Science method

Distillation - Science method

A chemical process for separating the components of a liquid mixture by boiling and collecting condensed vapors.
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Folks involved in the synthesis of organic compounds or anyone with organic lab setup expertise:
Would you recommend buying a chiller over a submersible water pump (a cheaper option-can buy a few for the same price for rotovap and distillation setup)
  1. If we purchase a chiller, can we connect multiple units (again rotovap and distillation units) at the same time?
Thank you.
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When I attended university, we used to have a chiller for our rotavap - worked great. Just remember to turn it off at night (our had a tendency to build up some ice if left on for too long).
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I noted that multiple articles cite using dichloromethane after essential oil extraction to separate oil from aqueous phase, I wanted to know why is it used while there are protocols that note separation through an essential Oil Separator integrated into the Clevenger apparatus while hydro distillation process is ongoing?
Thanks
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Oil viscosity could be too high so dissolving in DCM makes it easier to retrieve all of it.
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I am getting the total phenolics content and total flavonoids content of a sample. Should the TFC be always lower in value? I know that flavonoids are prt of phenolics but since the protocols and standards are different, the protocols somehow produced darker liquids for the TFC which of course gave higher absorbance reading.
The protocol I used:
TPC
The test sample (0.2 mL) was mixed with 0.6 mL of water and 0.2 mL of Folin-Ciocalteu’s phenol reagent (1 : 1). After 5 min, 1 mL of saturated sodium carbonate solution (8% w/v in water) was added to the mixture and the volume was made up to 3 mL with distilled water. The reaction was kept in the dark for 30 min and after centrifuging the absorbance of blue color from different samples was measured at 765 nm.
TFC
1 mL quercetin of each concentration or extract was added to the test tube containing 4 mL of distilled water. At the same time, 0.3 mL of 5% NaNO2 was added to the test tube and 0.3 mL of 10% AlCl3 after 5 min. Then, 2 mL of 1 M NaOH was added to the mixture after 6 min. The volume of the mixture was made 10 mL by immediately adding distilled water
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yes TFC should be always lower than TPC.
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I recently bought a mouse sRANKL (315-11-50UG) from, Preprotech. I would like to know how to reconstitute that. What solvent should I use? Is distilled water okay to store for a long time at -20°C or -80°C?
I checked the CoA, and they said that as soon I reconstitute the sRANKL with water, it can only be stored for up to 1 week. If I have to keep it for a long time, I have to dissolve it in 0.1 % BSA. But I am wondering if dissolving in BSA will hinder the experiment. I have to perform TRAP staining.
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You are most welcome
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the plant I'm trying to extract essential oil from have very tiny leaves which seep through the neck of the reservoir flask to the bottom flask where the distillation solvent is supposed to be
is there any solution to this problem please and thank you
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try to use that condenser above the funnel not next to like this photo
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Hi! I want to measure the sugar concentration of gummy bear. Is it possible to do by mixing the gummy with 100 ml distilled water and measure the concentration of solution over time until it reach constant. Do I need special process to do that since the gummy is in solid state.
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I hope you find this article is helpful
'Gummy candies production with natural sugar source: Effect of molasses types and gelatin ratios'
All the best.
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For lithium carbonate preparation it‘s been saying that %70 alcohol saturated with lithium carbonate. But ı can’t dissolve it in distilled water or alcohol.
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Thank you Wolfgang!
Bircan, have you find any solution to your answer?
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Yes, I am looking for low-cost ways. Some ideas are- centrifugation, flocculation-straining, and filtration. But which one of these will have the lowest cost?
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Filtering will probably work
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i don't have NaOH pellets to prepare for protein distillation but i found a Stock solution of 1M NaOH. Can it serve well in protein distillation?
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can caustic soda (used in soap making) be used in protein determination?
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ILs attract interest as separation agents, PILs in the field of distillation, in particular. From the literature it appears that: the process is regarded to the private case of the salt distillation. In case of distillable one, questions are arised. It is salt but it is vaporized. Initially only the acid or base is vaporized, and at a specific composition both start to vaporize and the composition of the vapor and liquid is the same. So what's going on from the thermodynamic point of view? Get we the vapor composition that related to the few liquid compositions?
Share your or colleagues research/es that is/are including experimental/theoretical data on distillable PIL and its engineering application, preferable in the distillation processes.
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Water content in IPA is 1.7%. I want to decrease it to less than 0.5%. I have tried simple distillation and also distillation using an entertainer such as ethylene glycol. No positive results were observed.
Secondly, One anomaly observed during distillation of the first cut which we discard is having water content - 3.4% and 1st main fraction - 3%. I do not understand how this water content increased to 3% from 1.7%.
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I think they use concentrated sulphuric acid to dehydrate ethanol once it as reached the distillation limiting value Solvent Recycling and Azeotropes (solvent--recycling.com) 5% water.
Never done it, but water and concentrated sulphuric are very exothermic, so great care will be needed.
Some people use anhydrous salts to remove traces of water, not sure that would work or silica gel - it is self indicating so you would 4know when it is saturated.
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I am using some industrial cable waste and there are two types of jelly that are inside these cables to avoid damage to small fibres inside them. They are,
1. Hydrotreated paraffin base distillate and polymethacrylate resin.
2. Hydrotreated paraffin base distillate and thermoplastic elastomer.
We tried several ways (with commonly available commercial materials) to wash them, but none of those techniques was successful. I am expecting some advice on techniques that can use to wash them.
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Thank you Vadym Chibrikov
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For sake of validation, I would like to compare one of the simulated streams with the experimental TBP curve. Is it possible somehow to generate a TBP curve in ChemCAD having only a CC-steady state license?
Best regards,
Marcin
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I am answering myself, but still, it may be useful as a reference. Menu Drawing\StreamBox and tick Petroleum Assay in Properties.
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Our Effluent treatment (ZLD) plant consist of stripper for solvent separation (bubble cap tray) but it's performance is not reasonable.
Feed COD = 24000 ppm
Distillate COD = 28000 ppm
Feed = 35KLD.
Reflux ratio = 3
Temperature = 115
Steam pressure to reboiler = 0.5
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If a columm is not working well, you may adjust the reflux ratio increasing it a little bit step by step until you find the expected stripping ratio, but you have to check if flooding is not occuring. Columm performance is a matter of number of plates, reflux ratio, and pressure drop
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I am working on the effects of sumac extract on animal models. I extracted sumac fruit using absolute ethanol and after filtration, I put the remaining contents in the rotary evaporator. Although there was a small amount of thick liquid left, it didn't freeze when I put it in the freezer ( even after I tried to dilute it by adding distilled water ), so I couldn't put it in the freeze dryer either. I would be happy if you share your experience with me.
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As vacuum and heat (how much?) are applied I find it hard to believe water or ethanol will remain. The liquid you see is probably fruit residues.
You can test this idea by placing same volume of 95% ethanol (95 ethanol + 5 water) in the rotovap and see if it evaporate
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I made a 20% TBA solution, and after stirring it enough, I can still see it settles at bottom.
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Addition of DMSO (Dimethyl Sulfoxide).
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I have insects stored for morphomolecular species identification in ethanol (EtOH). These weevils (Larinus spp.) were stored in 100% EtOH at the recommendation of more experienced entomologists. Now that I am trying to pin these weevils, they are quite brittle and difficult to pin without cracking an elytrum. It was suggested to me that I could dilute the EtOH in the storage vial to ~80% to 95% to rehydrate the weevils enough for pinning, but I am concerned this may result in DNA degradation.
Has anyone experienced a problem like this? Other than removing a leg prior to rehydration or pointing the weevils, does anyone have some advice on how to deal with this problem? Thank you in advance!
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Remove legs (1 or 2) prior to rehydration.
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As it is explained that exosome are robust in nature as they can withstand pH change or temperature change and can be stable in various buffer, so can we suspend exosome in pure water or distilled water and if we do, does its affects the markers present on it and if it does what are that changes occurs?
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Structural stability in different pHs doesn't mean that the exosomes will be stable enough and constant in hypotonic conditions (e.g pure distilled water). Various reactions and changes would be expected.
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Has anyone done any work about membrane distillation? If yes please tell me about the membrane that you used and the design of the equipment and it's measurements.
Please tell us the factors that we should take care of while we design such an equipment.
Thanks in advance
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Good day! That is pretty complex question. In our works we have used copolymer PVDF-TFE membranes because of hydrophobicity, thermal resistance and ability to be reused after cleaning and pore declogging. Also, we have used home-made pilot plant. Please follow the next references:
The requirement for such a plant are quite general: silicone tubes with foam thermoisolation, high speed pumps, the shortest runway for concentrate on the tubes, and steel cell. Some annotations may be dedicated to cell establishing - try plan your module in such a way to avoid blind spots in your cell by forming pathways. Please, feel free to correct me if I was mistaken, and also feel free to share your expertise.
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Please how I can done the simulation for the system multi effect distillation with solar energy(what software use it)
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You can use Matlab/Simulink Model.
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Compounds which are highly nonpolar and soluble in hexane . How to wash them because there is a lot of impurities in NMR between 1-3 ppm. Distill hexane is already used.
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You can try a few different things. I don't know how you got to this step, so you may have done some of these purifications already.
You can try non-aqueous reverse phase. This is reverse phase, where water is replaced by methanol or acetonitrile, ethanol, or THF and the strong solvent is replaced by dichloromethane or another solvent. Here is an example below- do a blank run before your sample to wash off any compounds retained from previous runs on your column, and loose C18 that has hydrolyzed from the silica. Do NOT use a polymeric reverse phase for this technique.
You can also try alumina instead of silica.
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My project is methanol conversion to jet fuel but I have problem with GC method to analyze liquid product which is hydrocarbon mixture.
for GC - simulated distillation cost for analysis is too expensive for me
I hope someone can help me
thank you.
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I think you can refer to ASTM D3710 "Standard Test Method for Boiling Range Distribution of Gasoline and Gasoline Fractions by Gas Chromatography" https://civilengineersstandard.com/wp-content/uploads/2019/02/D-3710.pdf
This document should give you hints to replicate the method in your lab.
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How do I make a link between the Photovoltaic thermal PV/T and Multi-effect distillation using Trnsys software?
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Thank you for the document. My answer is currently outside your problematic. I was looking at the analysis of the performance and lifetime of all the components of a cell.
Best wishes...
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I am running polarization tests to get tale plots of 304L SS and CP-Ti, and getting noisy anodic curves. the cathodic curve is fine, but the anodic curve has a good amount of noise in it. Why would just one of the curves have noise but not the other? I using HCl with a ph of 3 diluted in distilled water as the electrolyte.
Attached is a picture.
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It seems to be the result of pitting.
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hello, i want to isolate lactobacillus from feta cheese, can someone recommend a certain method ? I already isolated but there was no growth at all !!
- 1g of feta cheese was mixed by vortex with 9ml of distilled water , 1ml of the serial dilutions was added into MRS agar and spread by the loop .. incubated anaerobically for 72 under 37 C
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MnSO4 with distilled water for solution. Then this solution is in a 3 electrode system at a determined potential range for the CV technic. So which potential is Mn+3, which potential is Mn+2, and which potential is MnOxide...
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thank you for your answer
Christian Désilets
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Pressure is maintained at 0.65Mpa and 30-35°C while using the DME as a solvent. Idea is to distill it for reuse. So, need to evaporate the DME by incresing the temperature by 10°C (at this point pressure can be set to normal 0.1Mpa) and condensing back to liquid later.
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By using a proper thermodynamic model, which maybe available in process simulation softwares you can estimate plenity of DME thermophysical properties, including its heat of vaporization.
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I want to calculate the required PSVs for a plant with several distillation column, vessels and reactors, connected together. But before that I need to estimate relief load of each one of them under different scenarios like power failure or fire.
I need a reliable standard or reference for relief load calculation.
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Emergency relief in the process industries aims to protect equipment, the environment and operating personnel from abnormal conditions. Appropriate estimation of relief loads under extreme conditions is important for the correct sizing of relief valves and flare headers, and for the selection of disposal media. In addition, during debottlenecking or revamping of process units, adding a new relief valve and modifying the relief system can be very costly and, in terms of construction, difficult to implement. Following are the useful links.
Relief Flow=Unbalanced heating Duty/Latent heat of Vaporization.
Design Factor=Calculated relief Load/actual relief Load
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Hi! I am working with the CWP and I need to dialyze it with dialysis membrane of 6000-8000 Da. But I can't understand the term "20 volumes of distilled water. Please help me in finding the solution of this query that how much will be the precipitated proteins and how will I calculate the 20 vols of distilled water for dialysis against it.
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One time use is highly preferable.
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I m using the catalyst and plastic waste and heating it in furnance at high temperature, It is called catalytic degradation of plastic , im confused it with plastic waste composites. Please clarify the doubt that what are plastic waste composites then. or is it the same.
Also my second question is that the liquid product which is formed when plastic undergoes catalytic degradation, it needs to be purified? by fractional distillation or filtration if i am synthesizing biodiesel from it.
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Alisha Kakkar The cited chinese scientists discovered an elegant method to produce a highly interesting Fe-C nanocomposite.
The raw materials are iron rust + plastic waste, but the end product is not plastic. As far as I understand, it is iron atoms in a carbon coating.
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I have synthesized Selenium nanoparticles using a plant source. After drying them in Petri plates , these nanoparticles were scraped out. Because of that some of them are found as large thin sheets. It was found to be difficult to reduce their size and also they are not properly suspended in distilled water for antibacterial studies. Is there any solution for these?
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Instead of drying them on petri plates, you can try lyophilization or other minimally disruptive methods. Parvathi M a
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Is it mandatory to use RO + UV-treated double distilled water or MilliQ water? Or is it sufficient to use double-distilled water after autoclaving it?
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25 years ago, it used to work. We were feeding our quartz distillation machine with bulk RO water (in-house supply) which had been prepared from Munich's municipal water. Media then were filter sterilized into autoclaved bottles. No UV treatment was involved.
Depending on the price for off the shelf liquid media, you might want to calculate the efficiency and cost of the whole process, though
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I am researching into nano emulsification of Cannabinoids O/W formulation, using a Sonic Cell Disruptor (sonicator).
I am having issue to get proper homogenization depending on the ingredients.
When trying obtain ethosomes using hot method the API precipitates and coalesce as clump within the mixture.
  • API used is Solvent extraction of Cannabis Sativa "Butain Hash Oil (BHO)" it is not winterized.
  • (A): 1000mg of API is added to 3000mg of C2H5OH 94% / heated to 40*C to uniformly dissolve
  • (B): 1000mg of Veg. Glycerin USP is then added to (A) the API and C2H5OH. (when at 25*C this creates a "cloudy Goo" texture, liquid "translucent" at 35*C and above)
  • (C) A solution is created with phospholipids 1000mg (Lecithin powder hydrated in distilled water) and Distilled water 20ml (sonicated at 40*C for 5 mins) to obtain almost translucent yellow solution.
Here is the problem:
When (B) is added to (C), and sonification is applied, it seems that API coalesce within the said Mixture.
Any comment or other method would be much appreciated.
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May be you should using more purified API for your trial. I think that some impurities which contains in different proportion in vegetable source of starting material may have some infuence on sustainability of final emultion. From the my point of view it can bring some unwillingness error in your experiments.
p.s This is a really interesting area of research)))
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8.2 Liquid-liquid-extraction and acetylation
8.2.1 Transfer 100 ml of the distillate obtained in 8.1 into a 250 ml separating funnel (5.7).
8.2.2 Add 20 ml n-hexane(6.4), 0,5 ml triethylamine (6.9), and 1,5 ml acetic anhydride (6.6) to the solution and shake for 30 min on a mechanical shaker (5.4) with a shaking rate of at least 200 shakes per min.
8.2.3 After phase separation, transfer the organic layer to a 100 ml conical flask (5.6) and shake the aqueous layer for a further 30 min with an additional 20 ml of n-hexane(6.4)
8.2.4 Dehydrate the combined n-hexane extracts by adding anhydrous sodium sulfate (6.7) to the flask (5.6) and leaving to stand for approximately 10 min.
8.2.5 Filter (5.9) the n-hexane extract quantitatively, washing with n-hexane into a 50 ml volumetric flask (5.5).
8.2.6 Make up to volume (50 ml) with n-hexane.
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You may give it a try of course but, I guess partially organic soluble bases are recommended since your target extract will be in highly hydrophobic media after LLE and acetylation. Picoline or pyridine may be preferred instead. Excess KOH or NaOH treatment is also available at saponification of fatty acids and you may investigate the methodology before your application.
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I'm making a research on how to distill pyrolysis oil to produce diesel. Is simply heating the pyrolysis oil at the temperature that diesel from crude oil ussually evaporates at, or treating the pyrolysis oil like crude oil and using the same process (fractional distillation) to seperate the different fractions of crude oil on pyrolysis oil enough or do I need to do other process to seperate the diesel-like fraction out of the pyrolysis oil?
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In order to obtain fractions as components for diesel, you may conduct distillation at atmospheric pressure and in vacuum (for diesel components), but I think maybe it's better to carry out a hydrotreating step, to eliminate the olefins formed during the pyrolysis. In that way, you can have a higher yield in C15-C18.
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I am interested in understanding the impact on corrosivity of crude oils containing these two components. Specifically in Distillation Units equipment and piping (atmospheric and vacuum).
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I synthesized epoxy through Williamson reaction, but the yield is not good. The reaction condition is about 6 hours at 70 degrees by adding NaH (with minimal oil). It was washed with water and ethyl acetate, distilated, and finally, the mineral oil was removed with hexane. The desired powder came out, but the yield is less than 10%.
I would appreciate it if you could tell me if there is anything wrong with my experiment scheme.
thanks so much.
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By Controlling the side section you can achieve the maximum output at temp 50-100 °C and using alkylateng agent, you can improve the reaction rate. iodide salt can be added which yields an extremely reactive iodide after a halide exchange with the chloride.
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Sample tube: crude enzyme+ 1 % casein (100mM sodium bicarbonate buffer pH-9) than incubate for 30 minute add TCA (5% in distil water) than centrifuge than take readings at 600 nm.
Blank1: water + casein, same as above
Blank 2: water + enzyme, same as above.
take readings from spectro. (Run Sample and Blank simultaneously)
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It therefore measures the total reducing capacity of a sample, not just phenolic compounds. This reagent is part of the Lowry protein assay, and will also react with some nitrogen-containing compounds such as hydroxylamine and guanidine.
To determine the activity in a solid protease sample diluted in enzyme diluent, divide activity in units/mL by the concentration of solid used in this assay originally in mg/mL, which gives activity in terms of units/mg.
The phenolic compounds react with the Folin reagent which is formed by sodium tungstate and sodium molybdate in acid medium. Thus, this reaction produces a yellow complex that can be reduced with the phenolic compounds and identified with a spectrophotometric method at a wavelength of 765 nm (Cueva et al., 2010).
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I need to design a demethanizer for the given content . I cannot find any reference related to it . Is there any book where demethanizer design is given step by step . I am using rigrous distillation tower to simulate it in Aspen HYSYS and reflex ratio is around 70 and the condenser temperature is high which is impossible for such systems
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Parvin Salamzada Richardson and Coulson Chemical Engineering Book Vol 2 and this CHAPTER can also help you in such design: https://www.sciencedirect.com/science/article/pii/B9780080418650500192
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I want to simulate a mini distillation unit (water/ethanol) to produce 1 to 5kg/h of ethanol
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Sure, you can. The capacity of the plant you are simulating is your choice.
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I need help in reactive distillation of Phthalic anhydride & 2-Ethyl Hexanol to design a continuous plant for this esterification.
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Thanks to Both of you
Regards
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Hi, anyone can assist me on this for my design project. I am going to design a DC to purify acrylic acid, acetic acid and water. The boiling point of acetic acid and acrylic acid are too closed where I cant use simple distillation to separate. Will it be ok if I design vacuum distillation if I don't want to use azeotropic distillation?
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After extracting my essential oil i did not want to use rotary vapor some one told me i can use distillation to get better result so is that possible without losing quantity of the E.O or should i use the rotary vap ??
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I'm trying to separate isoamyl alcohol and optically active amyl alcohol from fusel oil. I have done a rigorous distillation to get maximum concentration in bottoms of block B3. Since the boiling point difference is very less , simple distillation won't work here (3-methyl -1-butanol is 131 deg_C and boiling point of 2-methyl-1-butanol is 128 deg_C) .
I thought of using crystallization process to separate them but it's not economically feasible process.
I have attached the simulation sheet and the results developed by Aspen.
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From what I can see, the default Aspen interaction parameters for VLE in this system probably don't work that well. Attached is a picture of a Pxy diagram @ T = 368.15K predicted using UNIFAC in Aspen. The green points are experimental data at 368.15K for this system from Thiede, S.; Horstmann, S.; Meisel, T.; Sinnema, J.; Gmehling, J. Ind. Eng. Chem. Res., 2010, 49`, 1844-1847. The agreement doesn't look all that good.
You might want to look into regressing your own interaction coefficients...distillation might look better than you're being led to believe.
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The raw materials I'm using are pineapples, bananas and mangoes.
I’m thinking of using a rotary evaporator. Is that good enough? if that so, what's the best temperature, rotation, and duration for the distillation process?
#bioethanol #distillation #fermentation #chemicalengineering #biofuels
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Yes. In order to remove the moisture content and increase the purity of ethanol.
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Does tin chloride take a long time to dissolve, and how long does it take for it to completely dissolve in solution?
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Dear Imene Saoula many thanks for sharing this interesting chemical question with the RG community. I assume that you are talking about tin(II) chloride (SnCl2), right? Pure SnCl2 dissolves quite easily and rapidly in deionized water. Preferably the water is first degassed by applying vacuum in order to remove dissolved oxygen. If you don't obtain a completely clear solution, chances are that you have unsoluble impurities present which could be e.g. metallic tin (gray particles) or tin(II) hydroxide (white). The latter could make the solution appear milky and opaque. If that is the case, try to add a few drops of hydrochloric acid (aqueous HCl) and see if the solution becomes clear.
Gooc luck with your experiments!
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The absorption spectrum of malachite green dye dissolved in distilled water showed correct lambda max (617 nm) at lower concentration only (10 ppm). The lambda max for 100 and 50 ppm shows variation (peak near 648 and 634 nm). What can be the possible reason?
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Counting on the @Adam Shapiro answer, flattening of the peak usually means you need to dilute your sample or use thinner covet. It also means you are missing data since you don’t know what does the peak look like, if its single or double, where is the maxima etc.
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I am currently studying the problem with the quality of distilled glycerin. When stored, it acquires a pink tint (see photo). We analyzed glycerol on a gas chromatography mass spectrometer. In the sample 1099/2, the following impurities were found:
1,2,3-Propanetriol, 1-acetate CAS No. 106-61-6;
3-Methoxy-1,2-propanediol CAS No. 623-39-2;
1,3-Dimethoxypropan-2-ol CAS No. 623-69-8;
2-tert-butylhydroquinone CAS No. 1948-33-0.
Which of these substances can give a pink color and why?
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James, thanks a lot!
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Hello, I am currently preparing 0.2M PBS solution, pH6.6 from 1.0M PBS solution, pH7.4. I adjusted the concentration by using M1V1=M2V2 formula by adding distilled water. Is this right? And can anyone help explain what acid solution should I use to lower the pH and what is the estimated volume or amount should I add ?
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Add 0.245 g of Potassium Phosphate Monobasic to the solution. Adjust solution to desired pH (typically pH ≈ 7.4). Add distilled water until the volume is 1.
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Actually I want to find the particle size of B4C powder, Al2O3 and Mg powder by particle size analyzer using a solvent. But I am facing problem to select the appropriate solvent for the same.
I have tried by using the distilled water but the powder is getting settled down within five seconds, therefore, the analysis of results not getting time to provide exact results.
Can anybody suggest me the suitable solvent which provide 20 to 30 seconds for settled down ?
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Hi Saty Dev Sir,
I am facing the same problem in particle size analyzing. I want to know the suitable solvent to avoid the problem.
Thank you
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I have digested 30mL of water in H2SO2 and the final volume is 100. After taking 5ml for distillation, the titration volume with HCL 0.01N for water sample was 1.7mL and for blank was 0.1mL.
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Kjeldahl nitrogen that method
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I am doing MTT to check cytotoxic activity of the chemical compound having anthraquinone and DCA in it. Yet, the component does not dissolve in distilled water as it turned into crystals in fume hood. Is there any solvent that could be used for drug treament concentrations to proceed the testing?.
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First of all you should identify the proper solvent of your tested drugs as well as you have to determine the concentration of that particular solvent that is not toxic for cells. Other than distilled water we also use DMSO (cell culture tested) as solvents.
Hope it will help you. All the best
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I will use it for insect DNA extraction. Can we use sterile distilled water to dissolve?
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Hi,
To synthesize ZnO nanoparticles by co-precipitation method. First, I dissolved ZnSO4.7H2O in distilled water. Then, I added 0.1 M NaOH to the solution dropwise to increase the PH of the solution to 12. But it remained constant at PH=5.8. By increasing the amount of NaOH it just marginally increased (PH = 6.3). However, after a while, it dropped to the previous level.
Is there any other substance that should be added to the solution?
Should I add the NaOH with a specific molar ratio concerning ZnSo4?
Thank you.
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Hi Mohamadreza Alikhani
The solubility product of Zn(OH)2 is given in handbooks as 3 x 10(-17). That means that a suspension of zinc hydroxide should have a pH around 8.3. In the presence of the large concentration of sodium sulfate formed in the precipitation reaction the solubility should be higher (higher ionic strength increases solubility of ionic precipitates) but still probably not much higher than 9.
Aiming for pH 12 is not useful. All you'll achieve if you manage to get to pH 12 will be a clear solution of sodium zincate, Na2Zn(OH)4, because zinc hydroxide is amphoteric and dissolves in excess base. You should try to add 2 millimoles of hydroxide for 1 millimole of zinc salt, both in solution form of course. 0.1 M solutions for both are a reasonable starting point, but you may find that a lower concentration gives you a cleaner precipitate. If you want a very fine precipitate it's best to mix the two solutions quickly rather than dropwise.
Good luck!
Emanuel Coper
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In general, when adsorbent materials are chemically modified we use distilled water to wash away the excess chemicals (e.g. after acid/base modifications, to wash away excess acid/base and confirm with achieving constant pH or pH = 7 in solution) and this usually requires a great amount of distilled water to properly clean the material.
What I would like to get comments on are;
1) Is there an advantage of using 'Hot distilled water' over the distilled water which is at room temperature?
2) What are the factors we need to consider about using hot/cold distilled water to wash the materials?
3) Are there any other methods available to improve the efficiency of the cleaning process of materials?
Comments, advises and publication recommendations regarding the concern are highly appreciated.
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Better performance of distilled water for washing will be achieved Since the dissolution increase directly with the increase of temperature
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I tried to make 0.1% DCPIP solution in
1. Distilled water and kept for 3 days but didn’t dissolve
2. Tried hot distilled water and again didn’t dissolve
3. Tried 1ml ethanol for 0.01gm DCPIP and failed this time also.
Is any other way to dissolve? Did I make any mistake? Or the DCPIP salt expired ??
Or any other way anyone know?
I didn’t try to dissolve it in NaHPO4 as I failed in Ethanol.
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Dear Sumona Akter thank you for sharing this very interesting technical question with the RG community. DCPIP (= 2,6-dichloro-phenolindophenol) is a neutral organic compound which in this form is insoluble in water. Thus it makes no difference if your stir the suspension in distilled water for 10 minutes or 3 days. 😥 Only the sodium salt of DCPIP is soluble in both water and ethanol. You can prepare a solution of the sodium salt in water by adding DCPIP in portions to a warm aqueous solution of sodium carbonate (Na2CO3).
Good luck with your experiments and best wishes, Frank Edelmann
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Hello
For my master thesis I´m trying to add a MVR to my Aspen Plus simulation.
I´m using a RadFrac Model for distillation. The head product is mainly water (97 wt.-%).
After trying several options suggested in literature or here, the simulation is still not converging.
Maybe someone can help or has some advices?
Thanks in advance
Stefan
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I would suggest to add a pseudo stream for the vapor phase on stage 2.
You can manipulate this stream any way you like without disturbing the column convergence itself.
You should add a pre-heater before the compressor to avoid condensation during compression. To specifiy a driving a driving temperature difference between compressed stream condensation and bottoms temperature, a desig-specification on compression ratio or compressor output pressure is helpful.
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I am getting confused that is it needed to add 70g ammonium sulfate in 100ml solvent or 100ml solution? Should I dissolve 70g solute in 100ml solvent or dissolve solute in less than 100ml solvent. I made solution wit 70g in 50ml of water initially but the overall volume became 100ml and the solution became supersaturated. What should be done. Guide me if I m wrong.
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Oussama Baaloudj thank you my friend the monster
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I have seen paper stating that it can remove KOH from the biochar or activated carbon with repeated washing of HCL and distilled water.
However, I do not understand how does washing of HCL and distilled water remove KOH from the biochar or activated carbon.
Do we have to filter the material after we put it in HCL and distilled water ?
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...we used an approach that was based on titration; see section "Pretreatment of biochar for ad-/desorption experiments" in: Sorption of copper (II) and sulphate to different biochars before and after composting with farmyard manure | Request PDF (researchgate.net).
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I have synthesized Ag nanoparticles using a green route [salt: plant extract = 9:1 and added 100 microlitres of starch solution (100mg starch dissolved in 1 ml distilled water) to it]. I had heated the mixture for an hour at 80 degrees centigrade. After recovering the nanoparticles by centrifuging the silver colloid and drying the precipitate, I tried resuspending them in distilled water (10 ml of water added to 1 mg of nanoparticles) by ultrasonication for 10 minutes at 270 Volt. The nanoparticles are settling at the bottom of the container which is the problem.
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Keep your material in liquid 'suspension'. Never dry. This will prevent the irreversible aggregation of nanoparticles. You can get different concentrations by dilution with the 'mother liquor' (never in DI water).
See (registration needed):
Dispersion and nanotechnology
Generalities on silver colloids are found in these webinars (registration needed):
Silver colloids and invisible ink
Metal colloids - their preparation, application and characterization
Be aware that the surface of silver is not silver metal but silver in the +1 oxidation state (and it’s – slightly soluble - Ag+) that’s the bactericide not silver metal.
This question or similar has been posed many times on RG. See, for example:
2 quotes from those greater than I...:
  • 'I think dry nanotechnology is probably a dead-end' Rudy Rucker Transhumanity Magazine (August 2002)
  • ‘If the particles are agglomerated and sub-micron it may be impossible to adequately disperse the particles……‘The energy barrier to redispersion is greater if the particles have been dried. Therefore the primary particles must remain dispersed in water….’ J H Adair, E. Suvaci, J Sindel, “Surface and Colloid Chemistry” Encyclopedia of materials: Science and Technology pp 8996 - 9006 Elsevier Science Ltd. 2001 ISBN 0-08-0431526
Chapter by a criminal:
This can be obtained by request to the aforesaid criminal.
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How to completely remove water from Isopropyl alcohol? I have isopropyl alcohol with 3% moisture. I need to remove water completely. Due to azeotrope with water, distillation not possible. I tried salt out process (addition of NaCl). But no effect on 3% water. However it works only on 70% IPA concentration increased to 80% only. Further removal of water not possible. Any other simple procedure for complete removal of water from IPA?
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In ancient times
1) I did some exploratory experiments using glycerol help eparate water from ethanol. I do not remember the results.
2) I used to a K-LTA (It is a comercial potassium exchanged Na-A (A zeolite -> now LTA). Some coleagues have been using this zeolite to dry solvents in laboratory scale. I think it is easy to buy in Sigma-Aldrich-Merck for example.
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Dears;
I solved CuSo4.5H2O in distilled water. After that I did UV spectroscopy experiment on this solution. The result graph is attached. Now, I have a question? In my solution, I have cu(aq) and so4(aq). which one is related to peak 809nm? Shouldn't this graph show two peaks for cu and so4?
thanks a lot.
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Dears, thank you for your answers.
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Hydrodistllation was used to erxtract essential oil from a natural product. What are the possible simple laboratory methods to isolate the essential oil from the distillate without loosing the oil through evaporation?
Thanks
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Hi Dr Lawrence Olusegun Ajala . The new technique is called Supercritical carbon dioxide extraction: It allows for extraction of essential oils from plants when steam distillation is impossible, this method consists of passing a stream of CO2 at high pressure through aromatic plant materials to burst the essence pockets and extract the aromatic substances. See the link: https://www.pranarom.fr/en/content/15-the-distillation-of-essential-oils
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currently i am using distilled water and then sonication followed by magnetic decantation . But magnetic character of NP's is getting lost . Can anyone suggest me something ie. a better solvent or washing method to wash off NaOH used in synthesis? Thanks in advance!
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In my opinion, it is the pH problem. You synthesized with NaOH to keep the pH higher than 10, but when you wash, the pH of water is much less.
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During sample preparation for GC-MS, Where i followed the given protocol:
10 mg of dried biomass + 1.7 ml methanol + 2 ml chlorofoam + 0.3 ml H2SO4 ----kept in water bath (100 degrees) for 140 min. Later, after cooling the reaction mixture, distilled water was added.
I saw only one sample giving proper phase separation (between organic phase and aqueous phase) ---see Pic 1
whilst others did not gave any phase separation, even though these samples were prepared by the same protocol---see Pic 2
Please note that the sample giving phase separation was that of the external standard (i.e. PHB; Polyhydroxybutyrate)
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How can I be sure that the percentage of ethanol that was used in the process of washing the nanoparticles is removed? What is the best ratio between ethanol and distilled water for the purification process?
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Dera Husham N Noori thanky for sharing your new question and concerns. I fully understand that this question puzzles you. However, there is no generally accepted ratio between distilled water and ethanol when washing nanoparticles. Researchers are absolutely free do do it their way and use different ratios. After all, the goal is to purify the nanoparticles and remove unreacted starting materials and by-products. It certainly doesn't hurt if you use more water and ethanol than what is absolutely necessary. Over time you will get more and more experienced and develop a feeling for what is appropriate.
Just isolate your nanoparticles by filtration, then re-disperse them in distilled water, centrifuge again and repeat this 2-3 times. Then repeat the whole procedure 2-3 times with ethanol and finally dry the product.
Please have a look at the answers given to the following closely related question which has been asked earlier on RG:
How do I remove impurities in nanoparticles?
I hope this helps. Good luck with your work and best wishes, Frank Edelmann
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We are used the protocol for urease extration adaptated (to C. neoformans) from Amin et al.,2013:
Briefly, the broth cultures were subjected to centrifugation (5,000 × g, 4 °C) and the recovered mass was washed twice using phosphate-buffered saline (pH 7.4) and then stored at -80 °C. Subsequently, was thawed to ambient (room) temperature, followed by mixing with 3 mL of distilled water and protease inhibitors (TLCK, Tosyl-L-lysyl-chloromethane hydrochloride) and sonication for 60 s. After centrifugation (15,000 × g, 4 °C), the supernatant was desalted by eluting through SephadexG-25 column. The resultant crude urease solution was mixed with an equal volume of glycerol and then preserved under refrigerator (4 °C) for further uses.
Okay, we ran the suggested protocol, but after 2 days, enzyme activity was no longer observed.
Then, we tried to exclude the TLCK from the protocol, again the activity was observed on the day of extraction, but after it lost the activity.
We also tried to activate urease with sodium bicarbonate and Ni solution, without success.
In another procedure, we repeated the protocol and lyophilized the solution resulting in a white solid. So we tested it on this day, we prepared a urease solution (10 mg / mL) and the activity was good, but after a few days, again the activity was lost.
We always work with refrigeration, and we are careful to keep the solution on ice when we handle it.
Please any suggestions?
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Something I would have done differently is to have used a pH-buffered solution during the procedure to maintain the pH at the optimal pH of the enzyme.
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Hello, I am still new to this, if I may ask, how do you do the dilution for gallic acid?
Just now I have 100ml of gallic acid stock solution from dissolving 0.500mg of Gallic acid + 10ml Methanol and diluted to volume with Distilled water.
I need to make 10, 40, 80, 140, and 200 microgram/millilitre for the standard curve but I do not have any idea how to do it, thank you..
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Thank you everyone for answering, Sir Juan Alemán I have a question, if 10 ml of standard stock solution needed to make 10 ug / mL of gallic acid, does that means I need 120 mL of stock solution to make 120 ug / mL gallic acid for the calibration curve?
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My team and I are new to HPLC/GC-MS quantification so we would appreciate some insight. Currently, we are trying to measure the concentration of organic acids within an organic solvent (tri-n-octylamine and oleyl alcohol (40% v/v)), aqueous solvent (water based microbial culture) and a pure substance (achieved through distillation). Will the reagents be different for each type of solvent? What solvents would be recommended for this procedure? Thanks.
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If the boiling points are too near together, the chromatography will be distorted.
Hexane and iso-octane are common solvents.
More polar solvents, such as acetonitril and toluene, can be employed, although developing the injection procedure with these solvents would likely take more effort.
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Hi everyone,
I need a dialysis tube for my synthesis. There is one piece of dialysis tube (12400 MWCO) that has been stored at 4 C fridge in distilled water for 2 years. I was wondering if this tube can be used for my synthesis or it,s properties (permeability, ..) have been changed.
I would appreciate any help in case you had a similar experience.
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If the dialysis tube is only used for in vitro synthesis, I have no objection, but not for synthesis in vivo.
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We're using S-300 HR (120ml column volume) pre-packed Gel filtration column connected to FPLC machine. The column is giving back pressure of above 20psi at 0.25ml/min flow rate. We've run the column with 0.1M acetic acid and 0.5M NaCl and then with milli Q water. The pressure was decreased to 3psi when ran with 0.1M acetic acid. When we ran the column with double distilled water, then the pressure was again increased to 15psi at a flow rate of 0.15ml/min. Please help how to regenerate the column again.
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I agree with Sebastian Schmitt about reversing the flow for cleaning, because the issue almost always will be at the top of the column. Also raise the adapter a few mm to allow the bed to expand when in reverse flow. The standard recommendation from the supplier is to use 200mM NaOH (I've not seen acid used before). Try at least 2 column volumes in reverse flow and then switch to water. Finally switch back to normal flow direction in water, adjust the adapter as required, and check the pressure. If all is well, re-equilibrate with your column buffer. If NaOH doesn't work you might need the more aggressive treatment with guanidinium hydrochloride as suggested above. If you are still having issues after all this, you may need to remove the top 2-3 mm of resin.
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I need to remove Hydroquinone inhibitors from Acrylic acid prior to use. For that I need to do vaccum distillation of Acrylic Acid under reduced pressure with copper shavings in the distillation flask. However, I am unable to find the specific temperature at which the distillation can be done. Boiling point of Acrlyic acid is 144 degree however it is also mentioned in some places that acrylic acid can be explosive if excessive heating is done. But any specific or recommended temperature for distillation is not mentioned anywhere. Have been searching for past 2 weeks. Kindly Help.
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Dear Bhuman, many thanks for sharing this interesting chemical problem with the RG community. Indeed, i would not suggest to distil acrylic acid at normal pressure. Please find cited below a protocol which has been published in "Organic Syntheses". The procedures published there are always very reliable because they have been checked by independent chemists. The boiling point of acrylic acid is given here as 69–71°/50 mm or 53–56°/25 mm.
(please see attached pdf file).
Good luck with your work and best wishes, Frank Edelmann
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Hi everyone,
I am trying to improve sustainability in my institute and I realized that there is an overuse of MilliQ water. I believe that for most of the operations done in a microbiology lab (buffers and bacterial media preparation, PCRs, restriction reactions, ligations, DNA assemblies, ...), using distilled water might be sufficient. I was wondering if someone has an overview of which water can be used for which protocol and maybe a list of the operations which really require MilliQ water.
Thank you very much in advance for your help!
Best,
Filippo
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For molecular reactions (PCR, restriction digests, etc.) it is best to use molecular grade water - purchased in a bottle & not out of a filtration set up.
For buffers & media, regular ddH2O from your filtration system is preferred, but dH2O is good enough.
For washing dishes, use tap water & rinse in dH2O.
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In preparing a liposome loaded with an aqueous extract to obtain a powdered sample, is it recommended to dissolve the extract in distilled water, then use same to hydrate the already formed lipid film? Thank you.
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Thank you Mohanad.
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I already try to sterile my fern for in vitro spore culture by:-
1. wash under running tap water
2. then shake with fungicide + distill water
3. rinse with distill water(3 times)
4. dip in 1 min 70% ethanol
5. dip in difference concentration of sodium hypochlorite (if higher concentration the it cannot grow but lower concentration cause fungus)
6. rinse with distill water (3 times)
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Hello Nurul,
thanky for posting this very interesting technical question on RG. In my opinion you did everything right. The following link has a detailed protocol for sterilization of fern spores using sodium hypochlorite solution:
Surface Sterilization of C-Fern Spores