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Calibration Techniques

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# Calibration Techniques - PowerPoint PPT Presentation

Calibration Techniques. 1. Calibration Curve Method 2. Standard Additions Method 3. Internal Standard Method. Calibration Curve Method. Most convenient when a large number of similar samples are to be analyzed. Most common technique. Facilitates calculation of Figures of Merit.

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## Calibration Techniques

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### Calibration Techniques

1. Calibration Curve Method

2. Standard Additions Method

3. Internal Standard Method

### Calibration Curve Method

Most convenient when a large number of similar samples are to be analyzed.

Most common technique.

Facilitates calculation of Figures of Merit.

### Calibration Curve Procedure

Prepare a series of standard solutions (analyte solutions with known concentrations).

Plot [analyte] vs. Analytical Signal.

Use signal for unknown to find [analyte].

### Example: Pb in Blood by GFAAS

Results of linear regression:

S = mC + b

m = 5.56 mAbs/ppb

b = 0.93 mAbs

A sample containing an unknown amount of Pb gives a signal of 27.5 mAbs. Calculate the Pb concentration.

S = mC + b

C = (S - b) / m

C = (27.5 mAbs – 0.92 mAbs) / 5.56 mAbs / ppb

C = 4.78 ppb

(3 significant figures)

Calculate the LOD for Pb

20 blank measurements gives an average signal

0.92 mAbs

with a standard deviation of

σbl = 0.36 mAbs

LOD = 3 σbl/m = 3 x 0.36 mAbs / 5.56 mAbs/ppb

LOD = 0.2 ppb

(1 significant figure)

Find the LDR for Pb

Lower end = LOD = 0.2 ppb

(include this point on the calibration curve)

SLOD = 5.56 x 0.2 + 0.93 = 2.0 mAbs

(0.2 ppb , 2.0 mAbs)

Find the LDR for Pb

Upper end = collect points beyond the linear region and estimate the 95% point.

Suppose a standard containing 18.5 ppb gives rise to s signal of 98.52 mAbs

This is approximately 5% below the expected value of 103.71 mAbs

(18.50 ppb , 98.52 mAbs)

Find the LDR for Pb

LDR = 0.2 ppb to 18.50 ppb

or

LDR = log(18.5) – log(0.2) = 1.97

2.0 orders of magnitude

or

2.0 decades

Find the Linearity

Calculate the slope of the log-log plot

Remember

S = mC + b

log(S) = log (mC + b)

b must be ZERO!!

log(S) = log(m) + log(C)

The original curve did not pass through the origin. We must subtract the blank signal from each point.

### Standard Addition Method

Most convenient when a small number of samples are to be analyzed.

Useful when the analyte is present in a complicated matrix and no ideal blank is available.

### Standard Addition Procedure

Add one or more increments of a standard solution to sample aliquots of the same size. Each mixture is then diluted to the same volume.

Prepare a plot of Analytical Signal versus:

volume of standard solution added, or

concentration of analyte added.

### Standard Addition Procedure

The x-intercept of the standard addition plot corresponds to the amount of analyte that must have been present in the sample (after accounting for dilution).

The standard addition method assumes:

the curve is linear over the concentration range

the y-intercept of a calibration curve would be 0

### Example: Fe in Drinking Water

The concentration of the Fe standard solution is 11.1 ppm

All solutions are diluted to a final volume of 50 mL

[Fe] = ?

x-intercept = -6.08 mL

Therefore, 10 mL of sample diluted to 50 mL would give a signal equivalent to 6.08 mL of standard diluted to 50 mL.

Vsam x [Fe]sam = Vstd x [Fe]std

10.0 mL x [Fe] = 6.08 mL x 11.1 ppm

[Fe] = 6.75 ppm

### Internal Standard Method

Most convenient when variations in analytical sample size, position, or matrix limit the precision of a technique.

May correct for certain types of noise.

### Internal Standard Procedure

Prepare a set of standard solutions for analyte (A) as with the calibration curve method, but add a constant amount of a second species (B) to each solution.

Prepare a plot of SA/SB versus [A].

### Notes

The resulting measurement will be independent of sample size and position.

Species A & B must not produce signals that interfere with each other. Usually they are separated by wavelength or time.

### Example: Pb by ICP Emission

Each Pb solution contains 100 ppm Cu.