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GB/T 3050-2000: Inorganic chemical products for industrial use. General method for determination of chloride content. Potentiometric method Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedure GB/T 3050: Historical versions
Similar standardsGB/T 3050-2000: Inorganic chemical products for industrial use. General method for determination of chloride content. Potentiometric method---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT3050-2000 GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 71.040.40 G 10 neq ISO 6227:1982 Inorganic chemical products for industrial use - General method for determination of chloride content - Potentiometric method ISSUED ON: JULY 31, 2000 IMPLEMENTED ON: MARCH 01, 2001 Issued by: State Bureau of Quality Technical Supervision Table of ContentsForeword ... 3 1 Scope ... 5 2 Normative reference ... 5 3 Method summary ... 5 4 Reagents and materials ... 6 5 Instruments and equipment... 8 6 Analytical procedures ... 8 7 Expression of analysis results ... 9 Appendix A (Normative) Preparation method of silver-silver sulfide electrode10 Appendix B (Normative) Selection of standard solution and electrode type ... 11 Appendix C (Normative) Example of test record format ... 12 Appendix D (Informative) Interference in the determination ... 13 Appendix E (Informative) Elimination method of ions interfering with determination ... 14 Inorganic chemical products for industrial use - General method for determination of chloride content - Potentiometric method1 ScopeThis standard specifies the general method for the determination of chloride content in inorganic chemical products - Potentiometric titration. This standard applies to test solutions, which have a chloride ion content of 1 mg/L ~ 1500 mg/L. The chloride (calculated as Cl) content in the test solution, which is used for titration, is 0.01 mg ~ 75 mg. When the concentration of the silver nitrate standard solution used is less than 0.02 mol/L, the titration shall be carried out in an ethanol-water solution. does not interfere with the determination. The ions that form insoluble precipitates or complexes with Ag+, as well as , etc. interfere with the determination. For the limit and elimination method, please refer to Appendix D (informative) and Appendix E (informative).2 Normative referenceThe provisions contained in the following standards constitute the provisions of this standard through quotation in this standard. When this standard is published, the versions shown are valid. All standards will be revised. All parties using this standard shall explore the possibility of using the latest version of the following standards. GB/T 603-1988 Chemical reagent - Preparations of reagent solutions for use in test methods GB/T 6682-1992 Water for laboratory use - Specifications (neq ISO 3696:1987)3 Method summaryIn acidic water or ethanol-water solution, use silver (silver-silver sulfide) electrode as the measuring electrode [see Appendix B (normative) for the selection of electrode types]; use calomel electrode as the reference electrode; use silver nitrate standard titration solution for titration. The end point of the reaction is determined by means of a potential jump.4 Reagents and materialsThe reagents and water, which are used in this standard, refer to analytical reagents and the grade 3 water, which are specified in GB/T 6682, unless otherwise specified. The preparations and products, which are used in this standard, shall be prepared in accordance with the provisions of GB/T 603, unless otherwise specified. 4.1 95% ethanol. 4.2 Saturated potassium nitrate solution. 4.3 Sodium hydroxide solution: 200 g/L. 4.4 Nitric acid solution 2 + 3. 4.5 Potassium chloride standard solution: c (KCl) = 0.1 mol/L. Accurately weigh 3.728 g of the reference potassium chloride (accurate to 0.001 g), which was previously baked at 130 °C to a constant weight. Place it in a beaker. After adding water to dissolve, transfer it into a 500 mL volumetric flask. Use water to dilute it to the mark. Shake well. Potassium chloride standard titration solution of 0.01 mol/L, 0.005 mol/L, 0.001 mol/L or other concentration: Accurately dilute the 0.1 mol/L potassium chloride standard titration solution to the required multiple. 4.6 Silver nitrate standard titration solution: c (AgNO3) = 0.1 mol/L. Silver nitrate standard titration solution of 0.01 mol/L, 0.005 mol/L, 0.001 mol/L or other concentrations: Accurately dilute the 0.1 mol/L silver nitrate standard titration solution to the required multiple. Calibration: Use a pipette to take 5 mL or 10 mL of the potassium chloride standard solution of the selected concentration. Place it in a 50 mL beaker. Add 1 drop of bromophenol blue indicator solution. Add 1 ~ 2 drops of nitric acid solution, to make the solution just yellow. Then add 15 mL or 30 mL of ethanol. Put in the electromagnetic stirrer. Place the beaker on the electromagnetic stirrer. Start the stirrer. Insert the measuring electrode and the reference electrode into the Where: c0 - The concentration of the potassium chloride standard solution taken, mol/L; V2 - The volume of the potassium chloride standard solution taken, mL. 4.7 Bromophenol blue indicator solution: 0.1% ethanol solution.5 Instruments and equipment5.1 Potentiometer: The accuracy is 2 mV/div. The range is -500 mV ~ +500 mV. 5.2 Reference electrode: Double-liquid junction type saturated calomel electrode, filled with saturated potassium chloride solution. During titration, the outer tube is filled with saturated potassium nitrate solution AND is connected to the calomel electrode. 5.3 Measuring electrode: Silver electrode or 0.5 mm silver wire (with 99.9% silver content; use shielded wire when connecting with potentiometer) When the concentration of the silver nitrate standard solution used is lower than 0.005 mol/L, it shall use a silver electrode with a silver sulfide coating. The preparation method is detailed in Appendix A (normative) 5.4 Micro burette: The graduation value is 0.02 mL or 0.01 mL.6 Analytical procedures6.1 Preparation of test solution Weigh an appropriate amount of the specimen. Treat it with an appropriate method. OR otherwise pipette an appropriate amount of the test solution after chemical treatment [to make the interference ion not greater than the specified limit, see Appendix D (informative)]. Place it in a beaker. Add 1 drop of Bromophenol blue indicator solution. Use sodium hydroxide solution or nitric acid solution to adjust the color of the solution just yellow. Transfer it to a volumetric flask of appropriate size. Add water to the mark. Shake well. This test solution is solution A. The concentration of chloride ions is 1 mg/L ~ 1.5 x 103 mg/L. 6.2 TitrationAppendix E(Informative) Elimination method of ions interfering with determination This Appendix cannot include the elimination methods of all interfering substances. It shall check the possible interference frequently. The processing methods described in E1 to E5 cannot cover all situations. E1 Iodine and bromine In addition to fluorine, iodine and bromine will react with silver nitrate, while titrating chlorine, which will interfere with the determination. The elimination method is to first use oxidant (such as hydrogen peroxide) to make oxidization, in a dilute nitric acid medium; then use an appropriate solvent to extract it. E2 Oxidant In an acidic solution, and etc., can oxidize Cl- to Cl2, which interferes with the determination. The elimination method is to control the pH of the tested solution, to make titration at pH 5 ~ 6. reacts with chlorine AND interferes with the determination. The elimination method is to slowly add an appropriate amount of 30%H2O2-1 mol/L HNO3 mixed solution (1 + 10) in the test solution, to make fade. The oxidant can oxidize the silver electrode. Use sodium sulfite, ascorbic acid solution or other reducing agents, that do not affect the measurement, to destroy the oxidant. E3 Nitrite and Ag+ generate AgNO2 precipitation. The elimination method of interference is to drop 10% sulfamic acid solution into the test solution; then heat and boil it, after there is no air bubble. E4 Cyanide, thiocyanate, sulfide, thiosulfate, sulfite, etc. The anions in these salts form insoluble precipitates with Ag+, which interfere with the determination. The elimination method is to slowly add an appropriate amount of 30% hydrogen peroxide solution in an alkaline medium; slowly heat it; finally boil until it, until there is no small bubble. E5 Ammonium salt and iron (III) salt ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. 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