Professional Documents
Culture Documents
01219
Test preparation
Before starting
The optional TitraStir Titration Stand can hold the Digital Titrator and stir the sample.
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
Sample collection
• Collect samples in clean glass bottles.
• Analyze the samples as soon as possible for best results.
• Prevent exposure of the sample to heat or light.
• If prompt analysis is not possible, keep the samples in a cool and dark location.
1
Test procedure
1. Insert a clean delivery 2. Hold the Digital Titrator 3. Fill a clean 125‑mL 4. Add the contents of one
tube into the 2.26 N Sodium with the cartridge tip up. Erlenmeyer flask to Potassium Iodide Powder
Thiosulfate Titrant Solution Turn the delivery knob to approximately the 75‑mL Pillow.
cartridge. Attach the eject air and a few drops of mark with deionized water
cartridge to the Digital titrant. Reset the counter to or tap water.
Titrator. zero and clean the tip. Note: The level of residual
chlorine in tap water will not
cause interference with the
test.
5. Swirl to mix. 6. Add the contents of one 7. Swirl to mix. 8. Use a TenSette pipet
Acid Reagent Powder with a new tip to add 0.2 mL
Pillow. of bleach sample to the
flask. Make sure to add the
sample below the solution
level.
9. Swirl to mix. 10. Put the end of the 11. Add one dropperful of 12. Swirl to mix.
The color of the solution delivery tube fully into the Starch Indicator Solution. The color of the solution
changes to dark brown. solution. Swirl the flask. changes to dark blue or
Turn the knob on the Digital green.
Titrator to add titrant to the
solution. Continue to swirl
the flask. Add titrant until the
color changes to pale
yellow.
Interferences
The test determines the hypochlorite ion (ClO–) and also the chlorite ion (ClO2 –).
However, the chlorite level in commercial bleach is not important (typically less than
0.2%). Other interferences are unlikely.
Interfering Interference level
substance
Caustic agent A high level of caustic can cause low results. To remove the interferences:
1. After the Acid Reagent Powder Pillow is added, examine the pH of the solution with pH Paper. The
pH must be less than 3.
2. If the pH is not less than 3, add more Acid Reagent, one pillow at a time, until the pH of the
solution is below 3.
Temperature For most accurate results, the temperature of the dilution water must be less than 20 °C (68 °F).
Accuracy check
Standard solution method
Use the standard solution method to validate the test procedure, reagents, apparatus and
technique.
Note: The strength of the Sodium Thiosulfate Standard Solution is validated with Potassium Iodide-
Iodate Standard Solution. It is recommended to validate the reagent accuracy with each new lot of
reagents.
Items to collect:
• Potassium Iodide-Iodate Standard Solution, 0.0125 N
• Potassium Iodide Powder Pillows
• Acid Reagent Powder Pillows
• 125-mL Erlenmeyer flask
• 50-mL volumetric pipet, Class A and pipet filler safety bulb
Precision
When a commercial bleach sample of 91.2 g/L (9.12 %) Cl2 is tested, one analyst caused
a standard deviation of ±1.5 g/L (±1.5 %) Cl2.
Summary of method
In acidic conditions, hypochlorite reacts with iodide to form an equivalent quantity of
triiodide (I3–). The released I3– is titrated with sodium thiosulfate to a colorless end point.
The quantity of sodium thiosulfate required is directly related to the hypochlorite
concentration in the sample.
Consumables and replacement items
Required reagents
Required apparatus
Recommended standards
© Hach Company/Hach Lange GmbH, 2007–2015. All rights reserved. 04/2015, Edition 8
Hardness, Calcium DOC316.53.01175
Test preparation
Before starting
Magnesium is not included in the results but must be in the sample for a sharp endpoint. If the sample does not contain
magnesium, add 1 to 2 drops of Magnesium Standard Solution, 10-g/L as CaCO3, to the sample before the test is started.
As an alternative to the CalVer 2 Calcium Indicator Powder Pillow, use a 0.1-g scoop of CalVer 2 Calcium Indicator Powder.
The optional TitraStir Titration Stand can hold the Digital Titrator and stir the sample.
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
Sample collection
• Collect samples in clean glass or plastic bottles that have been cleaned with a
detergent and rinsed with 1:1 nitric acid and deionized water.
• To preserve samples for later analysis, adjust the sample pH to 2 or less 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 7 with Potassium Hydroxide Standard Solution.
• Correct the test result for the dilution caused by the volume additions.
1
Test procedure
1. Select a sample volume 2. Insert a clean delivery 3. Hold the Digital Titrator 4. Use a graduated cylinder
and titration cartridge from tube into the digital titration with the cartridge tip up. or a pipet1 to measure the
Table 1 on page 3. cartridge. Attach the Turn the delivery knob to sample volume from Table 1
cartridge to the Digital eject air and a few drops of on page 3.
Titrator. titrant. Reset the counter to
zero and clean the tip.
5. Pour the sample into a 6. If the sample volume is 7. Swirl to mix. 8. If the sample volume is
clean, 250-mL Erlenmeyer 100 mL, add 2 mL of 8 N less than 100 mL, dilute to
flask. Potassium Hydroxide approximately 100 mL with
Standard Solution. If the deionized water.
sample volume is 50 mL or
less, add 1 mL of 8 N
Potassium Hydroxide
Standard Solution.
1 Titration accuracy has a direct relation to the accuracy of the sample volume measurement. For smaller
volumes, it is recommended to use a pipet to increase accuracy.
Interferences
WARNING
Chemical hazard. Potassium cyanide is toxic. Make sure to add potassium cyanide to the
sample after the Potassium Hydroxide has been added. Keep cyanide solutions at more
than pH 11 to prevent exposure to hydrogen cyanide gas. Dispose of reacted solutions
according to local, state and federal regulations.
An interfering substance can prevent the color change at the titration endpoint. A smaller
sample volume can often dilute the interfering substance to a level at which the
substance does not interfere. Table 4 shows the substances that can interfere with this
test.
Table 4 Interferences
Interfering substance Interference level
Acidity 10,000 mg/L acidity as CaCO3 does not interfere.
Alkalinity 10,000 mg/L alkalinity as CaCO3 does not interfere.
Aluminum Causes a slow endpoint. The sample can contain a maximum of 200 mg/L aluminum if sufficient
time is given for the color change.
Barium Barium is titrated at the same time with calcium and interferes with this test, but it is unusual to find
high levels of Barium in natural waters.
Chloride The chloride level in seawater does not interfere. Solutions that are saturated with chloride do not
show a sharp endpoint.
Cobalt Interferes directly and is included in the test result. Add 0.5 grams of potassium cyanide after the
Potassium Hydroxide during the test procedure to remove the interference from a maximum of
20 mg/L cobalt.
Copper Interferes at 0.1 mg/L copper. Add 0.5 grams of potassium cyanide after the Potassium Hydroxide
during the test procedure to remove the interference from a maximum of 100 mg/L copper.
Iron More than 8 mg/L iron causes an orange-red to green endpoint. Results are accurate to 20 mg/L
iron with this endpoint.
Magnesium The formation of magnesium hydroxide at the high test pH prevents interference from 200 mg/L
magnesium. Samples with more than 200 mg/L magnesium do not give a distinct endpoint.
Manganese Interferes at more than 5 mg/L manganese.
Nickel Interferes at 0.5 mg/L nickel. Add 0.5 grams of potassium cyanide after the Potassium Hydroxide
during the test procedure to remove the interference from a maximum of 200 mg/L nickel.
Orthophosphate Forms calcium phosphate and causes a slow endpoint. If sufficient time is given to let the calcium
phosphate dissolve during the titration, the orthophosphate will not interfere with the test.
Polyphosphates Interfere directly and are included in the test result.
Strontium Strontium is titrated at the same time with calcium and interferes with this test, but it is unusual to
find high levels of Strontium in natural waters.
Accuracy check
Standard additions method (sample spike)
Use the standard additions method to validate the test procedure, reagents, apparatus,
technique and to find if there is an interference in the sample.
Items to collect:
• Hardness Voluette Ampule Standard Solution, 10,000 mg/L as CaCO3
• Ampule Breaker
• Pipet, TenSette, 0.1–1.0 mL and pipet tips
Summary of method
Potassium hydroxide is added to the sample to adjust the pH to 12 to 13, which causes a
magnesium hydroxide precipitate to form. CalVer 2 Calcium Indicator is then added,
which reacts with calcium to give a red color. The EDTA titrant is added, which reacts
with all the free calcium. After the EDTA has reacted with all of the free calcium ions, the
EDTA removes the calcium from the indicator. The indicator color then changes from red
to blue.
Consumables and replacement items
Required reagents
Reagent set, 10–160 mg/L range (approximately 100 tests): — each 2447200
CalVer 2 Calcium Indicator Powder Pillows 1 pillow 100/pkg 85299
Potassium Hydroxide Standard Solution, 8 N 1–2 mL 100 mL MDB 28232H
EDTA Titration Cartridge, 0.0800 M varies each 1436401
Reagent set, 100–4000 mg/L range (approximately 100 tests): — each 2447500
CalVer 2 Calcium Indicator Powder Pillows 1 pillow 100/pkg 85299
Potassium Hydroxide Standard Solution, 8 N 1–2 mL 100 mL MDB 28232H
Required apparatus
Recommended standards
Calcium Hardness Standard Solution, 10,000-mg/L as CaCO3, 10-mL Voluette ampule 16/pkg 218710
Hardness Quality Control Standard, high range 500 mL 2833349
Hardness Quality Control Standard, low range 500 mL 2833449
© Hach Company/Hach Lange GmbH, 2007–2015. All rights reserved. 04/2015, Edition 8
Hardness, Total DOC316.53.01176
Test preparation
Before starting
As an alternative to the ManVer 2 Hardness Indicator Powder Pillow, use 4 drops of Hardness 2 Indicator Solution or a 0.1-g
scoop of ManVer 2 Hardness Indicator Powder.
The optional TitraStir Titration Stand can hold the Digital Titrator and stir the sample.
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
1
Test procedure
1. Select a sample volume 2. Insert a clean delivery 3. Hold the Digital Titrator 4. Use a graduated cylinder
and titration cartridge from tube into the digital titration with the cartridge tip up. or a pipet1 to measure the
Table 1 on page 3. cartridge. Attach the Turn the delivery knob to sample volume from Table 1
cartridge to the Digital eject air and a few drops of on page 3.
Titrator. titrant. Reset the counter to
zero and clean the tip.
5. Pour the sample into a 6. If the sample volume is 7. Add 2 mL of Hardness 1 8. Swirl to mix.
clean, 250-mL Erlenmeyer less than 100 mL, dilute to Buffer Solution.
flask. approximately 100 mL with
deionized water.
9. Add the contents of one 10. Swirl to mix. 11. Put the end of the 12. Use the multiplier in
ManVer 2 Hardness delivery tube fully into the Table 1 on page 3 to
Indicator Powder Pillow. solution. Swirl the flask. calculate the concentration.
Turn the knob on the Digital Digits used × digit multiplier
Titrator to add titrant to the = mg/L (or Gdh) total
solution. Continue to swirl hardness as CaCO3.
the flask. Add titrant until the
color changes from red to
pure blue. Record the
number of digits on the
counter.
1 Titration accuracy has a direct relation to the accuracy of the sample volume measurement. For smaller
volumes, it is recommended to use a pipet to increase accuracy.
Conversions units
To change the units or chemical form of the test result, multiply the test result by the
factor in Table 3.
Table 3 Conversions
mg/L Total Hardness as CaCO3 to... multiply by... Example
mg/L Total Hardness as Ca 0.40 1000 mg/L as CaCO3 x 0.40 = 400 mg/L Ca
German degrees hardness (Gdh) 0.056 1000 mg/L as CaCO3 × 0.056 = 56 Gdh
Grains per gallon (gpg) 0.058 1000 mg/L as CaCO3 x 0.058 = 58 gpg
mg/L Total Hardness as Mg 0.243 1000 mg/L as CaCO3 x 0.243 = 243 mg/L Mg
Hardness relationships
• mg/L Mg Hardness as CaCO3 = mg/L Total Hardness as CaCO3 – mg/L Ca
Hardness as CaCO3
• mg/L MgCO3= mg/L Mg Hardness as CaCO3 × 0.842
• mg/L Mg = mg/L MgCO3 × 0.29
WARNING
Chemical hazard. Potassium cyanide is toxic. Make sure to add potassium cyanide to the
sample after the Hardness 1 Buffer Solution has been added. Keep cyanide solutions at
more than pH 11 to prevent exposure to hydrogen cyanide gas. Dispose of reacted
solutions according to local, state and federal regulations.
An interfering substance can prevent the color change at the titration endpoint. A smaller
sample volume can often dilute the interfering substance to a level at which the
substance does not interfere. Table 4 shows the substances that can interfere with this
test.
Table 4 Interferences
Interfering substance Interference level
Acidity 10,000 mg/L acidity as CaCO3 does not interfere.
Alkalinity 10,000 mg/L alkalinity as CaCO3 does not interfere.
Aluminum Interferes when the sample contains more than 0.20 mg/L aluminum. Add 0.5 grams of potassium
cyanide after the Hardness 1 Buffer Solution during the test procedure to remove the interference
from a maximum of 1 mg/L aluminum.
As an alternative, add a CDTA powder pillow to remove the interference. Refer to Use CDTA to
remove metal interferences on page 5.
Barium Barium is titrated at the same time with calcium and interferes with this test, but it is unusual to find
high levels of Barium in natural waters.
Chloride The chloride level in seawater does not interfere. Solutions that are saturated with chloride do not
show a sharp endpoint.
Cobalt Interferes directly and is included in the test result. Add 0.5 grams of potassium cyanide after the
Hardness 1 Buffer Solution during the test procedure to remove the interference from a maximum of
20 mg/L cobalt.
As an alternative, add a CDTA powder pillow to remove the interference. Refer to Use CDTA to
remove metal interferences on page 5.
Copper Interferes when the sample contains 0.1 mg/L copper. Add 0.5 grams of potassium cyanide after the
Hardness 1 Buffer Solution during the test procedure to remove the interference from a maximum of
100 mg/L copper.
As an alternative, add a CDTA powder pillow to remove the interference. Refer to Use CDTA to
remove metal interferences on page 5.
Iron More than 8 mg/L iron causes an orange-red to green endpoint. Results are accurate to 20 mg/L
iron with this endpoint.
Manganese Interferes when the sample contains more than 5 mg/L manganese.
Nickel Interferes when the sample contains 0.5 mg/L nickel. Add 0.5 grams of potassium cyanide after the
Hardness 1 Buffer Solution during the test procedure to remove the interference from a maximum of
200 mg/L nickel.
As an alternative, add a CDTA powder pillow to remove the interference. Refer to Use CDTA to
remove metal interferences on page 5.
Orthophosphate Forms calcium phosphate and causes a slow endpoint. If sufficient time is given to let the calcium
phosphate dissolve during the titration, the orthophosphate will not interfere with the test.
Polyphosphates Interferes at all levels.
Polyvalent metal ions Although less common than calcium and magnesium, other polyvalent metal ions are titrated with
the calcium and magnesium and are included in the results.
Strontium Strontium is titrated at the same time with calcium and interferes with this test, but it is unusual to
find high levels of Strontium in natural waters.
Accuracy check
Standard additions method (sample spike)
Use the standard additions method to validate the test procedure, reagents, apparatus,
technique and to find if there is an interference in the sample.
1. Use a pipet to add 20.0 mL of the calcium chloride standard solution to a 250-mL
Erlenmeyer flask.
2. Dilute the standard solution to approximately 100 mL with deionized water.
3. Add one Hardness 1 Buffer Solution and one ManVer 2 Hardness Indicator Powder
Pillow. Swirl to mix.
4. Titrate the prepared standard solution to the endpoint. Calculate the concentration of
the standard solution. The correct result is 1000 mg/L or 55.9 Gdh as CaCO3.
5. Compare the actual result to the correct result. If much more or less titrant was used,
there can be a problem with user technique, reagents or apparatus.
Summary of method
A buffer solution (an organic amine and one of its salts) is added to the sample to adjust
the pH to 10.1. An organic dye, calmagite, is then added as the indicator for the test. The
organic dye reacts with calcium and magnesium ions to give a red-colored complex. The
EDTA (ethylenediaminetetraacetic acid) titrant is added, which reacts with all of the free
calcium and magnesium ions in the sample. After the EDTA has reacted with all of the
free magnesium ions, the EDTA removes the magnesium ions from the indicator. The
indicator color then changes from red to blue.
Consumables and replacement items
Required reagents
Reagent set, 10–160 mg/L range (approximately 100 tests): — each 2448000
ManVer 2 Hardness Indicator Powder Pillows 1 pillow 100/pkg 85199
Required apparatus
Recommended standards
© Hach Company/Hach Lange GmbH, 2007–2015. All rights reserved. 04/2015, Edition 8
Hardness, Total, Sequential DOC316.53.01230
Test preparation
Before starting
The first titration gives the results for calcium hardness and the second titration gives total hardness. The difference between
the values is the magnesium hardness level. All the concentration results are in mg/L as CaCO3. Refer to Conversions units
on page 5 for conversions to other units.
As an alternative to the CalVer 2 Calcium Indicator Powder Pillow, use a 0.1-g scoop of CalVer 2 Calcium Indicator Powder.
As an alternative to the ManVer 2 Hardness Indicator Powder Pillow, use 4 drops of Hardness 2 Indicator Solution or a 0.1-g
scoop of ManVer 2 Hardness Indicator Powder.
The optional TitraStir Titration Stand can hold the Digital Titrator and stir the sample.
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
1
• Before analysis, adjust the pH to 7 with Potassium Hydroxide Standard Solution.
• Correct the test result for the dilution caused by the volume additions.
Test procedure
1. Select a sample volume 2. Insert a clean delivery 3. Hold the Digital Titrator 4. Use a graduated cylinder
and titration cartridge from tube into the digital titration with the cartridge tip up. or a pipet1 to measure the
Table 1 on page 4. cartridge. Attach the Turn the delivery knob to sample volume from Table 1
cartridge to the Digital eject air and a few drops of on page 4.
Titrator. titrant. Reset the counter to
zero and clean the tip.
5. Pour the sample into a 6. If the sample volume is 7. Swirl to mix. 8. If the sample volume is
clean, 250-mL Erlenmeyer 100 mL, add 2 mL of 8 N less than 100 mL, dilute to
flask. Potassium Hydroxide approximately 100 mL with
Standard Solution. If the deionized water.
sample volume is 50 mL or
less, add 1 mL of 8 N
Potassium Hydroxide
Standard Solution.
1 Titration accuracy has a direct relation to the accuracy of the sample volume measurement. For smaller
volumes, it is recommended to use a pipet to increase accuracy.
13. Add 1 mL of 5.25 14. Add more acid, 1 drop 15. Add 2 mL of Hardness 16. Swirl to mix.
Sulfuric Acid Standard at a time until the color 1 Buffer Solution.
Solution. changes from pure blue to
purple, and then to red.
Swirl the flask to make sure
that all the precipitated
magnesium hydroxide has
dissolved.
Hardness relationships
• mg/L Mg Hardness as CaCO3 = mg/L Total Hardness as CaCO3 – mg/L Ca
Hardness as CaCO3
• mg/L MgCO3= mg/L Mg Hardness as CaCO3 × 0.842
• mg/L Mg = mg/L MgCO3 × 0.29
Interferences
WARNING
Chemical hazard. Do not use potassium cyanide to remove interferences because it will
form deadly hydrogen cyanide gas when the sulfuric acid solution is added.
An interfering substance can prevent the color change at the titration endpoint. A smaller
sample volume can often dilute the interfering substance to a level at which the
substance does not interfere. Table 4 shows the substances that can interfere with this
test.
Table 4 Interferences
Interfering substance Interference level
Acidity 10,000 mg/L acidity as CaCO3 does not interfere.
Alkalinity 10,000 mg/L alkalinity as CaCO3 does not interfere.
Aluminum Interferes at all levels. Add a DTA powder pillow to remove the interference. Refer to Use CDTA to
remove metal interferences on page 6.
Barium Barium is titrated at the same time with calcium and interferes with this test, but it is unusual to find
high levels of Barium in natural waters.
Chloride The chloride level in seawater does not interfere. Solutions that are saturated with chloride do not
show a sharp endpoint.
Cobalt Interferes at all levels. Add a DTA powder pillow to remove the interference. Refer to Use CDTA to
remove metal interferences on page 6.
Copper Interferes when the sample contains 0.10 and 0.20 mg/L copper.
Heavy metals Some transition and heavy metals have an effect in the indicator and prevent the color change at the
end point.
Iron Iron does not interfere until 15 mg/L. More than this level will cause a red-orange to green endpoint,
which is sharp and usable with a maximum of 30 mg/L iron. Change a 0.0800 M CDTA or 0.800 M
CDTA titration cartridge for the 0.0800 M EDTA or 0.800 M EDTA titration cartridges, respectively, if
iron interference is possible. For results in Gdh, divide the mg/L result by 17.9.
Manganese Interferes when the sample contains more than 20 mg/L manganese. Add a 0.1-gram scoop of
hydroxylamine hydrochloride to increase this level to 200 mg/L manganese.
Nickel Interferes at all levels. Add a DTA powder pillow to remove the interference. Refer to Use CDTA to
remove metal interferences on page 6.
Calcium and Total Hardness Reagent Set (approximately 100 tests): — each 2272100
Buffer Solution, Hardness 1 1 mL 100 mL MDB 42432
CalVer 2 Calcium Indicator Powder Pillows 1 100/pkg 94799
ManVer 2 Hardness Indicator Powder Pillows 1 100/pkg 85199
(x2) Potassium Hydroxide Standard Solution, 8 N 1 mL 100 mL MDB 28232H
EDTA Titration Cartridge, 0.0800 M varies each 1436401
EDTA Titration Cartridge, 0.800 M varies each 1439901
EDTA Titration Cartridge, 0.1428 M varies each 1496001
EDTA Titration Cartridge, 0.714 M varies each 1495901
Required apparatus
Recommended standards
© Hach Company/Hach Lange GmbH, 2007–2015. All rights reserved. 04/2015, Edition 8
Iron DOC316.53.01177
Test preparation
Before starting
The optional TitraStir Titration Stand can hold the Digital Titrator and stir the sample.
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
Sample collection
• Collect samples in clean glass or plastic bottles.
1
Test procedure
1. Select a sample volume 2. Insert a clean delivery 3. Hold the Digital Titrator 4. Use a graduated cylinder
and titration cartridge from tube into the digital titration with the cartridge tip up. or a pipet1 to measure the
Table 1 on page 3. cartridge. Attach the Turn the delivery knob to sample volume from Table 1
cartridge to the Digital eject air and a few drops of on page 3.
Titrator. titrant. Reset the counter to
zero and clean the tip.
5. Pour the sample into a 6. If the sample volume is 7. Add the contents of one 8. Swirl to mix.
clean, 125-mL Erlenmeyer less than 50 mL, dilute to Citrate Buffer Powder
flask. approximately 50 mL with Pillow.
deionized water.
9. Add the contents of one 10. Swirl to mix. 11. Add the contents of one 12. Swirl to mix.
Sodium Periodate Powder The color of the solution Sulfosalicylic Acid Powder The color of the solution
Pillow. changes to yellow if iron is Pillow. changes to red if iron is in
in the sample. the sample.
1 Titration accuracy has a direct relation to the accuracy of the sample volume measurement. For smaller
volumes, it is recommended to use a pipet to increase accuracy.
Accuracy check
Standard additions method (sample spike)
Use the standard additions method to validate the test procedure, reagents, apparatus,
technique and to find if there is an interference in the sample.
Items to collect:
• Iron Standard Solution, 1000 mg/L as Fe
• Pipet, TenSette, 0.1–1.0 mL and pipet tips
Summary of method
Ferrous iron Fe2+ is oxidized by sodium periodate to ferric ion Fe3+. The ferric ion
develops a red complex with sulfosalicylic acid. The red complex is removed by titration
with EDTA. Citric acid is used to buffer the solution and to make the ferric ion stable in the
solution.
Consumables and replacement items
Required reagents
Reagent set, 10–100 mg/L range (approximately 100 tests): — each 2449200
Citrate Buffer Powder Pillows 1 pillow 100/pkg 2081599
Sodium Periodate Powder Pillows 1 pillow 100/pkg 98499
Sulfosalicylic Acid Powder Pillows 1 pillow 100/pkg 2081669
TitraVer Standard Solution Titration Cartridge, 0.0716 M varies each 2081701
Reagent set, 100–1000 mg/L range (approximately 100 tests): — each 2449300
Citrate Buffer Powder Pillows 1 pillow 100/pkg 2081599
Sodium Periodate Powder Pillows 1 pillow 100/pkg 98499
Sulfosalicylic Acid Powder Pillows 1 pillow 100/pkg 2081669
TitraVer Standard Solution Titration Cartridge, 0.716 M varies each 2081801
Required apparatus
Recommended standards
© Hach Company/Hach Lange GmbH, 2007–2015. All rights reserved. 04/2015, Edition 8
Nitrite DOC316.53.01178
Test preparation
Before starting
The optional TitraStir Titration Stand can hold the Digital Titrator and stir the sample.
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
1
Test procedure
1. Select a sample volume 2. Insert a clean delivery 3. Hold the Digital Titrator 4. Use a graduated cylinder
from Table 1 on page 3. tube into the digital titration with the cartridge tip up. or a pipet1 to measure the
cartridge. Attach the Turn the delivery knob to sample volume from Table 1
cartridge to the Digital eject air and a few drops of on page 3.
Titrator. titrant. Reset the counter to
zero and clean the tip.
5. Pour the sample into a 6. Dilute to approximately 7. Add 5 drops of 5.25 N 8. Swirl to mix.
clean, 125-mL Erlenmeyer 75 mL with deionized water. Sulfuric Acid Standard
flask. Solution.
9. Add one drop of Ferroin 10. Swirl to mix. 11. Put the end of the 12. Use the multiplier in
Indicator Solution. delivery tube fully into the Table 1 on page 3 to
solution. Swirl the flask. calculate the concentration.
Turn the knob on the Digital Digits used × digit multiplier
Titrator to add titrant to the = mg/L sodium nitrite as
solution. Continue to swirl NaNO2.
the flask. Add titrant until the
color changes from orange
to pale blue. Record the
number of digits on the
counter.
Accuracy check
Standard solution method
Use the standard solution method to validate the test procedure, reagents, apparatus and
technique.
Items to collect:
• Sodium Nitrite, ACS
• 1000-mL volumetric flask, Class A
• 5-mL volumetric pipet, Class A and pipet filler safety bulb
• Deionized water
Summary of method
Ferroin indicator and acid is added to the sample. The sample is titrated with tetravalent
cerium ion, which is a strong oxidant. After the cerium oxidizes the nitrite, the indicator is
oxidized and causes a color change from orange to pale blue. The quantity of titrant used
changes in relation to the concentration of sodium nitrite in the sample.
Consumables and replacement items
Required reagents
Required apparatus
Recommended standards
© Hach Company/Hach Lange GmbH, 2007–2015. All rights reserved. 04/2015, Edition 8
Volatile Acids DOC316.53.01182
Test preparation
Before starting
Refer to the Volatile Acids Procedure, Sample Distillation in the distillation apparatus documentation to distill the sample. As
an alternative, refer to the distillation procedure in Standard Methods for the Examination of Water and Wastewater.
The final result is adjusted to give the correct answer based on a 70% correction factor. For higher recoveries, use the
esterification method.
The optional TitraStir Titration Stand can hold the Digital Titrator and stir the sample.
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
Sample collection
• Collect samples in clean glass or plastic bottles.
1
Test procedure
1. Collect 125 mL of 2. Select a sample volume 3. Insert a clean delivery 4. Hold the Digital Titrator
distillate. and titration cartridge from tube into the digital titration with the cartridge tip up.
Table 1 on page 3. cartridge. Attach the Turn the delivery knob to
cartridge to the Digital eject air and a few drops of
Titrator. titrant. Reset the counter to
zero and clean the tip.
5. Use a graduated cylinder 6. Pour the sample into a 7. If the sample volume is 8. Add the contents of one
or a pipet to measure the clean, 250-mL Erlenmeyer less than 150 mL, dilute to Phenolphthalein Indicator
sample volume from Table 1 flask. approximately 150 mL with Powder Pillow.
on page 3. deionized water.
9. Swirl to mix. 10. Put the end of the 11. Use the multiplier in
delivery tube fully into the Table 1 on page 3 to
solution. Swirl the flask. calculate the concentration.
Turn the knob on the Digital Digits used × digit multiplier
Titrator to add titrant to the = mg/L Volatile Acids (as
solution. Continue to swirl acetic acid, CH3COOH).
the flask. Add titrant until the
color changes to light pink.
Record the number of digits
on the counter.
Summary of method
The sample is acidified with sulfuric acid and distilled with deionized water. The distillate
is titrated to the phenolphthalein endpoint with sodium hydroxide standard.
Consumables and replacement items
Required reagents
Required apparatus
Recommended standards
Volatile Acids Standard Solution, 1000 mg/L as Acetic Acid 100 mL 1420542
© Hach Company/Hach Lange GmbH, 2007–2015. All rights reserved. 04/2015, Edition 8