Zinc

DOC316.53.01145

USEPA1 Zincon Method2

Method 8009

0.01 to 3.00 mg/L Zn

Powder Pillows

Scope and application: For water and wastewater. Digestion is required for a total zinc analysis.
1
2

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
Instrument-specific information
Table 1 shows all of the instruments that have the program for this test. The table also
shows sample cell and orientation requirements for reagent addition tests, such as
powder pillow or bulk reagent tests.
To use the table, select an instrument, then read across to find the applicable information
for this test.
Table 1 Instrument-specific information
Instrument

Sample cell orientation

Sample cell

DR 6000

The fill line is to the right.

2495402

DR 3800
DR 2800
DR 2700
DR 1900
DR 5000

The fill line is toward the user.

DR 3900
DR 900

The orientation mark is toward the user.

2401906

Before starting
Install the instrument cap on the DR 900 cell holder before ZERO or READ is pushed.
Clean all glassware with 6.0 N (1:1) hydrochloric acid, then fully rinse with deionized water to remove contaminants.
Use only glass-stoppered mixing cylinders in this procedure.
Make sure that the dropper that is used in this procedure is plastic. Droppers that have rubber bulbs can contaminate the
reagent.
The reagents that are used in this test contain potassium cyanide. Keep cyanide solutions at pH > 11 to prevent
exposure to hydrogen cyanide gas. Collect the reacted samples for proper disposal.
Review the Safety Data Sheets (MSDS/SDS) for the chemicals that are used. Use the recommended personal protective
equipment.
Do not use the Pour-Thru Cell or sipper module (for applicable instruments) with this test.
Dispose of reacted solutions according to local, state and federal regulations. Refer to the Safety Data Sheets for disposal
information for unused reagents. Refer to the environmental, health and safety staff for your facility and/or local regulatory
agencies for further disposal information.

Items to collect
Description

Quantity

Cyclohexanone

0.5 mL

ZincoVer 5 Reagent Powder Pillow, 20-mL

Mixing cylinder, graduated, 25-mL, glass stopper

Sample cells (For information about sample cells, adapters or light shields, refer to Instrumentspecific information on page 1.)

Refer to Consumables and replacement items on page 6 for order information.

Sample collection and storage

Collect samples in clean glass or plastic bottles that have been cleaned with 6 N (1:1)
hydrochloric acid and rinsed with deionized water.
To preserve samples for later analysis, adjust the sample pH to less than 2 with
concentrated nitric acid (about 2 mL per liter). No acid addition is necessary if the
sample is tested immediately.
Keep the preserved samples at room temperature for a maximum of 6 months.
Before analysis, adjust the pH to 45 with 5 N sodium hydroxide solution. Do not
exceed pH 5 as zinc can precipitate. Do not add the reagent to samples with pH less
than 4 because there is cyanide in the reagent.
Correct the test result for the dilution caused by the volume additions.

Powder pillow procedure

Start

1. Start program 780 Zinc.

For information about
sample cells, adapters or
light shields, refer to
Instrument-specific
information on page 1.
Note: Although the program
name can be different
between instruments, the
program number does not
change.

2. Fill a 25-mL graduated

mixing cylinder with 20 mL
of sample.

3. Add the contents of one

ZincoVer 5 Reagent Powder
Pillow to the mixing cylinder.
Close the cylinder.

4. Shake the cylinder

vigorously to dissolve the
powder completely.
Inconsistent readings can
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.

Zinc, Zincon Method (3.00 mg/L)

5. Blank preparation: Pour

10 mL of the solution into a
sample cell.

6. Prepared sample: Use a

plastic dropper to add
0.5 mL of cyclohexanone to
the solution in the mixing
cylinder.

7. Start the instrument

timer. A 30-second reaction
time starts.

8. During the reaction

period, close the mixing
cylinder and vigorously
shake the prepared sample.
The sample becomes
reddish-orange, brown or
blue, depending on the zinc
concentration.

9. Start the instrument

timer. A 3-minute reaction
time starts.
During the reaction period,
complete the next step.

10. Pour the prepared

sample solution from the
mixing cylinder into a
second sample cell.

11. When the timer expires,

clean the blank sample cell.

12. Insert the blank into the

cell holder.

Zero

13. Push ZERO. The

display shows 0.00 mg/L Zn.

Read

14. Clean the prepared

sample cell.

15. Insert the prepared

sample into the cell holder.

16. Push READ. Results

show in mg/L Zn.

Interferences
Interfering substance

Interference level

Aluminum

More than 6 mg/L

Cadmium

More than 0.5 mg/L

Copper

More than 5 mg/L

Iron (ferric)

More than 7 mg/L

Manganese

More than 5 mg/L

Zinc, Zincon Method (3.00 mg/L)

Interfering substance

Interference level

Nickel

More than 5 mg/L

Organic Material

Large amounts may interfere. Pretreat the sample with a digestion.

Highly buffered samples or

extreme sample pH

Can prevent the correct pH adjustment of the sample by the reagents. Sample pretreatment may be necessary. Adjust the pH to 45.

Amino-tri(methylene phosphonic
acid) (AMP)

Samples that contain AMP cause a negative interference. Digest the sample to remove
this interference (use the total phosphorus hot plate digestion, Method 8190).
Note: Be sure to adjust the pH of the sample after the digestion to pH 45 with sodium hydroxide
before the zinc analysis.

Digestion
For total zinc determinations, the sample must be digested with heat and acid to make
sure that all forms of the metal are measured. The steps that follow can be used for a
mild digestion.
Note: The following procedure is the USEPA mild digestion procedure. Refer to the Water Analysis
Guide for more digestion procedures.

1. Add concentrated nitric acid to the sample with a glass serological pipet and pipet
filler:

2.
3.
4.
5.
6.
7.

If the sample was acidified for preservation, add 3 mL of nitric acid to 1 liter of the
preserved sample.
If the sample was not acidified for preservation, add 5 mL of nitric acid to 1 liter of
sample.
Transfer 100 mL of acidified sample to a 250-mL Erlenmeyer flask.
Add 5 mL of 1:1 hydrochloric acid.
Put the sample on a hot plate at 95 C (203 F) until 1520 mL of the sample
remains. Make sure that the sample does not boil.
Put the cooled sample through a 0.45-m filter to remove any insoluble material.
Adjust the pH of the digested sample to pH 45 with 5.0 N sodium hydroxide. Do not
exceed pH 5 as zinc may precipitate.
Quantitatively transfer the sample to a 100-mL volumetric flask and dilute to the mark
with deionized water.

Accuracy check
Standard additions method (sample spike)
Use the standard additions method (for applicable instruments) to validate the test
procedure, reagents and instrument and to find if there is an interference in the sample.
Items to collect:

25-mg/L Zinc Voluette Ampule Standard Solution

Ampule breaker
Pipet, TenSette, 0.11.0 mL and tips
Mixing cylinders, 25-mL (3)

1. Use the test procedure to measure the concentration of the sample, then keep the
(unspiked) sample in the instrument.
2. Go to the Standard Additions option in the instrument menu.
3. Select the values for standard concentration, sample volume and spike volumes.
4. Open the standard solution.
5. Prepare three spiked samples: use the TenSette pipet to add 0.1 mL, 0.2 mL and
0.3 mL of the standard solution, respectively, to three 20-mL portions of fresh sample.
Mix well.

Zinc, Zincon Method (3.00 mg/L)

6. Use the test procedure to measure the concentration of each of the spiked samples.
Start with the smallest sample spike. Measure each of the spiked samples in the
instrument.
7. Select Graph to compare the expected results to the actual results.
Note: If the actual results are significantly different from the expected results, make sure that
the sample volumes and sample spikes are measured accurately. The sample volumes and
sample spikes that are used should agree with the selections in the standard additions menu. If
the results are not within acceptable limits, the sample may contain an interference.

Standard solution method

Use the standard solution method to validate the test procedure, the reagents and the
instrument.
Items to collect:

100-mg/L zinc standard solution

1-L volumetric flask, Class A
10-mL volumetric pipet, Class A and pipet filler safety bulb
Deionized water

1. Prepare a 1.00-mg/L zinc standard solution as follows:

a. Use a pipet to add 10.00 mL of 100-mg/L zinc standard solution into the
volumetric flask.
b. Dilute to the mark with deionized water. Mix well. Prepare this solution daily.
2. Use the test procedure to measure the concentration of the prepared standard
solution.
3. Compare the expected result to the actual result.
Note: The factory calibration can be adjusted slightly with the standard adjust option so that the
instrument shows the expected value of the standard solution. The adjusted calibration is then
used for all test results. This adjustment can increase the test accuracy when there are slight
variations in the reagents or instruments.

Method performance
The method performance data that follows was derived from laboratory tests that were
measured on a spectrophotometer during ideal test conditions. Users can get different
results under different test conditions.
Program

Standard

Precision (95% confidence interval)

Sensitivity
Concentration change per 0.010 Abs change

780

1.00 mg/L Zn

0.971.03 mg/L Zn

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. The measurement wavelength is 620 nm for
spectrophotometers or 610 nm for colorimeters.

Pollution prevention and waste management

Reacted samples contain potassium cyanide and must be disposed of as a hazardous
waste. Dispose of reacted solutions according to local, state and federal regulations.

Zinc, Zincon Method (3.00 mg/L)

Consumables and replacement items

Required reagents
Description

Quantity/test

Unit

Item no.

100 tests

2429300

0.5 mL

100 mL MDB

1403332

100/pkg

2106669

Quantity/test

Unit

Item no.

each

2088640

Description

Unit

Item no.

Water, deionized

4L

27256

100 mL

237842

Zinc Standard Solution, 10-mg/L Voluette Ampule, 25-mL as Zn

16/pkg

1424610

Zinc Standard Solution, 1000-mg/L

100 mL

1417742

Description

Unit

Item no.

Flask, Erlenmeyer, 250-mL

each

50546

Hot plate, 4-inch round, 120 V

each

1206701

Hydrochloric Acid Solution, 6.0 N (1:1)

500 mL

88449

Nitric Acid, concentrated

500 mL

15249

each

1970001

Zinc Reagent Set, 20-mL sample size, includes:

Cyclohexanone

ZincoVer 5 Reagent Powder Pillow, 20-mL

Required apparatus
Description
Mixing cylinder, graduated, 25-mL with stopper

Recommended standards

Zinc Standard Solution, 100-mg/L

Optional reagents and apparatus

Pipet, TenSette , 0.11.0 mL

Pipet tips for TenSette Pipet, 0.11.0 mL

50/pkg

2185696

Ampule Breaker, 10-mL Voluette Ampules

each

2196800

Pipet, volumetric, Class A, 10-mL

each

1451538

Pipet filler, safety bulb

each

1465100

Flask, volumetric, Class A, 1000-mL glass

each

1457453

FOR TECHNICAL ASSISTANCE, PRICE INFORMATION AND ORDERING:

In the U.S.A. Call toll-free 800-227-4224
Outside the U.S.A. Contact the HACH office or distributor serving you.
On the Worldwide Web www.hach.com; E-mail techhelp@hach.com

Hach Company/Hach Lange GmbH, 19892014. All rights reserved.

HACH COMPANY
WORLD HEADQUARTERS
Telephone: (970) 669-3050
FAX: (970) 669-2932

01/2014, Edition 8