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GENERAL55980
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Last modified
8/24/2016 8:40:55 PM
Creation date
11/23/2007 10:59:45 PM
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Template:
DRMS Permit Index
Permit No
M1988112
IBM Index Class Name
General Documents
Doc Name
STANDARD TEST METHODS FOR CYANIDE IN WATER AUTOMATED METHODS FOR TOTAL CYANIDE & DISSOCIABLE CYANIDE
Media Type
D
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No
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~~f D 4374 <br />- B llcm <br />SELYf xiEO <br />`f LOW AIR <br />~'/ -1-COnxECi OR -~ <br />\VYi-~_ _ <br />2 <m TLS SPXf PICAL JOixi <br />.- <br />I6an ..... .. . ..... ... .. ... . f <br />22 ,m-~j <br />ALUYIYUY BAR <br />N-COx HECTOR <br />-MOON <br />ABSOAPr10N Coo <br />ze ruxxs,2!mm I.L <br />Smm LD. \ <br />nu C <br />O HOPRON iAL TUBE <br />8 vEP11CGl TUBE <br />( WASTE 1PAP <br />o -GROOVE EpR ixlN fILM p15ix LAnON IA1, Smm AAOIUS bem.~mrtm°~1 y mm LD <br />b - HEALNL FLE MENi WELL- 10 me I D ~ IS mm <br />~ - OIAL ixE PYOYErFR WELL <br />FIG. 2 Continuous Thin Film Distillation Unit <br />8.3.4 Ethylene Diamine, and Isooctane, Trichlorotripttoro- <br />ethane, or Hexane. ' <br />8.4 Sodium Hydroxide (NaOH), for preservation and <br />other preparations: <br />8.4.1 Stock Solution, I.0 M dissolve 40 g of NaOH in <br />water and dilute to I L. <br />8.4.2 Working So/tttion, 0.01 M-Dilute 100 mL of the <br />stock solution (8.4.1) to 5 L. This solution is used in the <br />following: (a) absorption of HCN gas, (b) preparation of <br />cyanide standards, and (c) routine cleaning of the system <br />manifold. <br />8.5 Reagents for Standardization: <br />8.5.1 Silver Nitrate Solution, 0.0191 N Standard (I mL = <br />1 mg CN-)-Weigh 3.27 g of AgN03 crystals (oven dried), <br />dissolve in distilled water and dilute to I L. Keep in a dark <br />container. Standardize against standard sodium chloride <br />(NaCI) solution using the argentometric method (9) with <br />potassium chromate (K=Ct0!) indicator. One millilitre of <br />this solution ° I mg CN. <br />8.5.2 Ritodamine Indicator-Dissolve 20 mg oC 5-(p- <br />dimethylaminobenzylidene)rhodanine in L00 mL acetone.- <br />8.6 Simple Cyanide Standards, Potassium Cyanide, KCN: <br />8.6.1 Cyanide, Sock Solution, 1.0 g/L CN (Prepared <br />Fresh Every Month)-ln a 100-mL Oask dissolve 0.251 g of <br />potassium cyanide (KCN) in about 80 mL water. Add 4 to 5 <br />pellets of sodium hydroxide. Shake well to dissolve, then <br />dilute [o the mark. One millilitre of this stock E 1 mg CN-. <br />8.6.2 Standardization oJCyanide Stock Solution (8.6.1)- <br />Once amonth standardize against the primary standard <br />silver nitrate titrant using 10 mL o(KCN stock solution and <br />rhodanine indicator. - <br />8.6.3 Daily Working Standards, 50 and 100 µg/L CN-- <br />108 <br />With a micropipette take a 100-µL of stock solution and <br />dilute to 1000 mL with 0.02 M Na011. This will give a <br />concentration of 100 µg{1. CN. Take anllther 100 µL of the <br />stock solution and dilute to 2000 mL with 0.02 M NaOH to <br />obtain 50 µg/L. <br />8.7 Complex Cyanide Standards-Potassium ferricya- <br />nide, K3Fe (CN)6, or potassium ferrocyanide, K,Fe (CN)6.3 <br />HzO. <br />8.7.1 Preparation of Stock Solution, 1 g/L CN (Prepared <br />Every Week)-Dissolve 0.2109 g of potassium ferricyanide <br />or 0.2706 g of potassium ferrocyanide trihydrate in distilled <br />water. Add about four pellets of NaOH, mix well and dilute <br />to 100 mL. This solution must be ston;d in the dark and <br />preferably in a dark bottle. <br />8.7.2 Daily Working Standards, ]00 pg/L CN-With the <br />micropipette take 100 µL of the stock solution (8.7.1) and <br />dilute to 1000 mL with 0.02 M NaOH. <br />8.8 Acid Digestion Mixture-Prepare: I L of the acid <br />digestion mixture by dissolving 20(1 mL of (85 %) <br />orthophosphoric acid, 40 mL of (50 °S) hypophosphorus <br />acid, and 2 g of sulfamic acid in water. <br />8.9 Reagents jar Color Development: <br />8.9.1 Phosphate Buffer Solution, (0.6 M), (pH - 4.2)- <br />Dissolve 83 g of sodium phosphate monobasic in water, <br />dilute to I L. <br />8.9.2 Chloramine T Solution, 5%D Stack Solution-Care- <br />fully dissolve 5.0 g of chloramine-T it water and adjust <br />volume to 100 mL. Prepare weekly and .;tore in the dark. <br />8.9.2.1 Dai/y Working Solution, 0.4 %-Dilute 20 mL of <br />the stock to 250 mL. <br />8.9.3 Pyridine-Barbituric Acid Color F eagent-Place l5 g <br />of barbituric acid in a I-L flask, add just enough water to <br />LLA55 \\ <br />T-CONNEC70R <br />AESAYPLE~ <br />WASTE TUBE - <br />B Cm LOY4 <br /> <br />FIG, <br />wash t <br />75 mL <br />HCI (s <br />dilute <br />the da <br />9. Saf <br />9.1 <br />exactas <br />produy <br />should <br />escape <br />9.2 I <br />sP~led <br />the ey( <br />call a <br />give in <br />for on <br />(warm <br />9.3 <br />highly <br />dispose <br />10. <br />10.1 <br />Sampl <br />contai <br />10.2 <br />dcesn <br />hydro <br />to a 1 <br />~~ <br />
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