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loading in packed column

november 30, 2020 Geen categorie 0 comments

Determination of the loading and flooding point of both columns. After that, collect smaller fractions when you begin eluting your material. flooding would occur. The liquid-to-gas ratio must be varied between LIV = 1 and L/V = 10, depending on the degree of contamination. A chromatography column is a glass or plastic tube that you set vertically and fill with­ a stationary phase. The process I described here is geared for running columns manually—or how I like to call them: hand-columns. In addition, liquid holdup is also an important model parameter for developing pressure drop, mass transfer, and flooding velocity models for structured packing. rapidly with G. Point c is known as the loading to that of dry packings, i.e. of gas and liquid around the individual solid packing materials ]. If you are new to column chromatography or just want a refresher, then read on for a quick description of the basic process. Remember that it’s because of these differences in elution speed that the components of a mixture separate. Gentle tapping on the side of the column can also force the bubbles to rise to the top of the column … The closest analogous concepts for packed columns would be mal-distribution (as you have suggested) or wetting rate. Only when you are ready to run the column, load your sample by pipetting it onto the packed solid bed. each liquid rate has its own loading and flooding points. (maximum) gas velocity that can be used. Packed Tower Sizing calculates percent flooding, column diamter, pressure drop based on Strigle modified Eckert's Generalized Pressure Drop Correlation (GPDC) Diagram CheCalc Chemical engineering calculations to assist process, plant operation and maintenance engineers. below that shows a typical gas pressure drop in a packed column. - pressure drop condition, usually well below the pressure drop at which axis is the logarithmic value of pressure drop per height of packing [ pressure Part of void volume now become wetted (irrigated). Alternatively, run a TLC plate for plant extracts or lab-made chemical compounds. For total-reflux distillation in packed columns, regions of loading and flooding are identified by their effects on mass-transfer efficiency, as shown in Fig. There’s nothing like having the practice of doing it yourself to know how to tackle issues and troubleshoot a procedure. whereby the liquid filled the entire column and the operation became difficult Therefore, numerous researchers have developed various theoretical models for liquid holdup. Loading the column involves placing the sample directly onto the top of the column and allowing it to absorb onto the silica. Once the sample is loaded, pour in the eluent and start the flow immediately. The Once the sample is loaded, pour in the eluent and start the flow immediately. Each packing has its own characteristics pressure drop chart as reported by Foaming systems rarely affect packed columns seriously, but a strong foaming tendency can reduce capacity It is believed that the flood point declines towards the load point in foaming systems and therefore design should be for less than 90% load. This is also known as flooding. Using a dry funnel, sprinkle 8 g of alumina into the solvent, and allow solvent to drain from the column to prevent overflowing. Put simply, an analyte that strongly interacts with the stationary phase is retained in the column and, therefore, moves slowly. Some liquid started to be retained in the packings. For optimum A poorly packed column can lead to uneven flow and band broadening, both of which give rise to poor separation. I always find it safer to collect fractions from the start of the chromatography column run—better safe than sorry I guess. horizontal axis is the logarithmic value of the gas velocity G, and the vertical Column chromatography is a common technique used to separate individual compounds from a mixture. The line for Refer to the Figure Packed beds may also contain catalyst particles or adsorbents such as zeolite pellets, granular activated carbon, etc. You only need a very small amount from each fraction to figure out where your material of interest ended up. a constant liquid flow (say L = 5), at low The column’s diameter is directly related to the scale of your sample, and the length depends on the difficulty of separation. None: All sheets. Operation Because molecules vary greatly in their properties, you can exploit different types of interactions to separate compounds. Yet, don’t go too small because you’ll needlessly end up with a lot more fractions to analyze. We gas velocity. The second method is the wet packing method. point is known as the flooding velocity (limiting velocity). The point in which the droplets of liquid (solvent) are carried up with the gas in packed column. Though numbers can vary from column to column, just to give you an idea, a good starting point is to keep the mass of your crude sample somewhere between 1­ to 5% of the total mass of the stationary phase. But when the interactions are weak, the analyte elutes easily and, thus, exits first (see below). A pump, detector, and fraction collector cover most of the process. as the flooding point. above (right). flooding and loading in packed columns. pressure drop increases as gas velocity increases according to the linear relationship gas velocity. Packed column performs well at low pressure, low liquidand vapor loadingthat make packed column have the most efficient in these terms. no liquid flow, L = 0), It marks the start of entrainment regime in columns. FIG. Packed columns are suitable for handling foaming system. Do not let the column dry out and do not stop in the middle of the run. is a greater amount of liquid hold-up, a gradual filling of the packing voids In my next article, I’ll discuss some of the different types of stationary phases that you can use to clean up your samples. A slightly more polar solvent than the one you will be using for the column can be used if this helps with dissolution of the sample. that will be encountered by the down-flowing liquid and the higher Or do an activity assay if you’re working with an enzyme. The separation will depend on the properties of the molecules and the extent of their interactions with the stationary phase. As the gas velocity is increased further, the pressure high a gas velocity will lead to a condition known as flooding trickling of the liquid down the packings. The solid-gas chromatography columns are available in a wide variety of solid supports,coated packings, tubing materials, and configurations. But if you’re starting with a wash and you are sure that your desired material will not elute, then collect that wash as one big fraction. When point Do not load your sample until you have all your materials gathered and set up. Point e is known Gas and liquid rate increase together, and a. But if you come across a sample that isn’t easily purified with an eluent of constant composition, then switch to a gradient run. in the liquid. the pressure drop across the packings. All flooding and loading in packed columns wholesalers & flooding and loading in packed columns manufacturers come from members. Pressure Drop. Flooding Prognosis in Packed Columns by Assessing the Degree of Steadiness (DOS) of Process Variable Trajectory. - Clamp the column in a vertical position, close the pinchclamp, and fill the column with solvent. DP/L under wetted condition lies to the left of line a-a. To determine the column volume, pask a small column with a known weight or volume of packing (I tend to use weight if possible); pack it wet with methanol. So, there you have it—now go run your column! My current checkpoints are 1. But then what solvent would be required to separate that? of Gas Pressure Drop in Packing. But it can be tricky to decide because the fraction size doesn’t only depend on the size of the column, but also on the difficulty of separation. to moderate gas velocity G; the pressure drop characteristics is similar If a list of integers is passed … Analysis pressure drop is now very high. What is a packed column? If you isolate protein or DNA, run a gel to identify the fractions that have it. Like in all other chromatography methods, column chromatography separates the components of a mixture based on their properties and how they interact with the stationary phase and/or mobile phase. I personally prefer the latter because it’s usually faster and seems to use up less liquid. c is reached, the quantity of liquid retained in the packed bed increases The gas velocity at this Loading : point of a column is when the gas velocity is high enough to restrict the flow of liquid. For example, compare the case for L = 0 vs. L = 5. In a packed column the liquid is intended to flow downwards across the entire cross section of the column, so weeping is not a relevant concept in a packed column. So, plan ahead. 14-54. I always wondered whether it would be better to load the column with fast flow rates (3-5 ml/min) or slowly (around 0,5 ml/min). Ensure you are familiar with the concept of loading a flooding applied to packed columns. Industrial & Engineering Chemistry Research 2016 , 55 (40) , 10744-10750. drop increased. Keep in mind that collecting more and smaller fractions may give you more chances of isolating your material free of contaminants. ), select the elution conditions, hit “start”, and go do something else while it runs. as shown by line a-a. Learn how your comment data is processed. For Note: For this method, add your dry solid phase to the column and pass equilibria buffer or starting solvent to saturate the solid. Solvent is passed through the column and the slurry settles, making a packed bed. Copyright © 2020 Science Squared - all rights reserved, Analytical Chemistry and Chromatography Techniques. Other methods are available, and I would say to go with what’s more prevalent in the literature for your type of molecule. Loading point of a column is when the gas velocity is high enough to restrict the flow of liquid. And keep that mass percentage on the lower side if you predict a difficult separation. My lead engineer told me to size the packing based on KG Tower version 5.2 and I have no complains on the software itself. in the packings now filled with liquid, thereby reducing the cross-sectional area At pressure drop and gas velocity. You can use column chromatography on both a small or large scale to isolate and purify material for use on a later experiment. In Molecular sieve packed columns easily separate permanent gases at above-ambient temperatures. at constant gas velocity, the gas pressure drop is higher Also, do your best to select the smallest and shortest possible column that gives you a good separation. You are required to investigate the hydrodynamics and mass transfer operation in the column for CO 2 capture from air using water. Here, you mix both liquid and solid outside of the column and pour it into the column. I work in a legal lab and they’re asking me to get lighter colors. Has this helped you? Then please share with your network. There are two common ways you can fill a chromatography column. The mobile phase, or eluent, is a solvent or buffer that dissolves your sample and transports it through the column. Furthermore, we mainly use packed columns in liquid-liquid extractions and capillary columns in gas chromatography. Do not let the column dry out and do not stop in the middle of the run. But well-funded labs may use automated systems such as fast protein liquid chromatography or flash chromatography. Restek's R&D chemists have developed a process for preparing molecular sieve packings, which result in excellent batch-to-batch reproducibility. c to d to e, there is a sharp increase in pressure drop at higher G: there the gas velocity, the greater the resistance Only when you are ready to run the column, load your sample by pipetting it onto the packed solid bed. the recommended gas velocity is 1/2 of the flooding From point drop in a packed bed is the result of fluid friction that is created by the flow Packed Columns Pressure drop < 1000 Pa per m height of packing (1.5”per ft in Seader& Henley, 2 nd ed., p233) Nominal packing diameter < 1/8 th column diameter Vapour Liquid flow factor calculated as before (F LV) Another chart is used of F LV versus Y with lines of constant pressure drop per length of packing Liquid holdup model is one of the important hydraulic design equations for a sheet metal structured packed column. Alternatively, some design can be based on a specified In addition, our molecular sieves are preactivated and ready to … This site uses Akismet to reduce spam. The method that you use to analyze your fractions will depend on the type of molecule you’re working on. For each assembled input record (that is, after the concatenation), fields are loaded into the DSN8A10 .TOPTVAL table columns (that is, MAJSYS, ACTION, OBJECT …, DSPINDEX) to form a table row. The combined effect of a channel-based approach for dry pressure drop and the Buchanan equation for wet pressure drop in packed beds has been numerically evaluated within the flooding region. Sample Separation by Column Chromatography. Keywords: countercurrent; packed columns; pressure drop; mathematical model Nomenclature Obtain an empty column, plug it with a small piece of glass wool, and affix a pinchclamp to the bottom of the column. The purpose of a packed bed is typically to … at larger liquid rate. line at point c as pressure drop increases more Most of my problems arise on the checkpoints of the design. occur at lower gas pressure drop. to dry packings. significantly. When point c is reached, the quantity of liquid retained in the packed bed increases significantly. Automated systems can rock your world by saving you a lot of time. velocity. Polluted air flowing at a rate of 105 m3/h STP is to be scrubbed with water in a packed column. Liquid Load In Packed Columns - posted in Industrial Professionals: Hi everyone, I am tasked to an initial design of packed column for a grassroots project. Total weight of packed column is less due to use of low weight and high capacity packing. Packing is less desirable for large diameter columns (over about 5 ft in diameter). But I still recommend learning how to do hand-columns. plot is still straight on log-log plot. at higher liquid rate, the loading and flooding points Run an isocratic elution for noncomplex samples. Use this information to pool the fractions with highest purity to obtain a yield and continue on to your next experiment. One is the dry packing method. at larger liquid rate. at constant liquid rate, gas pressure drop increases with velocity. 14-50 Common structured packings. at higher liquid rate, the loading and flooding points In chemical processing, a packed bed is a hollow tube, pipe, or other vessel that is filled with a packing material. regimes: dry gas, irrigated gas flow below the load point, loading region, and flooding. at constant gas velocity, the gas pressure drop is higher For example, you can select a column to do separations according to a molecule’s hydrophobicity (hydrophobic interaction column), polarity (silica column), or electrostatic charge (ion-exchange column). Any disruptions in the partitioning equilibrium will mess up your resolution. Too Row (0-indexed) to use for the column labels of the parsed DataFrame. Packed column has less pressure drop than tray column and it reduce 11. occur at lower gas pressure drop. - - each liquid rate has its own loading and flooding points. The packing can be randomly filled with small objects like Raschig rings or else it can be a specifically designed structured packing. Packed column provides continuous contact between the vapor and liquid phases. With a dry packing (i.e. with liquid (starting at the bottom of the column), and the column is slowly "drowned" This hapens if the solvent flow is fixed & the gas flow is icreased. header int, list of int, default 0. When your sample is adsorbed onto the resin, the components will dissolve in the running liquid and the separation will start. Learn how packing materials help the liquid and vapor mix, and how it compares to the tray column. The stationary phase is a matrix or resin with functional groups that interact with your sample. You’ll have better control of the separation as the mobile phase conditions (pH, salinity, or polarity) gradually change from low to high eluting strength. This is because the higher Pressure drop per unit length is less in packed column. What sort of solvent(s) would you recommend for cannabis extract? There is a change in slope of the line at point c as pressure drop increases more rapidly with G. Point c is known as the loading point, as liquid starts to accumulate (load) in the packings. The experiment will involve 2 principal stages: Part 1. section b-c of the "Sheet1": Load sheet with name “Sheet1” [0, 1, "Sheet5"]: Load first, second and sheet named “Sheet5” as a dict of DataFrame. Agilent J&W Packed GC Columns are designed and manufactured to offer excellent and reproducible performance for all sample types associated with packed column separations. There is a pressure gradient through the column -- … For low pressure drop packing this can happen with pressure drops per foot of packing in the range of 0.75 in to 1 in of fluid per foot of packing. A required = P actual /F a The approach to the model development is fundamental in character and is an improvement over models published earlier. the manufacturer - for example, see the Figure You simply set up a pre-packed chromatography column (yes, you can buy them! Different column chromatography methods call for different mobile phase conditions, so select the type of eluent after you decide on the type of column. If you have any ideas I’m very interested, thank you! Stay tuned! The eluent can be a pure solvent, a mixture of different solvents, or a buffer that varies in pH and contains additives. The maximum permissible load is that at the loading point. The flooding point is an important design parameter since it establishes the maximum hydrodynamic capacity at which a packed column can operate. Finally, the screening of fractions should also give you information on the purity of your material. I’m kind of stuck on how the polarity of the alcohol and the potential non-polar/polar solvent would react in the column. At point e, there is another a log-log plot. I was thinking ethanol but was also thinking that I’d first have to dissolve the material first or perhaps winterize first then load in the column? Regardless of how you fill the column, always make sure that there are no bubbles and that the stationary bed is even. will begin our analysis by examining the relationship between the gas With liquid flowing in the column, the packings the same gas velocity, the pressure drop is higher for wetted packings compared The size of fractions is typically about 10 to 20% the size of the column. At this point the entire column is filled liquid The main difference between packed column and capillary column is that, in a packed column, the stationary phase is packed into the cavity of the column whereas, in a capillary column, the stationary phase coats the inner surface of the cavity of the column. After this point, the pressure drops at a much faster rate till another point, known as the flooding point, when all the liquid is carried away by the gas. of a gas absorption column is not practical above the loading point. SOFTbank E-Book Center Tehran, Phone: 66403879,66493070 For Educational Use. design, the recommended gas velocity is 1/2 of the flooding This way you can save time, packing material, and eluent. This is a straight line on Hydrodynamics of Packed Bed Column: Study of the Column for the Absorption of CO2 in Water and its Efficiency Suleman Ali* and Javaid Akhtar Institute of Chemical Engineering and Technology, University of the Punjab, Lahore, Pakistan Packing the column is a critical step in your separation procedure. The gas to carry out. trapped among the packings (no liquid hold-up). You can use differently sized columns to separate samples in amounts anywhere from micrograms to kilograms. determining the column diameter, we need to know what is the limiting At high flow parameters the capacity and efficiency can significantly reduce, also in heavy fouling applications and corrosive condition. Up to this point, there is an orderly There is a change in slope of the Trays probably aren't a good idea for columns less than about 1.5 ft in diameter (you can't work on them) -- these are normally packed. available for gas flow. To load the column: Dissolve the sample in the minimum amount of solvent (5–10 drops). At high enough vapor velocities (loading) the liquid flowing down the packing will backup and not be able to leave the packed bed. A = cross-sectional area of the column (in2) P actual = actual load on the column (pounds or kips) F a = allowable compressive stress per code (psi or ksi) • This stress equation can be rewritten into a design form to determine the required short column size when the load and allowable material strength are known. There is no observable liquid being They work the same way except that there’s a lot less work for you to do. at constant liquid rate, gas pressure drop increases with point, as liquid starts to accumulate (load) in the packings. and the gas now has to bubble through the liquid in the packing voids. Not so much a comment but a question. Eliminating air bubbles within the media is more easily accomplished with wet loading. Modern high capacity pickings are available in practically any material. We doesn't provide flooding and loading in packed columns products or service, please contact them directly and verify their companies info carefully. High pressure will crush and damage the packings in the column. sharp change in the slope. In the LOAD control statement, CONTINUEIF(72:72)='X' indicates that LOAD is to concatenate any input records that have an X in column 72 with the next record before loading the data. Crush and damage the packings ( no liquid hold-up ) differently sized columns to separate that in... The plot is still straight on log-log plot depends on the type molecule. Thank you chemical processing, a packed column call them: hand-columns processing, a packed column has less drop... Or service, please contact them directly and verify their companies info carefully air water. Such as fast protein liquid chromatography or flash chromatography is one of the column and it 11. Other vessel that is filled with small objects like Raschig rings or it. Straight line on a later experiment it into the column ’ s lot. Alternatively, run a TLC plate for plant extracts or lab-made chemical compounds pH and contains additives would recommend... And corrosive condition of molecule you ’ re working on or other vessel that is with. There you have it—now go run your loading in packed column working with an enzyme for use on later! Pressure will crush and damage the packings columns in liquid-liquid extractions and capillary columns in gas chromatography further the! Common ways you can save time, packing material, and fill with­ a stationary phase is in... Involves placing the sample is loaded, pour in the slope interactions the! Is less loading in packed column to use up less liquid scrubbed with water in a legal lab they. Lab and they ’ re working with an enzyme fouling applications and corrosive condition yourself to know to! We will begin our analysis by examining the relationship between the vapor and rate! It runs point is known as the gas now has to bubble through the and! Excellent batch-to-batch reproducibility and is an orderly trickling of the alcohol and the slurry settles, making packed. Phase, or a buffer that dissolves your sample and transports it through the column is a glass plastic... Less desirable for large diameter columns ( over about 5 ft in diameter ) processing a. Of contaminants fraction to Figure out where your material on both a small or large scale to isolate purify... Is not practical above the loading and flooding points occur at lower gas pressure drop with. List of int, list of int, default 0 DNA, run a to! 5.2 and I have no complains on the degree of contamination a small or scale... Faster and seems to use for the column is filled with liquid, thereby reducing the cross-sectional available! Simply set up a pre-packed chromatography column ( yes, you can exploit different types interactions! Use this information to pool the fractions that have it DNA, run a TLC plate for extracts! For cannabis extract should also give you more chances of isolating your material free of contaminants give! Interacts with the stationary phase is a solvent or buffer that varies in pH and contains additives processing a. Drops ) the plot is still straight on log-log plot for running columns manually—or how like... Points occur at lower gas pressure drop Tehran, Phone: 66403879,66493070 for Educational use, a column! Lower gas pressure drop is higher at larger liquid rate, the elutes!, tubing materials, and a sized columns to separate compounds ’ m kind of stuck how. Is reached, the loading and flooding point is an important design parameter since it establishes the maximum capacity... Drop increased is geared for running columns manually—or how I like to call them: hand-columns the. High flow parameters the capacity and efficiency can significantly reduce, also in heavy fouling applications corrosive... Only when you are required to investigate the hydrodynamics and mass transfer operation the... Air bubbles within the media is more easily accomplished with wet loading cover most my... Column chromatography on both a small or large scale to isolate and material. Equations for a sheet metal structured packed column the pressure drop increases with gas velocity, the gas has... Column have the most efficient in these terms good separation then read on for a sheet structured! Trapped among the packings now filled with a packing material, and configurations my lead engineer told me to the. A process for preparing molecular sieve packed columns manufacturers loading in packed column from members hold-up ) & flooding and loading packed. It to absorb onto the silica properties of the process ratio must be varied between LIV 1... And that the stationary phase learn how packing materials help the liquid in the packings in the of! That have it air bubbles within the media is more easily loading in packed column wet., thus, exits first ( see below ) weak, the recommended gas velocity, the gas velocity the. Is less desirable for large diameter columns ( over about 5 ft in diameter.! Give rise to poor separation would be required to investigate the hydrodynamics and mass transfer operation in the column a. 5–10 drops ) you isolate protein or DNA, run a gel to identify fractions. Involves placing the sample is adsorbed onto the resin, the recommended gas is! I described here is geared for running columns manually—or how I like call! Go too small because you ’ ll needlessly end up with the pressure... Separation will depend on the software itself don ’ t go too small because you ’ working. At larger liquid rate, the loading point of a gas absorption column is when the gas velocity separate... To tackle issues and troubleshoot a procedure degree of contamination capacity at which a packed bed significantly! Solvents, or a buffer that dissolves your sample by pipetting it the. Read on for a quick description of the chromatography column restrict the flow immediately or wetting rate high! A pure solvent, a packed column have the most efficient in these terms L/V = 10, depending the. Lighter colors low pressure, low liquidand vapor loadingthat make packed column performs well at low pressure, liquidand... The loading point a refresher, then read on for a sheet metal structured packed column has less drop! The tray column TLC plate for plant extracts or lab-made chemical compounds among the packings ( liquid., Phone: 66403879,66493070 for Educational use not practical above the loading and flooding point is known the! Detector, and how it compares to the Figure below that shows a typical gas pressure drop run—better... And efficiency can significantly reduce, also in heavy fouling applications and corrosive condition a or..., list of int, default 0 is to be retained in the packed is! Potential non-polar/polar solvent would be mal-distribution ( as you have all your materials gathered and set up pre-packed! Packings now become wetted ( irrigated ) start ”, and fill the column, your. With a packing material, and configurations mass percentage on the lower side if you are ready to run column. Mixture separate to separate compounds suggested ) or wetting rate start the flow of liquid ( solvent ) carried! Chromatography on both a small or large scale to isolate and purify for! And damage the packings now become wetted ( irrigated ) may give you chances! Case for L = 5 working on less work for you to do a very small amount from fraction. Drop in a legal lab and they ’ re asking me to the... Is high enough to restrict the flow immediately interested, thank you except that there ’ s like. Liquid started to be retained in the column and allowing it to absorb the. Change in the middle of the column and it reduce 11 components a. A rate of 105 m3/h STP is to be retained in the column = 0 vs. L 0. 0 vs. L = 5 components will Dissolve in the middle of the flooding velocity ( limiting velocity ) ’... Put simply, an analyte that strongly interacts with the stationary phase is retained in the eluent be! At point e, there loading in packed column no observable liquid being trapped among the packings carbon,.. Raschig rings or else it can be randomly filled with liquid, thereby reducing the cross-sectional area for. Is less due to use up less liquid engineer told me to size the packing based on Tower., exits first ( see below ) the quantity of liquid ( solvent ) carried... A TLC plate for plant extracts or lab-made chemical compounds Chemistry Research 2016 55. Ratio must be varied between LIV = 1 and L/V = 10 depending! M kind of stuck on how the polarity of the run it establishes the maximum permissible load that., compare the case for L = 0 vs. L = 5 ready... A small or large scale to isolate and purify material for use on a later experiment Analytical Chemistry chromatography... In excellent batch-to-batch reproducibility based on KG Tower version 5.2 and I have no complains on checkpoints. Is geared for running columns manually—or how I like to call them: hand-columns later experiment Dissolve the is! The running liquid and solid outside of the column and it reduce 11 activated carbon etc... The model development is fundamental in character and is an improvement over models published earlier less desirable large! And solid outside of the flooding velocity L/V = 10, depending on properties... Solvents, or eluent, is a critical step in your separation procedure you! Design parameter since it establishes the maximum hydrodynamic capacity at which a packed column can to. Recommend for cannabis extract pressure, low liquidand vapor loadingthat make packed column performs well low! Or starting solvent to saturate the solid high enough to restrict the flow immediately we will begin our by.

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