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FACULTY : ENGINEERING TECHNOLOGY EDITION:
LABORATORY: CIVILENGINEERING TECHNOLOGY REVISION NO:
2
EXPERIMENT: ANIONICSURFACTANT INENVIRONMENTAL SAMPLES
EFFECTIVE DATE: FEB2016AMENDMENT DATE:
FACULTY OF ENGINEERING TECHNOLOGYDEPARTMENT 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/TUTOR1)2)
DATE OF REPORT SUBMISSION
DISTRIBUTION OF MARKS FORLABORATORY REPORT
ATTENDANCE/PARTICIPATION/DISIPLINE: /5%
INTRODUCTION: /5%
PROCEDURE: /5%RESULTS & CALCULATIONS /15%
ANALYSIS /15%DISCUSSIONS: /20%ADDITIONAL QUESTIONS /15%CONCLUSION /10%
SUGGESTIONS & RECOMENDATIONS /5%
REFERENCES: /5%
TOTAL: /100%
EXAMINER COMMENTS: RECEIVED DATE AND STAMP:
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FACULTY : ENGINEERING TECHNOLOGY EDITION:
LABORATORY: CIVILENGINEERING TECHNOLOGY REVISION NO:
2
EXPERIMENT: ANIONICSURFACTANT INENVIRONMENTAL SAMPLES
EFFECTIVE DATE: FEB2016AMENDMENT 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 __________________________________________(Signature)Name : __________________________________Matrix No. : __________________________________
2) Group Member 1 __________________________________________(Signature)Name : __________________________________Matrix No : ___________________________________
3) Group Member 2 __________________________________________(Signature)Name : __________________________________Matrix No. : __________________________________
4) Group Member 3 __________________________________________(Signature)Name : __________________________________Matrix No. : __________________________________
8/16/2019 Exp 4 Determination of Anionic Surfactant in Water Sample
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FACULTY : ENGINEERING TECHNOLOGY EDITION:
LABORATORY: CIVILENGINEERING TECHNOLOGY REVISION NO:
2
EXPERIMENT: ANIONICSURFACTANT INENVIRONMENTAL SAMPLES
EFFECTIVE DATE: FEB2016AMENDMENT DATE:
1.0
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.
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.
3.0 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 (CHCl 3 ),
followed by an aqueous backwash and measurement of the blue color in
the CHCl 3 by the spectrophotometry at 653 nm. This method is applicable
at MBAS concentrations down to about 0.025 mg/L.
8/16/2019 Exp 4 Determination of Anionic Surfactant in Water Sample
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FACULTY : ENGINEERING TECHNOLOGY EDITION:
LABORATORY: CIVILENGINEERING TECHNOLOGY REVISION NO:
2
EXPERIMENT: ANIONICSURFACTANT INENVIRONMENTAL SAMPLES
EFFECTIVE DATE: FEB2016AMENDMENT DATE:
4.0
CHEMICAL / REAGENTS / INSTRUMENTS /APPARATUS4.1 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, H 2SO 4 1N. Add 28 mL concentrated H 2SO 4 to
distilled water, then dilute to 1 L.
iv) Chloroform, CHCl 3 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 H 2SO 4 , and 50 g NaH 2PO 4. 2H 2O. Shake to
dissolve and dilute to 1 L.
vii) Wash solution: Add 6.8 mL concentrate H 2SO 4 to 500 mL
distilled water. Add 50 g NaH 2PO 4 , H 2O and dilute to 1 L.
viii) Whatman #1PS (or equivalent hydrophobic filter paper)
ix) Distilled water
4.2
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 a red color filter exhibiting maximum
transmittance near 652 nm.
iii) Separatory funnels: 100 ml, preferably with inert TFE stopcocks
and stoppers.
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8/16/2019 Exp 4 Determination of Anionic Surfactant in Water Sample
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FACULTY : ENGINEERING TECHNOLOGY EDITION:
LABORATORY: CIVILENGINEERING TECHNOLOGY REVISION NO:
2
EXPERIMENT: ANIONICSURFACTANT INENVIRONMENTAL SAMPLES
EFFECTIVE DATE: FEB2016AMENDMENT DATE:
v) 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 between0.15 – 5 mg/L).
ii) Add 2 drop of phenophthalein then add (dropwise) NaOH untilpink colour develops.
iii) Add H 2SO 4 until pink colour disappears.
iv) Dispense 10 mL chloroform and 5 mL methylene blue to thecontainer.
v) Cap containers tightly, and mix for 30 seconds (rockingmotion).
vi) Filter mixture through Whatman #1PS (or equivalenthydrophobic filter paper). Collect filtrate in a 25 mL graduatedcylinder.
vii) Carefully tip the remained aqueous fraction from filter paperback into universal bottle used in steps (i) to (v).
viii) Add 5 mL chloroform, and repeat steps (v) to (vi). (New filtersmust be used).
ix) Add 2 mL wash solution to the chloroform extract, shake andfilter through the filter paper used in earlier steps. (Note: forsome sample types, this step can be omitted without affectingthe 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.
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FACULTY : ENGINEERING TECHNOLOGY EDITION:
LABORATORY: CIVILENGINEERING TECHNOLOGY REVISION NO:
2
EXPERIMENT: ANIONICSURFACTANT INENVIRONMENTAL SAMPLES
EFFECTIVE DATE: FEB2016AMENDMENT DATE:
6.0 RESULTS CALCULATIONS
6.1
Results
Table 6.1: Anionic surfactants (MBAS method)
TrialsAnionic surfactants (MBAS) (mg/L)
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.
8 DISCUSSIONS
Discuss your results both on the basis of any theory presented and on their
relevance to practical applications and current industrial practise. Commenton 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.
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FACULTY : ENGINEERING TECHNOLOGY EDITION:
LABORATORY: CIVILENGINEERING TECHNOLOGY REVISION NO:
2
EXPERIMENT: ANIONICSURFACTANT INENVIRONMENTAL SAMPLES
EFFECTIVE DATE: FEB2016AMENDMENT DATE:
9 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 :
Signature/ Tandatangan :Name/ Nama : DR. NOR HASLINA
HASHIM
Date/ Tarikh : FEBRUARY 2016
Approved by/ Disahkan oleh :
Signature/ Tandatangan :Name/ Nama : DR. SURAYA HANI ADNAN
Date/ Tarikh : FEBRUARY 2016
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