Método Prata

Silver
DR/2500
Method 8120
Powder Pillows
Scope and Application: For water and wastewater.
Colorimetric Method
(0.005 to 0.700 mg/L)
Tips and Techniques

Digestion is required in samples with interferences. See Digestion on page 4.
For more accurate results, determine a reagent blank value for each new lot of reagent. Follow the procedure using deionized
water in place of the sample. Subtract the reagent blank value from the final results or perform a reagent blank adjust. See the
DR/2500 instrument manual for more information on Running a Reagent Blank.
The graduated cylinder must be completely dry before beginning the test. If the Silver 1 Powder becomes moist, it will not dissolve
completely, which will inhibit color development.
The sample pH for this test must be between 9 and 10. Do not use a pH meter to adjust the sample pH as it will cause
contamination. See Digestion on page 4 for the procedure to adjust pH.
Generate a blank for each sample.
Wipe the outside of sample cells before each insertion into the instrument cell holder. Use a damp towel followed by a dry one to
remove fingerprints or other marks.
Powder Pillows
Method 8120
Hach Programs
1. Touch
Hach Programs
Select program
660 Silver
Touch Start.
Silver_PP_Other_CLR_Eng_Ody.fm
2. Add the contents of

one Silver 1 Powder
Pillow to a dry 50-mL
graduated mixing
cylinder.
If the Silver 1 Powder
becomes wet at this point,
the powder will not
dissolve completely,
which will inhibit color
development.
3. Add the contents of

one Silver 2 Reagent
Solution Pillow to the
cylinder. Swirl to
completely wet the
powder.
If clumps of dry powder
are present when the
sample is poured in, the
powder will not dissolve
completely, which will
inhibit color
development.
4. Use a 50-mL
graduated cylinder to
add 50 mL of sample to
the 50-mL graduated
mixing cylinder. Stopper
and invert repeatedly for
one minute.
Silver
Page 1 of 6
Silver
25 m
L
25 mL
25 mL
20 mL
20 mL
20 m
L
25 mL
20 mL
10 m
L
10 mL
10 mL
10 mL
5. Fill a cell to the 25-mL 6. Add the contents of

mark with the mixture. one Sodium Thiosulfate
(This is the blank.)
Powder Pillow to the
blank. Swirl for 30
seconds to mix.
7. Touch the timer icon. 8. Fill a second cell to
Touch OK.
A two-minute reaction
period will begin.
25 mL
25 mL
20 mL
Interferences
20 mL
Zero
10 mL
9. When the timer

beeps, place the blank
into the cell holder.
10. Touch Zero.
The display will show:

0.000 mg/L Ag
10 mL
11. Place the prepared

sample into the cell
holder.
Results will appear in
mg/L Ag.
Interference studies were conducted by preparing a known silver solution

(about 0.4 mg/L) and the potential interfering ion. The ion was said to interfere
when the resulting concentration changed by 10%.
Interfering Substance
Silver
Page 2 of 6
the 25-mL mark from the

remaining portion of the
mixture. (This is the
prepared sample.)
Interference Levels and Treatments
Aluminum
Negative interference above 30 mg/L
Ammonia
Cadmium
Calcium
Positive interference above 600 mg/L
Chloride
Negative interference above 19 mg/
Chromium6+
Copper
Iron
Silver
(continued)
Interfering Substance
Interference Levels and Treatments
Lead
Manganese
Magnesium
Mercury
Nickel
Zinc
Sample Collection, Storage, and Preservation
Accuracy Check
Collect samples in acid-cleaned glass or plastic bottles. Using pH paper,

adjust the pH to 2 or less with Concentrated Nitric Acid (Cat. No. 152-49)
(about 2 mL/liter). Store preserved samples at room temperature for up to 6
months. If the sample contains particulates or only dissolved metal content is
being determined, filter through a 0.45 mm filter at collection. After filtration,
adjust the pH to 2 or less as described above.
Before analysis, adjust the pH to 910 with 5.0 N Sodium Hydroxide
(Cat. No. 2450-32). (See step 13step 14 of the Digestion procedure on page 4.) Do
not use a pH meter because of silver contamination from the electrode. Correct
for volume additions; see Section 3.1.3 Correcting for Volume Additions on page 31.
Standard Additions Method (Sample Spike)

1. After reading test results, leave the sample cell (unspiked sample) in the
instrument.
2. Touch Options. Touch Standard Additions. A summary of the standard
additions procedure will appear.
3. Touch OK to accept the default values for standard concentration, sample
volume, and spike volumes. Touch Edit to change these values. After values
are accepted, the unspiked sample reading will appear in the top row. See
Standard Additions in the DR/2500 instrument manual for more information.
4. Add 5.00 mL of 1000 mg/L Silver Standard Solution to a 100-mL volumetric
Class A flask. Dilute to volume with deionized water. This is a 50.0 mg/L
standard solution.
5. Prepare three sample spikes. Fill three mixing cylinders (Cat. No. 1896-41)
with 50-mL of sample. Use the TenSette Pipet to add 0.1 mL, 0.2 mL, and
0.3 mL of standard, respectively, to each sample and mix thoroughly.
6. Analyze each sample spike as described in the procedure above, starting with
the 0.1 mL sample spike. Accept each standard additions reading by touching
Read. Each addition should reflect approximately 100% recovery.
7. After completing the sequence, touch Graph to view the best-fit line through
the standard additions data points, accounting for matrix interferences. Touch
View: Fit, then select Ideal Line and touch OK to view the relationship between
the sample spikes and the Ideal Line of 100% recovery.
See Section 3.2.2 Standard Additions on page 36 for more information.
Silver
Page 3 of 6
Silver
Standard Solution Method
Prepare a 0.5 mg/L silver standard solution as follows:
1. Pipet 0.50 mL of Silver Standard Solution, 1000 mg/L, into a 1000-mL
volumetric flask using a Class A volumetric pipet. Dilute to the mark with
deionized water. Prepare this solution daily. Perform the silver procedure as
described above.
2. To adjust the calibration curve using the reading obtained with the 0.5-mg/L
silver standard solution, touch Options on the current program menu. Touch
Standard Adjust.
3. Touch On. Touch OK to accept the displayed concentration. If an alternate
concentration is used, touch the number in the Adjust to field and enter the
actual concentration. Touch OK.
See Section 3.2.3 Adjusting the Standard Curve on page 38 for more information.
Method Performance
Precision
Standard: 0.500 mg/L Ag
Program
95% Confidence Limits of Distribution
660
0.4930.507 mg/L Ag
See Section 3.4.3 Precision on page 42 for more information, or if the standard
concentration did not fall within the specified range.
Sensitivity
Digestion
Warning: Always
wear safety glasses
and use a safety
shield, or operate the
Digesdahl within a
closed fume hood.
Follow the additional
safety precautions in
the Digesdahl
Digestion Apparatus
Manual.
Silver
Page 4 of 6
Portion of Curve
Abs
Concentration
Entire range
0.010
0.005 mg/L Ag
See Section 3.4.5 Sensitivity on page 43 for more information.

This digestion is for samples containing organic matter, thiosulfate or cyanide.
Possible sources for these compounds are wastewater, silver electroplating baths
and silver strike solutions. Digestion should be done with a Digesdahl Digestion
Apparatus.
Caution: Poisonous hydrogen cyanide gas may be generated during this
digestion. Use a fume hood.
1. Add an appropriate size sample to the 100-mL digestion flask for use with
the Digesdahl. Add several boiling chips to prevent bumping.
Note: Appropriate sample size is determined experimentally. The final sample concentration (after
dilution to 100 mL) should be 00.6 mg/L. Larger dilutions may be necessary for
electroplating baths and silver strike solutions. Do not exceed the maximum sample volume
of 25 mL. Several 25-mL aliquots may be digested in succession to concentrate a very dilute
sample.
2. Turn on the water aspirator and make sure there is suction in the
fractionating head.
Silver
3. Add 3 mL of concentrated sulfuric acid to the sample in the volumetric flask.
Immediately place the head on the digestion flask. Never use less than 3 mL
of acid.
4. Place the digestion flask on the heater. Turn the temperature dial to
440 C (825 F).
5. After the sample begins to char or the sulfuric acid reflux line becomes visible,
wait 35 minutes.
6. Visually confirm the presence of acid in the flask before adding hydrogen
peroxide!
7. Add 10 mL of 50% hydrogen peroxide to the sample via the capillary funnel
in the fractionating head.
8. After the hydrogen peroxide has boiled off, heat the sample until heavy white
sulfuric acid fumes are present. Continue heating and reduce the sample
volume to near dryness. Do not let the sample go completely dry at any time.
Note: If the sample goes to dryness, turn the Digesdahl off and cool completely. Add water to flask
before handling. Repeat digestion from the beginning.
Note: If only thiosulfate is present in the sample, proceed to step 1 of the Colorimetric procedure.
9. Add another 3 mL of sulfuric acid via the capillary funnel.

10. Add another 5 mL of hydrogen peroxide. Check the solution for digestion
completion. If digestion is not complete, continue adding hydrogen peroxide
in 5 to 10 mL portions. Several portions may be necessary.
Note: Digestion is complete when the digestate is colorless or the color of the digestate does not
change upon addition of hydrogen peroxide. Also, a completely digested sample will not
foam.
11. After digestion is complete and all the hydrogen peroxide is boiled off, reduce
the volume of the digestate to near dryness. Do not allow the sample to
become completely dry. Remove the flask from the heater. Cool to room
temperature.
12. Slowly add about 25 mL of deionized water to the cooled flask.
13. Add 2 drops of 1 g/L Phenolphthalein Indicator Solution. Add 2 drops of
1 g/L Thymolphthalein Indicator Solution.
14. Using sodium hydroxide, adjust the pH of the solution to 910. The solution
will be pink in this pH range.
Note: A purple color indicates a pH greater than 10. If this occurs, add a drop of sulfuric acid and
2 drops of each indicator; repeat pH adjustment. Initially, use 50% sodium hydroxide, then
1 N sodium hydroxide as the end point is approached.
15. Filter turbid digestates. Quantitatively transfer the filtrate (or unfiltered
sample) to a clean 100-mL volumetric flask. Dilute to the mark with deionized
water. The sample is ready for analysis.
Silver
Page 5 of 6
Silver
Summary of Method
Silver ions in basic solution react with cadion 2B to form a green to brown to
red-purple complex. The sodium thiosulfate acts as a decolorizing agent for the
blank. The Silver 1 and Silver 2 reagents contain the buffer, indicator, and
masking agents. Organic extractions are not necessary and this method does not
have as many interferences as the traditional dithizone method. Test results are
measured at 560 nm.
Required Reagents
Description
Quantity Required
per test
Unit
Cat. No.
Silver Reagent Set (50 tests)............................................................................................................................22966-00

Includes:
Silver 1 Reagent Powder Pillow.......................................................1 pillow........... 50/pkg...............22935-66
Silver 2 Reagent Solution Pillow......................................................1 pillow........... 50/pkg...............22936-66
Sodium Thiosulfate Powder Pillow ................................................1 pillow........... 50/pkg...............22937-66
Required Apparatus
Clippers, for opening powder pillows .................................................1....................... each........................968-00

Cylinder, graduated, 50-mL....................................................................1....................... each....................21179-41
Cylinder, graduated, mixing, 50-mL......................................................1....................... each......................1896-41
Sample Cells, 10-20-25 mL, w/cap.........................................................2....................... 6/pkg.................24019-06
Digestion Reagents
Hydrogen Peroxide, 50%................................................................................................... 490 mL...............21196-49

Phenolphthalein Indicator Solution, 1 g/L..................................................................... 15 mL SCDB .......1897-36
Sodium Hydroxide Solution, 50%.................................................................................... 500 mL.................2180-49
Sodium Hydroxide Solution, 1.00 N................................................................................ 100 mL MDB.......1045-32
Sulfuric Acid, ACS, concentrated..................................................................................... 2.5 L .......................979-09
Thymolphthalein Indicator Solution, 1 g/L ................................................................... 15 mL SCDB .....21853-36
Water, deionized ................................................................................................................. 4 liters....................272-56
Required Standards
Silver Standard Solution, 1000 mg/L Ag........................................................................ 100 mL...............14613-42

Water, deionized ................................................................................................................. 4 liters....................272-56
Digestion Apparatus
Boiling Chips, silicon carbide ........................................................................................... 500 g...................20557-34

Digesdahl Digestion Apparatus, 115 V ac, 50/60 Hz.................................................... each....................23130-20
Digesdahl Digestion Apparatus, 230 V ac, 50/60 Hz.................................................... each....................23130-21
Safety Shield, for Digesdahl.............................................................................................. each....................50030-00
2003. All rights reserved. Printed in the U.S.A.
Page 6 of 6
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Silver

Scope and Application: For water and wastewater.

Tips and Techniques

2. Add the contents of

3. Add the contents of

5. Fill a cell to the 25-mL 6. Add the contents of

7. Touch the timer icon. 8. Fill a second cell to

9. When the timer

10. Touch Zero.

The display will show:

11. Place the prepared

Interference studies were conducted by preparing a known silver solution

the 25-mL mark from the

Interference Levels and Treatments

Negative interference above 30 mg/L

Negative interference above 750 mg/L

Negative interference above 15 mg/L

Positive interference above 600 mg/L

Negative interference above 19 mg/

Negative interference above 90 mg/L

Negative interference above 7 mg/L

Negative interference above 30 mg/L

Interference Levels and Treatments

Negative interference above 13 mg/L

Negative interference above 19 mg/L

Positive interference above 2000 mg/L

Positive interference above 2 mg/L

Negative interference above 19 mg/L

Negative interference above 70 mg/L

Sample Collection, Storage, and Preservation

Collect samples in acid-cleaned glass or plastic bottles. Using pH paper,

Standard Additions Method (Sample Spike)

95% Confidence Limits of Distribution

See Section 3.4.5 Sensitivity on page 43 for more information.

9. Add another 3 mL of sulfuric acid via the capillary funnel.

Silver Reagent Set (50 tests)............................................................................................................................22966-00

Clippers, for opening powder pillows .................................................1....................... each........................968-00

Hydrogen Peroxide, 50%................................................................................................... 490 mL...............21196-49

Silver Standard Solution, 1000 mg/L Ag........................................................................ 100 mL...............14613-42

Boiling Chips, silicon carbide ........................................................................................... 500 g...................20557-34

2003. All rights reserved. Printed in the U.S.A.

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