Exp 4 Determination of Anionic Surfactant in Water Sample

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:

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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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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. : __________________________________


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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.


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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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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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6.0 RESULTS CALCULATIONS

6.1

Results

Table 6.1: Anionic surfactants (MBAS method)

TrialsAnionic surfactants (MBAS) (mg/L)

Blank Sample 1 Sample 2

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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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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

Exp 4 Determination of Anionic Surfactant in Water Sample

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