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Information INF07/124EN Rev.

Navigator 600
Silica analyzers
Mixing chemical solutions

1 Reagent solutions
C6H8O7.H2O, and stir to dissolve. Allow the solution to cool to
Warning. room temperature and then add 250 (5) ml of propan-2-ol
Handle concentrated sulfuric acid with great care; when (iso-propyl alcohol). Transfer the solution to a 2.5 liter plastic
diluting it, add it to the water. Do not add water to the bottle and make up to 2.5 liters with more high purity water.
acid. Wear appropriate protective clothing. Reduction solution ascorbic acid (BROWN channel)
Concentrated ammonia solution is extremely volatile and Dissolve 43 (1) g analytical reagent grade ascorbic acid,
toxic; it must always be handled under a fume hood. C6H8O6, in approximately 1 liter of high purity water. Add to
Wear appropriate protective clothing. this solution 0.18 (0.01) g analytical reagent grade disodium
EDTA, C10H14O8N2Na2.2H2O. When dissolved, add 4.0
A volume of 2.5 liters of each reagent solution maintains the (0.1) ml analytical reagent grade formic acid, H(COOH) and
analyzer in operation for a minimum of three months. The bottles transfer to a 2.5 liter plastic bottle. Dilute to 2.5 liters with
are color-coded to identify each reagent. more high purity water.
1st Acid 0.4M sulfuric acid (RED channel)
Place approximately 1 liter high purity water in a plastic Note. To ensure the reduction solution is fresh, a
beaker and carefully add 54.5 (0.5) ml analytical reagent solution of disodium EDTA and formic acid can be
grade concentrated sulfuric acid, H2SO4, (1.84 s.g.). Transfer prepared and stored and solid ascorbic acid added
the solution to a 2.5 liter plastic bottle and make up to 2.5 immediately before use. Ensure the solid is fully dissolved
liters with more high purity water. by shaking the bottle well.
Ammonium molybdate solution (VIOLET channel)
The 1st Acid and 2nd Acid reagents have a shelf life of several
Dissolve 37 (1) g analytical reagent grade ammonium
months; prepare the molybdate and reduction solutions for
molybdate, (NH4)6Mo7024.4H2O, in approximately 1 liter high
immediate use only.
purity water. Transfer the solution to a 2.5 liter plastic bottle,
add 7.5 (0.5) ml ammonia solution, NH4OH, (0.880 s.g.) Ensure all solutions are mixed thoroughly before use.
and make up to 2.5 liters with more high purity water.
Note. The reduction solution discolors over time but this does
2nd Acid 1.25M sulfuric acid (ORANGE channel)
not affect the performance of the analyzer.
Place approximately 1 liter of high purity water in a
polyethylene beaker. Surround the beaker with running cold
water and add 170 (2) ml of analytical reagent grade
concentrated sulfuric acid, H2SO4 (1.84 s.g.) slowly and
carefully. Stir the solution continuously during the addition.
Add 63 (1) g of analytical reagent grade citric acid crystals,
C6H8O7.H2O, and stir to dissolve. Allow the solution to cool to
room temperature and then add 250 (5) ml of propan-2-ol
(iso-propyl alcohol). Transfer the solution to a 2.5 liter plastic
bottle and make up to 2.5 liters with more high purity water.
2nd Acid 1.25M sulfuric acid (ORANGE channel) for
applications where Phosphate is present in the sample
Place approximately 1 liter of high purity water in a
polyethylene beaker. Surround the beaker with running cold
water and add 170 (2) ml of analytical reagent grade
concentrated sulfuric acid, H2SO4 (1.84 s.g.) slowly and
carefully. Stir the solution continuously during the addition.
Add 375 (5) g of analytical reagent grade citric acid crystals,

Confidential & Proprietary, 2011 Version


2 Secondary calibration solutions

2 Secondary calibration solutions 3 Cleaning solutions


It is important that the internal pipework of the analyzer is cleaned
Note. using the automatic cleaning schedule. Cleaning prevents gradual
The accuracy of the analyzer over its total range is fouling by molybdate precipitation in the pipework which can
governed by the choice of the secondary standard introduce errors. Problems such as noise can also be caused by
solution value. An analyzer calibrated at 200 g l1, for contaminated pipework.
example, will not exhibit the best accuracy at 2000 g l1.
For a multi-stream analyzer, chose a solution Warning. Sodium hydroxide is extremely caustic and must be
concentration that coincides with the point of greatest handled with great care. Wear appropriate protective clothing.
required accuracy. For a single-stream analyzer, chose a
value that corresponds to 80% of the high range value.
3.1 Regular cleaning solution
The high purity water used for diluting the standard (for automatic cleaning operation)
solution should contain less than 1 g l1 SiO2. If, this is To prepare 1 liter of regular cleaning solution:
not possible to obtain and the silica concentration is
1. Dissolve 5 g of analytical grade sodium hydroxide pellets,
known, make allowance for the background level in the
NaOH, in approximately 600 ml of high purity water in a
high purity water when calculating the actual silica
plastic container. Allow the solution to cool to ambient
concentration of the standard.
temperature.
2. Add to the solution 1 g analytical grade di-sodium EDTA and
A stock solution of 100 mg l1 silica, SiO2, can be obtained in one of stir to dissolve.
the following ways:
3. Transfer the solution to a 1 liter measuring cylinder and make
The preferred method: to the mark with more high purity water. Mix well and store in
Purchase a 100 mg l1 SiO2 stock solution from a proprietary a tightly stoppered plastic bottle.
chemical supplier.
If a stock solution of 1000 mg l1 silicon (Si) is available, it can 3.2 Extra strength cleaning solution
be diluted to obtain a 100 mg l1 SiO2 solution by taking 46.81 (for troubleshooting and more intense wet section cleaning)
ml and diluting to 1 liter with high purity water in a volumetric To prepare 1 liter of extra strength cleaning solution:
flask. The dilution factor is 21.39 times. 1. Dissolve 50 g of analytical grade sodium hydroxide pellets,
From sodium fluorosilicate: NaOH, in approximately 600 ml of high purity water in a
1. Dissolve 313 (1) mg of sodium fluorosilicate (Na2SiF6 plastic container. Allow the solution to cool to ambient
the purest grade available) in approximately 900 ml of temperature.
high purity water. Ensure that all solid has dissolved fully 2. Add to the solution 5 g analytical grade di-sodium EDTA and
by stirring the solution for several hours. stir to dissolve.
b. Transfer the solution to a 1 liter volumetric flask and 3. Transfer the solution to a 1 liter measuring cylinder and make
make up to the mark with more high purity water. to the mark with more high purity water. Mix well and store in
c. Store the solution in a polyethylene bottle. a tightly stoppered plastic bottle.
From sodium metasilicate:
1. Dissolve 353 (1) mg of sodium metasilicate penta
hydrate (Na2SiO3.5H2O the purest grade available) in
approximately 900 ml of high purity water. Ensure that
all solid has dissolved fully by stirring the solution for
several hours.
b. Transfer the solution to a 1 liter volumetric flask and
make up to the mark with more high purity water.
c. Store the solution in a polyethylene bottle.

Note.
Using polyethylene apparatus, dilute the appropriate
stock solution with high purity water to obtain the
secondary calibration solution.
Store all standard solutions in tightly stoppered
polyethylene bottles.
Stock solutions remain stable for approximately one year.
Prepare standard solutions for the analyzer immediately
before they are required for use.

2 INF07/124EN Rev. B | Navigator 600 | Silica analyzers | Mixing chemical solutions Confidential & Proprietary, 2011 Version
Notes

Notes

Confidential & Proprietary, 2011 Version Navigator 600 | Silica analyzers | Mixing chemical solutions | INF07/124EN Rev. B 3
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INF07/124EN Rev. B 12.2011


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