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FACULTY : ENGINEERING

TECHNOLOGY
LABORATORY: CIVIL
ENGINEERING TECHNOLOGY
EXPERIMENT: ANIONIC
SURFACTANT IN
ENVIRONMENTAL SAMPLES

EDITION:
REVISION NO:
EFFECTIVE DATE:

2
FEB
2016

AMENDMENT DATE:

FACULTY OF ENGINEERING TECHNOLOGY


DEPARTMENT OF CIVIL ENGINEERING TECHNOLOGY

WATER SAMPLING TECHNOLOGY LABORATORY


LABORATORY INSTRUCTION SHEETS

COURSE CODE

BNA 40503

EXPERIMENT CODE

EXPERIMENT 4

EXPERIMENT TITLE

ANIONIC SURFACTANTS IN WATER

DATE
GROUP NO.
LECTURER/INSTRUCTOR/TUTOR

1)
2)

DATE OF REPORT SUBMISSION

DISTRIBUTION OF MARKS FOR


LABORATORY REPORT

EXAMINER COMMENTS:

ATTENDANCE/PARTICIPATION/DISIPLINE:

/5%

INTRODUCTION:

/5%

PROCEDURE:

/5%

RESULTS & CALCULATIONS

/15%

ANALYSIS
DISCUSSIONS:
ADDITIONAL QUESTIONS
CONCLUSION

/15%
/20%
/15%
/10%

SUGGESTIONS & RECOMENDATIONS

/5%

REFERENCES:

/5%

TOTAL:

/100%

RECEIVED DATE AND STAMP:

FACULTY : ENGINEERING
TECHNOLOGY
LABORATORY: CIVIL
ENGINEERING TECHNOLOGY
EXPERIMENT: ANIONIC
SURFACTANT IN
ENVIRONMENTAL SAMPLES

EDITION:
REVISION NO:
EFFECTIVE DATE:

2
FEB
2016

AMENDMENT DATE:

STUDENT CODE OF ETHICS


DEPARTMENT OF CIVIL ENGINEERING TECHNOLOGY
FACULTY OF ENGINEERING TECHNOLOGY

I hereby declare that I have prepared this report with my own efforts. I also admit to
not accept or provide any assistance in preparing this report and anything that is
in it is true.
1) Group Leader
Name
:
Matrix No. :

__________________________________________(Signature)
__________________________________
__________________________________

2) Group Member 1
Name
:
Matrix No :

__________________________________________(Signature)
__________________________________
___________________________________

3) Group Member 2
Name
:
Matrix No. :

__________________________________________(Signature)
__________________________________
__________________________________

4) Group Member 3
Name
:
Matrix No. :

__________________________________________(Signature)
__________________________________
__________________________________

FACULTY : ENGINEERING
TECHNOLOGY
LABORATORY: CIVIL
ENGINEERING TECHNOLOGY
EXPERIMENT: ANIONIC
SURFACTANT IN
ENVIRONMENTAL SAMPLES

1.0

EDITION:
REVISION NO:
EFFECTIVE DATE:

2
FEB
2016

AMENDMENT DATE:

OBJECTIVES
a)

To analyze the anionic surfactant in aqueous solutions using Methylene


Blue Absorbing Substances (MBAS) method.

b)

To construct a calibration curve using known concentration of standard


solutions.

c)

To determine the anionic surfactant in water/wastewater sample using


constructed calibration curve.

2.0

LEARNING OUTCOMES
At the end of this course students are able to:
a)

Describe the importance of anionic surfactants in the environmental


studies.

3.0

b)

Measure the anionic surfactants of samples

c)

Identify problems and use their generic skill to solve problems.

d)

Develop their ability to work in group.

INTRODUCTION
3.1 Methylene blue active substances (MBAS) bring about the transfer of
methylene blue, a cationic dye, from an aqueous solution into an
immiscible organic liquid upon equilibration. This occurs through ion pair
formation by the MBAS anion and the methylene blue cation. The intensity
of the resulting blue color in the organic phase is a measure of MBAS.
3.2 Anionic surfactant is among the most prominent of many substances,
natural and synthetic, showing methylene blue activity.
3.3 This method is comprising three successive extractions from acid aqueous
medium containing excess methylene blue into chloroform (CHCl3),
followed by an aqueous backwash and measurement of the blue color in
the CHCl3 by the spectrophotometry at 653 nm. This method is applicable
at MBAS concentrations down to about 0.025 mg/L.
1

FACULTY : ENGINEERING
TECHNOLOGY
LABORATORY: CIVIL
ENGINEERING TECHNOLOGY
EXPERIMENT: ANIONIC
SURFACTANT IN
ENVIRONMENTAL SAMPLES

4.0

EDITION:
2

REVISION NO:

FEB
2016

EFFECTIVE DATE:
AMENDMENT DATE:

CHEMICAL / REAGENTS / INSTRUMENTS /APPARATUS


4.1

Chemicals / Reagents
i)

Stock standard Solution: Dissolve in water 0.10g sodium


dodecyl sulfate (SDS) and dilute to 1L. Store refrigerated to
minimize biodegradation.

ii)

Sodium hydroxide, NaOH, 1N. Dilute 40 g to 1L.

iii)

Sulphuric acid, H2SO4 1N. Add 28 mL concentrated H2SO4 to


distilled water, then dilute to 1 L.

iv)

Chloroform, CHCl3 AR. (Chloroform is toxic and suspected


carcinogen)

v)

Phenolphtalein, 1%: Dissolve 1 g in 50 mL of 95% ethanol. Mix


until dissolve and dilute to 100mL with distilled water in.

vi)

Methylene blue reagent: To a 1 L. flask add 30 mL of 0.1%


methylene blue solution. Add 500 mL distilled water, 6.8 mL
concentrated H2SO4, and 50 g NaH2PO4.

2H2O. Shake to

dissolve and dilute to 1 L.


vii)

Wash solution: Add 6.8 mL concentrate H2SO4 to 500 mL


distilled water. Add 50 g NaH2PO4, H2O and dilute to 1 L.

4.2

viii)

Whatman #1PS (or equivalent hydrophobic filter paper)

ix)

Distilled water

Apparatus/ instrument
i)

Spectrophotometer, (for use a 625 nm, providing a light path of


1 cm or longer

ii) Filter photometer, providing a light path of 1 cm or longer and

equipped

with

red

color

filter

exhibiting

maximum

transmittance near 652 nm.


iii) Separatory funnels: 100 ml, preferably with inert TFE stopcocks

and stoppers.

FACULTY : ENGINEERING
TECHNOLOGY
LABORATORY: CIVIL
ENGINEERING TECHNOLOGY
EXPERIMENT: ANIONIC
SURFACTANT IN
ENVIRONMENTAL SAMPLES

EDITION:
REVISION NO:
EFFECTIVE DATE:

2
FEB
2016

AMENDMENT DATE:

Analytical precautions
Because of inherent properties of surfactants, special analytical precautions
are necessary. Avoid foam formation because the surfactant concentration is
higher in the foam phase than in the associated bulk aqueous phase and the
latter may be significantly depleted. If foam is formed, let it subside by
standing, or collapse it by other appropriate means, and remix the liquid
phase before sampling. Adsorption of surfactant from aqueous solution onto
the wall of containers, when concentrations below about 1 mg/L are present,
may seriously deplete the bulk aqueous phase. Minimize adsorption errors, if
necessary, by rinsing container with sample, and for anionic surfactants by
adding alkali phosphate (e.g., 0.03 N KH2PO4).

5.0 PROCEDURE
5.1

Preparing of calibration curve


i)

Prepare an initial calibration curve consisting of at least five


standards covering the referenced or desired concentration
range.
Suggested amounts of working standard:
mL stock standard solution
completed to 100 mL distilled
water
0.5
1
2
3
5

ii)

Concentration
(mg/L)
0.5
1
2
3
5

Provided that linearity is demonstrated over the range of


interest (r = 0.995 or better).

iii)

Prepare a series of separatory funnels for a reagent blank and


selected standard.

iv)

Pipet portions of standard SDS solution into funnels.

FACULTY : ENGINEERING
TECHNOLOGY
LABORATORY: CIVIL
ENGINEERING TECHNOLOGY
EXPERIMENT: ANIONIC
SURFACTANT IN
ENVIRONMENTAL SAMPLES

v)

EDITION:
REVISION NO:
EFFECTIVE DATE:

2
FEB
2016

AMENDMENT DATE:

Add distilled water to make the total volume 10 mL in each


separatory funnel.

vi)

Treat each standard by follow step 5.2.

vii)

Plot a calibration curve of adsorbance vs micrograms SDS


taken, specifying the molecular weight of the SDS used.

5.2

MBAS method (ion pairing and extraction)

i)

Pipette 10 mL sample to separatory funnels (or other


volume so that total anionic surfactant sample is between
0.15 5 mg/L).

ii)

Add 2 drop of phenophthalein then add (dropwise) NaOH until


pink colour develops.

iii)

Add H2SO4 until pink colour disappears.

iv)

Dispense 10 mL chloroform and 5 mL methylene blue to the


container.

v)

Cap containers tightly, and mix for 30 seconds (rocking


motion).

vi)

Filter mixture through Whatman #1PS (or equivalent


hydrophobic filter paper). Collect filtrate in a 25 mL graduated
cylinder.

vii) Carefully tip the remained aqueous fraction from filter paper
back into universal bottle used in steps (i) to (v).
viii) Add 5 mL chloroform, and repeat steps (v) to (vi). (New filters
must be used).
ix)

Add 2 mL wash solution to the chloroform extract, shake and


filter through the filter paper used in earlier steps. (Note: for
some sample types, this step can be omitted without affecting
the result significantly).

x)

Make up volume to 15 mL with chloroform.

xi)

Measure absorbances at 652 nm against a blank of CHCl 3


(N.B. Use glass cuvettes).

xii) Calculate MBAS from standard curve.

FACULTY : ENGINEERING
TECHNOLOGY
LABORATORY: CIVIL
ENGINEERING TECHNOLOGY
EXPERIMENT: ANIONIC
SURFACTANT IN
ENVIRONMENTAL SAMPLES

EDITION:
2

REVISION NO:

FEB
2016

EFFECTIVE DATE:
AMENDMENT DATE:

6.0 RESULTS CALCULATIONS


6.1

Results
Table 6.1: Anionic surfactants (MBAS method)
Anionic surfactants (MBAS) (mg/L)
Trials

Blank

Sample 1

Sample 2

1
2
3
Average, mg/L

6.2

Calculation

From the calibration curve read microgram of apparent SDS (mol wt ____)
corresponding to the measured absorbance.

Report as MBAS, calculated as SDS, mol wt _________.


7

ANALYSIS
Please analyze the data and results obtained in this experiment.

DISCUSSIONS
Discuss your results both on the basis of any theory presented and on their
relevance to practical applications and current industrial practise. Comment
on the variation of your results and compare them with the recommended
standard values from the Department of Environment, Ministry of Natural
Resources and Environment or other international organization such as EPA,
WHO, EC, etc.

FACULTY : ENGINEERING
TECHNOLOGY
LABORATORY: CIVIL
ENGINEERING TECHNOLOGY
EXPERIMENT: ANIONIC
SURFACTANT IN
ENVIRONMENTAL SAMPLES

EDITION:
REVISION NO:
EFFECTIVE DATE:

2
FEB
2016

AMENDMENT DATE:

ADVANCED QUESTIONS
1. What is an anionic surfactant and gives 5 examples of anionic surfactant
and the application in industry?
2. What was the purpose of the blank sample?
3. Why is it important to determine anionic surfactant test in wastewater
treatment?
4. A sample is collected for anionic surfactant analysis and it is to be
performed on the following day. Describe how the sample can be
preserved. Why is it necessary to preserve the sample?
5. Gives another 3 options to analyse anionic surfactant other than MBAS
method?

10

CONCLUSION
Conclusion is merely a summary, presented in a logical order, of the
important findings already reported in the discussion section. It also relates to
the objectives stated earlier.

Prepared by/Disediakan oleh :

Approved by/Disahkan oleh :

Signature/Tandatangan :
Name/Nama : DR. NOR HASLINA
HASHIM

Signature/Tandatangan :
Name/Nama : DR. SURAYA HANI ADNAN
Date/ Date/Tarikh : FEBRUARY 2016

Date/Tarikh :

FEBRUARY 2016