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9. A 0.2056 g chocolate sample was digested (completely dissolved) in nitric aci

ID: 3303325 • Letter: 9

Question

9. A 0.2056 g chocolate sample was digested (completely dissolved) in nitric acid and the resulting solution diluted to a total volume of 10.00 mL. A series of solutions were then prepared with total constant volumes of 5.00 mL, each containing 1.00 mL of the chocolate solution plus variable volumes of a 475 ppb chromium standard. A standard addition calibration was obtained by measuring the constant volume solutions using ICP-MS to determine the chromium concentrations (results shown below). *See page 16 in textbook for ppb definition Vs ful) LINEST Output 1888.881 9950.456 63.61053 360.0394 0.995484 495.6791 S+X 30000 y 1888 3x + 9950.5 R2 =0.9955 9508 14062 17488 20037 24003 27661 25000 20 20000 15000 60 80 100 10000 DEVSQ= 60.72158 5000 0 0 6 [Crl (ppb) 8 A. what is the chromium concentration (in ppb) ± ,for the diluted (5 mL) sample? B. what is the chromium concentration (in ppb) ± 95% confidence interval for the diluted (5 mL) sample? C. What is the chromium concentration (in ppb) for the original (solid) chocolate sample?

Explanation / Answer

(a)

In the data given for the diluted 5mL sample, making use of the best fit equation, we get the following conc. values for the six solutions in series:

0, 0.573, 1.05, 1.405, 1.956, 2.46

The 95% C.I. is then : -0.52 to 3 ppb

(b)

From the given data

concentration of standard (Cs) in the dilute sample when,

V(ml)         Cs(ppb)

0                   0

0.02      125 x 0.02/5 = 0.5

0.04      125 x 0.04/5 = 1.0    

0.06      125 x 0.06/5 = 1.5

0.08      125 x 0.08/5 = 2.0

0.1         125 x 0.1/5 = 2.5

Concentration of chromium in dilute unknown sample Cx

with 0.5 ppb standard

Cx/(Cx + 0.5) = 9508/14062

Cx = 1.044 ppb

with 1.0 ppb standard

Cx/(Cx + 1.0) = 9508/17488

Cx = 1.191 ppb

with 1.5 ppb standard

Cx/(Cx + 1.5) = 9508/20037

Cx = 1.354 ppb

with 2.0 ppb standard

Cx/(Cx + 2.0) = 9508/24003

Cx = 1.312 ppb

with 2.5 ppb standard

Cx/(Cx + 2.5) = 9508/27661

Cx = 1.310 ppb

mean concentration = 1.242

standard deviation = sq.rt.(sum(x-X)/5)

= sq.rt.((0.0392 + 0.0026 + 0.0125 + 0.0049 + 0.0046)/5)

= 0.113

at 95% confidence level the range would be 1.102 to 1.382 ppb

(C)

For the original chocolate sample, we put y = 0 in the best fit equation.

Putting y=0, we get:

x = -1.386

The -ve sign is because of extrapolation into the -ve x axis.

So, [Cr] in chocolate sample = 1.386 ppb