DOC316.53.01145 Ed7
DOC316.53.01145 Ed7
DOC316.53.01145 Ed7
Zinc
USEPA1 Zincon Method2 (0.01 to 3.00 mg/L)
1 2
Scope and Application: For water and wastewater. Digestion is required for a total zinc analysis (see Digestion).
USEPA approved for wastewater analyses 3500 Zn B: Federal Register, 45(105) 36166 (May 29, 1980). Adapted from Standard Methods for the Examination of Water and Wastewater.
Test preparation
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1. Select the test. Insert an adapter if required (the Instrumentspecific information table). Refer to the user manual for orientation.
3. Add the contents of one ZincoVer 5 Reagent Powder Pillow to the mixing cylinder. Stopper.
4. Invert several times to dissolve the powder completely. Inconsistent readings may result if all the particles are not dissolved. The sample should be orange. If the sample is brown or blue, the zinc concentration is too high or an interfering metal is present. Dilute the sample and repeat the test.
6. Prepared sample: Use a plastic dropper to add 0.5 mL of cyclohexanone to the remaining solution in the mixing cylinder.
7. Start the instrument timer. A 30-second reaction period will begin. During the reaction period, stopper the mixing cylinder and vigorously shake the prepared sample. The sample will be reddish-orange, brown, or blue, depending on the zinc concentration.
8. Start the instrument timer. A three-minute reaction period will begin. During this reaction period, complete step 9.
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Zero
Read
9. Pour the prepared sample solution from the mixing cylinder into a second sample cell.
10. When the timer expires, wipe the blank and insert it into the cell holder.
11. ZERO the instrument. The display will show: 0.00 mg/L Zn
12. Wipe the prepared sample and insert it into the cell holder.
READ the results in mg/L Zn.
Interferences
Table 419 Interfering substances
Interfering substance Aluminum Cadmium Copper Iron (ferric) Manganese Nickel Organic Material Highly buffered or extreme sample pH Interference level Greater than 6 mg/L Greater than 0.5 mg/L Greater than 5 mg/L Greater than 7 mg/L Greater than 5 mg/L Greater than 5 mg/L Large amounts may interfere. Pretreat the sample with a mild digestion. May exceed the buffering capacity of the reagents and require sample pretreatment. Adjust pH to 45. Samples containing AMP cause a negative interference. Digest the sample to eliminate this interference (follow the total phosphorus hot plate digestion, Method 8190). Amino-tri(methylene phosphonic acid) (AMP)
Important Note: Be sure to adjust the pH of the sample after the digestion to pH 45 with sodium hydroxide before the zinc analysis. Correct the pH level for volume changes.
Accuracy check
Standard additions method (sample spike) Required for accuracy check: Zinc Page 3 of 6
Zinc
Zinc Voluette Ampule Standard, 25 mg/L Zn Ampule breaker TenSette Pipet 0.1 - 1.0 mL and tips 25-mL mixing cylinders
1. After reading test results, leave the sample cell (unspiked sample) in the instrument. 2. Select OPTIONS>MORE>STANDARD ADDITIONS from the instrument menu. 3. Press OK to accept the default values for standard concentration, sample volume, and spike volumes. Press EDIT to change these values. After values are accepted, the unspiked sample reading will appear in the top row. 4. Open one Voluette ampule standard. 5. Use the TenSette Pipet to prepare spiked samples: add 0.1 mL, 0.2 mL, and 0.3 mL of standard to three 20-mL portions of fresh sample. 6. Follow the test procedure for each of the spiked samples starting with the 0.1 mL sample spike. Measure each of the spiked samples in the instrument. 7. Select GRAPH to view the results. Select IDEAL LINE (or best-fit) to compare the standard addition results to the theoretical 100% recovery. Standard solution method
Note: Refer to the instrument user manual for specific software navigation instructions.
Required for accuracy check: 100 mg/L zinc standard solution 10.00 mL Class A pipet 1000-mL Class A volumetric flask
1. Prepare a 1.00-mg/L zinc standard solution as follows. Pipet 10.00 mL of Zinc Standard Solution, 100-mg/L, into a 1000-mL volumetric flask. Dilute to the mark with deionized water. Prepare this solution daily. 2. Follow the zinc procedure. 3. To adjust the calibration curve using the reading obtained with the 1.00-mg/L standard solution, navigate to Standard Adjust in the software (OPTIONS>(MORE)>STANDARD ADJUST). 4. Turn on the Standard Adjust feature and accept the displayed concentration. If an alternate concentration is used, enter the concentration and adjust the curve to that value.
Digestion
A sample digestion is required before an analysis for total zinc can be started. A digestion will make sure that all zinc compounds in the sample are in a chemical form that will be measured. Complete the following steps to digest the sample.
Note: The following procedure is the USEPA mild digestion. See the Water Analysis Guide for more digestion procedures.
1. If nitric acid has not been added to the sample previously, add 5 mL of concentrated nitric acid to one liter of sample (use a glass serological pipet and pipet filler). If the sample was acidified at collection, add 3 mL of nitric acid to one liter of sample. 2. Transfer 100 mL of acidified sample to a 250-mL Erlenmeyer flask.
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Zinc
3. Add 5 mL of 1:1 hydrochloric acid*. 4. Heat the sample on a hot plate* at 95 C (203 F) until 15-20 mL remain. Make sure the sample does not boil. 5. Filter the cooled sample with 0.45 m filter to remove any insoluble material. 6. Adjust the pH of the digested sample to pH 45 with 5.0 N sodium hydroxide. See Sample collection, preservation and storage for instructions. 7. Quantitatively transfer the sample to a 100-mL volumetric flask and dilute to the mark with deionized water.
Method performance
Program 780 Standard 1.00 mg/L Zn Precision 95% Confidence Limits of Distribution 0.971.03 mg/L Zn Sensitivity Concentration change per 0.010 Abs change 0.013 mg/L Zn
Summary of method
Zinc and other metals in the sample are complexed with cyanide. Adding cyclohexanone causes a selective release of zinc. The zinc reacts with 2-carboxy-2'-hydroxy-5'-sulfoformazyl benzene (zincon) indicator to form a blue-colored species. The blue color is masked by the brown color from the excess indicator. The intensity of the blue color is proportional to the amount of zinc present. Test results are measured at 620 nm.
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Zinc
Required apparatus
Description Cylinder, graduated, mixing, 25-mL Sample cell, 10 mL, square, matched pair Quantity 1 2 Unit each 2/pkg Catalog number 2088640 2495402
Recommended standards
Description Water, deionized Zinc Standard Solution, 100-mg/L Zinc Standard Solution, 10-mg/L Voluette Ampule, 25-mL as Zn Zinc Standard Solution, 1000-mg/L Unit 4L 100 mL 16/pkg 100 mL Catalog number 27256 237842 1424610 1417742
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Edition 7