HG/T 3937-2007 English PDF (HGT3937-2007)

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HG/T 3937-2007: 1, 6-Hexanediamine for industrial use
HG/T 3937-2007
HG
CHEMICAL INDUSTRY STANDARD OF
THE PEOPLE’S REPUBLIC OF CHINA
ICS 71.080.30
G 17
Registration number. 20519-2007
1,6-Hexanediamine for industrial use
ISSUED ON. APRIL 13, 2007
IMPLEMENTED ON. OCTOBER 01, 2007
Issued by. National Development and Reform Commission
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Normative references ... 4 
3 Traits ... 5 
4 Requirements ... 5 
5 Test methods ... 5 
6 Inspection rules ... 11 
7 Marking, packaging, transportation, storage ... 12 
8 Safety ... 13 
1,6-Hexanediamine for industrial use
1 Scope
This standard specifies the requirements, test methods, inspection rules,
marking, packaging, transportation, storage and safety of 1,6-Hexanediamine
for industrial use.
This standard applies to the production, inspection and sale of 1,6-
Hexanediamine for industrial use which is produced by catalytic hydrogenation
of adiponitrile which is used as raw material.
Molecular formula. C6H16N2
Relative molecular mass. 116.21 (according to 2005 international relative
atomic mass)
Structural formula. H2N(CH2)6NH2
2 Normative references
The provisions in following documents become the provisions of this standard
through reference in this standard. For the dated references, the subsequent
amendments (excluding corrections) or revisions do not apply to this standard;
however, parties who reach an agreement based on this standard are
encouraged to study if the latest versions of these documents are applicable.
For undated references, the latest edition of the referenced document applies.
GB 190-1990 Labels for packages of dangerous goods
GB/T 601-2002 Chemical reagent - Preparations of standard volumetric
solutions
GB/T 603-2002 Chemical reagent - Preparations of reagent solution for use
in test methods (neq ISO 6353-1.1982)
GB/T 1250 Methods for representation and determination of limit values
GB/T 3143-1982 Determination of the color of liquid chemistry product
(Hazen unit - platinum-cobalt chroma) (eqv ISO 2211.1973)
GB/T 3723 Sampling of chemical products for industrial use - Safety in
sampling (idt ISO 3165.1976)
hazardous situation. Operators shall take appropriate safety and health
measures.
5.2 General provisions
Unless otherwise stated, only the validated analytically pure reagents and the
grade III water as specified in GB/T 6682-1992 are used in the analysis.
The standard titration solution used in the test method, the standard solution for
the determination of impurities, the preparation and the product shall, when no
other requirements are specified, be prepared according to the provisions of
GB/T 601-2002 and GB/T 603-2002.
5.3 Appearance in molten state
Take appropriate amount of laboratory samples. Melt it at 60 °C. Pour it into the
colorimetric tube. Place the colorimetric tube in a 42 °C ~ 45 °C water bath.
Make visual observation immediately, to check whether it is a colorless
transparent liquid.
5.4 Determination of 1,6-Hexanediamine content
5.4.1 Summary of method
Using methyl red as an indicator, use the hydrochloric acid standard titration
solution for titration.
5.4.2 Reagents
5.4.2.1 Hydrochloric acid standard titration solution. c (HCl) = 0.5 mol/L.
5.4.2.2 Methyl red indicator solution 1 g/L.
5.4.3 Analytical procedures
Weigh 1.0 g ~ 14 g of laboratory sample, accurate to 0.0002 g. Place it in a 250
mL conical flask. Use 50 mL of water to dissolve it. Add 2 ~ 3 drops of methyl
red indicator solution. Use the hydrochloric acid standard titration solution to
titrate the solution, until the color of solution changes from yellow to red, which
is used as the end point.
5.4.4 Calculation of results
The mass fraction w1 of 1,6-Hexanediamine (C6H16N2), the value of which is
expressed in %, is calculated according to formula (1).
Where.
V - The volume of the hydrochloric acid standard titration solution (5.4.2.1),
in milliliters (mL);
c - The exact value of the concentration of the hydrochloric acid standard
titration solution, in moles per liter (mol/L);
m - The value of the mass of the sample, in grams (g),
M - The molar mass of the 1,6-Hexanediamine (1/2C6H16N2), in grams per
mole (g/mol) (M = 58.1).
Take the arithmetic mean of the results of two parallel determinations as the
determination result. The absolute difference between the results of the two
parallel determinations is not more than 0.1%.
5.5 Determination of chroma of aqueous solution
It is performed according to the provisions of GB/T 3143-1982. Weigh (70 ± 0.1)
g of laboratory sample which is in molten state. Dissolve it in water. Dilute it to
100 mL.
5.6 Determination of moisture
It is performed according to the provisions of GB/T 6283-1986. Add 5 mL of
glacial acetic acid into the titration cell. Place the titration cell in an ice water
bath.
Take the arithmetic mean of the results of two parallel determinations as the
determination result. The absolute difference between the results of the two
parallel determinations is not more than 15% of the arithmetic mean of the two
determined values.
5.7 Determination of crystallization points
It is performed according to the provisions of GB/T 7533-1993, wherein it allows
the main thermometer to use the locally-immersed thermometer.
Take the arithmetic mean of the results of two parallel determinations as taken
as the determination result. The absolute difference between the results of the
two parallel determinations is not more than 0.05 °C.
5.8 Determination of polarographic values
5.8.1 Summary of method
Use the polarographic instrument to measure the substances which produce
the polarographic wave near -1.5 V in the sample’s impurities. Use the
Solution B / mL 100 98 97 96
5.8.4.4 Determination of polarographic wave
Take 15 mL of 0# ~ 3# standard solution (i = 0, 1, 2, 3) in turn. Add it into the
electrolytic tank. Lead in nitrogen for 10 min to remove oxygen. Measure the
polarographic wave h (i, j) of it under the 6 sensitivities in the polarograph (j =
1, 2 ... 6).
5.8.4.5 Calculation of values
The polarographic value PI(t) corresponding to the 1# ~ 3# standard solution,
expressed as [mmol (isobutyraldehyde) / t (1,6-Hexanediamine)], is calculated
according to formula (2).
Where
m - The mass of isobutyraldehyde which is added to solution A, in grams (g);
T1 - The mass fraction of isobutyraldehyde (5.8.2.1), in percentage (%),
Vi - The volume of the solution A which is added to the 1# ~ 3# standard
solution, in milliliters (mL);
M - The molar mass of isobutyraldehyde, in grams per mole (g/mol) (M =
72.107);
T2 - The concentration of 1,6-Hexanediamine in solution B, in percentage
(%);
500 - The volume of the volumetric flask, in milliliters (mL).
The height difference of polarographic wave Δh (i, j) corresponding to 1# ~ 3#
standard solution, expressed in mm, is calculated according to formula (3).
Where
h (i, j) - The polarographic wave height measured for the 1# ~ 3# standard
solution at the jth sensitivity, in millimeters (mm).
h (0, j) - The polarographic wave height measured for the 0# standard
solution at the jth sensitivity, in millimeters (mm).
The coefficient f (i, j) corresponding to the 1# ~ 3# standard solution is calculated
fj - The arithmetic mean of the standard solution’s coefficients for the
selected sensitivity.
Take the arithmetic mean of the two determinatio...