Method 8185

SILICA, High Range (0 to 75.0 mg/L) For water and seawater

Silicomolybdate Method

1. Enter the stored 2. Press: 89 ENTER 3. Fill two sample 4. To the other cell,
program number for The display will show cells with 10 mL of add the contents of one
high range silica (SiO2). mg/L, SiO2 and the sample. Set one aside Molybdate Reagent
ZERO icon. as the blank. Powder Pillow for High
Press: PRGM
Note: Sample temperature Range Silica (the
The display will show: Note: For alternate form
(Si), press the CONC key. should be 15 to 25 °C prepared sample). Cap
PRGM ? (59 to 77 °F). and invert to mix.
Note: For most accurate
results, perform a Reagent
Blank Correction using
deionized water (see
Section 1).

5. Add the contents of 6. Press: 7. When the timer 8. The display will
one Acid Reagent TIMER ENTER beeps, add the contents show: 2:00 Timer 2
Powder Pillow for of one Citric Acid Press: ENTER
A 10-minute reaction
High Range Silica. Cap Powder Pillow to the
period will begin. A two-minute reaction
and invert to mix. prepared sample. Cap
period will begin.
Note: Silica or phosphate and invert to mix.
Note: Perform Steps 9-12
will cause a yellow color Note: The yellow color due
within three minutes after
to develop. to phosphate will
the timer beeps.
disappear.

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SILICA, High Range, continued

9. When the timer 10. Press: ZERO 11. Place the prepared 12. Press: READ
beeps, place the blank in The cursor will move to sample into the cell The cursor will move to
the cell holder. Tightly the right, then the holder. Tightly cover the the right, then the result
cover the sample cell display will show: sample cell with the in mg/L silica (SiO2)
with the instrument cap. instrument cap. will be displayed.
0.0 mg/L SiO2
Note: If Reagent Blank Note: Use of the Standard
Correction is on, the Adjust feature with each
display may flash “limit”. new lot of reagent is highly
See Section 1. recommended. See
Accuracy Check.

Sampling and Storage

Collect samples in clean plastic or glass bottles. Analyze samples
as soon as possible after collection. Store samples up to 28 days at
4 °C (39 °F) or below. Warm samples to room temperature before
analyzing.

Accuracy Check
Standard Additions Method
a) Open a High Range Silica Standard Solution, 1000 mg/L
SiO2.

b) Use the TenSette Pipet to add 0.1 mL, 0.3 mL, and 0.5 mL
of the standard to three 10-mL samples. Mix each
thoroughly.

c) Analyze each sample as described above. The silica

concentration should increase 10.0 mg/L for each 0.1 mL
of standard added.

d) If these increases do not occur, see Standard Additions in

Section 1 for more information.

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SILICA, High Range, continued
Standard Solution Method
To check the accuracy of the method, use the Silica Standard
Solutions, 25 and 50 mg/L as SiO2, listed under Optional
Reagents. Analyze according to the above procedure using
deionized water as the blank.

Standard Adjust
To adjust the calibration curve using the reading obtained with
the
50.0 mg/L standard solution, press the SETUP key and scroll
(using the arrow keys) to the STD setup option. Press ENTER to
activate the standard adjust option. Then enter 50.0 to edit the
standard concentration to match that of the standard used. Press
ENTER to complete the adjustment. See Section 1, Standard
Curve Adjustment for more information.

Method Performance
Precision
In a single laboratory, using a standard solution of 50.0 mg/L
SiO2 and two representative lots of reagent with the instrument, a
single operator obtained a standard deviation of ±1.0 mg/L silica.

Estimated Detection Limit

The estimated detection limit for program 89 is 1.00 mg/L SiO2.
For more information on the estimated detection limit, see
Section 1.
Interferences
Interfering Substance Interference Levels and Treatments
Color Eliminated by zeroing the instrument with the
original sample.
Iron High levels of Fe 2+ and Fe3+ interfere.
Phosphate Does not interfere below 50 mg/L PO43-. At 60 mg/L
PO43-, a negative 2% interference occurs. At 75 mg/L
PO43- the interference is negative 11%.
Sulfides (S2-) High levels interfere.
Turbidity Eliminated by zeroing the instrument with the
original sample.

Occasionally a sample contains silica which reacts very slowly

with molybdate. The nature of these “molybdate-unreactive”
forms is not known. A pretreatment with sodium bicarbonate,
then sulfuric acid will make these forms reactive to molybdate.
The pretreatment is given in Standard Methods for the

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SILICA, High Range, continued
Examination of Water and Wastewater under Silica-Digestion
with Sodium Bicarbonate. A longer reaction time with the sample
and the molybdate and acid reagents (before adding citric acid)
may help in lieu of the bicarbonate treatment.

Summary of Method
Silica and phosphate in the sample react with molybdate ion
under acidic conditions to form yellow silicomolybdic acid
complexes and phosphomolybdic acid complexes. Addition of
citric acid destroys the phosphate complexes. Silica is then
determined by measuring the remaining yellow color.

REQUIRED REAGENTS
Cat. No.
High Range Silica Reagent Set, 10-mL sample (100 tests) ......................................... 24296-00
Includes: (1) 21074-69, (1) 21062-69, (1) 21073-69
Quantity Required
Description Per Test Units Cat. No.
Acid Reagent Powder Pillows for High Range Silica .. 1..................... 100/pkg.......... 21074-69
Citric Acid Powder Pillows .......................................... 1..................... 100/pkg.......... 21062-69
Molybdate Reagent Powder Pillows for HR Silica ...... 1..................... 100/pkg.......... 21073-69

REQUIRED APPARATUS
Sample Cell, 10-20-25 mL, w/ cap ............................... 2......................... 6/pkg.......... 24019-06

OPTIONAL REAGENTS
Silica Standard Solution, 10 mg/L .........................................................500 mL............ 1403-49
Silica Standard Solution, 25 mg/L .........................................................236 mL.......... 21225-31
Silica Standard Solution, 50 mg/L .........................................................200 mL............ 1117-29
Silica Standard Solution, 1000 mg/L .....................................................500 mL.............. 194-49
Sodium Bicarbonate, ACS........................................................................ 454 g.............. 776-01
Sulfuric Acid Standard Solution, 1.000 N ...................................100 mL MDB............ 1270-32
Water, deionized............................................................................................4 L.............. 272-56

OPTIONAL APPARATUS
Pipet, TenSette, 0.1 to 1.0 mL..................................................................... each.......... 19700-01
Pipet Tips, for 19700-01 Pipet ................................................................ 50/pkg.......... 21856-96
Pipet Tips, for 19700-01 Pipet ....................................... .................... 1000/pkg.......... 21856-28
Standard Methods for the Examination of Water and Wastewater ............. each.......... 22708-00
Thermometer, -20 to 110 °C, Non-Mercury ................................................ each.......... 26357-02

For Technical Assistance, Price and Ordering

In the U.S.A.—Call 800-227-4224
Outside the U.S.A.—Contact the Hach office or distributor serving you.

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