Testing the Performance of an Ion Chromatography Column

Testing the Performance of an Ion Chromatography Column

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Testing the Performance of an Ion Chromatography Column


Ion column chromatography is used to separate both cations and anions.
The separation of ions is performed by using an ion exchange resin
(this lab uses an anion exchange resin which is a high molecular
weight polymer). The amount of time required for certain ions to move
through the column depends on the affinities of the ions. The mobile
phase’s anions, sodium bicarbonate in this lab, will force the ion
that’s being tested out of the column.


Procedure
---------

1. Given the choice of six 1000 ppm sodium salts, choose three. The
solutions to choose from are: sodium fluoride, sodium chloride, sodium
bromide, sodium sulfate, sodium phosphate, and sodium nitrate.

2. Prepare three 25 mL solutions each with one of the chosen sodium
salts, diluting with the carbonate buffer.

3. Run an IC on each one.

4. For day two, come up with an experiment that evaluates the column’s
performance. Look in textbooks to see what parameters can be tested.

The three anions we tested on day one were: fluoride, chloride, and
bromide. It took several tries to get some of the spectra to show up
correctly. On day two, our lab
consisted of making two solutions. Each lab had varying concentrations
of each of the three anions tested during the first day. The first
solution consisted of: 1 ppm chloride, 2 ppm fluoride, and 5 ppm
bromide. The second solution was: ½ ppm chloride, 4 ppm fluoride, and
10 ppm bromide.


Results
-------

The first solution ran was the bicarbonate buffer. This buffer showed
peaks as following:

Peak Number

Area %

RT (min)

Area

1

72.453

1.64

772,083

2

8.889

3.8

94,728

3

3.359

4.22

35,791

4

15.299

5.61

163,029

The first run of F-:

Peak Number

Area %

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RT (min)

Area

1

44.189

3.8

1,638,843

2

11.333

4.22

420,305

3

41.915

5.6

1,554,517

4

2.563

10.75

95,063

The first peak, with a retention time of 3.80 minutes, is the F-.
Peak #3 at 5.60 minutes is a Cl- contaminant.

The second run of F-:

Peak Number

Area %

RT (min)

Area

1

0.127

1.54

9,583

2

0.64

1.95

48,346

3

0.309

2.51

23,370

4

6.354

3.38

479,871

5

22.216

3.77

1,677,754

6

15.936

4.18

1.203,493

7

49.597

5.6

3,745,628

8

8.69

9

10.88


The page wasn’t fully copied, so I didn’t have the numbers to the last
two peaks. Once again, the peak at 3.77 is the F-. Peaks 4, 7, and 8
correspond to the buffer. The peak at 5.60 is also more Cl-
contaminant.

Chloride:

Peak Number

Area %

RT (min)

Area

1

6.802

3.08

409,572

2

1.782

3.78

107,276

3

16.648

4.21

1,002,379

4

0.701

4.54

42,198

5

74.067

5.58

4,459,512

The peak with the greatest area, peak #5, is from the chloride ion.

Bromide:

Peak Number

Area %

RT (min)

Area

1

6.811

3.78

90,057

2

8.485

4.2

112,178

3

43.667

5.53

577,337

4

22.294

8.7

294,762

5

18.743

16.62

247,815

The peak at 8.70 minutes is the bromide ion peak.

Buffer Day Two:

Peak Number

Area %

RT (min)

Area

1

6.325

3.34

42,716

2

22.765

3.8

153,743

3

3.339

4.19

22,548

4

34.748

5.18

234,669

5

14.112

5.66

95,304

6

18.71

8.67

126,359


Soln. #1:

Peak Number

Area %

RT (min)

Area

1

2.001

1.69

153,204

2

18.816

3.81

1,440,502

3

16.67

4.22

1,276,266

4

1.703

4.58

130,373

5

38.843

5.64

2,973,741

6

21.967

9.01

1,681,806

The peaks in this solution showed up where we expected them. The 2 ppm
F- peak was at 3.81 compared to the retention times of 3.77 and 3.80
of the two previous runs at 1 ppm. The 1 ppm Cl- peak showed up at
5.64, the 1 ppm Cl- peak before was at 5.58. Lastly, the 5 ppm Br- had
a retention time of 9.01 minutes compared to 8.70 for the 1 ppm
solution.

Soln. #2:

Peak Number

Area %

RT (min)

Area

1

0.609

2.15

74,491

2

1.963

2.56

240,216

3

25.847

3.66

3,162,306

4

13.296

4.06

1,626,647

5

0.726

4.42

88,762

6

28.436

5.47

3,478,956

7

28.414

8.76

3,476,353

8

0.625

10.71

76,502

9

0.084

11.63

10,276

The 4 ppm F- peak was at 3.66 minutes this time. The ½ ppm Cl- ion
showed up at 5.47 minutes. The 10 ppm Br- appeared at 8.76 minutes,
compared to 8.70 minutes for the 1 ppm solution and 9.01 minutes for
the 5 ppm solution.


Discussion
----------

Overall, the lab ran smoothly. All of the data suggests that even when
you vary the concentrations, the ion elutes out of the column at
relatively the same time. Let’s take


bromide as an example. When the concentration was 1 ppm, the ion
eluted at 8.70 minutes. By using 5 ppm sodium bromide, the retention
time was at 9.01 minutes. In the last solution, the bromide
concentration was 10 ppm, and the retention time was 8.76 minutes. The
retention times were all very similar, even though the concentrations
were varied.

To sum it all up, I think the column performance was pretty good. The
only slight problem we had was that some of the printouts had quite a
few extra peaks. I’m not exactly sure what caused these. Also, on both
of the sodium fluoride runs, there were obvious chloride peaks from
contamination. We made sure to use separate pipets for each solution,
so I’m not sure where that came from.
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