MACHEREY-NAGEL Special instruction Filvaton. Seinolteto- WessoanaytCrometogephe-Boanay May 2015, Parameter Cyanide Application Determination of Total Cyanide and WAD Cyanide Product group NANOCOLOR ® Remark ‘The term “cyanide” generally refers to one of three classifications of cyanide, which are: (1) total cyanide; (2) weak acid dissociable (WAD) cyanide; and (3) free cyanide, as shown in the following figure. Each of these forms of cyanide has specific analytical methodologies for its measurement, and it is important that the relationship between these forms be understood when analyzing cyanide-containing solutions. As indicated in this figure, for a given solution the total cyanide level is always greater than or equal to the WAD cyanide level, and likewise, the WAD cyanide level is always greater than or equal to the free cyanide concentration, Strong Metal Cyanide Complexes of Fe ‘Weak and Moderately Strong Metal-Cyanide Complexes of Ag, Cd, Cu,Hg, Ni and Zn Free cn Cyanide “| HCN General Classification of Cyanide Compounds ‘An approach to assessing the quality of water samples in many situations is to analyze for WAD cyanide since this includes the toxicologically and environmentally important forms of cyanide, including free cyanide and moderately and weakly complexed metal- cyanides. Total cyanide includes free cyanide, WAD cyanide plus the relatively non-toxic iron-cyanide complexes. Complete characterization of a cyanide solution generally includes analyses for pH, total cyanide, WAD cyanide, thiocyanate, cyanale, ammonia, nitrate and base metals such as copper, iron, nickel and zinc. 'WACHEREY-NAGEL GmbH & Go, KG Naumann NeanderSt ba ea55 Buren Gamany Germany ‘Suzana France: usa Sd mteration! NACHEREVNAGEL AG MACHEREY.NAGEL EURL — NACHEREY.NAGEL Ie Fax S4g2¢2t 900109 Fa “TaN RDGUBSG0S Fax: SaGaN0T P68 Fae $1484 821 1272MACHEREY-NAGEL wane : Fao: Rapid Tests: Water Analysis Chromatogranhy- Bioanalysis Special instruction Fivaton-Scnelest - Wasseranalk- Chromatogr - Boanaljtk Equipment = Three-necked flask, 00 mL. 9x NS 29/82 or 2x NS14,5/23/1 + 1x NS 29082 - Funnel tube, NS 14,5/23, immersion depth: 160 mm - Adapter, NS 14,5/23 to NS 29/32, if neccessary - Liebig condenser, both-sided NS 29/32 and jacket length 300 mm ~ Absorber, NS 29/32 [REF 916 68] = Gas washing bottle, 250 mL = Heating mantle for 500 mL flasks - Stand (complete) [e.g. REF 916 95] = Water suction pump - Glass stopper - Connecting tubes Reagents = Sodium hydroxide p. a, (NaOH) 1 moliL. ~ Zine sulphate heptahydrate p. a. (ZnSO, - 7 H:0) - Cadmium sulphate octahydrate p.a. (CdS, - 8 H,0) Zine powder p. a. (Zn) = EDTA solution p.a. (for example Titriplex® Il from Merck) ~ Potassium hydrogen phthalate p. a. (K"CO-HC:H,CO;) ~ Copperi|l) sulphate pentahydrate p. a. (CuSO, - 10 H20) = Tin(l) chloride p. a. (SnCl) ~ Hydrochloric acid 37% p. a. (HC!) ‘Sample Preparation ‘The apparatus for distillation can be seen at the end of this instruction. ‘Sample Preparation 1. Fill the absorber with 10 mL of NaOH (1 mol/L). for WAD Cyanide Fill he three-necked flask with the solutions listed here: 2.10 mL Zinc-Cadmium sulphate solution (100 g ZnSO, - 7 H,0 and 100 g CdSO, - 8 H,0 in 1 L distilled water) 3. 10 mL EDTA solution (100 g Titriplex® Ill in 940 mL warm distilled water) 4, 50 mL buffer (80 g Potassium hydrogen phthalate in 940 mL warm distilled water) 5. 100 mL of the sample. 6. Adjust pH value with HCl or NaH (both 1 mol/L) to pH 4.0 + 0.1. 7. Adjust a reflux cooler onto the three-necked flask. 8, Add 6.5 mL of HCI 37%, 9, Add 300 mg Zine powder. 10, Adjust the adsorber to the water suction pump and put it onto the three-necked flask. 14, Close the second opening. 12, To the third opening a purification/washing bottle filled with 100 mL of NaOH (1 mol/L) is connected, a glass feed tube leads to the round flask. 13, The air flow should be regulated in a way that the sodium hydroxide solution will not be pressed into the round flask. 14, Running time: 4h, 'WACHEREY-NAGEL GmbH & Go, KG Naumann NeanderSt ba ea55 Buren Gamany Sd mteration! NACHEREVNAGEL AG MACHEREY.NAGEL EURL — NACHEREY.NAGEL Ie Fax S4g2¢2t 900109 Fa “TaN RDGUBSG0S Fax: SaGaN0T P68 Fae $1484 821 1272MACHEREY-NAGEL Filtration : Rapid Tests: Water Analysis : Chromatography « Bioanalysis Special instruction Fivaton-Scnelest - Wasseranaltk- Chemalogiaphe - Boanalytk 415. Mter4h the residue is disconnected with care from the absorber, so that no NaOH can get info the ask 16, Fill the content of the absorber into a volumetric flask (100 mL) and adjust the pH to 6-7 with hydrochloric acid (1 moU/L). Fill up the volumetric flask to 100 mL using distilled water (aqua dest.). 17, Analysis 20 mL of this solution are used for test 1-30 NANOCOLOR® Cyanide, 4 mL for test NANOCOLOR® Cyanide 08 0-31 and 10 mL for test VISOCOLOR® ECO Cyanide. Measurement result = WAD Cyanide mg/L. 1. Fill the absorber with 10 mL of NaOH (1 mol/L) ‘Sample Preparation Fill the three-necked flask with the solutions listed here: for Total Cyanide 2. 40 mL of distilled water (aqua dest) 3, 10 mL of copper sulphate solution (200 g CuSO, : 5 HzO in 1 L of distilled water) 4, 2 mL of tin(ti)-chloride solution (fil 50 g of SnCI, -2 HO and 25 mL. of HCI 37% into a 100 mL volumetric flask and fil up with distilled water after dissolution) 100 mL of the sample Add 6,5 mL. of HCI 37%, ‘Adjust the adsorbtion flask to a water-operated vacuum pump and put it onto the cooler. 9. Close the second opening. 5. 6, Adjust a reflux cooler onto the round flask, 7, 8 10, To the third opening a purification/washing bottle filled with 100 mL of NaOH (1 mol/L) is connected, a glass feed tube leads to the round flask 14, The air flow should be regulated in a way that the sodium hydroxide solution will not be pressed into the round flask, 12, The mixture is boiled under reflux for 1 h. 13, After 1 h the residue is disconnected with care from the absorbtion flask, so that no NaOH can get into the flask. 14, Fillthe content of the absorber into a volumetric flask (100 mL) and adjust the pH to 6-7 with hydrochloric acid (1 mol/L) Fill up the volumetric flask to 100 mL using distiled water (aqua dest). 45, Analysis, 20 mL of this solution are used for test 1-30 NANOCOLOR® Gyanide, 4 ml. for test NANOCOLOR® Cyanide 08 0-31 and 10 mL for test VISOCOLOR® ECO Cyanide. Measurement result = Total Cyanide mg/L 'WACHEREY-NAGEL GmbH & Go, KG Naumann NeanderSt ba ea55 Buren Gamany Sd mteration! NACHEREVNAGEL AG MACHEREY.NAGEL EURL — NACHEREY.NAGEL Ie Fax S4g2¢2t 900109 Fa “TaN RDGUBSG0S Fax: SaGaN0T P68 Fae $1484 821 1272