海水硅酸盐测定方法

QuikChem® Method 31-114-27-1-D DETERMINATION OF SILICATE IN BRACKISH OR SEAWATER BY FLOW INJECTION ANALYSIS

Written by Matt Wolters

Applications Group

Revision Date:

17 September 2003

LACHAT INSTRUMENTS

5600 LINDBURGH DRIVE

QuikChem® Method 31-114-27-1-D

Silicate in Brackish or Seawater

10 to 1700 µg Si/L

– Principle –

Soluble silica species react with molybdate at 45°C and a pH of 1.2 to form a yellow silicamolybdate complex. This complex is subsequently reduced with stannous chloride to form a heteropoly blue complex which has an absorbance maximum at 820 nm. The absorbance is proportional to the concentration of “molybdate reactive” silica.

Though the method is written for brackish water and seawater, it is also applicable to non-saline sample matrixes. The method is calibrated using standards prepared in deionized water. Once calibrated, samples of varying salinities (0 to 35 ppt) may be analyzed. The determination of background absorbance is necessary only for samples, which have color absorbing at 820 nm.

– Interferences –

1. Orthophosphate is a known interferent in this method. The selectivity of this method

against orthophosphate is 79. A sample containing greater than 142 µg P/L as orthophosphate would result in a positive interference greater than that of the method detection limit.

2. Turbidity may positively interfere with this method. Filtration can remove this

interference.

– Special Apparatus –

Please see Parts and Price list for Ordering Information

1. Standards Tubes, Polystyrene (Lachat Part No. 21049)

2. Sample Tubes, Polystyrene (Lachat Part No. 21042)

3. All reagent, standard, and sample containers must be non-glass (polystyrene or

polypropylene)

Unit

4. Heating

CONTENTS

1. SCOPE AND APPLICATION (1)

2. INTERFERENCES (1)

3. SAFETY (1)

4. EQUIPMENT AND SUPPLIES (1)

5. REAGENTS AND STANDARDS (2)

5.1.PREPARATION OF REAGENTS (2)

5.2.PREPARATION OF STANDARDS (3)

6. SAMPLE COLLECTION, PRESERVATION AND STORAGE (4)

7. PROCEDURE (5)

7.1.CALIBRATION PROCEDURE (5)

7.2.SYSTEM NOTES (5)

8. DATA ANALYSIS AND CALCULATIONS (6)

9. METHOD PERFORMANCE (6)

10. REFERENCES (6)

11. TABLE, DIAGRAMS, FLOWCHARTS, AND VALIDATION DATA (7)

11.1.DATA SYSTEM PARAMETERS FOR QUIKCHEM 8000 (7)

11.2.SUPPORT DATA FOR QUIKCHEM 8000 (8)

11.3.SILICATE MANIFOLD DIAGRAM (13)

QuikChem® Method 31-114-27-1-D

DETERMINATION OF SILICATE IN BRACKISH OR SEAWATER

BY FLOW INJECTION ANALYSIS

1. SCOPE AND APPLICATION

1.1. This method covers the determination of silicate in brackish or seawaters.

1.2. The method is based on reactions that are specific for the orthophosphate ion.

1.3. The applicable range is 10 to 1700 µg Si/L. The method detection limit is 1.43 µg Si/L;

claiming 2.1 µg Si/L due to carryover. The method throughput is 36 injections per hour.

2. INTERFERENCES

2.1. Orthophosphate is a known interferent in this method. The selectivity of this method

against orthophosphate is 79. A sample containing greater than 142 µg P/L as

orthophosphate would result in a positive interference greater than that of the method

detection limit.

2.2. Turbidity may positively interfere with this method. Filtration can remove this

interference.

3. SAFETY

3.1. The toxicity or carcinogenicity of each reagent used in this method has not been fully

established. Each chemical should be regarded as a potential health hazard and exposure

should be as low as reasonably achievable. Cautions are included for known extremely

hazardous materials.

3.2. Each laboratory is responsible for maintaining a current awareness file of the

Occupational Health and Safety Act (OSHA) regulations regarding the safe handling of

the chemicals specified in this method. A reference file of Material Safety Data sheets

(MSDS) should be made available to all personnel involved in the chemical analysis.

The preparation of a formal safety plan is also advisable.

3.3. The following chemicals have the potential to be highly toxic or hazardous, for detailed

explanation consult the MSDS.

3.3.1. Hydroxylamine hydrochloride

3.3.2. Sulfuric Acid

3.3.3. Oxalic Acid

4. EQUIPMENT AND SUPPLIES

4.1. Balance -- analytical, capable of accurately weighing to the nearest 0.0001 g.

4.2. Glassware -- Class A volumetric flasks and pipettes or plastic containers as required.

Samples may be stored in plastic or glass.