 -274.6 0.1145 25.0 0.9
8 0.1715 -273.3 0.0570 25.0 1.3
13 0.2000 -272.6 0.0285 25.0 0.3

91 4.5500 -253.3 0.4000 25.0 2.6 7.10

97 4.9500 -250.4 0.4000 25.0 2.9 9.41
102 5.3500 -246.4 0.4000 25.0 4.0 12.16
108 5.7500 -241.5 0.4000 25.0 4.9 14.38
6.117514 -235.8 15.13 EQP
113 6.1500 -235.3 0.4000 25.0 6.2 15.10
118 6.5500 -227.6 0.4000 25.0 7.7 14.00
123 6.9500 -222.6 0.4000 25.0 5.0 11.28

158 9.7500 -212.9 0.4000 25.0 0.5

164 10.0000 -212.8 0.2500 25.0 0.1

Comments
 The sensor is first conditioned according to the operating instructions.
 For a quick check of the sensor, ca. 0.03-0.09 g sodium sulfate has been dissolved in 50 mL deionized
water and titrated with 0.05 M Pb(NO3)2 after acidifying with 0.1 M HCl

 Subsequently, the sample SLES has been titrated in water:ethanol 30 mL:30mL.

 Clean the electrode with deionized water, and -if needed- condition it in deionized water for 2-3 min. before
starting the next sample.

METTLER TOLEDO Page 3 of 4

M768 v1.0
 Method
Titration Application Note

001 Title 006 Calculation R1

Type General titration Result Sulfate in SLES
Compatible with T5/T7/T9 Result unit mg/g
ID M768 Formula R1 = Q*C/m
Title Sulfate in SLES Constant C = M/z
… M M[Sulfate]
Z z[Sulfate]
002 Sample Decimal places 3
Result limits No
Number of IDs 1
Extra statistical calculations No
ID 1 SLES
Send to buffer No
Entry type Weight
Write to SmartTag None
Lower limit 2.0 g
Condition No
Upper limit 3.0 g
Density 1.0 g/mL
Correction factor 1.0 007 End of sample
Temperature 25.0 °C
Entry Arbitrary
Titrator reader None
Number of sample factors 0

003 Titration stand (Manual stand)

Type Manual stand
Titration stand Manual stand 1

004 Stir
Speed 30 %
Duration 30 s

005 Titration (EQP) [1]

Titrant
Titrant Pb(NO3)2
Concentration 0.05 mol/L
Sensor
Type ISE
Sensor perfectION Pb
Unit mV
Ion charge 2
Temperature acquisition
Temperature sensor No
Stir
Speed 30 %
Predispense
Mode Volume
Volume 0.2 mL
Wait time 15 s
Control
Control User
Titrant addition Dynamic
dE (set value) 8.0 mV
dV (min) 0.1 mL
dV (max) 0.4 mL
Mode Equilibrium controlled
dE 1.0 mV
dt 2s
t (min) 5s
t (max) 30 s
Evaluation and recognition
Procedure Standard
Threshold 10 mV/mL
Tendency Positive
Ranges 0
Add. EQP criteria Last EQP
Last jumps 1
Termination
At Vmax 10 mL
At potential No
At slope No
After number of recognized EQPs No
Combined termination criteria No
Accompanying stating
Accompanying stating No
Condition
Condition No

METTLER TOLEDO Page 4 of 4

M768 v1.0