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FLUORIDE IN SOIL AND SLUDGE (SAMPLE PREPARATION AND EXTRACTION (1) PREPARE…
FLUORIDE IN SOIL AND SLUDGE
REAGENTS PREPARATION
SHELF LIFE
COMMERCIALLY AVAILABLE
CALIBRATION AND AQC STANDARD PREPARATION
STOCK SOLUTIONS
ADDITION OF ACID TO SAMPLE THOUGHT TO POTENTIALLY CONTAIN HAZARDOUS MATERIAL
RANGE OF APPLICATION
APPARATUS
SAMPLE COLLECTION AND PRESERVATION
COLLECTED FROM FIELD AT A DEPTH OF 250 MM (LD SAMPLES) OR 150 MM(OA SAMPLES)
SAMPLE PRE-TREATMENT
SLUDGE SAMPLES ARE DRIED
DRYING AND GRINDING OF THE LAND SAMPLES
SAMPLE PREPARATION AND EXTRACTION
1) PREPARE WORKSHEETS FOR FLUORIDE 00541 & 90660. LABEL POTS WITH PRE-PRINTED LABELS
2) CREATE COMPOSITE FOR 00541,TRANSFER TO INSTRUMENT, SELECTING INSTRUMENT FROM DROP DOWN MENU
3) INVERT SOIL SAMPLE POT 3 TIMES TO DISTRIBUTE LAND EVENLY WEIGH SOIL OR DRIED SLUDGE INTO A TARED POT RECORD MASS ON WORKSHEET
BLANKS - ACID WASHED SAND
4) ADD 20 ML OF 0.5M SULPHURIC ACID TO EACH POT USING A CALIBRATED DISPENSER
5) MIX SAMPLE BY SWIRLING SIX TIMES DURING NEXT 15 MINUTES
6) ADD DEIONISED WATER USING CALIBRATED DISPENSER LEAVE FOR MINIMUM 1 HOUR TO ALLOW FULL REACTION
SAMPLES ANALYSED DAY EXTRACTED
SETTING UP INSTRUMENT
1) ON INSTRUMENT PC DOUBLE CLICK INSTRUMENT SOFTWARE IMPORT DATA SELECT YOUR WORKSHEET
AT THE BEGGINING OF EACH RUN PLACE WASHES
2) PLACE IN SAMPLE RACK
3) PRESS START TO BEGIN ANALYSIS
4) AFTER ANALYSIS IS COMPLETE CREATE REPORT SAVE REPORT IN FOLDER ON INSTRUMENT PC DESKTOP MAKE SURE THAT THE CALIBRATION FOR EACH SAMPLE IS WITHIN LIMITS
5) TRANSFER ANALYSIS RESULTS TO AQWINDOWS GO TO DATA ENTRY TO SUBMIT RESULTS
ONE BLANK FOR EVERY 20 SAMPLES OR PART THEREOF
EACH BLANK ASSOCIATED WITH ONE AQC SPIKE
6) CREATE A GRIDSCREEN TO CALCULATE FLUORIDE DRY WEIGHT
CALCULATION OF RESULTS
INSTRUMENT READING PRESENTED AS MG/L F
ADDITIONAL CALCULATION SET UP IN SOFTWARE TO CALCULATE RESULTS TO MG/KG F
((INSTRUMENT READING [MG/L F = PPM] - ASSOCIATED BLANK RESULT [MG/L])X10000)/(DRY WEIGHT [G] X SAMPLE VOLUME = 100 [ML])
ENTER SAMPLE MASS IN TO MASS COLUMN. ENTER BLANK RESULTS FROM THE INSTRUMENT TO BLANK MG/L COLUMN. ENTER RESULTS FOR AQCS.
EDIT GRIDSCREEN SO BLANKS AND AQCS IN THE SAME POSITION AS ANALYSED
CHECK THE BLANK RESULTS ZERO AND TRANSFER YOUR RESULTS
CLEANING AND MAINTENANCE
DAILY
REAGENTS
WEEKLY
APPARATAUS
MONTHLY
ELECTRODE MAINTENANCE
CALCULATION OF RESULTS
ANALYTICAL QUALITY CONTROL
GIVE A DAILY CHECK ON RESULTS AND ALSO TO PRODUCE LONG-TERM STATISTICAL DATA, WHICH CAN BE USED TO ASSESS METHOD PERFORMANCE AND TO AID THE INTERPRETATION OF RESULTS
WITHIN EACH SAMPLE RUN THE FOLLOWING AQC STANDARDS MUST BE ANALYSED
BLANK
BLANK RESULTS PLOTTED ONTO A CONTROL CHART
ONE INVESTIGATION LIMIT
RESULTS ABOVE THIS LIMIT MUST BE INVESTIGATED
ONE BLANK FOR EVERY 20 SAMPLES
EACH BLANK ASSOCIATED WITH 1 AQC SPIKE
IN-HOUSE REFERENCE MATERIAL (AQC-SPIKE)
1 IN 20 AND AT THE END OF THE BATCH
RESULT PLOTTED ON APPROPRIATE CONTROL CHART
NOT CARRIED OUT FOR SLUDGE
FIRST RESULT OUTSIDE +/- 3S, SECOND SUCCESSIVE RESULT OUTSIDE +/- 2S, OR THE 8TH RESULT ON THE SAME SIDE OF THE MEAN INDICATION THAT METHOD OUT OF CONTROL
REJECT ALL THE ASSOCIATED DATA UNLESS IT CAN BE PROVEN THAT ONLY THE AQC HAS BEEN AFFECTED.