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Apparatus:
1. Stoppered volumetric flasks, 50 ml, 250 ml, 500 ml and 1000 ml.
2. Flask, 250 ml, with stopper.
3. Pipettes, 1 ml, 5 ml, 10 ml and 25 ml volumetric and 5 ml graduated.
4. Burettes, 10 ml and 50 ml.
5. Photoelectric colorimeter or spectrometer, (wavelength, 412 nm).
6. Test tubes / Vial, colorimeter tubes or spectrometer tubes.
7. Shaking Water bath, at (40 ± 2) °C.
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56/1 S.M. MALEH ROAD, OSMAN TOWER, NARAYANGANJ
8. Filters, made from heat resistant glass having a pore size between 40 mm and
100 mm (pore symbol P100 in accordance with ISO 4793).
9. Balance, accurate to 0. 2 mg.
Reagents:
Distilled water or grade 3 water complying with ISO 3696.
Formaldehyde solution, appx. 37% or 3, 70,000ppm (W/V or W/W).
Acetylacetone reagent (Nash reagent).
Dissolve 150 g of ammonium acetate in about 800 ml of water; add 3 ml of glacial
acetic acid and 2 ml of acetylacetone, transfer into a 1000 ml volumetric flask and
make up to the mark with water. Store in a brown bottle.
Note: The reagent darkens in color slightly on standing over the first 12 h. For this
reason the reagent should be held 12 h before use. Period of time, at least 6 weeks.
Then take successively 5ml Nash reagent with 0.15 ppm, 0.30 ppm, 1.5 ppm, 3.0
ppm, 6.0 ppm & take six vials, clean it carefully.
Keep the Vial in a water bath at (40 2)°C for (30 5) min and then at ambient
temperature for (30 5) min.
Measure the absorbance in a 10 mm absorption cell at a wavelength of 412 nm
against water.
Then showing the successful calibration, have to be save it. Save procedure is
Click File save settings As new method Save as method OK.
Fill up Reference side & sample side for auto zero, showing -0.041 to -0.043A.
Then successively contact with 0.15 ppm, 0.30 ppm, 1.5 ppm, 3.0 ppm, 6.0 ppm.
*** W/O considered cal. Point & QC point, all points are Spike.
# During sample run, must be prepare 1st & 2nd step solution.
1st step:
1. Sample (1.0g sample with 100ml DW in a CF).
2. Spike (0.75ppm) [take 1ml from 75ppm in a 100ml VF, up to mark 100ml with DW].
3. MB (100ml DW in a CF).
2nd step:
1. QC (1.5ppm) [Take 5ml from 1.5ppm + 5ml NR in a Vial].
2. Spike (Take 5ml soln from op. 2 of step 1 + 5ml NR in a Vial).
3. MB [Take 5ml soln from op. 3 of step 1 + 5ml NR in a Vial].
4. Sample (5ml sample extracted soln from op.1 of step 1 + 5ml NR in a Vial].
5. SB (5ml sample extracted soln from op.1 of step 1 + 5ml DW in a Vial].
Requirements:
JIS L1041 A, B.
For babies in size 98 or below ( 0-3 years); (A-A0) < 0.05 abs
Formaldehyde test by UV-Vis RL: <0.02 (5 mg/kg)
Spectrophotometric Analysis
ISO 14184-1, 2.
For children above 3 years (104-170) ); 75 mg/kg
RL: 16 mg/kg)
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56/1 S.M. MALEH ROAD, OSMAN TOWER, NARAYANGANJ
Where,
SV = sample value in ppm.
SB = sample Blank in ppm.
MB = Method Blank in ppm.
SW = sample weight in gm.
Where,
As= Sample absorbance
Ab= Blank absorbance
MB = Method blank