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Corrosion

Management
Manual

Test Kit
Model CM-1
2
CONTENTS
Page
Temperature .............................................................5
Total Dissolved Solids .............................................6
Hardness, Calcium ...................................................8
Alkalinity, Total.....................................................10
pH...........................................................................13
Langlier Saturation Index and
Aggressive Index Calculations ........................15
Phosphate (ortho) ...................................................21
Silica ......................................................................23

Material Safety Data Sheets and Labels


As part of good laboratory practice, please familiarize yourself with
reagents used in these procedures. Read all product labels and
material safety data sheets for all chemicals before using them.
Please use appropriate safety equipment.

3
INTRODUCTION
Corrosive conditions in water supplies can introduce lead, copper and
other heavy metals in to water systems. Consequently, it is necessary to
test drinking water to maintain optimal corrosion control. This kit
includes equipment, reagents and methods for analyzing parameter of
particular importance in controlling corrosive conditions in water:
temperature, total dissolved solids, calcium hardness, total alkalinity and
pH.

By analyzing for these parameters, it is possible to calculate a solution's


ability to dissolve or deposit calcium carbonate by using the Langlier
Saturation Index (LI). The LI is a useful measurement because calcium
carbonate scale (film) can form a protective coating on the inside of the
pipe, insulating the pipe from the water.

Total alkalinity and calcium hardness tests are performed by the easy,
convenient drop-count titration method.

TDS and pH determinations are done with Hach's Pocket Pals. Just dip
the bottom of these simple-to-use instruments in the sample and read the
result from the display.

This kit also contains orthophosphate and silica tests, which allows the
water supplier to test for the concentration of these corrosion inhibitors.
These colorimetric tests help optimize the inhibitor concentration, by
minimizing unnecessary addition of inhibitor. Results are obtained by
matching the developed sample color to a precalibrated disc. The color
disc fits into a color comparator made of durable black plastic. The
orthophosphate analysis can be upgraded to use Hach's DR/100
Colorimeter method, which is USEPA approved. A thermometer is
included for temperature readings.

With this kit analyst can obtain data necessary for making efficient and
timely water management decisions. Packaged in a durable case, this kit
can be used anywhere analysis is needed in the water treatment plant.

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TEMPERATURE
Use the water temperature (in °C) in the Langlier Index calculation. If
necessary, use the table below to convert from °F to °C.

CELSIUS TO FAHRENHEIT DEGREES


°C °F °C °F °C °F
0 32.0 14 57.2 28 82.4
1 33.8 15 59.0 29 84.2
2 35.6 16 60.8 30 86.0
3 37.4 17 62.6 31 87.8
4 39.2 18 64.4 32 89.6
5 41.0 19 66.2 33 91.4
6 42.8 20 68.0 34 93.2
7 44.6 21 69.8 35 95.0
8 46.4 22 71.6 36 96.8
9 48.2 23 73.4 37 98.6
10 50.0 24 75.2 38 100.4
11 51.8 25 77.0 39 102.2
12 53.6 26 78.8 40 104.0
13 55.4 27 80.6

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TOTAL DISSOLVED
SOLIDS
PROCEDURE FOR POCKET PAL TDS TESTER

1. Slide the on/off switch to on. (See Figure 1.) See Note A for
periodic calibration and verification of accuracy.

ON-OFF SWITCH

IMMERSION
LEVEL PROTECTIVE
CAP

FIGURE 1

2. Remove the protective cap from the bottom.

3. Immerse the bottom of the Pocket Pal 1-1.5 inches (2.5-3.8 cm) into
the sample.

4. Gently stir the sample for several seconds with the Pocket Pal.
When the digital display stabilizes, read the display. Multiply the
reading by 10 to determine the TDS value in mg/L. This result is
used in the Langlier calculation.

5. Rinse the bottom of the Pocket Pal and replace the protective cap.
6
Notes
A. Before use and for periodic calibration, measure a solution with a
known TDS value. If necessary, adjust the calibration with a small
screwdriver through the hole in the back. (See Figure 2.)

B. Periodically clean the stainless steel probe with alcohol to maintain


optimal performance.

C. Battery Replacement:

1. Remove the case top from the Pocket pal. See Figure 3.
CAUTION: Do not overextend the attached wires.
2. Replace the four batteries (positive terminals up) with Eveready
E675E, Duracell RM675 or equivalent.

BATTERY
CASE BATTERIES (4)

CALIBRATION
TRIMMER

FIGURE 2 FIGURE 3

D. To convert the TDS value in mg/L to µS/cm, multiply the TDS value
by 2.

7
CALCIUM HARDNESS
Calcium Hardness is the amount of dissolved minerals in water
expressed as milligrams per liter (mg/L) calcium carbonate.

CALCIUM HARDNESS INTERFERENCE CHART


Interference Interference at levels above:
Aluminum Causes slow end point; tolerates up to 200 mg/L if
sufficient time is allowed for color change.
Barium/strontium Titrated as calcium; seldom high enough to cause
interference.
Iron 8 mg/L- causes orange-red to green end point;
accurate results obtained up to 20 mg/L.
Manganese 5 mg/L
Magnesium 200 mg/L- indistinct end point.
Orthophosphate Causes slow end point; allow enough time for
calcium phosphate to redissolve.
Polyphosphates Interfere directly; must be absent.
Temperature Titrate samples coulder than 20 °C (68 °F) slowly
near the end point.
Depending on the sample hardness, varying the sample size can provide
the desired test range and accuracy. Use the table below to determine the
proper range and sample size.

Sample Size for Calcium Hardness Testing


Range (in mg/L) Sample Size Multiplier
Low Range (0-100) 46 mL (2 bottles) 2.5
Low Range (0-200) 23 mL (1 bottle) 5
High Range (200-400) 11.7 mL (2 tubes) 10
High Range (400-800)* 5.8 mL (1 tube) 20
This method can determine concentrations higher than 800 mg/L; exercise care in counting the number of drops.

PROCEDURE FOR LOW RANGE CALCIUM HARDNESS


(0-100 and 0-200 mg/L)

1. Fill the mixing bottle to the 23-mL mark with sample. Pour the
contents of the bottle into the 125-mL flask. (If the calcium hardness
of the sample is 0-1000 mg/L, fill the bottle to the 23-mL mark twice
and pour the contents into the flask. Proceed to Step 2.)

8
2. Add 4 drops of 8 N Potassium Hydroxide Solution to the flask.
Swirl to mix.

3. Add the contents of two CalVer 2 Calcium Indicator Powder Pillows.


Swirl to mix. (See Figure 1.) The sample should be pink. If it is
blue, no calcium hardness is present.

4. Add 0.035 N EDTA Titrant dropwise to the flask. Swirl the flask as
each drop is added and count each drop. Add drops until the sample
changes from pink to blue.

5. The calcium hardness (mg/L) is equal to the number of drops of


EDTA titrant needed to cause the color change multiplied by the
appropriate multiplier.

For a 23-mL sample: Calcium Hardness = No. of drops in Step 4 x 5


For a 46-mL sample: Calcium Hardness = No. of drops in Step 5 x 25

PROCEDURE FOR HIGH RANGE CALCIUM HARDNESS


(200-400 and 400-800 mg/L)

1. Fill the plastic measure tube full of sample. Pour the contents of the
bottle into the mixing bottle. (If the calcium hardness of the sample
is 200-400 mg/L, fill the measuring tube twice and pour the contents
into the mixing bottle. Proceed to Step 2.)

2. Add 2 drops of 8 N Potassium Hydroxide Solution to the mixing


bottle. Swirl to mix (see page 25, Figure 2).

3. Add the contents of one CalVer 2 Calcium Indicator Powder Pillow.


Swirl to mix. The sample should be pink. If it is blue, no calcium
hardness is present.

4. Add 0.035 N EDTA Titrant dropwise to the flask. Swirl the bottle as
each drop is added and count each drop. Add drops until the sample
changes from pink to blue.

5. The calcium hardness (mg/L) is equal to the number of drops of


EDTA titrant needed to cause the color change multiplied by the
appropriate multiplier.

For a 5.8-mL sample: Calcium Hardness = No. of drops in Step 4 x 20


For a 11.7-mL sample: Calcium Hardness = No. of drops in Step 4 x 10

9
ALKALINITY
Alkalinity refers to the amount of titratable bases in water expressed as
milligrams per liter of equivalent calcium carbonate. The presence of
carbonates, bicarbonates, and hydroxides is the most common cause of
alkalinity in natural water. Salts of weak acids such as borates, silicates
and phosphates also may contribute. Alkalinity is significant in the
treatment process of potable water and waste water. Alkalinity is
expressed as phenolphthalein alkalinity or as total alkalinity. The
phenolphthalein alkalinity is determined by titration with sulfuric acid to
a pH of 8.3 (the phenolphthalein end point) and registers the total
hydroxide and one half of the carbonate present. The total alkalinity is
determined by titration to a pH of 4.5. The total alkalinity includes all
carbonate, bicarbonate and hydroxide alkalinity.

Depending on the sample alkalinity, varying the sample size can provide
the desired test range and accuracy. Use the table below to determine the
proper range and sample size.

Sample Size for Alkalinity Testing


Range (in mg/L) Sample Size Multiplier
Low Range (0-100) 46 mL (2 bottles) 2.5
Low Range (100-200) 23 mL (1 bottle) 5
High Range (200-400) 11.7 mL (2 tubes) 10
High Range (400-800) 5.8 mL (1 tube) 20

PROCEDURE FOR LOW RANGE ALKALINITY


(0-100 and 100-200 mg/L)

1. Fill the mixing bottle to the 23-mL mark with sample. Pour the
contents of the bottle into the 125-mL flask. (If the alkalinity of the
sample is 0-100 mg/L, fill the mixing bottle twice and pour the
contents into the flask. Proceed to Step 2.)

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2. Add the contents of 2 Phenolphthalein Indicator Powder Pillows to
the flask. Swirl to mix.

3. If the water remains colorless, the phenolphthalein alkalinity = 0.


Proceed to Step 6.

4. If the water turns pink, add 0.035 N Sulfuric Acid Standard Solution
dropwise, swirling to mix after each drop. Count each drop. Add
drops until the water becomes colorless.

5. The phenolphthalein alkalinity (mg/L) is equal to the number of


drops used in Step 4 multiplied the appropriate multiplier.

For a 23-mL sample: Phenolphthalein = No. of drops in Step 4 x 5


For a 46-mL sample: Phenolphthalein = No. of drops in Step 4 x 2.5

6. Add the contents of 2 Bromcresol Green-Methyl Red Indicator


Powder Pillows to the same flask and swirl to mix. The color will
change to blue-green.

7. Add 0.035 N Sulfuric Acid Standard Solution dropwise until the


sample turns pink. Count each drop and swirl the flask after each
addition. See note A.

8. The total alkalinity (Methyl-Orange) in mg/L is equal to the total


number of drops in Step 4 and 7 multiplied by the appropriate
multiplier.

For a 23-mL sample: Total Alkalinity = (No. of drops in Steps 4 and 7) x 5


For a 46-mL sample: Total Alkalinity = (No. of drops in Steps 4 and 7) x 2.5

PROCEDURE FOR HIGH RANGE ALKALINITY


(200-400 and 400-800 mg/L)

1. Fill the plastic measuring tube full of sample. Pour the contents of
the tube into a mixing bottle. (If the alkalinity of the sample is 200-
400 mg/L, fill the measuring tube twice and pour the contents into
the mixing bottle. Proceed to Step 2.)

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2. Add the contents of 1 Phenolphthalein Indicator Powder Pillow.
Swirl to mix (see page 25, Figure 2).

3. If the sample remains colorless, the phenolphthalein alkalinity = 0.


Proceed to Step 6.

4. If the sample turns pink, add 0.035 N Sulfuric Acid Standard


Solution dropwise, swirling to mix after each drop. Count each drop.
Add drops until the water becomes colorless.

5. The phenolphthalein alkalinity (mg/L) is equal to the number of


drops used in Step 4 multiplied by the appropriate multiplier.

For a 5.8-mL sample: Phenolphthalein = No. of drops in Step 4 x 20


For a 11.7-mL sample: Phenolphthalein = No. of drops in Step 4 x 10

6. Add the contents of 1 Bromcresol Green-Methyl Red Indicator


Powder Pillow to the mixing bottle. Swirl to mix. The color will
change to blue-green.

7. Add 0.035 N Sulfuric Acid Standard Solution, dropwise, until the


sample turns pink. Count each drop and swirl the bottle after each
addition. See note A.

8. The total alkalinity (Methyl-Orange) in mg/L is equal to the number


of drops used in Step 4 and 7 multiplied by the appropriate
multiplier.

For a 5.8-mL sample: Total Alkalinity = (No. of drops in Steps 4 and 7) x 20


For a 11.7-mL sample: Total Alkalinity = (No. of drops in Steps 4 and 7) x 10

Note A: To determine the indicator color at the total alkalinity end point,
mix the contents of one 4.5 pH Buffer Pillow (Cat. No. 865-68) with
50 mL of demineralized water in a 125-mL flask. Add two Bromcresol
Green-Methyl Red Indicator Pillow. Use the color of the Buffer/
Indicator solution as a reference for the 4.5 end point color when titrating
samples.

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pH
PROCEDURE FOR POCKET PAL PH TESTER

1. Slide the on/off switch to on. (See Figure 1.)

ON-OFF SWITCH

IMMERSION
LEVEL PROTECTIVE
CAP

FIGURE 1

2. Remove the protective cap from the bottom.

3. Immerse the bottom of the Pocket Pal 1-1.5 inches (2.5-3.8 cm) into
the sample. See Note A for accuracy verification.

4. Using the Pocket Pal, gently stir the sample for several seconds.
When the display stabilizes after stirring, read the pH value. This
value is pH "actual" in the Langlier calculation. See Note B.

5. Rinse the bottom of the Pocket Pal and replace the protective cap.
See Note C for longer life.

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Notes:

A. Before use and for periodic calibration, prepare a pH 7.00 buffer


solution. Use the Pocket Pal to read the pH. If necessary, adjust the
reading to 7.0 with a small screwdriver through the hole in the back
of the instrument. See Figure 2.

B. Large differences in pH readings may be caused by a dry electrode


or low batteries. To improve performance, dip to immersion level in
tap water at least once a week.

C. Place several drops of water in the protective cap to prevent the glass
bulb from drying out. This will provide faster response and longer
Pocket Pal life.

D. Battery Replacement:

1. Remove the case top from the Pocket pal. See Figure 3.
CAUTION: Do not overextend the attached wires.
2. Replace the four batteries (positive terminals up) with Eveready
E675E, Duracell RM675 or equivalent.

BATTERY
CASE BATTERIES (4)

CALIBRATION
TRIMMER

FIGURE 2 FIGURE 3

14
LANGELIER AND
AGGRESSIVE INDICES
LANGELIER SATURATION INDEX
The Langelier Saturation Index (LI), a measure of a solution’s ability to
dissolve or deposit calcium carbonate, often is used as an indicator of the
corrosivity of water. The index is not related directly to corrosion, but is
related to the deposition of a calcium carbonate film or scale which can
insulate pipes, boilers, and other components of a system from contact
with water. When no protective scale is formed water is considered to be
aggressive, and corrosion can occur. Highly corrosive water can cause
system failures or result in health problems from dissolved lead and other
heavy metals. On the other hand, an excess of scale can damage water
systems, necessitating repair or replacement.

In developing the LI, Langelier derived an equation for the pH at which


water is saturated with calcium carbonate (pHs). This equation is based
on the equilibrium expressions for calcium carbonate solubility and
bicarbonate dissociation. To approximate actual conditions more
closely, pHs calculations were modified to include the effects of
temperature and ionic strength.

The Langelier Index is defined as the difference between actual pH


(measured) and calculated pHs. The magnitude and sign of the LI value
show a water’s tendency to form or dissolve scale and thus inhibit or
encourage corrosion.

Although information obtained from the LI is not quantitative, it can be


useful in estimating water treatment requirements for low pressure
boilers, cooling towers and water treatment plants-as well as serving as a
general indicator of the corrosivity of water.

Parameter Measurement
The Langelier Saturation Index can be calculated easily by using Hach
products to determine the pH of calcium carbonate saturation (pHs) and
the actual pH of a solution. Using a simple formula, the pH is derived
from the values for calcium hardness, total alkalinity at pH 4.5,

15
temperature and total filterable residue (total dissolved solids). All of
these procedures are included in this manual.

Temperature: Temperature can be measured in degrees centigrade with


a laboratory thermometer. If only a Fahrenheit thermometer is available,
conversion to degrees Celsius will be necessary. [°C = 5/9 x (°F - 32)] or
use the conversion chart in the Temperature Section of this manual.

Calculation
After the preceding parameters have been determined, calculate the pH,
from the following formula:

pHs = A + B – C – D

Where:

Constant A takes into account the effect of temperature. It is found by


selecting the value from Table 1 (see Aggressive Index) that corresponds
to the measured temperature in degrees centigrade.

Constant B is a correction for the ionic strength of the sample. It is


determined using Table 2 (see Aggressive Index) by taking the value that
corresponds to the measured total filterable residue or the estimated
TDS.

Value C is obtained by using the calcium hardness (in mg/L CaCO3) of


the sample and referring to Table 3 (see Aggressive Index).

Value D is obtained by using the total alkalinity (in mg/L CaCO3) of the
sample and referring to Table 3.

The Langelier Saturation Index is the difference between the pHactual, of


the solution and pHs calculated above.

pHactual – pHs = LI

Interpretation
The LI is a gauge of whether a water will precipitate or dissolve calcium
carbonate. If the pHs is equal to the actual pH, the water is considered
“balanced”. This means that calcium carbonate will not be dissolved or
precipitated. If the pHs is less than the actual pH (the LI is a positive
number), the water will tend to deposit calcium carbonate and is scale-
forming (nonaggressive). If the pHs is greater than the actual pH (the LI

16
is a negative number), the water is not saturated and will dissolve
calcium carbonate (aggressive). In summary:

pHs = pHactual, water is balanced


pHs < pHactual, water is scale forming (nonaggressive)
pHs > pHactual, water is not scale forming (aggressive)

It is important to remember that the LI value is not a quantitative


measure of calcium carbonate saturation or corrosion.

Because the protective scale formation is dependent on pH, bicarbonate


ion, calcium carbonate, dissolved solids and temperature; each may
affect the water’s corrosive tendencies independently. Soft, low
alkalinity waters with either low or excessively high pH are corrosive
even though this may not be predicted by the LI. This is because
insufficient amounts of calcium carbonate and alkalinity are available to
form a protective scale.

Waters having high pH values and sufficient hardness and alkalinity also
may be corrosive even if the LI predicts the opposite. This is the result
of calcium and magnesium complexes that cannot actively participate in
the scale forming process. Analytical procedures do not distinguish
between these complexes and available calcium and magnesium, and so
the LI value is not accurate in such situations.

Corrosive tendencies may be exhibited also by water containing high


concentrations of sulfate, chloride and other ions which interfere with
uniform carbonate film formation.

As a result of these and other problems, the LI is useful only for


determining the corrosivity of waters containing more than 40 mg/L of
alkalinity, sufficient calcium ion concentration and ranging between pH
6.5 and 9.5.

AGGRESSIVE INDEX
The Aggressive Index (AI) originally developed for monitoring water to
be transported through asbestos pipe, is sometimes substituted for the
Langelier Index as an indicator of corrosivity of water. The AI is derived
from the actual pH, calcium hardness and total alkalinity. (Use
procedures contained in this handbook). Where it is applicable, it is
simpler and more convenient than the LI. Since the AI does not include
the effects of temperature or dissolved solids, it is less accurate as an
analytical tool than the LI.

17
Calculation
After obtaining the pH, total alkalinity, and calcium hardness, use the
following formula to calculate the AI:

AI = pHactual + C + D

Where:

Value C is obtained by using the measured value for calcium hardness in


mg/L CaCO3 and referring to Table 3.
Parameter Measurement*

Value D is obtained by using the measured value for total alkalinity in


mg/L CaCO3 and referring to Table 3.

Interpretation
As with LI, the AI is not a quantitative measure of corrosion but is a
general indicator of the tendency for corrosion to occur and should be
used with proper reservation. An AI of 12 or above indicates
nonaggressive (not corrosive) water; AI values below 10 indicate
extremely aggressive (corrosive) conditions. Values of 10-11.9 suggest
that the water is moderately aggressive. Corrosivity characteristics of
water as indicated by the LI and AI are compared in Table 4.

Table 1
Water Temperature, °C A
0 ...............................................................................................2.60
4 ...............................................................................................2.50
8 ...............................................................................................2.40
12 .............................................................................................2.30
16 .............................................................................................2.20
20 .............................................................................................2.10
25 .............................................................................................2.00
30 .............................................................................................1.90
40 .............................................................................................1.70
50 .............................................................................................1.55
60 .............................................................................................1.40
70 .............................................................................................1.25
80 .............................................................................................1.15

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Table 2
TDS, mg/L B
0 ...............................................................................................9.70
100 ...........................................................................................9.77
200 ...........................................................................................9.83
400 ...........................................................................................9.86
600 ...........................................................................................9.89
1000 .........................................................................................9.90

Table 3
Calcium Hardness and
Total Alkalinity in mg/L CaCO3 C or D
10 .............................................................................................1.00
20 .............................................................................................1.30
30 .............................................................................................1.48
40 .............................................................................................1.60
50 .............................................................................................1.70
60 .............................................................................................1.78
70 .............................................................................................1.84
80 .............................................................................................1.90
100 ...........................................................................................2.00
200 ...........................................................................................2.30
300 ...........................................................................................2.48
400 ...........................................................................................2.60
500 ...........................................................................................2.70
600 ...........................................................................................2.78
700 ...........................................................................................2.84
800 ...........................................................................................2.90
900 ...........................................................................................2.95
1000 .........................................................................................3.00
Note: Factor C is the logarithm (base 10) of the calcium hardness expressed in mg/L.
Note: Factor D is the logarithm (base 10) of the total alkalinity expressed in mg/L.

19
Table 4
Corrosive Characteristics Langelier Index Aggressive Index
Highly aggressive < -2.0 < 10.0
Moderately aggressive -2.0 to 0.0 10.00 to 12.0
Nonaggressive >0.0 >12.0

References
1. Langelier, W. F., “The Analytical Control of Anticorrosion Water Treatment”
Journal of American Water Works Association 1936, 28, 1500.
2. Larson, T.E.; Buswell A. M. “Calcium Carbonate Saturation Index and Alkalinity
Interpretations” Journal of American Water Works Association 1942, 34, 1667.
3. Langelier, W. F., “Chemical Equilibria in Water Treatment” Journal of American
Water Works Association 1946, 38, 169.
4. Maguire, J. J.; Polsky, J. W. “Simplified Plant Control Test for Boiler Water
Dissolved Solids” Combustion 1947, May, 35.
5. Betz Handbook of Industrial Water Conditioning 1962, 6th ed., Betz Laboratories:
Trevose, PA.
6. Robinson, R. A.; Stokes, R. H. Electrolyte Solutions 1965, Butterworth & Co. LTD:
London.
7. Federal Register 1980, 45 (168), August 27, 1980, p. 57338.

20
PHOSPHATE
If a corrosion inhibitor is used, it will be necessary to analyze for
orthophosphate or silica, depending on the type of corrosion inhibitor
used.

This kit includes colorimetric methods to perform these analyses. The


analytical method for orthophosphate (reactive phosphorus) can be used
with Hach's DR/100 colorimeter method, which is USEPA approved.

PROCEDURE FOR LOW RANGE PHOSPHATE (0 to 5 mg/L)

1. Fill both color viewing tubes to the 5-mL mark with the water to be
tested.

2. Use the clippers to open on PhosVer 3 Phosphate Reagent Powder


Pillow. Add the contents of the pillow to one of the tubes. Swirl to
mix. Allow at least one minute, but not more than five minutes, for
color development. If phosphate is present, a blue-violet color will
develop.

3. Insert the tube with the prepared sample into the right top opening of
the color comparator (prepared Sample Position in Figure 1).

FIGURE 1

4. Insert the tube of untreated water sample into the left top opening of
the comparator (Untreated Sample Position in Figure 1).
21
5. Hold the comparator up to a light source such as the sky or a lamp
and view through the two openings in front. Rotate the disc to obtain
a color match. Divide the reading in the scale window by 10 to
obtain the mg/L phosphate (PO4)
mg/L PO4 = reading on scale
10

6. To obtain the value as mg/L phosphorus (P), divide the phosphate


(PO4) value by 3.

PROCEDURE FOR HIGH RANGE PHOSPHATE (0 to 50 mg/L)

1. Rinse a color viewing tube with demineralized water. Rinse the


plastic dropper several times with the water to be tested. If the
sample is turbid, pass through filter paper before analysis.

2. Fill the dropper to the 0.5-mL mark with the water to be tested.
Discharge the contents of the dropper into the rinsed color viewing
tube.

3. Add demineralized water to the 5-mL mark on the viewing tube.


Swirl the tube to mix.

4. Use the clippers to open one PhosVer 3 Phosphate Reagent Powder


Pillow. Add the contents of the pillow to one of the tubes. Swirl to
mix. Allow at least one minute, but not more than five minutes, for
color development. If phosphate is present, a blue-violet color will
develop.

5. Insert the tube of prepared sample into the right top opening of the
comparator (Prepared Sample Position in Figure 1).

6. Fill the other viewing tube to the 5-mL mark with demineralized
water. Insert this tube into the left top opening of the color
comparator (Untreated Sample Position in Figure 1).

7. Hold the comparator up to a light source such as the sky or a lamp


and view through the two openings in front. Rotate the disc to obtain
a color match. Read the mg/L phosphate (PO4) through the scale
window.
mg/L = reading on scale
8. To obtain the value as mg/L phosphorus (P), divide the phosphate
value (PO4) by 3.

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SILICA
The Citric Acid Powder Pillow used in these procedures eliminates
phosphate interference up to 50 mg/L phosphate. Higher concentrations
of phosphate cause these negative errors: 60 mg/L phosphate- 2%;
75 mg/L phosphate- 11%. If larger amounts of phosphate are present,
dilute the sample as instructed tin the High Range test to minimize
phosphate interference.

PROCEDURE FOR MEDIUM RANGE SILICA


(0 to 40 mg/L SiO2)

1. Fill both sample tubes to the 5-mL mark with the water to be tested.

2. Use the clippers to open one Molybdate Reagent Powder Pillow and
one Acid Reagent Powder Pillow. Add the contents of both pillows
to one of the tubes. Swirl to mix.

3. Let the sample stand for 10 minutes to allow color development. If


silica or phosphate is present, a yellow color will develop.

4. Open one Citric Acid Powder Pillow and add the contents of the
pillow to the same sample tube. Swirl to mix. Allow the solution to
stand for two minutes. The citric acid will destroy the yellow color
due to phosphate.

5. Add the contents of one Silica 3 Reagent Powder Pillow to the same
tube. Swirl to mix.

6. Allow five minutes for color development. If silica is present, a blue


color will develop.

23
7. Insert the tube of prepared sample into the right top opening of the
color comparator (Prepared Sample Position in Figure 1).

8. Insert the tube of untreated water into the top left opening of the
color comparator (Untreated Sample Position in Figure 1).

9. Hold the comparator up to a light source such as the sky or a lamp


and view through the two openings in the front. Rotate the disc to
obtain a color match. Read the mg/L silica (SiO2) through the scale
window.

FIGURE 1

PROCEDURE FOR HIGH RANGE SILICA


(0 to 800 mg/L SiO2)

1. Fill the dropper to the 1-mL mark with the water to be tested (1 cc =
1 mL). Transfer the contents of the dropper to the square mixing
bottle.

2. Fill the mixing bottle to the 20-mL mark with demineralized water.
Swirl to mix as shown in Figure 2.

3. Fill both sample tubes to the 5-mL mark with the diluted water
sample form Step 2.

4. Use the clippers to open one Molybdate Reagent Powder Pillow and
one Acid Reagent Powder Pillow. Add the contents of both pillows
to one of the tubes. Swirl to mix.

5. Let the sample stand for 10 minutes to allow color development. If


silica or phosphate is present, a yellow color will develop.
24
FIGURE 2

6. Open one Citric Acid Powder Pillow and add the contents of the
pillow to the same sample tube. Swirl to mix. Allow the solution to
stand for two minutes. The citric acid will destroy the yellow color
due to phosphate.

7. Add the contents of one Silica 3 Reagent Powder Pillow to the same
tube. Swirl to mix.

8. Allow five minutes for color development. If silica is present, a blue


color will develop.

9. Insert the tube of prepared sample into the right top opening of the
color comparator (Prepared Sample Position in Figure 1).

10. Insert the tube of untreated water into the top left opening of the
color comparator (Untreated Sample Position in Figure 1).

11. Hold the comparator up to a light source such as the sky or a lamp
and view through the two openings in the front. Rotate the disc to
obtain a color match. Read the mg/L silica (SiO2) through the scale
window.

12. To obtain the mg/L silica, multiply the reading in Step 11 by 20.

Mg/L Silica = Reading on Scale x 20

25
REAGENTS AND
APPARATUS
Parameter Cat No. Description Unit

pH 44350-00 pH Pocket Pal each

Temperature 1877-01 Thermometer each

TDS 44400-00 TDS Pocket Pal each

Hardness (Ca) 947-99 CalVer 2 Calcium Indicator pkg/100


Powder Pillows
282-37 Potassium Hydroxide Solution, 8N 118 mL
23499-37 EDTA Titrant, 0.035N 118 mL MDB
968-00 Clippers each
438-00 Measuring Tube, plastic, 5.83 mL each
2327-06 Bottle, mixing, 10-, 15-, 20-, each
23-mL marks
505-13 Erlenmeyer Flask, 125 mL each

Alkalinity 942-99 Phenolphthalein Powder Pillows pk/100


943-99 Bromcresol Green-Methyl Red pk/100
Powder Pillows
23497-37 Sulfuric Acid Standard, 0.035 N 118 mL
438-00 Measuring Tube, 5.83 mL each
2327-06 Bottle, mixing, 10-, 15-, 20-, each
23-mL marks

Orthophos- 2209-99 PhosVer 3 Reagent Powder pk/100


phate Pillows for 5-mL samples
968-00 Clippers each
1732-00 Color Comparator each
46600-04 Color Viewing Tube, 5-mL mark pkg/4
14197-05 Dropper, 0.5 & 1-mL marks pkg/5
24898-00 Color Disc, Phosver 3, 0-50 mg/L each

26
Silica 14545-99 Acid Reagent Powder Pillows pk/100
14549-99 Citric Acid Powder Pillows pk/100
14299-00 Demineralizer Bottle 177 mL
14546-99 Molybdate Reagent Powder Pillows pk/100
271-69 Silica 3 Reagent Powder Pillows pk/100
2327-06 Bottle, mixing, 10-, 15-, 20-, each
23-mL marks
1732-00 Color Comparator each
1741-00 Color Disc, Silica, 0-40 mg/L each
46600-04 Color Viewing Tube, 5-mL mark pkg/4
14197-05 Dropper, 0.5 & 1-mL marks pkg/5

27
HOW TO ORDER

HACH COMPANY
WORLD HEADQUARTERS
P.O. Box 389
Loveland, Colorado 80539-0389
Telephone: (970) 669-3050
FAX: (970) 669-2932

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

PRINTED IN U.S.A 3/92, rev1 11/01 rb

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