Potassium Permanganate Titration Developed in 1957 by AATCC Commit- cartridge and full facepiece should be 7.3.2 Boil the solution for 15 min and tee RA34; reaffirmed 1962, 1968, 1972, readily available for emergency use. cool. 1975, 1979, 2002; editorially revised 4.4 Exposure to chemicals used in this 7.3.3 Filter the solution through a filter (with title change) 1983; editorially re- procedure must be controlled at or below funnel (see 5.1) into a 1 L volumetric vised and reaffirmed 1985, 1992; re- levels set by governmental authorities flask. Dilute to the mark with water. vised 1987 (with title change), 1997. (e.g., Occupational Safety and Health 7.3.4 Store solutions of potassium per- Administration’s [OSHA] permissible manganate in brown bottles or otherwise exposure limits [PEL] as found in 29 protect the solutions from light. CFR 1910.1000 of January 1, 1989). In 7.4 Standardization of 0.588N potas- 1. Purpose and Scope addition, the American Conference of sium permanganate solution. Make three 1.1 This test method determines the Governmental Industrial Hygienists determinations as follows. concentration of hydrogen peroxide (ACGIH) Threshold Limit Values (TLVs) comprised of time weighted averages 7.4.1 Pipette 100 mL 0.100N sodium (H2O2) in aqueous solutions, particularly oxalate solution into a 250 mL Erlen- (TLV-TWA), short term exposure limits those used in textile bleaching. meyer flask and add 10 ± 1 mL 20% sul- (TLV-STEL) and ceiling limits (TLV-C) are recommended as a general guide for furic acid. 2. Principle air contaminant exposure which should 7.4.2 Heat to boiling. Remove from be met (see 11.1). heat and immediately titrate with the po- 2.1 A specimen is acidified with sulfu- tassium permanganate solution being ric acid and titrated with standardized po- standardized, adding the titrant drop by tassium permanganate solution. The con- 5. Apparatus drop at the beginning and at the end of centration of hydrogen peroxide is 5.1 Filter funnel, fritted glass, fine po- the titration. The end-point is a faint but calculated using the volume and normal- rosity, 250 mL. permanent pink color. ity of the permanganate solution used. 5.2 Filtration flask, 2000 mL. 7.4.3 Calculate the normality of the po- tassium permanganate solution to the near- est 0.001 using the following equation: 3. Terminology 6. Reagents Nk = (Vo)(No)/(Vk) 3.1 bleaching, n.—elimination of un- 6.1 Sodium oxalate (Na2C2O4), crys- wanted coloring matter from a textile tals, CP. where: substrate by oxidative or reductive chem- 6.2 Sulfuric acid (H2SO4), 95-98%. Vo = volume of the sodium oxalate ical treatment. 6.3 Potassium permanganate (KMnO4), solution used, in mL crystals. No = normality of the sodium oxalate 4. Safety Precautions solution NOTE: These safety precautions are 7. Preparation of Reagents Vk = volume of the potassium per- for information purposes only. The safety manganate solution used, in mL 7.1 Standard 0.100N sodium oxalate precautions are ancillary to the testing solution. 7.4.4 Average the three normality values procedures and are not intended to be all 7.1.1 Dry at least 7 g sodium oxalate in and use that average for all calculations. inclusive. It is the user’s responsibility to an oven at 105 ± 1°C for 4 h and cool in a use safe and proper techniques in han- desiccator. dling materials in this test method. Manu- 7.1.2 Weigh 6.7000 ± 0.0002 g sodium 8. Procedure facturers MUST be consulted for specific oxalate (see 7.1.1) and dissolve in 250- details such as material safety data sheets 300 mL distilled or deionized water at 70 8.1 Weigh 10 ± 0.1 g of the aqueous and other manufacturer’s recommenda- ± 10°C. hydrogen peroxide specimen into a tions. All OSHA standards and rules 7.1.3 Cool and quantitatively transfer 250 mL flask (see 11.3). must also be consulted and followed. to a 1 L volumetric flask and cover. Al- 8.2 Add 20 ± 1 mL 20% sulfuric acid 4.1 Good laboratory practices should low to stand at least 12 h, then dilute to to the flask (see 7.2). Gently mix by be followed. Wear safety glasses in all the mark with distilled or deionized swirling or stirring. laboratory areas. water. 8.3 Titrate the solution with standard- 4.2 All chemicals should be handled 7.2 Sulfuric acid, approximately 20% ized potassium permanganate solution with care. Sodium oxalate, potassium by volume (see Section 4 for safety pre- (see 7.3 and 7.4) to a faint pink color permanganate and sulfuric acid are corro- cautions). which lasts at least 30 s. Record the vol- sive. When preparing the dilute solutions 7.2.1 Slowly add 200 mL 95-98% sul- ume of titrant in milliliters as Vt. from pure or concentrated reagents, use furic acid to 800 mL water with stirring. 8.3.1 If less than 2 mL of titrant are chemical goggles or face shield, impervi- Cool to 20 ± 2°C. used, repeat the procedure using either a ous gloves, and an impervious apron. 7.2.2 Add water to 1 L. standardized potassium permanganate so- CAUTION: Always add acid to water. 7.3 Potassium permanganate solution lution of known lower normality or a 4.3 An eyewash/safety shower should 0.588N (see 11.2). larger specimen. be located nearby and a high efficiency 7.3.1 Weigh 18.6 ± 0.1 g potassium 8.4 Titrate a blank, and record the mL particulate respirator with organic vapor permanganate and add it to 900 mL water. titrant required as Vb.