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Topic: Re: Quantitative analysis of Ca2+ in Milk  (Read 22719 times)

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Offline ivychen1989

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Re: Quantitative analysis of Ca2+ in Milk
« on: May 02, 2006, 04:20:30 AM »
For school, I am supposed to design an experiment.  I've chosen to do a quantitative analysis of Ca2+ in Milk, comparing the concentration of Ca2+ after the milk has been heated to different temperatures.  Does anyone know if there would be any problems in me letting the milk cool before doing titrations?  (I don't want to crack the glassware if I change the temperature in the conical flask too fast when titrating.)

Please say if someone knows of anything terribly wrong with the back titration I've come up with:
1.  10.0mL of milk and 20.0 mL of standardized EDTA (about 0.05molL-1) mixed thoroughly together so that all the Ca2+ complexes with the EDTA
2.  20mL of KOH added to bring pH up to 13, so that the Mg2+ in the milk precipitates as Mg(OH)2 (and will not interfere with the titration)
3.  2mL of hydroxyl naphthol blue indicator (turning the solution blue)
4.  titrate with standard calcium chloride solution (about 0.05molL-1) until the colour of the solution changes to violet (when the extra Ca2+ begins to form a red complex with the indicator)

Would I be able to keep the KOH (for a few weeks) or will it react with the CO2 in the air?  (I'll be able to keep the other solutions,right?)
Would the temperatures 20, 40, 60, 80, 100 degrees Celsius be reasonable to heat my milk to?
If anyone knows of any scientific work related to this topic, could they post it up?

Thanks for any help/suggestions.

Offline Borek

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Re: Quantitative analysis of Ca2+ in Milk
« Reply #1 on: May 02, 2006, 05:17:30 AM »
While there is nothing particularly wrong with the titration I wonder what you will be really determining in the experiment. Amount of calcium per sample will not change, that's mass conservation law. Perhaps during heating some of the calcium can get binded to peptides present in the milk, but you will most likely destroy this equilibrium adding strong base.

Thus it will be very surprising for me if the results will show any dependence between concentration and heating - but keep us posted, I will be happy to be mistaken on that one ;)
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Offline xiankai

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Re: Re: Quantitative analysis of Ca2+ in Milk
« Reply #2 on: May 03, 2006, 04:43:54 AM »
this has also been done before, u can take a look at others' attempts

http://www.chemicalforums.com/index.php?topic=7158.0
one learns best by teaching

Offline ivychen1989

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Re: Quantitative analysis of Ca2+ in Milk
« Reply #3 on: May 06, 2006, 02:06:10 AM »
I've only been allowed to do a rough trial using beakers and measuring cylinders, so I haven't been able to tell if there are any differences in the calcium concentration.  The method works, as in I've been able to figure out a concentration similar to the one written on the milk bottle).
I'll write more when I've done my proper, accurate experiment.

Davo89

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Re: Quantitative analysis of Ca2+ in Milk
« Reply #4 on: May 16, 2006, 07:18:41 PM »
i was wondering around how much calcium chloride solution in mL's is needed???

Offline Borek

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Re: Quantitative analysis of Ca2+ in Milk
« Reply #5 on: May 17, 2006, 03:37:29 AM »
i was wondering around how much calcium chloride solution in mL's is needed???

Depends on amount of calcium in the milk, concentration of EDTA and concetration of CaCl2.
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Davo89

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Re: Quantitative analysis of Ca2+ in Milk
« Reply #6 on: May 17, 2006, 11:11:03 PM »
Jus need a rough estimate really but it's the same concentrations and volumes as is in the procedure at top of page (practically repeating the experiment)

thx

Offline ivychen1989

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Re: Quantitative analysis of Ca2+ in Milk
« Reply #7 on: May 18, 2006, 02:30:13 AM »
Well, right now I've only used one bottle of milk, and have yet to try it all out on another.  I also titrated after heating milk at 30, 50, 70, and 90 degrees Celsius to see if there was a trend in my results (the calcium concentration decreased then increased again as heating temperatures increased).  My results are as follows:

20 degrees          0.0311 mol/L
30 degrees          0.0310 mol/L
40 degrees          0.0305 mol/L
50 degrees          0.0297 mol/L
60 degrees          0.0289 mol/L
70 degrees          0.0291 mol/L
80 degrees          0.0294 mol/L
90 degrees          0.0302 mol/L
100 degrees        0.0308 mol/L

Does anyone know/can guess reasons why this would be?
I'll put up my results for the next bottle when I've finished.

i was wondering around how much calcium chloride solution in mL's is needed???

As for how much calcium chloride solution is needed, definitely no more than 15mL for each titration, and I made 1000 mL for the whole thing, though I may run out during my analysis using the second bottle, because I did extra titrations for 4 different temperatures (and I had not taken that into account when I decided on the standard calcium volume I needed).

Offline ivychen1989

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Re: Quantitative analysis of Ca2+ in Milk
« Reply #8 on: May 20, 2006, 12:00:41 AM »
Today (Saturday) I went to school and finished off my investigation.  Here are my results for my second bottle of milk.  The trend shown in both bottles are similar, although the calcium concentrations are higher from my second bottle.

20 degrees      0.0313
30 degrees      0.0311
40 degrees      0.0305
50 degrees      0.0297
60 degrees      0.0293
70 degrees      0.0296
80 degrees      0.0299
90 degrees      0.0305
100 degrees    0.0313

I really can't think of reasons why the trend is like this.

Offline Borek

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Re: Quantitative analysis of Ca2+ in Milk
« Reply #9 on: May 20, 2006, 04:46:48 AM »
What was the complete procedure? And I mean not only just determination, but whole procedure starting from the moment you've bought the milk ;)
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Offline ivychen1989

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Re: Quantitative analysis of Ca2+ in Milk
« Reply #10 on: May 20, 2006, 06:06:55 AM »
Well, I first made all the solutions I needed, the EDTA and calcium chloride.  I standardized the EDTA I made with a magnesium sulfate solution that I'd made, and I made my standard calcium chloride solution by dissolving calcium carbonate in hydrochloric acid.

I bought my first bottle of milk at the dairy, and I took it home and put it in the fridge.  Then I carried it to school the day after, and put it in the school's fridge about an hour and a half afterwards (it's been so cold lately and the classes didn't have the heaters on, so I don't think this would have affected anything).

Throughout that week, I titrated the milk.  Depending on how many titrations I had time to do (one, two, or three different temperatures), I would pour out the milk that I needed into a large beaker; the rest of the milk stayed in the fridge.

To heat the milk, I poured some milk into another beaker and put the beaker on a hotplate (which was far from my large beaker of milk).  Once a thermometer showed that the milk had reached the temperature I wanted, I would take the beaker off the hotplate and placed it in a cold water bath.

Once the milk's temperature had decreased to 20 degrees Celsius, I would pipette the milk into conical flasks that already had the EDTA, KOH and indicator in them.  I titrated four times for each temperature to firstly get a rough idea of the titre values, then the other tree titrations gave me concordant results.

I bought my second bottle of milk on Thursday, and kept it in my fridge until this morning, when I brought the bottle to school, where I kept most of it in the fridge and only took out enough milk for me to heat at three different temperatures.  So I went back to the fridge to fill up my beaker twice after that.

I did the temperatures in this order both times: 20, 40, 60, 80, 100, 30, 50, 70, 90 degrees Celsius.

Offline Borek

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Re: Quantitative analysis of Ca2+ in Milk
« Reply #11 on: May 20, 2006, 06:48:55 AM »
So basically milk was stored for some unknown time in undefined, albeit low temperatures, than it was heated for few minutes to the higher temperature, cooled and titrated?

I am surprised you have found any dependence. The only thing I can think of is some additional equilibrium taking place between Ca2+ and other substances present in the milk, equilibrium that is somehow affected by the heating (and protein denaturation?).

Note that amount of calcium in your samples was always the same, that's mass conservation law. Only thing that can change is free calciium concentration, or, more precisely - concentration of calcium that can be titrated with EDTA at the pH, temperature and speed of your titration procedure.

Interesting.
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Offline billnotgatez

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Re: Quantitative analysis of Ca2+ in Milk
« Reply #12 on: May 20, 2006, 01:02:42 PM »
One could infer that there is something in milk (protein? or fat?) that sequesters calcium when heated to a specific temperature. How often did you replicate each temperature treatment? Since the temperatures observed are not naturally occurring in animals one wonders what the importance of this analysis considering how pasteurization is done.



Offline ivychen1989

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Re: Quantitative analysis of Ca2+ in Milk
« Reply #13 on: May 21, 2006, 01:50:17 AM »
So basically milk was stored for some unknown time in undefined, albeit low temperatures, than it was heated for few minutes to the higher temperature, cooled and titrated?
I am surprised you have found any dependence.

Yeah, but I made sure that I did all the titrations before the milk's best-before-date.  And other students in my class have been doing the same type of investigation (though using different brands of milk); out of the three I spoke to, two have gotten similar trends to mine, and one has gotten no trend.

How often did you replicate each temperature treatment? Since the temperatures observed are not naturally occurring in animals one wonders what the importance of this analysis considering how pasteurization is done.

Each temperature was done once for each bottle, so twice.  I did this investigation because of the old-wives-tale that we shouldn't boil milk because heating it decreases the calcium concentration, which is, of course, bad.

Thanks for the suggestions, I'll see if I can find anything in the milk that might have made the calcium unable to react with the EDTA.

Offline Borek

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Re: Quantitative analysis of Ca2+ in Milk
« Reply #14 on: May 21, 2006, 04:58:41 AM »
I did this investigation because of the old-wives-tale that we shouldn't boil milk because heating it decreases the calcium concentration, which is, of course, bad.

As the amount of titratable calcium goes up in the higher temperatures, tale seems to be wrong according to your results.

But it doesn't mean your results support the idea of not heating the milk to 60 deg C where you have found minimum concentration - as you don't know what amount of calcium can be freed when the milk is digested.

I digged some and this may be of help:

http://www.afns.ualberta.ca/Courses/Nufs403/PDFs/chapter2.pdf

(it supports the original tale in a way - although one need to check the solubility of calcium phosphate in gastric juices).
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