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GB/T 601-2016 English PDF (GBT601-2016)

GB/T 601-2016 English PDF (GBT601-2016)

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GB/T 601-2016: Chemical reagent -- Preparations of reference titration solutions

This 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.
GB/T 601-2016
NATIONAL STANDARD OF THE
PEOPLE 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 Republic of China;
Standardization Administration of the People's Republic of
China.
Table of Contents
Foreword ... 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 ... 71
Foreword
This Standard was drafted in accordance with the rules given in GB/T
1.1-2009.
This Standard replaces GB/T 601-2002 Chemical reagent ?€? Preparations of reference titration solutions. Compared with GB/T 601-2002, the major
technical changes are as follows:
?€? The relevant contents in general provisions 3.2, 3.6, 3.8, 3.9 and 3.10 have been modified (SEE 3.2, 3.6, 3.8, 3.9 and 3.10 of the present
edition; and 3.2, 3.6, 3.8, 3.9 and 3.10 of the 2002 edition);
?€? ?€?The blank test is performed at the same time?€? has been added to the
method 1 of the reference titration solution of sodium carbonate, and
the method 2 (direct preparation with working reference reagent) has
been added (SEE 4.4.1.2 and 4.4.2 of the present edition; and 4.4.2
of the 2002 edition);
?€? The preparation method and calibration method 2 of the reference
titration solution of iodine have been modified (SEE 4.9.1 and 4.9.2.2 of the present edition; and 4.9.1 and 4.9.2.2 of the 2002 edition);
?€? The preparation method of the reference titration solution of sodium
thiosulfate has been modified (SEE 4.6.1 of the present edition; and
4.6.1 of the 2002 edition);
?€? The reference titration solution of sodium oxalate has been added to
oxalic acid side by side, and the method 2 (direct preparation of the
reference titration solution of sodium oxalate with working reference
reagent) has been added (SEE 4.11.1.1 and 4.11.2 of the present
edition; and 4.11 of the 2002 edition);
?€? The method 1 has been added to the reference titration solution of
ammonium ferric sulfate (II), and ?€?the blank test is performed at the
same time?€? has been added to the method 2 (SEE 4.13.3.1 and
4.13.3.2 of the present edition; and 4.13 of the 2002 edition);
?€? The method 2 (direct preparation with working reference reagent) has
been added to the reference titration solution of ethylene diamine
tetraacetic acid, and the effective number of bits of the molar mass of the working reference reagent zinc oxide has been modified (SEE
4.15.1.2.1, 4.15.1.2.2 and 4.15.2 of the present edition; and 4.15.2.1
and 4.15.2.2 of the 2002 edition);
?€? Two concentrations of 0.05mol/L and 0.02mol/L have been added to the
Chemical reagent -
Preparations of reference titration solutions
Warning: Some of the testing procedures specified in this Standard may
result in hazardous conditions and the users are responsible for taking appropriate safety and health measures.
1 Scope
This 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 references
The 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 balance
verified by comparison (SEE Appendix C).
3.7 The relative expansion uncertainty of the concentrations of the
reference titration solutions in this Standard is not greater than 0.2% (k = 2), and the evaluation method is shown in Appendix D.
3.8 This Standard uses the working reference reagent to calibrate the
concentrations of the reference titration solutions. When the accuracy of the concentrations of the reference titration solutions is required to be higher, the standard substance (the expansion uncertainty shall be less than 0.05%) may be used instead of the working reference reagent for calibration or direct preparation, and when calculating the concentrations of the reference titration solutions, its mass fraction is substituted into the calculation formula. 3.9 When the concentration of the reference titration solution is less than or equal to 0.02mol/L (except 0.02mol/L reference titration solutions of ethylene diamine tetraacetic acid and zinc chloride), the reference titration solution with a high concentration shall be diluted with boiling and cooling water (a reference titration solution without non-aqueous solvent) prior to use, and recalibrated if necessary. When it is necessary to use the reference titration solution other than the concentration specified in this Standard, it may be prepared and calibrated by referring to the preparation method of the
corresponding reference titration solution in this Standard.
3.10 Storage:
a) Unless otherwise specified, the sealed storage time of the reference titration solutions at 10??C to 30??C is generally not more than 6 months; the sealed storage time of the reference titration solutions of iodine and sodium nitrite [c(NaNO2) = 0.1mol/L] is 4 months; and the sealed storage time of the reference titration solutions of perchloric acid, potassium hydroxide-ethanol, and ammonium ferric sulfate (III) is 2 months.
Reference titration solutions that exceed the storage time may be used
after recalibration.
b) The storage time of the reference titration solution unsealed and used at 10??C to 30??C is generally not more than 2 months (CLOSE immediately
after pouring out the solution); for the reference titration solutions of iodine and potassium hydroxide-ethanol, it is generally not more than 1 month; for the reference titration solution of sodium nitrite [c(NaNO2) = 0.1mol/L], it is generally not more than 15d; and the reference titration solution of perchloric acid is used on the same day after unsealing.
c) When the standard titration solution shows turbidity, precipitation, color change, etc., it shall be re-prepared.
3.11 The container for storing the reference titration solutions shall not have physical and chemical effects with the solutions, and the thinnest part of the Where:
V1 ?€? Volume of the reference titration solution of sodium thiosulfate, in milliliter (mL);
V2 ?€? Volume of the reference titration solution of sodium thiosulfate consumed by blank test, in milliliter (mL);
c1 ?€? Concentration of the reference titration solution of sodium thiosulfate, in mole per liter (mol/L);
V ?€? Volume of bromine solution, in milliliter (mL).
4.8 Reference titration solution of potassium bromate [c(1/6 KBrO3) =
0.1mol/L]
4.8.1 Preparation
WEIGH 3g of potassium bromate, DISSOLVE it in 1,000mL of water, and
SHAKE well.
4.8.2 Calibration
WEIGH 35.00mL to 40.00mL of prepared potassium bromate solution,
PLACE it in an iodine flask, ADD 2g of potassium iodide and 5mL of
hydrochloric acid solution (20%), SHAKE well, and PLACE it in the dark for 5min. ADD 150mL of water (15??C to 20??C), TITRATE with the reference
titration solution of sodium thiosulfate [c(Na2S2O3) = 0.1mol/L], ADD 2mL of starch indicator solution (10g/L) near the endpoint, and CONTINUE titration until the blue color of the solution disappears. The blank test is performed at the same time.
The concentration of the reference titration solution of potassium bromate [c(1/6 KBrO3)] is calculated according to Formula (10):
Where:
V1 ?€? Volume of the reference titration solution of sodium thiosulfate, in milliliter (mL);
V2 ?€? Volume of the reference titration solution of sodium thiosulfate consumed 300mL of sulfuric acid solution (20%), ADD 700mL of water, and SHAKE well. 4.13.3 Calibration (calibration prior to use)
4.13.3.1 Method 1
WEIGH 0.18g of the working reference reagent, potassium dichromate, dried in an electric oven at 120??C??2??C to a constant-weight, DISSOLVE it in 25mL of water, ADD 10mL of sulfur-phosphorus mixed acid solution, ADD 70mL of water, TITRATE with the prepared ammonium ferric sulfate (II) solution until the orange color disappears, ADD 2 drops of N-phenylanthranilic acid
indicator solution (2g/L), and CONTINUE titration until the solution turns from purple to bright green.
The concentration of the reference titration solution of ammonium ferric sulfate (II) {c[(NH4)2 Fe(SO4)2]} is calculated according to Formula (18): Where:
m ?€? Mass of potassium dichromate, in gram (g);
V ?€? Volume of ammonium ferric sulfate (II) solution, in milliliter (mL); M - Molar mass of potassium dichromate, in gram per mole (g/mol) [M (1/6 K2Cr2O7) = 49.031].
4.13.3.2 Method 2
WEIGH 35.00mL to 40.00mL of prepared ammonium ferric sulfate (II) solution, ADD 25mL of anaerobic water, TITRATE with the reference titration solution of potassium permanganate [c(1/5 KMnO4) = 0.1mol/L] until the solution is pink, and KEEP it for 30s. The blank test is performed at the same time. The concentration of the reference titration solution of ammonium ferric sulfate (II) {c[(NH4)2 Fe(SO4)2]} is calculated according to Formula (19): Where:
V1 ?€? Volume of the reference titration solution of potassium permanganate, in milliliter (mL);
V2 ?€? Volume of the reference titration solution of potassium permanganate consumed by blank test, in milliliter (mL);
m ?€? Mass of zinc oxide, in gram (g);
V1 ?€? Volume of ethylene diamine tetraacetic acid solution, in milliliter (mL); V2 ?€? Volume of the ethylene diamine tetraacetic acid solution consumed by blank test, in milliliter (mL);
M - Molar mass of zinc oxide, in gram per mole (g/mol) [M (ZnO) = 81.408]. 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):
Where:
m ?€? Mass of zinc oxide, in gram (g);
V1 ?€? Volume of zinc oxide solution, in milliliter (mL);
V2 ?€? Volume of ethylene diamine tetraacetic acid solution, in milliliter (mL); V3 ?€? Volume of the ethylene diamine tetraacetic acid solution consumed by blank test, in milliliter (mL);
M - Molar mass of zinc oxide, in gram per mole (g/mol) [M (ZnO) = 81.408]. 4.15.2 Method 2
According to the amount specified in Table 15, WEIGH the working reference reagent, ethylene diamine tetraacetic acid, placed in a humidistat with a Where:
m ?€? Mass of ethylene diamine tetraacetic acid, in gram (g);
V1 ?€? Volume of magnesium chloride (or magnesium sulfate) solution, in
milliliter (mL);
V2 ?€? Volume of the magnesium chloride (or magnesium sulfate) solution
consumed by blank test, in milliliter (mL);
M - Molar mass of ethylene diamine tetraacetic acid, in gram per mole (g/mol) [M (EDTA) = 372.24].
4.18 Reference titration solution of lead nitrate {c[Pb(NO3)2] =
0.05mol/L}
4.18.1 Preparation
WEIGH 17g of lead nitrate, DISSOLVE it in 1,000mL of nitric acid solution (1+2000), and SHAKE well.
4.18.2 Calibration
WEIGH 35.00mL to 40.00mL of prepared lead nitrate solution, ADD 3mL of
acetic acid (glacial acetic acid) and 5g of hexamethylenetetramine, ADD 70mL of water and 2 drops of xylenol orange indicator solution (2g/L), and TITRATE with the reference titration solution of ethylene diamine tetraacetic acid [c(EDTA) = 0.05mol/L] until the solution is bright yellow. The blank test is performed at the same time.
The concentration of the reference titration solution of lead nitrate
{c[Pb(NO3)2]} is calculated according to Formula (27):
Where:
V1 ?€? Volume of the reference titration solution of ethylene diamine tetraacetic acid, in milliliter (mL);
V2 ?€? Volume of the reference titration solution of ethylene diamine tetraacetic acid consumed by blank test, in milliliter (mL);
c1 ?€? Concentration of the reference titration solution of ethylene diamine tetraacetic acid, in mole per liter (mol/L);
Where:
m ?€? Mass of sodium chloride, in gram (g);
V ?€? Volume of sodium chloride solution, in milliliter (mL);
M ?€? Molar mass of sodium chloride, in gram per mole (g/mol) [M (NaCl) = 58.442].
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]
4.20.1 Preparation
WEIGH 8.2g of sodium thiocyanate (or 9.7g of potassium thiocyanate or 7.9g of ammonium thiocyanate), DISSOLVE it in 1,000mL of water, and SHAKE
well.
4.20.2 Calibration
4.20.2.1 Method 1
DETERMINE according to the provisions of GB/T 9725-2007. Wherein:
WEIGH 0.6g of the working reference reagent, silver nitrate, dried in a sulfuric acid desiccator to a constant-weight, DISSOLVE it in 90mL of water, ADD 10mL of starch solution (10g/L) and 10mL of nitric acid solution (25%), USE the 216-type silver electrode as an indicator electrode and the 217-type double salt bridge saturated calomel electrode as a reference electrode, and TITRATE with the sodium thiocyanate (or potassium thiocyanate or
ammonium thiocyanate) solution. CALCULATE V0 according to the provisions of 6.2.2 of GB/T 9725-2007.
The concentration (c) of the reference titration solution of sodium thiocyanate (or potassium thiocyanate or ammonium thiocyanate) is calculated according to Formula (30):
Where:
m ?€? Mass of silver nitrate, in gram (g);
V0 ?€? Volume of sodium thiocyanate (or potassium thiocyanate or ammonium blank test is performed at the same time.
The concentration of the reference titration solution of sodium nitrite [c(NaNO2)] is calculated according to Formula (35):
Where:
m ?€? Mass of p-aminobenzene sulfonic acid, in gram (g);
V1 ?€? Volume of sodium nitrite solution, in milliliter (mL);
V2 ?€? Volume of the sodium nitrite solution consumed by blank test, in milliliter (mL);
M - Molar mass of p-aminobenzene sulfonic acid, in gram per mole (g/mol) {M[C6H4(NH2)(SO3H)] = 173.19}.
4.24 Reference titration solution of perchloric acid [c(HClO4) =
0.1mol/L]
4.24.1 Preparation
4.24.1.1 Method 1
WEIGH 8.7mL of perchloric acid, INJECT 500mL of acetic acid (glacial acetic acid) under stirring, and MIX well. Dropwise ADD 20mL of acetic anhydride, and STIR until the solution is homogeneous. After cooling, USE an acetic acid (glacial acetic acid) to dilute to 1,000mL.
4.24.1.2 Method 2 1
WEIGH 8.7mL of perchloric acid, INJECT 950mL of acetic acid (glacial acetic acid) under stirring, and MIX well. TAKE 5mL, two portions in total. USE pyridine as a solvent, and DETERMINE the mass fraction of water according to the provisions of GB/T 606. CALCULATE the amount of acetic anhydride added in the perchloric acid solution from the average value (w1) of the results of the two parallel deter...

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