Lonza Lonza Test Method Effective 16-Nov-1989 Version 3.0 Doc. No USAD-7788 Total Formaldehyde in Glydant Plus (W-153) Page 1 of 5 WORK INSTRUCTION: Total Formaldehyde of Glydant Plus DEFINITION Colorimetric determination of total formaldehyde in Glydant Plus. REAGENTS Formaldehyde 37% (Reagent Grade) Ammonium acetate, reagent grade Acetylacetone (2,4-Pentanedione), reagent grade Glacial acetic acid, reagent grade APPARATU: Visible spectrophotometer 1 cm spectrophotometer cells (Quartz only! Disposable plastic cell will not work.) Volumetric pipettes Volumetric flasks 400 mL glass beakers Analytical balance Hot plate Microsoft Excel Program PROCEDURE Pr q 1. Transfer seventy-five (75) grams of ammonium acetate, 1.5 ml’s of glacial acetic acid and 1.0 ml’s of acetylacetone [2,4-Pentanedione] reagent to a 500 mL volumetric flask. 2. Bring the contents to volume with distilled water and mix well. 100 tock Standard Preparation: 1. Weigh 2.70 grams of 37 % formaldehyde solution into a one (1) liter flask. 2. Dilute to volume with distilled water and mix well. Uncontrolled Copy May not be effective after 17 Jul 2006Lonza Lonza Test Method Effective 16-Nov-1999 Version 3.0 Doc. No USAD-7788 Total Formaldehyde in Glydant Plus (W-153) Page 2 of 5 A. Standards Preparation 1. 100 ppm Working Standard a. Pipette 10.00 mL’s of 1000 ppm stock standard into a 100.00 mL volumetric flask. b. Dilute to volume with distilled water and mix well. 2. 5,10, 20 ppm Colorimetric Standards a. Pipette 5,00 mL’s, 10.00 mL’s, and 20.00 mls of the 100 ppm working standard into separate 100.00 mL volumetric flasks. b. Dilute each to volume with distilled water and mix well. B. Sample Preparation 1. Onan analytical balance weigh 0.5000 - 0.5500 grams of sample into a one (1) liter volumetric flask. 2. Bring to volume with distilled water and mix well. 3. Pipette 10.00 mL’s of sample solution into a 100.00 mL volumetric flask. 4. Dilute to volume with distilled water and mix well. C. Coloration of Standards, Sample(s) and Blank 1. Pipette 10.00 mL’s of each colorimetric standard into separate 25.00 mL. volumetric flasks. 2, Pipette 10.00 mL’s of the sample solution(s) into separate 25.00 mL volumetric flasks. 3. Prepare a reagent blank by pipetting 10.00 mls of distilled water into a separate 25.00 mL volumetric flask. 4, Pipette 10.00 mL’s of acetylacetone reagent into each standard, sample(s) and blank flasks. 5. Immediately place the flasks into a boiling water bath (400 mL beaker) for twenty (20) minutes for color development. Use one (1) 400 mL beaker to hold two (2) flasks max. 6. Cool the flasks in an ice bath for one (1) minute. 7. Dilute the flasks to volume with distilled water and mix well. D. Color Absorbance Readings 1. Tum the spectrophotometer on and allow fifteen (15) minutes to warm up. 2. Set the wavelength to 413 nm. 3. Measure the absorbance of the standards, sample(s) and blank @ 413 against a Uncontrolled Copy May not be effective after 17 Jul 2006Lonza Lonza Test Method Effective 16-Nov-1999 Version 3.0 Doc. No USAD-7788 Total Formaldehyde in Glydant Plus_(W-153) Page 3 of 5 | distilled i water reference. CALCULATIONS 1. Calibration Curve standard: Ac = Ast - Ab Where Ac = corrected absorbance standards absorbance ‘Ab = absorbance of blank a. Ifyou used water as the reference, calculate the corrected absorbance for each “** If the blank was the reference you do not correct the absorbance. b. Use the Microsoft Excel program and login the standard results for 5, 10 and 20 ppm in the appropriate light blue cells. c. Check the calibration curve to see if the numbers are valid. To do this make sure the green cell reads 0.999 mit 2. Sample Results a. If you used water as the reference, calculate the corrected absorbance for each sample: Ac’ = As - Ab Where Ac’ = corrected absorbance As = samples absorbance ‘Ab = absorbance of blank “""* If the blank was the reference you do not correct the absorbance. b, Use the Microsoft Excel program and login the sample result and sample weight in the appropriate yellow cells. c. When all the information has been entered into the program, the total formaldehyde Uncontrolled Copy May not be effective after 17 Jul 2006Lonza Lonza Test Method Effective 16-Nov-1999 Version 3.0 Dos. No USAD-7788 Total Formaldehyde in Glydant Plus (W-153) Page 4 of 5 blue cell. result will appear in the dat METHOD NOTES 1. The following steps are critical for proper color development: a, Begin heating the standards/samples immediately after adding the acetylacetone reagent. 'b. Heating temperatures and times MUST be followed. 2. Read absorbance of standards/samples immediately upon cooling. 3. The amount of color development is dependent on the age of the acetylacetone and 1000 ppm stock standard reagents. Each sol acetylacetone reagent in a refrigerator when not in use. is valid for two (2) weeks MAX! Store the 4. Accuracy can only be obtained if a standard curve is run daily. 5. When this method is rigidly followed the standard calibration curve is linear and very consistent from one day to another. 6. The calculation to convert the formaldehyde concentration from the calibration curve to the formaldehyde concentration in the original sample are based upon the dilution’s listed in this method; if other dilution’s are done, the calculation must be changed. 7. The following number of flasks and pipettes are required to perform a daily calibration curve: a. Four (4) 100.00 mL volumetric flasks with stoppers. b. Four (4) 25.00 mL volumetric flasks with stoppers. ©. Six (6) 10.00 ml pipettes.”* Uncontrolled Copy May not be effective after 17 Jul 2006Lonza Lonza Test Method Effective 16-Nov-1999 Version 3.0 Doc. No USAD-7788 Total Formaldehyde in Glydant Plus (W-153) Page 5 of 5 d. One (1) 20.00 ml pipette. s . One (1) 5.00 mL pipette. 8. The following pieces of glassware are required to perform a sample analysis: a. One (1) 100.00 mL volumetric flask with stopper. b. One (1) 25.00 mL volumetric flask with stopper. ¢. Two (2) 10.00 mL pipettes.* ‘Save and reuse the 10.00 mL pipette for transferring the acetylacetone reagent. 9. Use ONLY the Quartz 1 cm spectrophotometer cells. The disposable plastic cells do not work. Uncontrolled Copy May not be effective after 17 Jul 2008