HG/T 3696.1-2002 Preparation of standard titration solutions for chemical analysis of inorganic chemical products
Some standard content:
1Cs 71. 060. 01:71. 060. 99
Registration No.: 10941~10943—2002
Chemical Industry Standard of the People's Republic of China
HG/T3696.1-3696.3—2002
Inorganic Chemical Products
Preparation of Standard Titration Solutions, Standard Solutions for Impurities and Preparations and Products for Chemical Analysis
Published on September 28, 2002
Implemented on June 1, 2003
Published by the State Economic and Trade Commission of the People's Republic of ChinaRegistration No.: 10941—2002
HG/T 3696. 1—2002
Cited Standards
3General Provisions
4Preparation and Standardization of Standard Titration Solutions
Sodium Oxychloride Standard Titration Solution
Hydrochloric Acid Standard Titration Solution
Sulfuric Acid Standard Titration Solution
Sodium Carbonate Standard Titration Solution
Potassium Dichromate Standard Titration Solution
Sodium Thiosulfate Standard Titration Solution
Bromide Standard Titration Solution
Potassium Iodide Standard Titration Solution
Oxalic Acid Standard Titration Solution
Potassium Permanganate Standard Titration Solution
Ammonium Ferrous Sulfate Standard Titration Solution
HG/T 3696. 1—2002
Standard titration solution of cerium sulfate (or ammonium cerium sulfate) Standard titration solution of disodium ethylenediaminetetraacetate (EDTA) Standard titration solution of zinc chloride
Standard titration solution of magnesium chloride (or magnesium sulfate) Standard titration solution of lead nitrate
Standard titration solution of copper sulfate
Standard titration solution of silver nitrate
Standard titration solution of sodium chloride
Standard titration solution of sodium thiocyanate (or potassium thiocyanate or ammonium thiocyanate) Standard titration solution of sodium nitrate
Standard titration solution of perchloric acid
Standard titration solution of 4.25% mercuric nitrate Appendix A (Standard Appendix)
Appendix B (Standard Appendix)
Appendix (Suggestive Appendix)
Appendix D (Suggestive Appendix)
Appendix E (Suggestive Appendix)
Temperature compensation limit value of standard titration solution prepared directly with working reference reagent and standard solution concentration
Comparison method of some standard titration solutions
Determination method of potentiometric titration endpoint and data recording example Treatment method of mercury-containing waste liquid
Registration number: 10941--2002
HG/T 3696.1—2002
This standard is formulated based on the non-equivalent use of the American Society for Testing and Materials standard A51ME200--1907 Preparation, calibration of commonly used standard and reagent solutions for chemical analysis and the preparation, calibration and storage of titration solutions in this standard. Compared with ASTM E 200--1997, this standard has the following differences: sodium carbonate, bromine, potassium bromate, potassium iodate, oxalic acid, ammonium ferrous sulfate, zinc chloride, magnesium chloride (or magnesium sulfate), lead nitrate, copper sulfate, sodium chloride, sodium nitrate, mercuric nitrate and other standard titration solutions are added. Appendix A (standard appendix) standard titration solutions prepared directly from working reference reagents are added. - Added Appendix (standard appendix) temperature correction values for different concentrations of standard titration solutions (in LL). - Added Appendix (informative appendix) comparison method of some standard titration solutions. - Added Appendix I (informative appendix) determination method of potentiometric titration integral point and data recording example. - Added Appendix E (informative appendix) treatment method of waste liquid. Appendix A and Appendix B of the standard are standard appendices, and Appendix C, Appendix D and Appendix E are informative appendices. This standard was proposed by the Policy and Regulations Department of the State Administration of Petroleum and Chemical Industry. This standard is under the technical jurisdiction of the Inorganic Chemical Branch of the National Technical Committee on Chemical Standardization. The drafting units of this standard are: Tianjin Chemical Research and Design Institute, Tianjin Entry-Exit Inspection and Quarantine Bureau, Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanle Entry-Exit Inspection and Quarantine Bureau, Hunan Chemical Reagent General Factory, Chongqing Minfeng Agrochemical Co., Ltd. The drafting and completion units of this standard are: Shandong Dacheng Pesticide Co., Ltd. The main drafters of this standard are: Lu Siwei, Liu Zhuocong, Yixing Yuchengmin, Zhang Ping, Zhao Zuliang, Bing Zhaowu, Du Jian. This standard is the first to be issued, and the National Technical Committee on Chemical Standardization Optical, Mechanical and Chemical Branch is responsible for the interpretation of this standard. 3
Chemical Industry Standard of the People's Republic of China
Inorganic Chemical Products
Preparation of Standard Volumetric Solutions for Chemical Analysis
Inorganic Chemical prduets
Preparatinns of standard volumetric solutions: solutions for chemical analysis1Scope
This standard specifies the preparation and calibration methods of standard volumetric solutions for chemical analysis of inorganic chemical products. HG/T 3696.1—2002
This standard is applicable to the preparation of standard volumetric solutions with accurate concentrations, which are used to determine the main content and impurity content of inorganic chemical products by titration, and can also be used for the standards of other chemical products. 2Referenced Standards
The provisions contained in the following standards constitute the provisions of this standard by being cited in this standard. When this standard is revised, the versions shown are valid. All standards will be revised. The parties using this standard shall discuss the possibility of using the latest version of the following standards. G1/T1250-1989 Method of expressing and determining the limit value GB/16682-1992 Specifications and test methods for water used in analytical laboratories (c9JSO3696:1987) JIG/T3696.3----2002 Preparation of preparations and products for chemical analysis of inorganic chemical products 3 General provisions
3.1 The water used in this standard, unless otherwise specified, shall comply with the specifications of grade 3 water in GB/T6682: 3.2 The purity of the reagents used in this standard shall be above analytical purity 3.3 The analytical balance, titration tank, volumetric flask and pipette used in the work shall be calibrated regularly. 3.4 The reference reagent used in the calibration of this standard is the reference reagent for volumetric analysis, and the reagent used in the preparation of standard titration solutions is above analytical purity
3.5 The concentration of the standard titration solution prepared in this standard refers to the concentration at 20°C. During calibration and use, if there is a temperature difference, it should be corrected according to Appendix R of the standard). 3.6 When calibrating the concentration of the standard titration solution, three parallel measurements should be made by two people. The relative difference between the relative value of the parallel measurement results of each person and the average value shall not be greater than 0.2, and the difference between the average values of the two people's measurement results shall not be greater than 0.2. The results are averaged, and the concentration value is taken to four significant figures. 3.7 The relative error between the concentration of the prepared standard titration solution and the specified concentration shall not be greater than 5. 3.8 When preparing a standard titration solution with a concentration equal to or lower than 0.02moi/L, the high-concentration standard titration solution should be diluted with boiled and cooled water before use, and the standard should be recalibrated. 3.9 When the iodine is added, the temperature of the solution should not be too high, and the titration should be carried out between 15-20%. 3.10 The storage time of standard titration solution for chemical product analysis at room temperature (15-25℃) shall not exceed two months. 4 Preparation and calibration of standard titration solution
4.1 Standard titration solution of sodium hydroxide
Approved by the State Economic and Trade Commission of the People's Republic of China on September 28, 2002, and implemented on June 1, 2003
HG/T3696.1—2002
4.1.1 Preparation
Weigh 500g of sodium hydroxide and add it to 500mL of water. Shake the hook and pour it into a polyethylene container. Seal it and place it in a container until the solution becomes clear. Use a plastic tube to siphon the volume of supernatant liquid specified in Table 1 into a polyethylene container, add 100 mL of carbon dioxide-free water, shake the spoon, and prepare the concentration of the standard titration solution containing iron oxide (NaOH) 4.1.2 Calibration 4.1.2.1 Determination method Preparation 1 U00 mL liquid required for testing
Volume of saturated sodium hydroxide solution
Mass pressure of standard potassium hydrogen phthalate required for calibration
Volume of water without carbon dioxide used to dissolve standard potassium hydrogen phthalate
Weigh the amount of standard potassium hydrogen phthalate (accurate to 0.0001g) dried to constant weight at 105-110℃ as specified in Table 1. Add 2 drops of 10R/1.phenol-resistant indicator solution to the specified volume of water without carbon dioxide, and titrate with the prepared sodium hydroxide standard titration solution until the solution turns pink. Perform a blank test at the same time.
4.1.2.2 Calculation
The concentration of sodium hydroxide standard titration solution is calculated according to formula (1): c(NaOH)-
Where: Na0)-\
(V, -V)X 0. 204 2
The concentration of sodium hydroxide standard titration solution: mol/L The volume of sodium hydroxide standard titration solution consumed during titration, TmL The volume of sodium hydroxide standard titration solution consumed during blank test, mI.; Weigh the mass of standard potassium hydrogen phthalate, denoted as 1([)
The mass of potassium hydrogen phthalate in grams equivalent to 1.00mL sodium hydroxide standard titration solution [c(Na0)H)=1.000mol/I.
4.2 Hydrochloric acid standard titration solution
4.2.1 Preparation
Transfer the volume of hydrochloric acid specified in Table 2: inject into 100)ml water and shake the hook. Table 2 HCl to be prepared for standard hydrochloric acid solution 4.2.2 Calibration Volume of hydrochloric acid required to prepare 1 000 ml solution Mass of basic anhydrous sodium carbonate required for calibration 4.2.2.1 Determination method Weigh the amount of standard anhydrous sodium carbonate (accurate to 0.0001) burned to the desired value at 270-300℃ as specified in Table 2, dissolve in 50 ml of water, add 10 drops of green-methyl red mixed indicator solution, and titrate with the prepared hydrochloric acid standard titration solution until the solution changes from green to dark red. Boil for 2 min. Cool and continue titrating until the solution turns dark red again. At the same time, perform a vacuum test. 6
4. 2. 2. 2 Calculation
HG/T 3696. 1—2002
Concentration of hydrochloric acid standard titration solution is calculated using formula (2): (HC) -
(V1--V.)X0.052 99
Wherein: r(HC1) "Concentration of standard hydrochloric acid titration solution.mol/L; V.--Volume of standard hydrochloric acid titration solution consumed during titration, ml..
Volume of standard hydrochloric acid titration solution consumed during a single-room test, mL. Weigh the mass of standard sodium carbonate in water, &; (2)
The mass of anhydrous sodium carbonate in grams equivalent to 1.00ml standard hydrochloric acid titration solution [ct[C1)=1.000mol/1].
4.3 Standard sulfuric acid titration solution
4.3.1 Preparation
Pipette the specified volume of sulfuric acid according to 3, slowly pour it into 1000㎡l. water under constant stirring, cool, and shake the spoon. Table 3
Preparation of standard sulfuric acid titration solution
Concentration Lr(1/2H: S0,))
4.3.2 Calibration
4.3.2.1 Determination method
Prepare 1000ml solution
The volume of sulfuric acid
The mass of standard anhydrous sodium carbonate
Weigh the standard anhydrous sodium carbonate with constant weight at 270～300℃ ignition rate (accurate to 0.0001g) specified in Table 3, dissolve in 50ml water, add 10 drops of green powder·toluene red mixed indicator solution, and titrate with the prepared sulfuric acid standard titration solution until the solution changes from green to dark red. Boil for 2min. After cooling, continue to titrate until the solution turns red again. Perform a blank test in between. 4.3.2.2 The concentration of fresh sulfuric acid standard titration solution is calculated according to formula (3): e(1/2H,S0)=(V.-V)X0. 052 99
where: r(1/2HS0)
Liquidity of sulfuric acid standard titration solution, mol/L: Volume of sulfuric acid standard titration solution consumed during titration, ml: Volume of sulfuric acid standard titration solution consumed during the test, nI. Weigh the mass of standard anhydrous sodium carbonate in g and 1.00mL sulfuric acid standard titration solution [c(1/2HzS0, — 1.000m01/L = the mass of anhydrous sodium carbonate expressed in grams.
4.4 Standard Sodium Carbonate Titration Solution
4.4.1 Preparation
Weigh the amount of anhydrous sodium carbonate specified in Table 4, dissolve it in 1000ml. water, and shake the hook. The concentration of the sodium carbonate standard titration solution to be prepared is _e(L/2Na:CX),)]
4.4.2 Calibration
4. 4. 2. 1. Determination method
HG/T 3696. 1-2002
Concentration of hydrochloric acid standard titration solution required for calibration
Preparation of 10:1 ml. solution
The quality of sodium carbonate solution
The volume of carbon dioxide-free water used to dissolve anhydrous sodium carbonate
Take 30.00~35.00 ml. Prepare a standard sodium carbonate titration solution. Add the volume of water specified in Table 1, add 10 drops of bromocresol and methyl red mixed indicator solution, and titrate with the hydrochloric acid standard titration solution of the current concentration until the solution changes from green to dark red, boil for 2 minutes, cool and continue to titrate until the solution turns dark red again. At the same time, perform a blank test. 4. 4. 2. 2 Calculation
The concentration of sodium carbonate standard titration solution is calculated according to formula (4): c(1/2Ne;CO,)-(VV)e
The concentration of sodium carbonate standard titration solution: mol/L; (1/2Na.C0.)--
.-The actual concentration of hydrochloric acid standard titration shock, ma1/1.V,——The volume of acid standard titration solution consumed during titration, mL The volume of hydrochloric acid standard titration solution consumed during blank test, ml.; VbZxz.net
The volume of sodium carbonate solution transferred for calibration, mL. 4.5 Potassium dichromate standard titration solution
r01/6K,Crz0,)=0.1mol/1
4. 5. 1 Preparation
Weigh 3g potassium dichromate, dissolve it in 1000mL water, and shake the spoon. 4.5.2 Calibration
4.5.2.1 Determination method
Pipette 30.00~35.00mL of prepared potassium diazirate solution [e(1/6K,Cr2(),)-0.1mol/L.-, place in a 500ml iodine rat bottle, add 2g potassium iodide and 20mL of 20% thiol capping solution. Stir well, place in a dark place for 10min, add 150mL water and titrate with sodium thiosulfate standard solution [c(NaS.0,)=0.1mpl/1.j. When near the end point, add 3ml of 5g/I starch indicator solution. Continue titrating until the solution turns from blue to bright green. Perform a blank test at the same time. 4.5.2.2 Calculation The concentration of potassium dichromate standard titration solution is calculated according to formula (5): (V-Ve/(1/6K.Gr0,)-//GK.C)//GK.C ... 12002
Weigh 26g sodium thiosulfate (NaS,..5H0) (or 16g anhydrous sodium thiosulfate), add 0.g standard sodium carbonate, dissolve in 10ml water, slowly boil for 10min, and then filter for use after leaving for two weeks. 4.6.2 Calibration
4.6.2.1 Determination method
Weigh 0.158 (120±5)%℃ dried to constant weight of potassium quaternary ammonium sulfate (accurate to 0.0001g), and place in a 500ml iodine volumetric flask. Add 2g potassium iodide and 20ml 20% sulfuric acid solution to 25ml water. Shake well, place in a dark place for 10min, add 1150ml water, and titrate with the prepared sodium thiosulfate standard titration solution (NaSO4)-0.1mol/1.1. When near the end point, add 3mL 5/L starch indicator solution, and continue titrating until the solution changes from pale green to bright green. At the same time, perform a blank test. 4.6.2.2 Calculation
The concentration of sodium thiosulfate standard titration solution is calculated according to formula (6): c(Na2S20s)=(V2-V2)X0.0490)t
Where: NaS)-
. The concentration of sodium thiosulfate standard titration solution, mol/L: Vi
- The volume of sodium thiosulfate standard titration solution consumed during titration, ml.：V，-the volume of sodium thiosulfate standard titration solution consumed in blank test, ml：-the weight of standard potassium dichromate, denominator + 0. 049 03
4.7 Bromine standard titration solution
The mass of potassium dichromate in grams equivalent to 1.00mL sodium thiosulfate standard titration solution Lc(NaS.0,)=1.000mol/L].
c(1/6KBr,)-0. 1 mol/1.
4.7.1 Preparation
Weigh 3g potassium bromate and 25g potassium bromide, dissolve in 1000mL water, and shake the hook. 4.7.2 Calibration
4.7.2.1 Determination method
Take 30.00~35.00ml of the prepared solution [c (1/6KHr0.) - 0.1mal/L], place it in a 500ml iodine volumetric flask, add 5mL of potassium 2-sulfonate and (20%) hydrochloric acid solution, and add 5 tin. Add 150mL of water: titrate with sodium thiocyanate standard titration solution c (>a5, (),) - 0.1mal/L, add 3mL of 5/L starch indicator solution when near the end point, and continue titrating until the blue color of the solution disappears. At the same time, perform a vacuum test.
4.7.2.2 Calculation
The concentration of bromine standard titration solution is calculated according to formula (7): c(1/6KBrO,)=(VV,)el
Wherein: c(1/6KBrO,）
.Concentration of standard titration solution, mol/I; Actual concentration of sodium thiosulfate standard titration solution, mol/L: Volume of sodium thiosulfate standard titration solution consumed during titration, mL; Volume of sodium thiosulfate standard titration solution consumed during blank test, ml.V-
Volume of the standard solution transferred for calibration, ml:
4.8 Potassium bromate standard titration solution
c(1/6KBrO, -0.1 m1/L
4.8.1 Preparation
HG/T3696.1—2002
Weigh 3g potassium bromate, dissolve in 1000m1. water, shake for about 4.8.2 Calibration
4.8.2.1 Determination method
Pipette 30.00～~35.00ml of prepared potassium bromate solution [c(1/6KBr)-0.1mol/1.] into a 500m1 iodine volumetric flask, add 2g potassium iodide and 5mL of 20% hydrochloric acid solution. Shake well, and place in a dark place for 5min. Add 150ml water, titrate with sodium thiosulfate standard titration solution -c(Na,S,0,)-0.1mol/L", add 3ml of 5g/L starch indicator solution when near the end point, and continue titrating until the blue color of the solution disappears. At the same time, perform a blank test.
4.8.2.2 Calculation
The concentration of potassium bromide standard titration solution is calculated according to formula (8): (Vr-V.)ei
e(1/6KBr0.)=
Formula: (1/6KBr0)
4.9 Iodine standard titration solution
The concentration of potassium bromide standard titration solution, mal/L: The actual concentration of sodium thiosulfate standard titration solution, mal/L; The volume of sodium thiosulfate standard titration solution consumed during titration, mL; The volume of sodium thiosulfate standard titration solution consumed during the empty test, m[.; The volume of potassium thiosulfate sol transferred for calibration, mlc(1/212)=0.1 mol/L
4.9.1 Preparation
Weigh 13g iodine and 35g iodine, dissolve in 100mL water, dilute to 1000nL, shake, store in a brown stoppered bottle, 4.9.2 Calibration
4. 9. 2. 1 Determination method
Weigh 0.15g of standard iodine trioxide (accurate to 0.0001g) that has been dried to constant weight in a sulfuric acid desiccator in advance. Place it in a 250ml iodine volumetric flask and add 1ml sodium hydroxide solution (Na(H2O) = 1mol/L) to dissolve it. Add 50mL water and 2 drops of 10g/L phenol indicator solution. Neutralize with sulfuric acid solution L(1/2HSC,)-1mol/1.1, add 3ml of sodium bicarbonate and 5K/L starch indicator solution 311L, and titrate with the prepared iodine standard titration solution L(1/2I) = (.1mol/L) until the solution turns light blue. Perform a blank test at the same time. 4.9.2.2 Calculation
The concentration of the iodine standard titration solution is calculated according to formula (9):
(1/212)-(VV)×0. D49 46
Wherein: 1/21)—
concentration of iodine standard titration solution, mol/L.; volume of iodine standard titration solution consumed during titration, mLI-:Vvolume of iodine standard titration solution consumed during blank test, mL(9)
Weigh the standard mass of arsenic trioxide·g;
the mass of arsenic trioxide in grams equivalent to 1.00m.read standard titration solution [c(1/21,)=1.000mol/L.70.949 4G-
The mass of one.
4.10 Potassium iodate standard titration solution
4.10.1 Preparation
Weigh the amount of potassium iodate specified in Table 5 and drop it into 1000ml of water. Shake the hook for 10
To prepare the potassium iodate standard titration solution
The liquid concentration is "1/61
4.10.2 Calibration
4.10.2.1 Determination method
HG/T 3696.1
Prepare 1600ml of liquid
The mass of potassium iodate required
The volume of potassium iodate solution required to be transferred
11. 00-- 13. 00
30.00--35.00
Pipette the prepared potassium iodide solution according to the specified volume of length 5 and place it in a 500ml iodine volumetric flask. Add water to about 35mL and 2% hydrochloric acid solution, 5ml, shake well, and place in a dark place for 5 minutes. Add 150 ml of water and titrate with sodium thiosulfate standard titration solution [Va: 5 (,)-0.1mol/l, add 3ml of 5g/1. starch indicator solution when near the end point, continue titrating until the blue color disappears, and do a blank test at the same time.
4.10.2.2 Calculation
The concentration of potassium iodate standard titration solution is calculated according to formula (10): r1/6K0,)-
Where: 1/6KI0)
(V:-V.)el
The concentration of potassium iodate standard titration solution, ol/1.! The actual concentration of sodium thiosulfate standard titration solution.mol/L; The volume of sodium thiosulfate standard titration solution consumed during titration, ml.: The volume of sodium thiosulfate standard titration solution consumed during blank test, mL: The volume of potassium iodate solution transferred for calibration, I1I. 4.11 Oxalic acid standard titration solution
r(1/2cH2O3)-0.1 mol/1.
4.11.1 Preparation
Weigh 6.4 g oxalic acid (CH4)·2Hz0), dissolve in 1000 ml water, shake and 4.11.2 Calibration
4.11.2.1 Determination method
Move 30.00-35.00 ml 1. Prepare the oxalic acid standard titration solution [e(1/2(zH2O3)-0.1m(1/1.7, add 101ml of 8+92 sulfuric acid solution, and titrate with potassium permanganate standard titration solution [(1/5KMn03)-0.1mal/1]. When near the end point, heat to 65°C: continue titrating until the solution turns pink and keep for 30 seconds. Perform a blank test at the same time.4. 11.2.2 Calculation The concentration of the oxalic acid standard titration solution is calculated according to formula (11): c(1/2C H 0)=VV)n
Wu Zhong; c(1/2C:H.0.)-
The concentration of the oxalic acid standard titration solution, mal/L: The actual viscosity of the permanganate standard titration solution, mol/L.: The volume of potassium permanganate standard titration solution consumed during titration, mL: The volume of potassium permanganate standard titration solution consumed during blank test, mL-; The volume of the oxalic acid standard titration solution transferred for calibration, 4. 12
2 Potassium permanganate standard titration solution
r(1/5Kn0,) =(, 1 mol/I
4.12.1 Preparation
HG/T 3696. 1-2002
Weigh 3.3% potassium permanganate, dissolve in 1050 μm water, slowly boil for 1 minute, cool and store in a dark place for two weeks, filter through a filter plate with a pore size of 5~10 μm glass sand into a clean brown bottle. Note: The filter plate used to filter the potassium permanganate solution should have a pore size of 5~10 μm. The sand should be slowly boiled with the same potassium permanganate solution in advance and the collected solution should also be washed twice with potassium permanganate solution. 4. 12. 2 Calibration
4.12.2.1 Determination method
Weigh 0.2% sodium bicarbonate (accurate to 0.0001 mmol) at 105-110°C and dissolve it in 10 ml of 8+92% sulfuric acid solution. Titrate with prepared potassium permanganate standard titration solution (1/5KMn), 0.1 mol/l]. Heat to 65°C when approaching the end point. Continue titrating until the solution turns pink: keep it without fading for 30 minutes, and perform a blank test at the same time. 4.12.2.2 Calculation
The concentration of potassium permanganate standard titration solution is calculated according to formula (12): e(1/5KMnO) - (V,-V)X0. 06700 - the concentration of potassium permanganate standard titration solution, 11ol/L: : <1/5KMnO,) -
V. - the volume of potassium permanganate standard titration solution consumed in titration, ml -; V… - the volume of potassium permanganate standard titration solution consumed in the case test, 1. Weigh the mass of standard sodium oxalate. Name:
(12)
0.0670) - the mass of sodium oxalate in grams equivalent to 1.00ml potassium permanganate standard titration solution c (1/5KMnO): 1.039mol/L7,
4. 13 Ammonium ferrous sulfate standard titration solution
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