HG/T 3696.1-2011 PDF in English
HG/T 3696.1-2011 (HG/T3696.1-2011, HGT 3696.1-2011, HGT3696.1-2011)
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Inorganic chemicals for industrical use. Preparations of standard and reagent solutions for chemical analysis. Part 1: Preparations of standard volumetric solutions
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HG/T 3696.1-2011: PDF in English (HGT 3696.1-2011) HG/T 3696.1-2011
CHEMICAL INDUSTRY STANDARD OF
THE PEOPLE’S REPUBLIC OF CHINA
ICS 71.060.01;71.060.99
G 10
Filing No.: 34581-2012
Replacing HG/T 3696.1-2002
Inorganic chemicals for industrial use - Preparation of
standard and reagent solutions for chemical analysis - Part
1: Preparations of standard volumetric solutions
ISSUED ON: DECEMBER 20, 2011
IMPLEMENTED ON: JULY 01, 2012
Issued by: Ministry of Industry and Information Technology of PRC
Table of Contents
Foreword ... 4
1 Scope ... 6
2 Normative references ... 6
3 General provisions ... 6
4 Warning ... 7
5 Preparation and calibration of standard titration solution ... 8
5.1 Sodium hydroxide standard titration solution ... 8
5.2 Hydrochloric acid standard titration solution ... 9
5.3 Sulfuric acid standard titration solution ... 10
5.4 Sodium carbonate standard titration solution ... 11
5.5 Potassium dichromate standard titration solution [c(1/6 K2Cr2) ≈ 0.1 mol/L] ... 12
5.6 Sodium thiosulfate standard titration solution [c(Na2S2O3) ≈ 0.1 mol/L] ... 14
5.7 Bromine standard titration solution [c(1/2Br2) ≈ 0.1 mol/L] ... 15
5.8 Potassium bromate standard titration solution [c(1/6KBrO3) ≈ 0.1 mol/L] ... 16
5.9 Iodine standard titration solution [c(1/2I2) ≈ 0.1 mol/L] ... 17
5.10 Potassium carbonate standard titration solution ... 19
5.11 Oxalic acid standard titration solution [c(1/2C2H2O4) ≈ 0.1 mol/L] ... 21
5.12 Potassium permanganate standard titration solution [c(1/5KMnO4) ≈ 0.1 mol/L]
... 22
5.13 Ammonium ferrous sulfate standard titration solution {c[(NH4)2Fe(SO4)2] ≈ 0.1
mol/L} ... 23
5.14 Cerium sulfate (or cerium ammonium sulfate) standard titration solution {c[Ce(SO4)2]
≈ 0.1 mol/L, c[2(NH4)2(SO4) • Ce(SO4)2] ≈ 0.1 mol/L} ... 24
5.15 Disodium ethylenediaminetetraacetate (EDTA) standard titration solution ... 26
5.16 Zinc chloride standard titration solution [c(ZnCl2) ≈ 0.1 mol/L] ... 28
5.17 Magnesium chloride (or magnesium sulfate) standard titration solution [c(MgCl2) ≈
0.1 mol/L, c(MgSO4) ≈ 0.1 mol/L] ... 29
5.18 Lead nitrate standard titration solution {c[Pb(NO3)2] ≈ 0.05 mol/L} ... 30
5.19 Copper sulfate standard titration solution [c(CuSO4) ≈ 0.1 mol/L] ... 31
5.20 Silver nitrate standard titration solution [c(AgNO3) ≈ 0.1 mol/L] ... 32
5.21 Sodium chloride standard titration solution [c(NaCl) ≈ 0.1 mol/L] ... 33
5.22 Sodium thiocyanate (or potassium thiocyanate or ammonium thiocyanate) standard
titration solution [c(NaSCN) ≈ 0.1 mol/L, c(KSCN) ≈ 0.1 mol/L, c(NH4SCN) ≈ 0.1
mol/L] ... 34
5.23 Sodium nitrite standard titration solution ... 36
5.24 Perchloric acid standard titration solution [c(HCIO4) ≈ 0.1 mol/L] ... 38
5.25 Mercury nitrate standard titration solution {c[1/2Hg(NO3)2] ≈ 0.1 mol/L} ... 39
5.26 Sodium oxalate standard titration solution ... 40
Appendix A (Normative) Corrected value of volume of standard titration solution at
different temperatures ... 42
Appendix B (Informative) Determination of potentiometric titration end point and
example of data recording ... 43
Appendix C (Informative) Treatment method of mercury-containing waste liquid ... 45
Inorganic chemicals for industrial use - Preparation of
standard and reagent solutions for chemical analysis - Part
1: Preparations of standard volumetric solutions
1 Scope
This Part specifies the preparation and calibration methods of the main standard titration
solutions, which are used by the volumetric method, for chemical analysis of inorganic
chemical products.
This Part is applicable to the preparation of standard titration solutions of accurate
concentration for volumetric determination of the main content and impurity content of
inorganic chemical products. It can also be used for chemical analysis of other chemical
products.
2 Normative references
The following documents are essential to the application of this document. For the dated
documents, only the versions with the dates indicated are applicable to this document;
for the undated documents, only the latest version (including all the amendments) is
applicable to this standard.
GB/T 6682-2008 Water for analytical laboratory use - Specification and test
methods
GB/T 8170 Rules of rounding off for numerical values & expression and judgement
of limiting values
HG/T 3696.3-2011 Inorganic chemicals for industrial use - Preparations of standard
and reagent solutions for chemical analysis - Part 3: Preparations of reagent
solutions
3 General provisions
3.1 The water used in this Part, unless other requirements are specified, shall meet the
specifications of grade-3 water in GB/T 6682-2008.
3.2 The reference reagents, which are used in the calibration in this Part, are the
reference reagents for volumetric analysis; the other reagents used are all reagents of
analytical grade or above.
3.3 Analytical balances, weights, burettes, volumetric flasks, single-marked pipettes,
which are used in work, need to be calibrated regularly.
3.4 The concentration of the standard titration solution, which is prepared in this Part,
except for perchloric acid, refers to the concentration at 20 °C. During calibration and
use, if there is a difference in temperature, it shall be corrected, according to Appendix
A.
3.5 When calibrating the concentration of the standard titration solution, two people
shall do three parallels at the same time. The ratio -- of the range of the three parallel
measurement data for each person TO the average value -- shall not be greater than
0.2%; the ratio -- of the difference between the measurement results of two persons TO
the average value of the measurement results of the two persons -- shall not be greater
than 0.2%. The results are averaged; the concentration value takes four significant
figures.
3.6 The concentration value of the prepared standard titration solution shall be within
±5% of the specified concentration value.
3.7 When preparing a standard titration solution, which has a concentration equal to or
lower than 0.02 mol/L, it shall use water, which was boiled and cooled, to make volume
of the standard titration solution, which has high concentration, to the mark, before use;
AND dilute it. If necessary, re-calibrate it.
3.8 The standard titration solution, which is specified in this Part, shall generally not be
stored for more than two months at room temperature (unless otherwise specified). The
standard titration solution, which is stored more than two months, shall be re-calibrated;
it shall be re-prepared, when the solution appears turbid, precipitated, changes in color.
3.9 During the iodometric reaction, the temperature of the solution shall not be too high;
the titration shall generally be carried out, between 15 °C and 20 °C.
3.10 During calibration or titration, the titration speed shall generally be maintained at
6 mL/min ~ 8 mL/min.
4 Warning
Some of the reagents, which are used in the preparation method of this Part, are
toxic or corrosive, so be careful when handling! If splashed on the skin, rinse
immediately with water; in severe cases, seek medical attention immediately.
5.8.2.1 Determination method
Accurately add 30.00 mL ~ 35.00 mL of prepared potassium bromate standard titration
solution [c(1/6KBrO3) ≈ 0.1 mol/L]. Put it in a 500 mL iodine flask. Add 2 g of
potassium iodide and 5 mL of hydrochloric acid solution (20%). Use water to seal it.
Shake well. Place it in a dark place for 5 min. Quickly add 150 mL of water. Use sodium
thiosulfate standard titration solution [c(Na2S2O3) ≈ 0.1 mol/L]. Add 3 mL of starch
indicator solution (5 g/L), when approaching the end point. Continue to titrate until the
blue color of the solution disappears. At the same time, carry out a blank test.
5.8.2.2 Result calculation
The concentration of potassium bromate standard titration solution [c(1/6KBrO3)] is
expressed in moles per liter (mol/L), which is calculated according to formula (10):
Where:
c1 - The exact value of the concentration of the standard titration solution of sodium
thiosulfate, in moles per liter (mol/L);
V1 - The value of the volume of the standard titration solution of sodium thiosulfate,
which is consumed during titration, in milliliters (mL);
V2 - The value of the volume of the standard titration solution of sodium thiosulfate,
which is consumed by the blank test, in milliliters (mL);
V - The value of the volume of potassium bromate standard titration solution, which
is accurately added during calibration, in milliliters (mL).
5.9 Iodine standard titration solution [c(1/2I2) ≈ 0.1 mol/L]
5.9.1 Preparation
Weigh 13 g of iodine and 35 g of potassium carbonate. Dissolve it in 100 mL of water.
Use water to dilute it to 1000 mL. Shake well. Store it in a brown stoppered bottle.
5.9.2 Calibration
5.9.2.1 Method 1
5.9.2.1.1 Determination method
Weigh 0.15 g of benchmark arsenic trioxide, which was pre-dried in a sulfuric acid
desiccator to a constant mass, accurate to 0.0001 g. Put it in a 250 mL iodine volumetric
flask. Add 4 mL of sodium hydroxide solution [c(NaOH) ≈ 1 mol/L] to dissolve it. Add
50 mL of water. Add 2 drops of phenolphthalein indicator solution (10 g/L). Use sulfuric
acid solution [c(1/2H2SO4) ≈ 1 mol/L] to neutralize it. Add 3 g of sodium bicarbonate
and 3 mL of starch indicator solution (5 g/L). Use the prepared iodine standard titration
solution [c(1/2I2) ≈ 0.1 mol/L] to titrate it, until the solution is light blue. At the same
time, carry out a blank test.
5.9.2.1.2 Result calculation
The concentration of iodine standard titration solution [c(1/2I2)] is expressed in moles
per liter (mol/L), which is calculated according to formula (11):
Where:
V1 - The value of the volume of iodine standard titration solution, which is consumed
during titration, in milliliters (mL);
V2 - The value of the volume of the iodine standard titration solution, which is
consumed by the blank test, in milliliters (mL);
m - The mass of the weighed benchmark arsenic trioxide, in grams (g);
M - The value of the molar mass of arsenic trioxide (1/4As2O3), in grams per mole
(g/mol) (M = 49.46).
5.9.2.2 Method 2
5.9.2.2.1 Determination method
Accurately add 30.00 mL ~ 35.00 mL of sodium thiosulfate standard titration solution
[c(Na2S2O3) ≈ 0.1 mol/L]. Place it in a 500 mL iodine volumetric flask. Add 150 mL of
water. Use the prepared carbon standard titration solution [c(1/2I2) ≈ 0.1 mol/L] to
titrate it. Add 3 mL of starch indicator solution (5 g/L), when approaching the end point.
Continue to titrate, until the solution turns blue.
At the same time, carry out a blank test of iodine consumed by water. Take 200 mL of
water. Add 0.05 mL of prepared iodine standard titration solution [c(1/2I2) ≈ 0.1 mol/L]
and 3 mL of starch indicator solution (5 g/L). Use sodium thiosulfate standard titration
solution [c(Na2S2O3) ≈ 0.1 mol/L] to titrate, until the blue color of the solution
disappears.
5.9.2.2.2 Result calculation
The concentration of the iodine standard titration solution [c(1/2I2) is expressed in
moles per liter (mol/L), which is calculated according to formula (12):
Where:
m - The mass of the weighed reference potassium carbonate, in grams (g);
V - The value of the volume of potassium carbonate solution, in milliliters (mL);
M - The value of the molar mass of potassium iodate (1/6KIO3), in grams per mole
(g/mol) (M = 35.67).
5.11 Oxalic acid standard titration solution [c(1/2C2H2O4) ≈ 0.1 mol/L]
5.11.1 Preparation
Weigh 6.4 g of oxalic acid (C2H2O4 • 2H2O). Dissolve it in 1000 mL of water. Shake
well.
5.11.2 Calibration
5.11.2.1 Determination method
Accurately add 30.00 mL ~ 35.00 mL of the prepared oxalic acid standard titration
solution [c(1/2C2H2O4) ≈ 0.1 mol/L]. Add 100 mL of sulfuric acid solution (8 + 92).
Use potassium permanganate standard titration solution [c(1/5KMnO4) ≈ 0.1 mol/L] for
titration. Heat it to 65 °C, when approaching the end point. Continue to titrate until the
solution turns pink for 30 s. At the same time, carry out a blank test.
5.11.2.2 Result calculation
The concentration of oxalic acid standard titration solution [c(1/2C2H2O4)] is expressed
in moles per liter (mol/L), which is calculated according to formula (15):
Where:
c1 - The exact value of the concentration of potassium permanganate standard
titration solution, in mole per liter (mol/L);
V1 - The value of the volume of potassium permanganate standard titration solution,
which is consumed during titration, in milliliters (mL);
V2 - The value of the volume of the potassium permanganate standard titration
solution, which is consumed by the blank test, in milliliters (mL);
V - The value of the volume of the oxalic acid standard titration solution, which is
accurately added during calibration, in milliliters (mL).
5.12 Potassium permanganate standard titration solution
[c(1/5KMnO4) ≈ 0.1 mol/L]
5.12.1 Preparation
Weigh 3.3 g of potassium permanganate. Dissolve it in 1050 mL of water. Slowly boil
for 15 min. Cool and store in a dark place for two weeks. Use a glass sand crucible,
which has a filter plate aperture of 5 μm ~ 10 μm, to filter it into a clean brown bottle.
The pore size of the filter plate, which is used for filtering the potassium permanganate
standard titration solution, is 5 μm ~ 10 μm. The glass sand crucible shall be slowly
boiled by the same potassium permanganate standard titration solution, for 5 minutes
in advance. The collection bottle shall also be washed two to three times, by this
potassium permanganate standard titration solution.
5.12.2 Calibration
5.12.2.1 Method 1
5.12.2.1.1 Determination method
Weigh 0.2 g of standard sodium oxalate, which was dried to a constant mass in a 105 °C
~ 110 °C electric heating constant temperature drying oven, accurate to 0.0001 g.
Dissolve it in 100 mL of sulfuric acid solution (8 + 92). Use the prepared potassium
permanganate standard titration solution [c(1/5KMnO4) ≈ 0.1 mol/L] for titration. Heat
it to 65 °C, when approaching the end point. Continue to titrate, until the solution is
pink, which is kept for 30 s without fading. At the same time, carry out a blank test.
5.12.2.1.2 Result calculation
The concentration of potassium permanganate standard titration solution
[c(1/5KMnO4)] is expressed in moles per liter (mol/L), which is calculated according
to formula (16):
Where:
V1 - The value of the volume of potassium permanganate standard titration solution,
which is consumed during titration, in milliliters (mL);
V2 - The value of the volume of the potassium permanganate standard titration
solution, which is consumed by the blank test, in milliliters (mL);
Add 300 mL of water. Heat to dissolve. Add 650 mL of water. Shake well.
5.14.2 Calibration
5.14.2.1 Method 1
5.14.2.1.1 Determination method
Weigh 0.2 g of benchmark sodium oxalate, which is dried to the constant mass in an
electric heating constant temperature drying oven at 105 °C ~ 110 °C, accurate to
0.0001 g. Dissolve it in 75 mL of water. Add 4 mL of sulfuric acid solution (20%) and
10 mL of hydrochloric acid. Heat it to 65 °C ~ 70 °C. Use the prepared cerium sulfate
standard titration solution (or cerium ammonium sulfate) to titrate it, until the solution
turns pale yellow. Add 3 drops of ferrous-o-phenanthroline indicator solution, to make
the solution become orange-red. Continue to titrate, until the solution is light blue. At
the same time, carry out a blank test.
5.14.2.1.2 Result calculation
The concentration (c) of cerium sulfate (or cerium ammonium sulfate) standard titration
solution is expressed in moles per liter (mol/L), which is calculated according to
formula (19):
Where:
V1 - The value of the volume of the cerium sulfate (or cerium ammonium sulfate)
standard titration solution, which is consumed during titration, in milliliters (mL);
V2 - The value of the volume of the cerium sulfate (or cerium ammonium sulfate)
standard titration solution, which is consumed by the blank test, in milliliters (mL);
m - The mass of the weighed benchmark sodium oxalate, in grams (g);
M - Numerical value of the molar mass of sodium oxalate (1/2Na2C2O4), in grams
per mole (g/mol) (M = 66.70).
5.14.2.2 Method 2
5.14.2.2.1 Determination method
Accurately add 30.00 mL ~ 35.00 mL of prepared cerium sulfate (or cerium ammonium
sulfate) standard titration solution. Put it in a 500 mL iodine volumetric flask. Add 2 g
of potassium iodide, 20 mL of sulfuric acid solution (20%). Use water to seal it. Shake
well. Place it in a dark place for 5 min. Add 150 mL of water. Use sodium thiosulfate
standard titration solution [c(Na2S2O3) ≈ 0.1 mol/L] to titrate. Add 3 mL of starch
5.15.2.1 Disodium EDTA standard titration solution [c(EDTA) ≈ 0.1 mol/L,
c(EDTA) ≈ 0.05 mol/L]
5.15.2.1.1 Determination method
According to Table 7, weigh the specified amount of standard zinc oxide, which was
burnt in a high temperature furnace at 800 °C ± 20 °C to a constant mass, accurate to
0.0001 g. Use a small amount of water to wet it. Add 2 mL of hydrochloric acid solution
(20%) to dissolve it. Add 100 mL of water. Use ammonia solution (10%) to neutralize
it to pH = 7 ~ 8. Add 10 mL of ammonia-ammonium chloride buffer solution A (pH ≈
10) and 5 drops of chrome black T indicator solution (5 g/L) or a small amount of
chrome black T indicator. Use the prepared disodium EDTA solution [c(EDTA) ≈ 0.1
mol/L] to titrate it, until the solution changes from purple to pure blue. At the same time,
carry out a blank test.
5.15.2.1.2 Result calculation
Concentration of disodium EDTA standard titration solution [c(EDTA)] is expressed in
moles per liter (mol/L), which is calculated according to formula (21)
Where:
V1 - The value of the volume of disodium EDTA standard titration solution, which
is consumed during titration, in milliliters (mL);
V2 - The value of the volume of the disodium EDTA standard titration solution,
which is consumed by the blank test, in milliliters (mL);
m - The mass of the weighed benchmark zinc oxide, in grams (g);
M - Numerical value of the molar mass of zinc oxide (ZnO), in grams per mole
(g/mol) (M = 81.39).
5.15.2.2 Disodium EDTA standard titration solution [c(EDTA) ≈ 0.02 mol/L]
5.15.2.2.1 Determination method
According to Table 7, weigh the specified amount of standard zinc oxide, which was
burnt in a high-temperature furnace at 800 °C ± 20 °C to a constant mass, accurate to
0.0001 g. Use a small amount of water to wet it. Add hydrochloric acid solution (20%)
dropwise, to dissolve it. Transfer the whole into a 250 mL volumetric flask. Use water
to dilute it to the mark. Shake well. Accurately add 30.00 mL ~ 35.00 mL of this solution.
Add 70 mL of water. Use ammonia solution (10%) to neutralize it to pH = 7 ~ 8. Add
10 mL of ammonia-ammonium chloride buffer solution A (pH ≈ 10) and 5 drops of
The concentration of zinc chloride standard titration solution [c(ZnCl2)] is expressed in
moles per liter (mol/L), which is calculated according to formula (23):
Where:
c1 - The exact value of the concentration of the disodium EDTA standard titration
solution, in moles per liter (mol/L);
V1 - The value of the volume of disodium EDTA standard titration solution, which
is consumed during titration, in milliliters (mL);
V2 - The value of the volume of the disodium EDTA standard titration solution,
which is consumed by the blank test, in milliliters (mL);
V - The value of the volume of zinc chloride standard titration solution, which is
accurately added during calibration, in milliliters (mL).
5.17 Magnesium chloride (or magnesium sulfate) standard titration
solution [c(MgCl2) ≈ 0.1 mol/L, c(MgSO4) ≈ 0.1 mol/L]
5.17.1 Preparation
Weigh 21 g of magnesium chloride (MgCl2 • 6H2O), [or 25 g of magnesium sulfate
(MgSO4 • 7H2O). Dissolve it in 1000 mL of hydrochloric acid solution (0.5 + 999.5).
After standing for one month, use a 16 µm ~ 30 µm glass sand crucible to filter it. Shake
well.
5.17.2 Calibration
5.17.2.1 Determination method
Accurately add 30.00 mL ~ 35.00 mL of prepared magnesium chloride (or magnesium
sulfate) standard titration solution. Add 70 mL of water and 10 mL of ammonia-
ammonium chloride buffer solution A (pH ≈ 10), 5 drops of chrome black T indicator
solution (5 g /L) or a small amount of chrome black T indicator. Use the disodium EDTA
standard titration solution [c(EDTA) ≈ 0.1 mol/L] to titrate, until the solution changes
from purple to pure blue. At the same time, carry out a blank test.
5.17.2.2 Result calculation
The concentration (c) of the magnesium chloride (or magnesium sulfate) standard
titration solution is expressed in moles per liter (mol/L), which is calculated according
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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