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The study showed that the flux decrease was significant with every variation of the process parameter. In general, the decrease in flux over time is caused by the impurities deposited on the surface and inner pores of the membrane.

Fig 1. Schematic Illustration of Ultrafiltration Cell with control temperature.

Blocking Mechanism

This strengthens the evidence that fatty acids which are still dissociated at pH 7 enter the pores and cause blockages in the membrane pores. If there is an interaction between fatty acids and membranes, it forms a negative charge induction in the membrane.

Conclusions

Nomenclatures

Ultrafiltration of palm oil-oleic acid-glycerin solutions: Fouling mechanism identification, of palm oil-oleic acid-glycerin solutions: Fouling mechanism identification, fouling mechanism analysis and membrane characterizations. Ultrafiltration of protein and humic substances: effect of solution chemistry on fouling and flux decline.

Paper ID CE19004 /Review of a paper, First Round Result with Rejection/

Technical aspects

Comments to the authors (You may use another sheet of paper.)

Recommendation (Tick one) 1. Accepted without modifications

Comments to the editors (These comments will not be sent to the authors)

Please use dot, instead of comma, for writing numbers with decimals
Please use degree sign ° to describe “degree”, and do not use superscripted zero “0”, superscripted uppercase
Please write “min” or “mins” in the whole manuscript, to describe “minute” or “minutes”
Please write “h” in the whole manuscript, to describe “hour” or “hours”
Do not replace the word “or” using the symbol “/” !!
Abstract: please write “transmembane pressure (TMP)”, and then write it consistently as TMP, TMP and TMP
Abstract: “…Experiments were carried out at…”
Abstract: “…free fatty acid (FFA)…”
Section 1 paragraph 1: What are the disadvantages of crude glycerin? Add more references!
Section 1 paragraph 1: …free fatty acid (FFA), fatty acid methyl ester (FAME, or biodiesel)…
Section 1 paragraph 1: Add space to split the word “alcoholand”
Section 1 paragraph 2: You mentioned about “other purification processes”, but no references at all !!
Section 1 paragraph 3: “Separation of glycerin from FAME by UF and microfiltration…”
Section 1 paragraph 3: What is the reference number for the citation “[Saleh]” ???
Section 1 paragraph 3: ASTM stands for what? Please write it down
Section 1 paragraph 3: Please consistently write FFA, FFA, and FFA throughout the entire manuscript!
Section 1 paragraph 3: The proper name of the polymer is “polyethersulfone”, with lowercase l, and with “f”
Section 1 paragraph 3: Describe the details on the results and findings from Mah et al [10, 11]
Section 2.1 paragraph 1: You use a membrane with relatively wide pore (1000 Da MWCO) to separate glycerol (92 Da) from water (18 Da) and other small molecules??? Such a FATAL error in planning the experiment
Figure 1: What is the hexagon in circle? Describe!
Section 2.2 paragraph 2: “…for 60 mins…”
Section 2.2 paragraph 2: “…inside the UF cell…”
Section 2.2 paragraph 2: “…collected for 120 mins, with interval of 5 mins…”
Section 2.2 paragraph 2: Permeate FLUX! Not “fluxes”
Equation 1: remove the “x”
Section 2.2 paragraph 3: delete “transmembrane pressure” and then write it consistently as TMP, TMP and TMP
Section 2.2 paragraph 3: “…carried out for 60 mins, with interval of 10 mins.”
Section 2.3 paragraph 1: “gas chromatography (GC, Shimadzu TQ8030).”
Section 3 paragraph 1: What is the reason and justification of using the Hermia model? Write it down!
Section 2.3 paragraph 2: Use uppercase “C” for the beginning of Section 2.3 paragraph 2!
Section 2.3 paragraph 2: Change “/” with “or”
Section 2.3 paragraph 2: Equation 1? This is wrong, maybe you refer to Equation 3?
Table 1: Please use lowercase letters in all words, except for the beginning of the sentences
Section 4: Delete “transmembrane pressure”, and then write it consistently as TMP, TMP and TMP
Section 4: “…sampled every 5 mins… for its composition by using GC.”
Title of Section 4.1.1: Delete “transmembrane pressure”, and then write it consistently as TMP, TMP and TMP
Section 4.1.1 paragraph 1: “UF process is one method to…using TMP as a driving force”
Change the label of x axis in Figures 2, 3, 4, 5 with “mins”
Section 4.1.1 beginning of paragraph 2: Which figure confirms the correlation between flux and TMP?
Section 4.1.1 paragraph 2: “30-60 mins”
Section 4.1.1 paragraph 2: “…as the result of the increasing deposit and impurities…”
Section 4.1.1 paragraph 2: “The impurities were carried away…”
Please repeat all the experiments with a replicate (duplo) or two replicates (triplo), because all the results in Figures 2, 3, and 4 are insignificant, not worth mentioning
Table 2: Maximum rejection of mediocre 70%, due to filtering small molecules by using wide and sparse sieve…
Table 3: Where are the fitting for all the data shown in Table 3?? There should be a set of 12 (twelve) plots!
Section 4.2 paragraph 2: “…which tend to dissociate at acidic environment…”
Section 4.2 paragraph 3: Please change “minutes” to mins!
Section 4.2 paragraph 3: “The foulant is the piled up… in irregular…”
Section 4.2 paragraph 4: Add references that support the negative charge induction caused by the interaction between fatty acid and membrane!
Section 4.2 paragraph 4: “This condition may also cause changes in the fluid resistance to the membrane [8].”
Nomenclature: Please use UPPERCASE for the letters in the beginning of a sentence!
Nomenclature: Permeate FLUX! Not “fluxE”

There is no innovation, and it is also carelessly planned, as the authors used a commercial membrane with a 1000 Da MWCO (molecular weight cutoff) to filter glycerol (92 Da, much smaller molecule, compared to the membrane pore diameter) . . Section heading 4.1.1: Delete "transmembrane pressure" and then write it consistently as TMP, TMP, and TMP.

Recommendation (Tick one)

Introduction
Materials and Method 1. Materials

Ultrafiltration Membrane
Analysis

Model of Blocking Mechanism
Results and Discussion

Effect of Trans Membrane Pressure (TMP) on permeate fluxes Ultrafiltration process is one method to separate substances which have different
Temperature effect on permeate fluxes
Effect of pH on permeate fluxes
Rejection

The hydrophobic property is in contrast to the hydrophilic properties of the membrane properties used in this study. The adsorption forms on the membrane surface as well as at the entrance of the membrane pore and then causes high flux decline and membrane fouling [8,17–18].

Comments to the editors (These comments will not be sent to the authors) Recommended

Title of the article: PURIFICATION OF GLYCERIN-RICH SOLUTION FROM PALM OIL BASED PRODUCTION BIODIESEL BY ULTRAFILTRATION MEMBRANE.

Title of paper

In the introduction, what are the current limitations of using UF for glycerol purification? what is the objective of this study? Or what is this study trying to improve? Reduce the effect of flux decline or just
For all equations in the manuscript, after each equation, please specify each papameter, its name, and unit
In the method section, Gas Chromatography was used for analysis. Operating condition for this analysis applied for glycerol must be mentioned here
The paragraph right after the results and discussion, ‘For flux decline study and blocking mechanism… in raw glycerin.’ This part should be moved to method section
Since the objectives of this study was missing in the introduction. The conclusion should say if the objectives are achieved
Is using UF a good solution for glycerol purification? Since flux decline occurs very soon after the system start for all studied parameters at various range
Comments to the editors (These comments will not be sent to the authors) This paper need to improve more its formatting

3-10-2020 Department of Chemical Engineering, Diponegoro University Mail - REVISION of paper ID CE19004 / Review of a paper, first round Re.

REVISION of Paper ID CE19004 /Review of a paper, First Round Result with Rejection/

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PURIFICATION OF GLYCERIN-RICH SOLUTION FROM PALM OIL BASED PRODUCTION BIODIESEL BY ULTRAFILTRATION

MEMBRANE

Materials and Methods 1. Materials

UF Membrane
Model of Blocking Mechanism

XX(Y) In equation (2), R (%) is the rejection of FFA or impurities, Cf (mg/L) is the concentration of FFA or impurities in the feed, Cp (mg/L) is the concentration of FFA or impurities in the permeate . Hermia's model defined the fouling mechanism, particularly in the porous membrane filtration of the dead-end system.

Table 1. Linearization equation of blocking models based on Hermia’s model [16]

Result and Discussion

Flux decline and rejection

Effect of TMP on Permeate Flux
Temperature Effect on Permeate Flux
Effect of pH on Permeate Flux
Rejection

Blocking Mechanism

The hydrophobicity of FFA has different characteristics from the hydrophilic properties of the membrane used in this study. It has been found that the hydrophobic properties of the impurity (FFA) can increase the repulsion forces on the membrane, which ultimately affects the flow tendency that occurs during the filtration process (mass transfer mechanism). Furthermore, increasing temperature can lead to an increase in the mobility of the polymer bond within the membrane matrix [12,23].

Adsorption forms on the membrane surface as well as at the entrance of the membrane pores and then causes high flux drop and membrane fouling. At pH 9, this phenomenon may be due to the fact that dissociated fatty acid molecules (at pH 9, fatty acid molecules are almost completely dissociated) block the membrane micropores. It shows that the liquid resistance to the membrane is greater and causes more severe fouling than in the alkaline condition.

Table 2. Summary of rejection data in various variations of process parameters.

Time (mins)pH = 6.33

Conclusions

Both pressure and temperature did not have a significant effect on the flux drop due to the dominance of the mass transfer mechanism, which is caused by the nature of impurities themselves. Effects of palm oil-based fatty acids on fouling of ultrafiltration membranes during clarification of glycerin-rich solution. Ultrafiltration of Palm Oil-Oleic Acid-Glycerin Solutions: Fouling Mechanism Identification, Palm Oil-Oleic Acid-Glycerin Solutions: Fouling Mechanism Identification, Fouling Mechanism Analysis and Membrane Characterizations.

A Feasibility Investigation on Ultrafiltration of Palm Oil and Removal of Oleic Acid from Glycerol Investigation on Ultrafiltration of Palm Oil and Removal of Oleic Acid from Glycerol Solutions: Flux Drop, Fouling Pattern, Rejection and Membrane Characterizations. Flux Profiles and Mathematical Modeling of Fouling Mechanism for Ultrafiltration Mathematical Modeling of Fouling Mechanism for Ultrafiltration of KonjacGlucomannan. Analysis of membrane pore blocking models applied to ultrafiltration of membrane pore blocking models applied to PEG ultrafiltration. Separation and purification technology.

Address all the concerns/recommendations of the reviewers

All amendments made are to be highlighted in red color in the revised paper

Reviewer # 1 Final

Recommendation

Accepted without modification

Accepted with minor corrections

Accepted with major modification

Rejected

Please write “min” or “mins” in the whole manuscript, to describe “minute” or “minutes
Please write “h” in the whole manuscript, to describe
Do not use unit with the “/” character! For example use
Abstract: please write “transmembane pressure (TMP)”, and then write it consistently as TMP, TMP
Section 1 paragraph 1: Please mention what are the components classified as MONG. It should be written as
of 10 13. Section 1 paragraph 1: What are the disadvantages of

who explored pervaporation as a new process to handle and purify viscous and hygroscopic liquid (ethylene glycol) which is quite similar to glycerin. However, we believe that the paper you suggest is not similar to our process.

Section 1 paragraph 3: Please use uppercase A for the beginning of the sentence “A similar result was also

Section 2.2 paragraph 3: delete “transmembrane pressure” and then write it consistently as TMP, TMP

Section 3 paragraph 1: What is the reason and

Section 4.1.1 beginning of paragraph 2: Which figure confirms the correlation between flux and TMP?

Section 4.1.1 paragraph 2: “…as the result of the increasing deposit and impurities…”

Table 2: Maximum rejection of mediocre 70%, due to filtering small molecules by using wide and sparse

Table 3: Where are the fitting for all the data shown in Table 3?? There should be a set of 12 (twelve) plots!

Section 4.2 paragraph 2: “…which tend to dissociate at acidic environment…”

Section 4.2 paragraph 4: Add references that support the negative charge induction caused by the interaction

Section 4.2 paragraph 4: “This condition may also cause changes in the fluid resistance to the membrane [8].”

Nomenclature: Please use UPPERCASE for the letters in the beginning of a sentence!

Reviewer # 2 Final

Reply/Action taken

Reviewer # 3 Final

Provide the fixed value of pH and temperature at varied TMP Y The fixed value of pH and temperature has been provided. Give a fixed value of pressure and temperature Y The values of pressure and temperature are given. What is the initial pH of the feed sample. Y The initial pH of the feed sample is given.

Note and discuss the rejection obtained in this study with other publications on glycerin rejection.

Reviewer # 4 Final

Reviewer # 5 Final

Final

Paper ID CE19004 /A progress of Review Process/

10/3/2020 Institut for Kemiteknik, Diponegoro University Mail - Papir ID CE19004 /Review of a paper, Second Round Result/.

Paper ID CE19004 /Review of a paper, Second Round Result/

2/3 This message (including any attachments) is intended solely for the use of the individual or entity to whom it is addressed and may contain information that is non-public, proprietary, privileged, confidential and exempt from disclosure under applicable law or may to constitute as a product of the lawyer's work. If you have received this communication in error, notify us immediately by telephone and (i) destroy this message if it is a facsimile or (ii) delete this message immediately if this is an electronic communication. However, in the attached file, there were only reports from reviewer 1 and reviewer 5, and I could not find the report from reviewer 3.

Subject: Re: Paper ID CE19004 /Review of a paper, Second Round Result/

Communications aspects

There are a number of issues that have not been addressed well enough by the authors, so REJECT is still recommended.

Review of JESTEC CE19004.R1 - Purification of glycerin-rich solution from palm oil based production biodiesel by ultrafiltration membrane

Section 1, paragraph 4: Similar works have been done before

Section 1, subsection 4: Write reason/justification why no pretreatment was done to achieve >95% pure concentration. This is why the ultrafiltration trials in this study (with no modification initiated) should only give 70% rejection, as the permeate streams contain not only glycerin, but also 300 Da fatty acids, also water (most likely).

Section 3.1.1, paragraph 4: Any data for contact angle of free fatty acids that reflect their hydrophobic properties?

Figure 4, Y-axis: “glycerin”, not “glycerinE”

Section 3.1.3: Edit the excess square bracket

Abbreviation: add PO, OA, NGOM, FAME into the list

27 is the correct one (with abbreviated name) and the format of other references should be changed.

The research showed that the flux drop was significant at all variations of the process parameter. It showed that the flux drop became worse in the presence of the acidic environment. In addition, investigation of the blocking mechanism of the UF membrane in crude glycerin purification was addressed.

Determination based on the accumulation of the solute on the membrane surface is representative of cake or gel formation [10]. This behavior can occur due to the nature of the impurities, as described in section 3.1.3. To improve UF performance, pretreatment of crude glycerin or membrane surface modification is required.

Revision of Paper ID CE19004 /Review of a paper, Second Round Result/

Result and Discussion 1. Flux decline and rejection

In general, the decline in flux over time is caused by impurities that accumulate on the surface and inside the pores of the membrane. In addition, an increase in temperature can lead to an increase in polymer bond mobility within the membrane matrix [16,30]. In addition, the flux can directly increase along with the decrease in viscosity, which can lead to an increase in the impurity concentration both on the surface and in the internal pores of the membrane.

Adsorption occurs at the membrane surface as well as at the inlet 0. A previous researcher used a mixture of PO+OA as an impurity, which has a larger molecular size and droplet size than FFA. A larger molecule and droplet size could lead to an increase in impurity rejection [18]. Effect of low molecular weight organic solute concentration on flux reduction of a polyethersulfone ultrafiltration membrane.

Fig. 2confirms the correlation between flux and TMP, wherein increasing TMP causes an increase in the flux

Reply/Action taken 1. The title is not reflecting the content of the

Section 1, paragraph 1: How come reference #10 jumps up, and bypassing references number 6, 7, 8 and
Section 1, paragraph 2: Beside those aforementioned processes, there is also an emerging process to remove
of 7 saponification, acidification, neutralization, extraction, and

Section 1, paragraph 4: What do you mean by “To the best of our knowledge, the applications of PES UF for separation
Section 1, paragraph 4: Similar works have been done before
Section 1, paragraph 4: Write reasons/justifications on why no pretreatment was taken, in order to obtain
Section 2.1: You use a membrane with 1000 Da molecular weight cut-off, to separate glycerin (92 Da)

of 7 ultrafiltration experiments in this study (without any

Table 1: in the column of “Physical Concept”, use uppercase S and D for the 3 rd line (Formation of
Section 3.1.1, paragraph 4: Any data for contact angle of free fatty acids that reflect their hydrophobic
Reference #5: Be consistent! Remove the DOI in order to make the format of this reference is in unison with
Reference #20: The name of the first author must be
Reference #31: Use uppercase M and uppercase S for

The word "purification" in the old title (and in Section 1, paragraph 4, the last three lines) should be removed, as the product is not truly pure. Abbreviation: add PO, OA, NGOM, FAME to the list Y The list in abbreviation is 16. Abbreviation: add PO, OA, NGOM, FAME to the list Y The list in abbreviation is.

Is the requirement to use the abbreviated name of the journal, or to use the full name of the journal stated. Or, maybe reference #27 is correct (using the abbreviated name), and the format of the other references needs to be changed. Add citation/ref N Our previous study was presented at an international conference and will be published in the IOP Conference Proceedings. it wasn't published yet so we can't add this to the reference section.

11. Table 1: in the column of “Physical Concept”, use uppercase S and D for the 3 rd line (Formation of Surface Deposit)

Paper ID (CE19004) Review process is completed

FOULING BEHAVIOR OF POLYETHERSULPHONE ULTRAFILTRATION MEMBRANE IN THE SEPARATION OF

BASED BIODIESEL PRODUCTION

The objectives of the research were to study the influence of process parameters (TMP, temperature and pH) on membrane performance (flow and rejection) for crude glycerin purification. Flux drop, rejection and blocking mechanism were observed for various process parameters. A determination based on solute accumulation on the membrane surface is representative of cake or gel formation [14].

This phenomenon is conceivable due to the nature of the raw material (glycerin) and the majority of impurities (FFA) in crude glycerin. The constant of the blocking mechanism and the corresponding correlation coefficients (R2) during filtration are listed in Table 3. It is believed that the standard blocking mechanism is responsible for a significant flux drop, since in that condition the impurity molecule penetrates to the inner wall of the membrane. pore and forms a deposit that can lead to clogging of the active area of the membrane pore [38-39].