Calibration Procedure Formaldehyde.docx

RUSSEL GARMENTS 56/1 S.M. MALEH ROAD, OSMAN TOWER, NARAYANGANJ

PREPARATION OF STD. SOLUTION & CALIBRATION PROCEDURE - At 1st, UPS line ON Computer UPS ON Formaldehyde m.c ON Double click perkin Elmer software Select Analyst Ok Click W/L Quant Idle mode if M.c connected / not Initializing Click data collection Add 412 /415 then Response 2. - Accessory: No work. - Connection: No work. - Sample Info. : 5 then click Enter Click format sample table Click column select (Sample ID, Description, Type, Analyte, Concentration, Ordinate) Ok. -Type Standard-1: 0.15ppm Standard-2: 0.30ppm Standard-3: 1.50ppm Standard-4: 3.0ppm Standard-5: 6.0ppm. - Beer`s law: components name- formaldehyde standard. -Force through zero option-Click it. - Type of curve: Linear. - Unit: ppm. - R2 (Correlation) = 0.995 - Start click OK. [Correlation co-efficient (R2) value good 0.995-1.0] Note: 1st, sample side & 2nd, Reference/Blank side. 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.

RUSSEL GARMENTS 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.  Preparation of formaldehyde stock solution 1500 mg/l: 3.8 ml of formaldehyde solution (37%) dilute to one litre with water in a 1L VF. Record the accurate concentration of this standardized stock solution. This stock solution will keep for up to four weeks and is used to prepare standard dilutions.  Preparation of formaldehyde standard solution 75 mg/l: Take 5ml formaldehyde stock solution from 1500ppm in a 100ml volumetric flask, upto mark 100ml with DW. 1500 ppm (S2 ) 75ppm (S1 ) Here, S1 = 1500ppm, S2 = 75ppm, Total volumeV2= 100ml, V1 =? V1S1= V2S2; So, V1 = V2S2 / S1 = 100 x 75 / 1500 = 5ml.  At 1st, take five VF of 100ml & clean it carefully. Mark it level on VF successively with 0.15 ppm, 0.30 ppm, 1.5 ppm, 3.0 ppm, 6.0 ppm.

RUSSEL GARMENTS 56/1 S.M. MALEH ROAD, OSMAN TOWER, NARAYANGANJ

1. Preparation of formaldehyde standard solution 1.5 mg/l: Take 2ml formaldehyde standard solution from 75ppm in a 100ml volumetric flask, upto mark 100ml with DW. 75 ppm 1.5 ppm S1 S2 Here, S1 = 75ppm, S2 = 1.5 ppm, Total volumeV2= 100ml, V1 =? V1S1= V2S2; So, V1 = V2S2 / S1 = 100 x 1.5 / 75 = 2ml.

2. Preparation of formaldehyde standard solution 0.3 mg/l: Take 20ml formaldehyde standard solution from 1.5 ppm in a 100ml volumetric flask, upto mark 100ml with DW. 1.5 ppm 0.3 ppm S1 S2 Here, S1 = 1.5ppm, S2 = 0.3 ppm, Total volumeV2= 100ml, V1 =? V1S1= V2S2; So, V1 = V2S2 / S1 = 100 x 0.3 / 1.5 = 20 ml.

3. Preparation of formaldehyde standard solution 0.15 mg/l: Take 10ml formaldehyde standard solution from 1.5 ppm in a 100ml volumetric flask, upto mark 100ml with DW. 1.5 ppm 0.15 ppm S1 S2 Here, S1 = 1.5ppm, V1S1= V2S2

S2 = 0.15 ppm, Total volumeV2= 100ml, V1 =? So, V1 = V2S2 / S1 = 100 x 0.15 / 1.5 = 10 ml.

4. Preparation of formaldehyde standard solution 6.0 mg/l: Take 8.0 ml formaldehyde standard solution from 75 ppm in a 100ml volumetric flask, upto mark 100ml with DW. 75 ppm 6.0 ppm S1 S2 Here, S1 = 75 ppm, S2 = 6.0 ppm, Total volumeV2= 100ml, V1 =? V1S1= V2S2 So, V1 = V2S2 / S1 = 100 x 6.0 / 75 = 8.0 ml.

5. Preparation of formaldehyde standard solution 3.0 mg/l: Take 50 ml formaldehyde standard solution from 6.0 ppm in a 100ml volumetric flask, upto mark 100ml with DW. 6.0 ppm - S1 3.0 ppm – S2 Here, S1 = 6.0 ppm, S2 = 3.0 ppm, Total volumeV2= 100ml, V1 =? V1S1= V2S2 So, V1 = V2S2 / S1 = 100 x 3.0 / 6.0 = 50 ml.

RUSSEL GARMENTS 56/1 S.M. MALEH ROAD, OSMAN TOWER, NARAYANGANJ

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. RB: Take 5ml Nash reagent & 5 ml DW in a vial. 1. Take 5ml solution from standard 0.15 ppm & 5ml NR in a Vial. 2. Take 5ml solution from standard 0.30 ppm & 5ml NR in a Vial. 3. Take 5ml solution from standard 1.5 ppm & 5ml NR in a Vial. 4. Take 5ml solution from standard 3.0 ppm & 5ml NR in a Vial. 5. Take 5ml solution from standard 6.0 ppm & 5ml NR in a Vial. 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. Now we have to sample test against under this calibration.

RUSSEL GARMENTS 56/1 S.M. MALEH ROAD, OSMAN TOWER, NARAYANGANJ

Standard Formaldehyde Conc. & abs: Standard Std-1 Std-2 Std-3 Std-4 Std-5 Std-6 Std-7 Std-8

Conc. (ppm) 0.15 0.30 0.75 1.50 2.25 3.0 4.5 6.0

Abs 0.02 0.041 0.100 0.200 0.300 0.400 0.600 0.800

Range ( abs ± 0.03) -0.01 to 0.05 0.011 to 0.071 0.07 to 0.13 0.17 to 0.23 0.27 to 0.33 0.37 to 0.43 0.57 to 0.63 0.77 to 0.83

Reagent Blank (RB): During calibration, auto zero is done by 5ml DW + 5ml NR in a Vial. Keep it in WB 400C x 30`. Take it at D/Z for 20`, comedown RT. 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. # How to make QC (1.5ppm)? Take 2ml formaldehyde standard solution from 75ppm in a 100ml volumetric flask, up to mark 100ml with DW. 75 ppm 2ml 1.5 ppm S1 S2 Here, S1 = 75ppm, S2 = 1.5 ppm, Total volumeV2= 100ml, V1 =? V1S1= V2S2; So, V1 = V2S2 / S1 = 100 x 1.5 / 75 = 2ml. Take 5ml from 1.5ppm + 5ml NR in a Vial. Keep it in WB 400C x 30`. Take it at D/Z for 20`, comedown RT. *QC point is catched as to middle point.

RUSSEL GARMENTS 56/1 S.M. MALEH ROAD, OSMAN TOWER, NARAYANGANJ

# How to make Spike (0.75ppm)? 75 ppm 1ml 0.75 ppm S1 S2 Here, S1 = 75ppm, S2 = 0.75 ppm, Total volumeV2= 100ml, V1 =? V1S1= V2S2; So, V1 = V2S2 / S1 = 100 x 0.75 / 75 = 1ml. Take 1ml formaldehyde standard solution from 75ppm in a 100ml volumetric flask, up to mark 100ml with DW. Keep it in WB 400C x 1h. Take it at D/Z for 20`, comedown RT. Take 5ml soln from 0.75ppm + 5ml NR in a Vial. Keep it in WB at 400C x 30`. Take it at D/Z for 20`, comedown RT. *** W/O considered cal. Point & QC point, all points are Spike. Denotes as sample, such as 0.75ppm, 2.25ppm, 4.5ppm. # How to make MB? 100ml DW in a C/F. Keep it in WB 400C x 1h. Take it at D/Z for 20`, comedown RT. Take 5ml water soln + 5ml NR in a Vial. Keep it in WB 400C x 30`. Take it at D/Z for 20`, comedown RT. # How to make sample Blank (SB)? Take 5ml sample extracted soln + 5ml DW in a Vial. Keep it in WB 400C x 30`. Take it at D/Z for 20`, comedown RT.

RUSSEL GARMENTS 56/1 S.M. MALEH ROAD, OSMAN TOWER, NARAYANGANJ

# 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). Keep those in WB 400C x 1h, with 30-40rpm. Take those at D/Z for 20`, comedown RT.

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]. Keep those in WB at 400C x 30min Take those at D/Z for 20`, comedown RT. Then measure. # How to do sample run against calibration? At 1st, when sample run then auto zero is done by only water. Fill up Reference side & sample side for auto zero, showing -0.034 to -0.039A. Then successively contact with 1. QC 2. Spike 3. MB

4. Sample

5. SB

Requirements: Formaldehyde test by UV-Vis Spectrophotometric Analysis

JIS L1041 A, B. For babies in size 98 or below ( 0-3 years); RL: <0.02 (5 mg/kg) ISO 14184-1, 2. For children above 3 years (104-170) ); RL: 16 mg/kg)

(A-A0) < 0.05 abs

75 mg/kg

RUSSEL GARMENTS 56/1 S.M. MALEH ROAD, OSMAN TOWER, NARAYANGANJ

Calculations of ISO method We know that, Formaldehyde content (F) in ppm = {(SV – SB) – MB} x 100 / SW. Where, SV = sample value in ppm. SB = sample Blank in ppm. MB = Method Blank in ppm. SW = sample weight in gm. Given from data, SV = 0.4967 ppm SB = 0.0357 ppm MB= 0.1026 ppm SW = 1.0 g F = {(0.4967- 0.0357) – 0.1026} x 100 / 1.0. = 36 ppm.

Calculations of JIS method We know that, Corrected Absorbance (A) = = (As – Ab) – MB. Where, As= Sample absorbance Ab= Blank absorbance MB = Method blank Given from data, As= 0.08 abs Ab= 0.0045 abs MB = 0.015 abs A = (0.08 – 0.0045) – 0.015. = 0.07 abs.