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Here is the assignment I have:

You are working for Matrix Pro - a company involved in analytical assessment and method development for the clean-up of contaminated waters.

You received water samples from a potential client. The samples may contain the following ions: $\ce{H+, Ba^2+, OH^─}$

The potential client requested a qualitative analysis of the sample as well as the development of a treatment technique that will bring the pH value to neutral and eliminate the barium ions. For comparison another water sample (considered to be non-contaminated) was also sent for similar qualitative analysis.

Assignment

  1. Develop an experimental procedure to comply with the request of the potential client.

  2. Draw a flow chart.

  3. Tabulate all your observations and data.

What I'm not sure about is finding the amount of barium present in the unknown sample so I can determine the amount of precipitating reagent to add. I just want to know what type of analysis to do. Chromatography? Spectrophotometry? Something else?

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    $\begingroup$ You could add some sodium sulfate solution to a sample of the water to see if barium sulfate precipitates. It wouldn't be difficult or expensive to do this quantitatively for that matter. $\endgroup$ – airhuff Apr 11 '17 at 2:01
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Because the client is ultimately interested in removing the barium by precipitation, gravimetric analysis is likely a suitable solution. This can be done in a few hours in a lab with basic equipment like a filter flask, a drying oven, an analytical balance and the appropriate reagents.

You can take advantage of the fact that barium sulfate is very insoluble in water by adding some saturated solution of sodium sulfate to a known volume of a sample of the water. Then just filter out the barium sulfate onto some pre-weighed filter paper, dry, weigh, and calculate the mass of barium (from the measured mass and the molecular weight of barium sulfate) per volume of water. You should repeat the analysis to be sure you added enough sodium sulfate solution to precipitate all of the barium.

If there is little or no precipitate found, you have a couple options. Firstly, you can optimize the gravimetric analysis by using large volumes of sample with a small filter and a good analytical balance. Also be sure to pre-filter the sample prior to adding the sodium sulfate in case there are suspended particulates, which would get measured just as if they were barium.

If a gravimetric analysis does not provide the detection limit required by the client, the next best options are atomic absorption spectroscopy (AAS) and inductively coupled plasma - atomic emission spectroscopy (ICP-AES). As these analyses can be done very cheaply (~\$10-$30 per sample) you may actually want to do this to begin with. The down side of outsourcing is that the turnaround time could be weeks, or the price could quadruple if you need results fast.

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  • $\begingroup$ maybe... It depends on what the Ba level is in the contaminated water, and what the highest level acceptable in the "cleaned-up" waste. $\endgroup$ – MaxW May 4 '17 at 6:47
  • $\begingroup$ Gravimetric analysis of $\ce{Ba^{2+}}$ was one of the practice exercises in my quantitative analytics lab. We had to use filter crucibles because $\ce{BaSO_4}$ is usually very fine-grained and to allow for heating at 900 K for several hours to remove water. $\endgroup$ – TAR86 May 4 '17 at 19:17
  • $\begingroup$ @TAR86 , My first response is: 900K ?! I guess that would get it dry in a hurry. The way I've described it is basically an ASTM standard method that my lab has probably done thousands of times over the years. So long as there is sufficient $\ce{Ba^2+}$ in solution, gravimetric analysis can actually give much better precision that AA or particulary ICP. $\endgroup$ – airhuff May 4 '17 at 19:31

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