Nickel DOC316.53.

01063

1-(2 Pyridylazo)-2-Napthol (PAN) Method1 Method 8150

0.006 to 1.000 mg/L Ni Powder Pillows
Scope and application: For water and wastewater.
1 Adapted from Watanabe, H., Talanta, 21 295 (1974).

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.
To make sure that all forms of the metal are measured, digest the sample with heat and acid. Use the mild or vigorous
digestion. Refer to the Water Analysis Guide for more information.
For spectrophotometers, this method can measure the cobalt concentration on the same sample with Program Number 110.
Review the Safety Data Sheets (MSDS/SDS) for the chemicals that are used. Use the recommended personal protective
equipment.
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

EDTA Powder Pillow 2

Phthalate-Phosphate Reagent Powder Pillow 2

1
Items to collect (continued)
Description Quantity

PAN Indicator Solution 0.3% 1 mL

Deionized water 25 mL
Stoppers 2
Sample cells (For information about sample cells, adapters or light shields, refer to Instrument-
2
specific 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.
• If the sample temperature is less than 10 °C (50 °F), warm the sample to room
temperature before analysis.
• 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 3–8 with 5.0 N sodium hydroxide standard solution.
Do not exceed pH 8 to prevent precipitation of the metal.
• Correct the test result for the dilution caused by the volume additions.

Test procedure

Start

1. Start program 2. Prepare the blank: Fill a 3. Prepare the sample: Fill 4. Add the contents of one
340 Nickel, PAN. For sample cell with 10 mL of a second sample cell with Phthalate-Phosphate
information about sample deionized water. 10 mL of sample. Reagent Powder Pillow to
cells, adapters or light each cell.
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 Nickel, PAN Method (1.000 mg/L)

5. Close the sample cells. 6. Add 0.5 mL of 0.3% PAN 7. Put the stopper on the 8. Start the instrument
Immediately shake to Indicator Solution to each sample cells. Invert several timer. A 15-minute reaction
dissolve the reagent. cell. times to mix. time starts.
If the sample contains iron, During color development
make sure that all the the sample solution color
powder is dissolved before may vary from yellow-
the PAN Indicator Solution orange to dark red, based
is added. on the chemical makeup of
the sample. The blank will
be yellow.

9. When the timer expires, 10. Close the sample cells. 11. Clean the blank sample 12. Insert the blank into the
add the contents of one Shake to dissolve the cell. cell holder.
EDTA Reagent Powder reagent powder.
Pillow to each cell.

Zero Read

13. Push ZERO. The 14. Clean the prepared 15. Insert the prepared 16. Push READ. Results
display shows 0.00 mg/L Ni sample cell. sample into the cell holder. show in mg/L Ni and Co
and Co (spectrophotometers) or
(spectrophotometers) or mg/L Ni (colorimeters).
mg/L Ni (colorimeters) *.

* Spectrophotometers "zero" at 560 nm and 620 nm. Colorimeters "zero" at 560 nm.

Nickel, PAN Method (1.000 mg/L) 3

Interferences
Interfering substance Interference level
Al3+ 32 mg/L
Ca2+ 1000 mg/L as (CaCO3)
Cd2+ 20 mg/L
Cl– 8000 mg/L
Chelating agents (e.g., EDTA) Interfere at all levels. Use either the Digesdahl or vigorous digestion to remove
this interference.
Cr3+ 20 mg/L
Cr6+ 40 mg/L
Cu2+ 15 mg/L
F– 20 mg/L
Fe3+ 10 mg/L. If the sample contains iron, make sure that all the powder is dissolved
before the PAN Indicator is added.
Fe2+ Interferes directly and must not be present.
K+ 500 mg/L
Mg2+ 400 mg/L
Mn2+ 25 mg/L
Mo6+ 60 mg/L
Na+ 5000 mg/L
Pb2+ 20 mg/L
Zn2+ 30 mg/L
Highly buffered samples or extreme Can prevent the correct pH adjustment of the sample by the reagents. Sample
sample pH pre-treatment may be necessary.

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:
• 1000-mg/L Nickel Standard Solution
• 100-mL volumetric flask, Class A
• 5-mL volumetric pipet, Class A and pipet filler
• Deionized water
• Pipet, TenSette®, 0.1–1.0 mL and tips
• Mixing cylinders, 25-mL (3)

1. Prepare a 50 mg/L nickel standard solution as follows:

a. Use a pipet to add 5.00 mL of a 1000 mg/L nickel standard solution into a 100-mL
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 sample, then keep the
(unspiked) sample in the instrument.
3. Go to the Standard Additions option in the instrument menu.
4. Select the values for standard concentration, sample volume and spike volumes.

4 Nickel, PAN Method (1.000 mg/L)

 5. Prepare three spiked samples: use the TenSette pipet to add 0.1 mL, 0.2 mL and
0.3 mL of the prepared standard solution, respectively, to three 25-mL portions of
fresh sample. Mix well.
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:
• 1000-mg/L Nickel Standard Solution
• 1-L volumetric flask, Class A
• 100-mL volumetric flask, Class A
• 10-mL volumetric pipet, Class A and pipet filler
• 5-mL volumetric pipet, Class A and pipet filler
• Deionized water

1. Prepare a 5.00-mg/L nickel stock solution as follows:

a. Use a pipet to add 5.00 mL of a 1000-mg/L nickel standard solution into a 1-L
volumetric flask.
b. Dilute to the mark with deionized water. Mix well. Prepare the stock solution each
day.
2. Prepare a 0.5 mg/L nickel standard solution as follows:
a. Use a pipet to add 10.00 mL of the 5.00-mg/L nickel stock solution into a 100-mL
volumetric flask.
b. Dilute to the mark with deionized water. Mix well. Prepare the standard solution
each day.
3. Use the test procedure to measure the concentration of the prepared standard
solution.
4. 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
340 0.500 mg/L Ni 0.492–0.508 mg/L Ni 0.006 mg/L Ni

Summary of method
After pyrophosphate is added to buffer the sample and mask any Fe3+, the nickel reacts
with 1-(2-Pyridylazo)-2-Naphthol indicator. The indicator forms complexes with most
metals present. After color development, EDTA is added to destroy all metal-PAN
complexes except nickel and cobalt. Spectrophotometers automatically adjust for cobalt

Nickel, PAN Method (1.000 mg/L) 5

 interference by measuring the absorbance of the sample at both 560 nm and 620 nm.
This method is unique because both nickel and cobalt can be determined on the same
sample with a spectrophotometer. The measurement wavelength is 560 nm for
colorimeters.
Consumables and replacement items
Required reagents

Description Quantity/test Unit Item no.

Cobalt/Nickel Reagent Set, PAN, 10-mL, includes: — 100/pkg 2651600

Includes:
EDTA Reagent Powder Pillow 2 100/pkg 700599
Phthalate-Phosphate Reagent Powder Pillow, 10-mL 2 100/pkg 2615199
PAN Indicator Solution, 0.3% 1 mL 100 mL MDB 2150232
Water, deionized varies 4L 27256

Required apparatus

Description Quantity/test Unit Item no.

Stoppers for 18-mm tubes and AccuVac Ampuls 2 6/pkg 173106

Recommended standards

Description Unit Item no.

Nickel Standard Solution, 1000-mg/L Ni (NIST) 100 mL 1417642

Optional reagents and apparatus

Description Unit Item no.

Mixing cylinder, graduated, 25-mL each 189640

Flask, volumetric, Class A, 100-mL glass each 1457442
Pipet, volumetric 5.00-mL each 1451537
Pipet filler, safety bulb each 1465100
Pipet, volumetric, Class A, 10-mL each 1451538
Flask, volumetric, Class A, 1000-mL glass each 1457453
Water, deionized 4L 27256
Nitric Acid Solution, 1:1 500 mL 254049
Sodium Hydroxide Standard Solution, 5.0 N 100 mL MDB 245032

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© Hach Company/Hach Lange GmbH, 1989–2014. All rights reserved. 01/2014, Edition 9