Waste Water Analysis WI

Waste Water Analysis WI
KL-3-550-000-W76
Revision Level: 4.0

UNCONTROLLED
1.0 Safety Instructions

PPE are required to be worn by the Lab associate in the laboratory during lab
operation. Refer to SS Analytical Lab Operation WI KL-3-550-000-W61 for the
suitable personal protective equipment (PPE) to be used in the SS Analytical Lab.
2.0 Purpose
This document is to provide a written description on the metal trace, pH, COD, TSS,
Chromium Hexavalent, Sulfate, Chloride, Fluoride and Ammonia Nitrogen analysis
for waste water sample at SS Analytical Lab.
3.0 Scope
This procedure applies to metal trace, pH, COD, TSS, Chromium Hexavalent, Sulfate,
Chloride, Fluoride and Ammonia Nitrogen analysis for waste water sample at SS
Analytical Lab.
4.0 Definitions
o
o
o
o
o
o
o
o
SS
Site Services
UPW
Ultra pure water
COD
Chemical oxygen demand
TSS
Total Suspended Solid
Cd
Cadmium
ICP-OES Inductively Couple Plasma - Optical Emission Spectrometer
WI
Work instruction
TISAB Total Ionic Strength Adjustment Buffer
5.0 Apparatus & Materials

5.1
5.2
5.3
5.4
5.5
5.6
5.7
5.8
5.9
5.10
5.11
5.12
5.13
UPW
Analytical Grade nitric acid 68-70%
pH Electrode Solution
Buffer Solution for pH 4.0
Cd standard solution 1000 mg/L
Multielements standard solution 100 mg/L
COD standard solution 1000 mg/L
COD Digestion Reagent Vials for Low Range (3150mg/L)
COD Digestion Reagent Vials for High Range (201500mg/L)
COD Digestion Reagent Vials for High Range Plus (015000mg/L)
ChromaVer 3 Reagent Powder Pillow
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5.14
5.15
5.16
5.17
5.18
5.19
5.20
5.21
5.22
5.23
5.24
5.25
5.26
5.27
5.28
5.29
5.30
5.31
5.32
5.33
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SulfaVer 4 Reagent Powder Pillow
Mercuric Thiocyanate Solution
Ferric Ion Solution
SPADNS 2 reagent
Nitrogen, Ammonia Standard Solution100 mg/L as NH3-N
Ammonia-free water
AmVer Diluent Reagent Test 'N Tube for High Range Ammonia Nitrogen
Ammonia Salicylate Reagent Powder Pillow
Ammonia Cyanurate Reagent Powder Pillow
500ml volumetric flask
1ml adjustable pipette
Syringe
0.45m syringe filter
15ml high clarity centrifuge tube
Beaker
Square sample cell
Round sample cell
TISAB II solution
6.0 Cadmium Analysis

6.1 Calibration Standards Preparation
6.1.1 Prepare calibration blank, calibration standard Cd 5ppb, calibration
standard Cd 20ppb, calibration standard Cd 60ppb, calibration standard
Cd 120ppb, QC standard Cd 10ppb and QC standard Cd 100ppb with 2%
of nitric acid 68-70%. Refer to Appendix 17.2 for details.
6.2 Sample preparation prior to cadmium analysis with ICP-OES
6.2.1 Pipette 9.80mL of waste water sample (Cd<120ppb) into the 15ml High
Clarity Centrifuge Tube using 10mL adjustable pipette. For Cd level >
120ppb or unknown, dilution is required.
6.2.2 Pipette 0.20mL of nitric acid 68-70% into the 15ml High Clarity
Centrifuge Tube using 1mL adjustable pipette.
6.2.3 Cap the tube and invert the tube for few times.
6.2.4 Leave the samples in the tube for about 5 minutes.
6.2.5 Open the cap and filter the resulted samples using 0.45m filter.
Note: The in-house method is reference to APHA 3030E Method.
6.3 Cadmium analysis with ICP-OES
6.3.1 After sample preparation, analyze the waste water sample using ICPOES. Refer to ICP-OES Start Up Shut Down PM WI KL-3-550-000W109 for ICP-OES operation.
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7.0 Metal Trace Analysis

7.1 Calibration Standards Preparation
7.1.1 Prepare minimum 3 points calibration curve. The calibration range will
depend on the sample concentration. Refer to Appendix 17.3 for
example of calibration standards preparation for metal trace analysis.
7.2 Sample preparation prior to metal trace analysis with ICP-OES
7.2.1 Pipette 9.80mL of waste water sample into the 15ml High Clarity
7.2.2 Pipette 0.20mL of nitric acid 68-70% into the 15ml High Clarity
7.2.3 Cap the tube and invert the tube for few times.
7.2.4 Leave the samples in the tube for about 5 minutes.
7.2.5 Open the cap and filter the resulted samples using 0.45m filter.
Note: The in-house method is reference to APHA 3030E Method.
7.3 Metal trace analysis with ICP-OES
7.3.1 After sample preparation, analyze the waste water sample using ICPOES. Refer to ICP-OES Start Up Shut Down PM WI KL-3-550-000W109 for ICP-OES operation.
8.0 pH Analysis
8.1 Turn on pH meter.
8.2 Wait until AR appears on the Display Screen of the meter.
8.3 Press Calibrate
button prior to calibrate with buffer solution.
8.4 Remove the pH probe from electrode solution and rinse with UPW (ultrapure
water), then wipe with dry and clean tissue.
8.5 Calibrate pH probe with buffer pH4, 7 and 10 (in sequence). Refer to SS Lab
Analytical Instrument WI KL-3-550-000-W62 for pH Calibration Instruction.
8.6 Preparation of waste water sample prior to analysis.
8.6.1 Rinse beaker with UPW and followed with some waste water sample
from bottle that would be analyzed.
8.6.2 Rinse pH probe with UPW, then wiped with dry and clean tissue and
followed by rinsing with some waste water sample that would be
analyzed.
8.6.3 Pour waste water sample that would be analyzed into beaker to level that
can cover the pH probe bulb.
8.7 Immerse the probe inside the waste water sample in the beaker.
8.8 Shake the sample gently and measure the pH with the pH probe in stand.
8.9
8.10
8.11
8.12
Press
to start the measurement.
Wait until pH and AR stops flashing on the Display Screen.
Record pH reading.
For next sample, repeat Step 8.6 to 8.11.
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8.13 QC check with buffer pH7 before every batch of sample analysis is
recommended.
9.0 COD Analysis
9.1 Blank Preparation
9.1.1 For Low Range and High Range COD Digestion, Reagent vials, use
pipette to add 2ml UPW into vials. For High Range Plus COD Digestion,
Reagent vials, pipette 0.2ml into vials.
9.1.2 Close vials cap tightly and invert it gently for a few several time until
solution mix well.
9.1.3 Continue with step 9.3.
9.2 Sample Preparation
9.2.1 Turn on the DRB200 Reactor. Preheat to150 C.
9.2.2 Homogenize the sample if contain larger amount of solids.
9.2.3 Chloride removal
9.2.3.1 Pour about 20ml of sample into a 50ml beaker.
9.2.3.2 Put the magnetic bar into the beaker.
9.2.3.3 Put the beaker on the hotplate and start stirring the sample
without heating.
9.2.3.4 Add a pinch of silver nitrate into the sample till the liquid
becomes clear.
9.2.3.4.1 Photo A indicates that the sample still contains
chloride and the liquid is still cloudy. Need to
continue to add silver nitrate until achieve photo B.
Photo B indicates that the liquid in the mixture has
become clear. When this is observed, proceed to
next step.
9.2.3.5
9.2.3.6
9.2.3.7
9.2.3.8
Prepare conical flask, syringe and syringe filter.

Add a pinch of silver nitrate into the conical flask (to verify if
filtrate still contains chloride).
Filter the sample mixture into the conical flask using syringe
filter.
If the filtrate is free of chloride, the silver nitrate in the conical
flask will dissolve and no white precipitation will be observed.
On the other hand, if the filtrate still contains chloride, white
precipitation is observed.
9.2.3.8.1 Photo below indicates that filtrate is free of chloride.
Silver nitrate fully dissolve and no white
precipitation.
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9.2.3.9
9.2.3.10
9.2.3.11
9.2.3.12
9.2.3.13
If there is trace of chloride, then repeat step 9.2.3.1 to 9.2.3.8

with the filtrate.
If no chloride found in the filtrate, then use clean pipette to add
2.00mL of sample into Low Range/High Range COD
Digestion, Reagent vials. For High Range Plus COD Digestion,
Reagent vials, pipette 0.2mL into vials.
Cap the vials tightly.
Invert it gently for several times.
Continue with step 9.3.
9.3 Put the vials on the reactor and heated it at 150 C for 120 minutes.
9.4 After 2 hours, wait for about 20 minutes for the vials to cool to 120C or less.
9.5 Invert each vial several times while still warm. Place vials into rack and cool to
room temperature. Then proceed to COD Determination.
9.6 COD Determination by HACH Spectrophotometer
9.6.1 Select the appropriate range of test: 430 COD LR or 435 COD HR on
spectrophotometer.
9.6.2 Clean the outside of the vials with a damp towel followed with a dry one.
9.6.3 Insert the blank into the 16 mm Cell Holder.
9.6.4 Press ZERO. The display will show 0.0 mg/L COD.
9.6.5 Insert the sample vial into the 16mm Cell Holder.
9.6.6 Press READ. Results are in mg/L COD.
9.6.7 If using High Range Plus COD Digestion, Reagent Vials, multiply the
result by 10.
9.7 Accuracy Check Standard Solution Method
9.7.1 Check the accuracy of the 3 to 150 mg/L range with a 100 mg/L
standard. Dilute 10 mL of 1000 mg/L COD Standard Solution to 100 mL
to produce a 100 mg/L standard. Use 2 mL as the sample volume. The
result should be 100 mg/L COD.
9.7.2 Check the accuracy of the 20 to 1,500 mg/L range by using either a
300 mg/L or 1000 mg/L COD Standard Solution. Use 2 mL of one of
these solutions as the sample volume; the expected result will be 300 or
1000 mg/L COD respectively.
Note: The method above is reference to HACH Method 8000
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10.0 TSS Analysis

10.1 HACH Method
10.1.1 Blank Preparation
10.1.1.1 Pipette 10ml of UPW into a square sample cell. Remove gas
bubbles in the water by swirling or tapping the bottom of the
cell on a table.
10.1.1.2 Continue with step 10.1.3.
10.1.2 Sample Preparation
10.1.2.1 Stir the sample and immediately pipette 10 mL of the
homogenize sample into a square sample cell. Remove gas
bubbles in the water by swirling or tapping the bottom of the
cell on a table.
10.1.2.2 Continue with step 10.1.3.
10.1.3 TSS Determination by HACH Spectrophotometer
10.1.3.1 Select the test: 630 Suspended Solids on spectrophotometer.
10.1.3.2 Insert the blank into the cell holder with the fill line facing
right.
10.1.3.3 Press ZERO. The display will show: 0 mg/L TSS.
10.1.3.4 Insert the prepared sample into the cell holder with the fill line
facing right.
10.1.3.5 Press READ. Results are in mg/L TSS.
Note: The method above is reference to HACH Method 8006.
10.2 APHA Method
10.2.1 Preparation of filter paper
10.2.1.1 Assemble the glass base on top of the filtrate flask and connect
it to the vacuum pump.
10.2.1.2 Insert the filter paper with wrinkled side up in filter holder
using forceps.
10.2.1.3 Put the glass funnel on top of the filter holder and apply the
clamp to the filtration apparatus.
10.2.1.4 Apply vacuum and wash filter paper with the three successive
20ml portions of UPW.
10.2.1.5 Continue suction to remove all traces of water.
10.2.1.6 Remove filter paper using forceps and transfer to an inert
aluminum weighing dish.
10.2.1.7 Dry the filter paper in the oven at 103-105C for 1 hour.
10.2.1.8 Cool in desiccator to balance the temperature and weigh.
10.2.1.9 Repeat cycle of drying, cooling, desiccating, and weighing until
a constant weight is obtained or until the weight change is less
than 4% of the previous weighing or 0.5mg, whichever is less.
10.2.1.10 Store the filter paper in desiccator until needed.
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10.2.2.1 Assemble filtering apparatus and filter paper from 10.2.1.10
before begin suction.
10.2.2.2 Wet the filter paper with a small volume of UPW to seat it.
10.2.2.3 Stir the sample with a magnetic stirrer at speed to shear larger
particles.
10.2.2.4 While stirring, pipette a measured volume onto the seated filter
paper. Choose a point both mid depth and midway between
wall and vortex.
10.2.2.5 Wash filter paper with three successive 10ml volumes of UPW,
allow complete drainage between washings.
10.2.2.6 Continue suction for about 3 minutes after filtration is
complete.
10.2.2.7 Carefully remove filter paper from filtration apparatus and
transfer to an aluminum weighing dish as a support.
10.2.2.8 Dry for at least 1 hour at 103-105C in an oven, cool in
desiccators to balance temperature and weigh.
10.2.2.9 Repeat cycle of drying, cooling, desiccating, and weighing until
a constant weigh is obtained or until the weight change is less
than 4% of the previous weighing or 0.5mg, whichever is less.
10.2.3 Data reprocessing
10.2.3.1 Calculate the total suspended solid obtained as below:
mg total suspended solid/L =
(A-B) X 1000
Sample volume, mL
Where,
A = weight of filter paper + dried residue, mg
B = weight of filter paper, mg
Note: The method above is reference to APHA 2540D Method.
Remark: APHA method only will be used for TSS analysis upon customer
request or for random sampling only.
11.0 Chromium, Hexavalent Analysis

11.1.1 Pipette 10ml of sample into a square sample cell.
11.1.2 Add the contents of one ChromaVer 3 Reagent Powder Pillow to the
sample cell. Swirl to mix. A purple color will form if hexavalent
chromium is present.
11.1.3 Start the instrument timer. A five-minute reaction period will begin.
11.2.1 Pipette 10ml of UPW into a second square sample cell.
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11.3 Chromium, Hexavalent Determination by HACH Spectrophotometer
11.3.1 Select the test: 90 Chromium, Hex. on spectrophotometer.
11.3.2 When the timer (5 minutes) expires, insert the blank into the cell holder.
11.3.3 ZERO the instrument. The display will show: 0.000 mg/L Cr6+
11.3.4 Insert the prepared sample into the cell holder.
11.3.5 READ the results in mg/L Cr6+.
12.0 Sulfate Analysis

12.1.1 Pipette 10ml of sample into a round sample cell.
12.1.2 Add the contents of one SulfaVer 4 Reagent Powder Pillow to the
sample cell. Swirl vigorously to dissolve the powder. White turbidity
will form if sulfate is present.
12.1.3 Start the instrument timer. A five-minute reaction period will begin. Do
not disturb the cell during this time.
12.2.1 Pipette 10ml of UPW into a second round sample cell.
12.3 Sulfate Determination by HACH Spectrophotometer
12.3.1 Select the test: 680 Sulfate on spectrophotometer.
12.3.2 When the timer (5 minutes) expires, wipe the blank and insert it in the
cell holder (fill lines face right.)
12.3.3 ZERO the instrument. The display will show: 0 mg/L SO42
12.3.4 Within five minutes after the timer expires, wipe the cell and insert the
prepared sample in the cell holder.
12.3.5 READ the results in mg/L SO42.
13.0 Chloride Analysis

13.1 Sample and Blank Preparation
13.1.1 Sample Preparation: Pipette 10ml of sample into a square sample cell.
13.1.2 Blank Preparation: Pipette 10ml of UPW into another square sample cell.
13.1.3 Pipette 0.8 mL of Mercuric Thiocyanate Solution into each sample cell.
13.1.4 Swirl to mix.
13.1.5 Pipette 0.4 mL of Ferric Ion Solution into each sample cell.
13.1.6 Swirl to mix. An orange color will develop if chloride is present.
13.1.7 Start the instrument timer. A two-minute reaction time will begin.
13.1 Chloride Determination by HACH Spectrophotometer
13.2.1 Select the test: 70 Chloride on spectrophotometer.
13.2.2 Within five minutes after the timer expires, wipe the blank sample cell
and insert it into the cell holder with the fill line facing right.
13.2.3 Press ZERO. The display will show: 0.0 mg/L Cl
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13.2.4 Wipe the prepared sample cell and insert it into the cell holder with the
fill line facing right.
13.2.5 Press READ. Results are in mg/L Cl.
14.0 Fluoride Analysis

14.1 ISE Method
14.1.1.1 Pipette 20ml of sample to a clean 50ml beaker.
14.1.1.2 Pipette 20ml of TISAB II solution and add into the sample
beaker.
Note: Ensure there is no cross contamination during pipetting
the sample and TISAB II solution.
14.1.1.3 Sample is ready for analysis.
14.1.2 QC Sample preparation
14.1.2.1 Pipette 40ml of QC standard solution into another 50ml beaker
and proceed to sample analysis. Refer to Appendix 17.4.2 for
example of QC standards preparation for Fluoride analysis.
14.1.3 Sample Analysis
14.1.2.1 Power on the meter. Press the mode button and set the
measurement mode to ISE.
14.1.2.2 Rinse the electrode with UPW and wipe it to dry. Ensure not to
touch the sensing surface at the bottom of the electrode.
14.1.2.3 Perform a QC check using the QC sample solution prepared in
14.1.2.
14.1.2.3.1 Put magnetic bar into the QC sample beaker, place it
on the stirrer and stir the solution thoroughly.
14.1.2.3.2 Place the electrode into the solution and press
measure (esc) to measure the sample and wait for it
to stabilize.
Note: If the QC check failed, prepare a new QC standard
solution as per 17.4.2 and repeat steps 14.1.2.3. If the
subsequent QC check failed, recalibrate the instrument
as per instrument calibration instruction in SS Lab
Analytical Instrument WI KL-3-550-000-W62 and redo
the sample analysis.
14.1.2.4 Remove the electrode from the solution and rinse it with UPW
and wipe it to dry.
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14.1.2.5
14.1.2.6
14.1.2.7
14.1.2.8
14.1.2.9
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Put magnetic bar into the sample beaker prepared in 4.1.1,
place it on the stirrer and stir the solution thoroughly.
Place the electrode into the sample beaker.
Press measure (esc) to measure the sample and wait for it to
stabilize.
Repeat steps 14.1.2.4 to 14.1.2.7 for other samples.
When all samples have been measured, store the electrode
according to electrode storage instruction in SS Lab Analytical
Instrument WI KL-3-550-000-W62.
14.2 HACH method

14.2.1 Sample and Blank Preparation
14.2.1.1 Sample Preparation: Pipette 10ml of sample into a dry square
sample cell.
14.2.1.2 For sample with Fluoride level > 2 mg/L, dilution is required.
14.2.1.3 Blank Preparation: Pipette 10ml of UPW into another dry
square sample cell.
14.2.1.4 Pipette 2.0 mL of SPADNS 2 reagent to each sample cell.
14.2.1.5 Swirl to mix.
14.2.1.6 Start the instrument timer. A 1-minute reaction time starts.
14.2.2 Fluoride Determination by HACH Spectrophotometer
14.2.2.1 Select the test: 190 Fluoride on spectrophotometer.
14.2.2.2 When the timer (1 minute) expires, clean the blank sample cell.
14.2.2.3 Insert the blank into the cell holder.
14.2.2.4 Press ZERO. The display will show 0.00 mg/L F.
14.2.2.5 Clean the prepared sample cell.
14.2.2.6 Insert the prepared sample into the cell holder.
14.2.2.7 Press READ. Results show in mg/L F.
Remark: ISE method is the preferred method for Fluoride analysis. HACH method
only will be used upon customer request or when the ISE electrode is out of
service.
15.0 Ammonia Nitrogen Analysis

15.1 Sample and Blank Preparation
15.1.1 Blank Preparation: Pipette 0.1ml of ammonia-free water into one
AmVer Diluent Reagent Test 'N Tube for High Range Ammonia
Nitrogen.
15.1.2 Sample Preparation: Pipette 0.1ml of sample into another AmVer
Diluent Reagent Test 'N Tube for High Range Ammonia Nitrogen.
15.1.3 Add the contents of one Ammonia Salicylate Reagent Powder Pillow to
each vial.
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15.1.4 Add the contents of one Ammonia Cyanurate Reagent Powder Pillow to
each vial.
15.1.5 Put the caps on both vials. Shake thoroughly to dissolve the powder.
15.1.6 Start the instrument timer. A 20-minute reaction time starts.
15.2 Ammonia Nitrogen Determination by HACH Spectrophotometer

15.2.1 Select the test: 343 N, Ammonia HR TNT on spectrophotometer.
15.2.2 Clean the blank vial.
15.2.3 Insert the blank vial into the cell holder.
15.2.4 Press ZERO. The display will show: 0.0 mg/L NH3N.
15.2.5 Clean the sample vial.
15.2.6 Insert the sample vial into the cell holder.
15.2.7 Press READ. Results show in mg/L NH3N.
16.0 Reference Document

16.1
16.2
16.3
16.4
SS Analytical Lab Operation WI KL-3-550-000-W61

SS Lab Analytical Instrument WI KL-3-550-000-W62
ICP-OES Start Up Shut Down PM WI KL-3-550-000-W109
Standard Methods for the Examination of Water and Wastewater APHA
Handbook
16.5 HACH DR 2800 & DR 3900 Spectrophotometer Procedures Manual
17.0 Appendix
17.1 Sample dilution method
17.1.1 Example Metal Buffer Sample with 250X dilution
17.1.1.1 Fill some UPW into 500mL volumetric flask.
17.1.1.2 Pipette 2.00mL of waste water sample into the 500mL
volumetric flask using 5mL adjustable pipette.
17.1.1.3 Top up the volumetric flask to the mark using UPW.
17.1.1.4 Stopper the volumetric flask and invert the volumetric flask for
few times.
17.2 Example of Standard Solution Preparation for cadmium analysis
Standard
Solution
Standard
Concentration
Stock Standard
Solution
10ppm
Intermediate
Standard
Solution
1ppm
Amount of
Standard Solution
Add 1mL of
1000ppm Standard
Solution
Add 10mL of
10ppm Standard
Solution
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Amount of Acid & UPW

Top up to 100mL with UPW

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120ppb
Add 12mL of
1ppm Standard
Solution
Add 2mL of nitric acid 68-70% and top up

to 100mL with UPW
60ppb
Add 6mL of 1ppm

Standard Solution

to 100mL with UPW
20ppb
Add 2mL of 1ppm

Standard Solution

to 100mL with UPW
5ppb
Add 0.5mL of
1ppm Standard
Solution

to 100mL with UPW
10ppb
Add 1mL of 1ppm

Standard Solution

to 100mL with UPW
100ppb
Add 10mL of
1ppm Standard
Solution

to 100mL with UPW
Calibration
Standard
QC Standard
Note: The standard concentration may vary with different trace metals.
17.3 Example of Standard Solution Preparation for metal trace (multielements)
analysis
Standard
Solution
Standard
Concentration
Stock Standard
Solution
10ppm
Calibration
Standard
Amount of
Multielements
Standard Solution
Add 10mL of
100ppm Standard
Solution
Amount of Acid & UPW
500ppb
Add 5mL of
10ppm Standard
Solution

to 100mL with UPW
200ppb
Add 2mL of
10ppm Standard
Solution

to 100mL with UPW
100ppb
Add 1mL of
10ppm Standard
Solution

to 100mL with UPW
17.4 Example of Standard Solution Preparation for Fluoride Analysis by ISE Method
17.4.1 Calibration Standard Solution Preparation
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Fluoride with TISAB II Standards solution can directly be use as
calibration standard solution. The standards do not require the addition
of TISAB II because TISAB II has already been added.
17.4.2 Quality Control (QC) Standard Solution Preparation

17.4.2.1 Prepare a QC standard solution from 1000ppm Fluoride
Standard solution in any concentration to suit the sample and
calibration range. Refer table below for example of Fluoride
QC standard solution preparation:
Standard
Solution
Fluoride Stock
Standard
Solution
Fluoride QC
Standard
solution
Amount of
Standard
1000ppm Standard
Concentration
Solution
Add 10mL of
100ppm
1000ppm Standard
Solution
Add 2mL of 100ppm
2ppm
Stock Standard
Solution
Amount of UPW
Top up to 100mL
with UPW
Top up to 100mL
with UPW
17.4.2.2 Mix the standard prepared in 17.4.2.1 with TISAB II solution

with a ratio of 1:1. Refer table below for example of Fluoride
QC standard in TISAB II solution preparation:
Standard Solution
Fluoride QC
Standard in TISAB
II solution
Fluoride QC
Standard volume
TISAB II
solution volume
Mixed solution
volume
250ml
250ml
500mL
17.4.2.3 Verify the QC standard prepared with Fluoride with TISAB II

Standards solution.
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1.0 Safety Instructions

5.0 Apparatus & Materials

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