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Zincon Method* USEPA approved for wastewater analysis** (digestion needed; see Section 2)
2. Press: 97 ENTER
* Adapted from Standard Methods for the Examination of Water and Wastewater.
** Federal Register, 45 (105) 36166 (May 29, 1980).
603
ZINC, continued
5. Measure 10 mL of
the orange solution into
another sample cell
(the blank).
6. Add 0.5 mL of
cyclohexanone to the
remaining orange
solution in the first
sample cell (the
prepared sample).
8. Press:
Shake vigorously for 30
TIMER ENTER
seconds (the prepared
A 3-minute reaction
sample).
period will begin.
604
ZINC, continued
Sampling and Storage
Collect samples in acid-washed plastic bottles. For storage,
adjust the pH to 2 or less with nitric acid (about 2 mL per liter).
The preserved samples can be stored up to six months at room
temperature.
Adjust the pH to 4 to 5 with 5.0 N sodium hydroxide before
analysis. Do not exceed pH 5, as zinc may be lost as a
precipitate. Correct the test result for volume additions; see
Sampling and Storage, Volume Additions, in Section 1 for more
information.
If only dissolved zinc is to be determined, filter the sample before
the acid addition.
Accuracy Check
Standard Additions Method
a) Snap the neck off a Zinc PourRite Ampule Standard, 25
mg/L Zn.
b) Use the TenSette Pipet to add 0.1, 0.2, and 0.3 mL of
standard to three 25-mL samples. Mix each thoroughly.
c) Analyze each sample as described above. The zinc
concentration should increase 0.1 mg/L for each 0.1 mL of
standard added.
d) If these increases do not occur, see Standard Additions in
Section 1 for more information.
Standard Solution Method
Prepare a 0.50 mg/L zinc standard solution by diluting 5.00 mL
of Zinc Standard Solution, 100 mg/L as Zn, to 1000 mL with
deionized water in a Class A 1000-mL volumetric flask. Prepare
this solution daily. Use this solution as the sample and perform
the zinc procedure as described above.
Method Performance
Precision
In a single laboratory, using a standard solution of 1.50 mg/L Zn
and two representative lots of reagent with the instrument, a
single operator obtained a standard deviation of 0.02 mg/L Zn.
Estimated Detection Limit (EDL)
The EDL for program 97 is 0.02 mg/L Zn. For more information
on derivation and use of Hachs estimated detection limit, see
Section 1.
605
ZINC, continued
Interferences
The following may interfere when present in concentrations
exceeding those listed below.
Interfering Substance
Aluminum
6 mg/L
Cadmium
0.5 mg/L
Copper
5 mg/L
Iron (ferric)
7 mg/L
Manganese
5 mg/L
Nickel
5 mg/L
Organic material
606
ZINC, continued
Summary of Method
Zinc and other metals in the sample complex with cyanide.
Adding cyclohexanone selectively releases zinc. The zinc then
reacts with the
2-carboxy-2-hydroxy-5-sulfoforamazyl benzene (zincon)
indicator and forms a blue color that is proportional to the zinc
concentration.
REQUIRED REAGENTS
Zinc Reagent Set, 20 mL size (100 tests)......................................................................24293-00
Includes: (1) 14033-32, (1) 21066-69
Description
Quantity Required
Per Test
Units
Cat. No.
ZINC, continued
OPTIONAL APPARATUS (continued)
Description
Units
Cat. No.
608