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GB/T 601-2016: Chemical reagent - Preparations of reference titration solutions Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedure Status: Valid GB/T 601: Historical versions
GB/T 601-2016: Chemical reagent - Preparations of reference titration solutions---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/GBT601-2016NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 71.040.40; 71.040.30 G 60 Replacing GB/T 601-2002 Chemical reagent - Preparations of reference titration solutions Issued on. OCTOBER 13, 2016 Implemented on. MAY 1, 2017 Issued by. General Administration of Quality Supervision, Inspection and Quarantine of the People’s Republic of China; Standardization Administration of the People's Republic of China. Table of ContentsForeword... 5 1 Scope... 8 2 Normative references... 8 3 General rules... 9 4 Preparation and calibration of reference titration solutions... 11 4.1 Reference titration solution of sodium hydroxide... 11 4.2 Reference titration solution of hydrochloric acid... 12 4.3 Reference titration solution of sulfuric acid... 13 4.4 Reference titration solution of sodium carbonate... 14 4.5 Reference titration solution of potassium dichromate [c(1/6 K2Cr2O7) = 0.1mol/L]... 16 4.6 Reference titration solution of sodium thiosulfate [c(Na2S2O3) = 0.1mol/L] ... 17 4.7 Reference titration solution of bromine [c(1/2 Br2) = 0.1mol/L]... 18 4.8 Reference titration solution of potassium bromate [c(1/6 KBrO3) = 0.1mol/L]... 19 4.9 Reference titration solution of iodine [c(1/2 I2) = 0.1mol/L]... 20 4.10 Reference titration solution of potassium iodate... 21 4.11 Reference titration solution of oxalic acid (or sodium oxalate) [c(1/2 H2C2O4) = 0.1mol/L or c(1/2 Na2C2O4) = 0.1mol/L]... 23 4.12 Reference titration solution of potassium permanganate [c(1/5 KMnO4) = 0.1mol/L]... 24 4.13 Reference titration solution of ammonium ferric sulfate (II) {c[(NH4)2 Fe(SO4)2] = 0.1mol/L}... 25 4.14 Reference titration solution of cerous sulfate (or ammonium cerous sulfate) {c[Ce(SO4)2] = 0.1mol/L or c[2(NH4)2 SO4 · Ce(SO4)2] = 0.1mol/L}... 27 4.15 Reference titration solution of ethylene diamine tetraacetic acid... 28 4.16 Reference titration solution of zinc chloride... 30 4.17 Reference titration solution of magnesium chloride (or magnesium sulfate) [c(MgCl2) = 0.1mol/L or c(MgSO4) = 0.1mol/L]... 32 4.18 Reference titration solution of lead nitrate {c[Pb(NO3)2] = 0.05mol/L}. 33 4.19 Reference titration solution of sodium chloride [c(NaCl) = 0.1mol/L]... 34 4.20 Reference titration solution of sodium thiocyanate (or potassium thiocyanate, ammonium thiocyanate) [c(NaSCN) = 0.1mol/L, c(KSCN) = 0.1mol/L, c(NH4SCN) = 0.1mol/L]... 35 4.21 Reference titration solution of silver nitrate [c(AgNO3) = 0.1mol/L]... 36 4.22 Reference titration solution of mercury nitrate... 37 4.23 Reference titration solution of sodium nitrite... 38 4.24 Reference titration solution of perchloric acid [c(HClO4) = 0.1mol/L]... 41 4.25 Reference titration solution of potassium hydroxide-ethanol [c(KOH) = 0.1mol/L]... 43 4.26 Reference titration solution of hydrochloric acid-ethanol [c(HCl) = 0.5mol/L]... 44 4.27 Reference titration solution of ammonium ferric sulfate (III) {c[NH4Fe(SO4)2] = 0.1mol/L}... 45 Appendix A (Normative) Correction value of the reference titration solution volume at different temperatures... 47 Appendix B (Normative) Method for determining burette capacity... 49 Appendix C (Informative) Comparison of some reference titration solutions. 51 Appendix D (Informative) Assessment on expansion uncertainty of reference titration solution concentrations... 60 Appendix E (Informative) Method for processing mercury-containing waste liquid... 70 Appendix F (Informative) Assessment on expansion uncertainty of the glass gauge capacity... 711 ScopeThis Standard specifies the preparation and calibration methods of the reference titration solutions of chemical reagents. This Standard applies to the preparation and calibration of the reference titration solutions for determining the purity and impurity content of chemical reagents by titration. Other fields are also available.2 Normative referencesThe following documents are essential for the application of this document. For dated references, only the dated editions apply to this document. For undated references, the latest editions (including all amendments) apply to this document. GB/T 603 Chemical reagent – Preparations of reagent solutions for use in test methods GB/T 606 Chemical reagent – General method for the determination of water (Karl Fischer method) GB/T 6379.6-2009 Accuracy (trueness and precision) of measurement methods and results – Part 6.Use in practice of accuracy values GB/T 6682 Water for analytical laboratory use – Specification and test methods GB/T 9725-2007 Chemical reagent – General rule for potentiometric titration JJG 130 Liquid-in-glass thermometers for working JJG 196-2006 Working glass container JJG 1036 Electronic balance3 General rules3.1 Unless otherwise specified, the grade of reagents used in this Standard shall be above AR (including AR). The preparations and products used shall be prepared in accordance with the provisions of GB/T 603.The experimental water shall meet the specifications of the Grade III water in GB/T 6682. 3.2 All the concentrations of the reference titration solutions prepared according to this Standard, except the reference titration solution of perchloric acid, the reference titration solution of hydrochloric acid-ethanol, and the reference titration solution of sodium nitrite, refer to the concentrations at 20°C. 3.3 When calibrating and using reference titration solutions, the titration rate shall generally be maintained at 6mL/min to 8mL/min. 3.4 When the mass of the working reference reagent is less than or equal to 0.5g, it is weighed accurately to 0.01mg; when it is greater than 0.5g, it is weighed accurately to 0.1mg. 3.5 The concentrations for preparing the reference titration solutions shall be within ± 5% of the specified concentration.4 Preparation and calibration of reference titrationsolutions 4.1 Reference titration solution of sodium hydroxide 4.1.1 Preparation WEIGH 110g of sodium hydroxide, DISSOLVE it in 100mL of carbon dioxide-free water, SHAKE well, INJECT it into a polyethylene container, and SEAL it until the solution is clear. According to the amount specified in Table 1, USE a plastic tube to weigh the supernatant, DILUTE to 1,000mL with carbon 4.1.2 Calibration According to the amount specified in Table 2, WEIGH the working reference reagent, potassium hydrogen phthalate, dried in an electric oven at 105°C to 110°C to a constant-weight, ADD carbon dioxide-free water to dissolve, ADD 2 drops of phenolphthalein indicator solution (10g/L), TITRATE with the prepared sodium hydroxide solution until the solution is pink, and HOLD for 30s. The blank test is performed at the same time. 4.2.2 Calibration According to the amount specified in Table 4, WEIGH the working reference reagent, anhydrous sodium carbonate, that has been burnt in a high-temperature furnace at 270°C to 300°C to a constant-weight, DISSOLVE it in 50mL of water, ADD 10 drops of bromocresol green-methyl red indicator solution, and TITRATE with the prepared hydrochloric acid solution until the solution turns from green to dark red, BOIL for 2min, COVER the rubber stopper of the soda lime tube, COOL and CONTINUE titration until the solution becomes dark red again. The blank test is performed at the same time. 4.3 Reference titration solution of sulfuric acid 4.3.1 Preparation According to the amount specified in Table 5, WEIGH the sulfuric acid, INJECT it into 1,000mL of water slowly, COOL and SHAKE well. 4.3.2 Calibration According to the amount specified in Table 6, WEIGH the working reference reagent, anhydrous sodium carbonate, that has been burnt in a high-temperature furnace at 270°C to 300°C to a constant-weight, DISSOLVE it in 50mL of water, ADD 10 drops of bromocresol green-methyl red indicator solution, and TITRATE with the prepared sulfuric acid solution until the solution turns from green to dark red, BOIL for 2min, COVER the rubber stopper of the soda lime tube, COOL and CONTINUE titration until the solution becomes dark red again. The blank test is performed at the same time. 4.4 Reference titration solution of sodium carbonate 4.4.1 Method 1 4.6 Reference titration solution of sodium thiosulfate [c(Na2S2O3) = 0.1mol/L] 4.7 Reference titration solution of bromine [c(1/2 Br2) = 0.1mol/L] 4.7.1 Preparation WEIGH 3g of potassium bromate and 25g of potassium bromide, DISSOLVE it in 1,000mL of water, and SHAKE well. 4.10 Reference titration solution of potassium iodate 4.10.1 Method 1 4.10.1.1 Preparation According to the amount specified in Table 10, WEIGH the potassium iodate, DISSOLVE it into 1,000mL of water, and SHAKE well. 4.12.2 Calibration WEIGH 0.25g of the working reference reagent, sodium oxalate, dried in an electric oven at 105°C to 110°C to a constant-weight, DISSOLVE it in 100mL of sulfuric acid solution (8+92), TITRATE with the prepared potassium permanganate solution, HEAT to about 65°C near the endpoint, CONTINUE titration until the solution is pink, and KEEP it for 30s. The blank test is performed at the same time. 4.14.1 Preparation WEIGH 40g of cerium sulfate tetrahydrate (or 67g of ammonium cerous sulfate), ADD 30mL of water and 28mL of sulfuric acid, ADD another 300mL of water, HEAT to dissolve, ADD another 650mL of water, and SHAKE well. 4.14.2 Calibration WEIGH 0.25g of the working reference reagent, sodium oxalate, dried in an electric oven at 105°C to 110°C to a constant-weight, DISSOLVE it in 75mL of water, ADD 4mL of sulfuric acid solution (20%) and 10mL of hydrochloric acid, HEAT to 65°C to 70°C, and TITRATE with the prepared cerous sulfate (or ammonium cerous sulfate) solution until the solution is pale yellow. 4.15 Reference titration solution of ethylene diamine tetraacetic acid 4.15.1 Method 1 4.15.1.1 Preparation According to the amount specified in Table 13, WEIGH the ethylene diamine tetraacetic acid, ADD 1,000mL of water, HEAT to dissolve, COOL, and SHAKE well. 4.15.1.2 Calibration 4.15.1.2.1 Reference titration solution of ethylene diamine tetraacetic acid [c(EDTA) = 0.1mol/L, c(EDTA) = 0.05mol/L] According to the amount specified in Table 14, WEIGH the working reference reagent, zinc oxide, that has been burnt in a high-temperature furnace at 800°C±50°C to a constant-weight, WET with a small amount of water, ADD 2mL of hydrochloric acid solution (20%) to dissolve, ADD 100mL of water, USE an ammonia solution (10%) to adjust the pH of the solution to 7 to 8, ADD 10mL of ammonia-ammonium chloride buffer solution A (pH ≈ 10) and 5 drops of chrome black T indicator solution (5g/L), and TITRATE with the prepared ethylene diamine tetraacetic acid solution until the solution turns from purple to pure blue. The blank test is performed at the same time. 4.15.1.2.2 Reference titration solution of ethylene diamine tetraacetic acid [c(EDTA) = 0.02mol/L] WEIGH 0.42g of the working reference reagent, zinc oxide, that has been burnt in a high-temperature furnace at 800°C±50°C to a constant-weight, WET with a small amount of water, ADD 3mL of hydrochloric acid solution (20%) to dissolve, PIPETTE into a 250mL volumetric flask, DILUTE to the scale, and SHAKE well. TAKE 35.00mL to 40.00mL, ADD 70mL of water, USE an ammonia solution (10%) to adjust the pH of the solution to 7 to 8, ADD 10mL of ammonia-ammonium chloride buffer solution A (pH ≈ 10) and 5 drops of chrome black T indicator solution (5g/L), and TITRATE with the prepared ethylene diamine tetraacetic acid solution until the solution turns from purple to pure blue. The blank test is performed at the same time. The concentration of the reference titration solution of ethylene diamine tetraacetic acid [c(EDTA)] is calculated according to Formula (22). 4.22.2 Calibration According to the amount specified in Table 20, WEIGH the working reference reagent, sodium chloride, that has been burnt in a high-temperature furnace at 500°C to 600°C to a constant-weight, DISSOLVE it in 100mL of water, and ADD 3 to 4 drops of bromophenol blue indicator solution. If the solution is bluish violet, dropwise ADD a nitric acid solution (8+92) until the solution turns yellow, then ADD excessive 5 to 6 drops. 4.26.2 Calibration (calibration prior to use) 4.26.2.1 Method 1 WEIGH 0.95g of the working reference reagent, anhydrous sodium carbonate, that has been burnt in a high-temperature furnace at 270°C to 300°C to a constant-weight, DISSOLVE it in 50mL of water, ADD 10 drops of bromocresol green-methyl red indicator solution, and TITRATE with the prepared hydrochloric acid-ethanol solution until the solution turns from green to dark red, BOIL for 2min, COVER the rubber stopper of the soda lime tube, COOL and CONTINUE titration until the solution becomes dark red again. 4.27.2 Calibration WEIGH 35.00mL to 40.00mL of prepared ammonium ferric sulfate (III) solution. ADD 10mL of hydrochloric acid solution (1+1). HEAT to near boiling. Dropwise ADD a stannous chloride solution (400g/L) until the solution is colorless. ADD excessive 1 to 2 drops, COOL, ADD 10mL of saturated solution of mercury chloride, and SHAKE well. LET it stand for 2min to 3min. ADD 10mL of sulfur-phosphorous mixed acid solution (SEE 4.13.1.1). DILUTE to 100mL. ADD 1mL of sodium diphenylamine sulfonate indicator solution (5g/L). TITRATE with the reference titration solution of potassium dichromate [c(1/6 K2Cr2O7) = 0.1mol/L] until the solution is purple, and KEEP it for 30s. The blank test is performed at the same time. (COLLECT the waste liquid, and SEE Appendix E for the treatment method.) The concentration of the reference titration solution of ammonium ferric ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. 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