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GB/T 4649-2018 PDF in English


GB/T 4649-2018 (GB/T4649-2018, GBT 4649-2018, GBT4649-2018)
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GB/T 4649-2018: PDF in English (GBT 4649-2018)

GB/T 4649-2018
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.080.60
G 16
Replacing GB/T 4649-2008
Ethylene glycol for industrial use
ISSUED ON: MAY 14, 2018
IMPLEMENTED ON: DECEMBER 01, 2018
Issued by: State Administration for Market Regulation;
Standardization Administration of the PRC.
Table of Contents
Foreword ... 3 
1 Scope ... 6 
2 Normative references ... 6 
3 Technical requirements ... 7 
4 Test methods ... 8 
5 Inspection rules ... 11 
6 Marks, labels, and accompanying documents ... 11 
7 Packaging, transportation, and storage ... 12 
Appendix A (Normative) Determination of color ... 13 
Appendix B (Normative) Determination of density ... 15 
Appendix C (Normative) Determination of ash content ... 16 
Appendix D (Normative) Determination of chloride ion ... 17 
Appendix E (Informative) Safety ... 19 
Foreword
This Standard is drafted in accordance with the rules given in GB/T 1.1-2009.
This Standard replaces GB/T 4649-2008 “Ethylene glycol for industrial use -
Specification”.
Compared with GB/T 4649-2008, the main changes of this Standard are as
follows:
- Delete the description of production process of ethylene glycol (see Clause
1; Clause 1 of the 2008 edition);
- Delete the technical requirements for qualified products (see Table 1; Table
1 of the 2008 edition);
- CHANGE “Superior product” to “Polyester grade” and “First-class product”
to “Industrial grade” (see Table 1; Table 1 of the 2008 edition);
- CHANGE the appearance requirement of polyester grade and industrial
grade products from “Colorless and transparent without mechanical
impurities” to “Transparent liquid, without mechanical impurities” (see Table
1; Table 1 of the 2008 edition);
- CHANGE the content index of polyester grade ethylene glycol from
“≥99.8%” to “≥99.9%”, and the content index of diethylene glycol from
“≤0.10%” to “≤0.050%”. CHANGE the diethylene glycol content of industrial
grade ethylene glycol from “≤0.80%” to “≤0.600%”, and the water content
index from “≤0.10%” to “≤0.08%” (see Table 1; Table 1 of the 2008 edition);
- ADD 1,2-butanediol, 1,4-butanediol, 1,2-hexanediol, and vinyl carbonate
items with the index “Report” (see Table 1; Table 1 of the 2008 edition);
- ADD 250 nm for the polyester grade ultraviolet transmittance with the index
“Report” (see Table 1; Table 1 of the 2008 edition);
- For polyester grade, ADD chloride ion item and test method, with the index
“≤0.5 mg/kg” (see Table 1 and 4.14; 5.7 of the 2008 edition);
- CHANGE the unit of measurement for items such as acidity, iron, ash
content, aldehyde content from “%” to “mg/kg” (see Table 1; Table 1 of the
2008 edition);
- Modify the gravimetric test requirements for the dispute of appearance
visual determination results (see 4.3; 4.1 of the 2008 edition);
Ethylene glycol for industrial use
Caution - This Standard does not address all possible safety problems.
Producers must explain to users the hazards of the product and the safety
and protective measures in use. The users of this Standard are
responsible for taking appropriate safety and health measures and
ensuring compliance with the conditions specified in relevant national
regulations.
1 Scope
This Standard specifies the technical requirements, test methods, inspection
rules, marks, labels, and accompanying documents, packaging, transportation,
and storage of ethylene glycol for industrial use.
This Standard applies to ethylene glycol used as monomers for the production
of polyesters and alkyds and as electrolytes, antifreezes, plasticizers, solvents,
etc. for electrolytic capacitors.
2 Normative references
The following documents are indispensable for the application of this document.
For the dated references, only the editions with the dates indicated are
applicable to this document. For the undated references, the latest edition
(including all the amendments) are applicable to this document.
GB/T 2013-2010 Standard test method for density of liquid petrochemical
products
GB/T 3049 Chemical products for industrial use - General method for
determination of iron content - 1,10-Phenanthroline spectrophotometric
method
GB/T 3143 Color determination method of liquid chemicals (Hazen unit -
Platinum-cobalt scale)
GB/T 3723 Sampling of chemical products for industrial use - Safety in
sampling
GB/T 4472-2011 Determination of density and relative density for chemical
products
4.2 General provision
Unless otherwise stated, only reagents confirmed as analytically pure and
Grade 3 water meeting GB/T 6682 are used in the analysis.
4.3 Determination of appearance
TAKE 50 mL~60 mL of the sample of ethylene glycol for industrial use; PLACE
it in a clean and dry 100 mL colorimetric tube; under the transmission of sunlight
or fluorescent lamp, visually inspect it directly.
In case of dispute, TAKE 100 g±0.5 g of sample; USE a constant-weight No. 4
glass filter crucible to suction-filter. The suction-filtration rate shall be controlled
so that the filtrate is in the form of drops. USE distilled water to wash the glass
filter crucible 4 times~5 times. The dosage each time is about 20 mL. Then,
TRANSFER the glass filter crucible into an oven; DRY at 105 °C±2 °C for at
least 45 min; TAKE out; COOL in a desiccator for 30 min and weigh, accurate
to 0.0001 g. DRY the glass filter crucible for 30 min again; TAKE out; COOL in
a desiccator for 30 min and weigh. This is repeated until the difference between
the two consecutive weighs does not exceed 0.0004 g. Compared with the
glass filter crucible before filtration, when the increment is not more than 0.001
g, it is considered that there is no mechanical impurity.
4.4 Determination of ethylene glycol, diethylene glycol, 1,4-butanediol,
1,2-butanediol, 1,2-hexanediol, vinyl carbonate content
According to the provisions of GB/T 14571.2, carry out the determination.
4.5 Determination of color
According to the provisions of Appendix A, carry out the determination.
4.6 Determination of density
According to the provisions of Appendix B, carry out the determination.
4.7 Determination of boiling range
It shall be carried out according to the provisions of GB/T 7534-2004. The heat
source is a 500 W electric furnace or a gas lamp. The master thermometer is a
rod-shaped glass thermometer with a scale value of 150 °C~220 °C and a
division value of 0.1 °C. The distance between the tip of the temperature
sensing bulb and the first scale line is at least 100 mm. The 104C-75
thermometer recommended in Table 1 of GB/T 7534-2004 may also be used.
The difference between two repeated determination results, for the initial boiling
point, shall be no more than 0.5 °C, and for the dry point, shall be no more than
It shall be carried out according to the provisions of GB/T 14571.5 or Appendix
D. When the result is controversial, GB/T 14571.5 is used as the arbitration
method.
5 Inspection rules
5.1 Inspection classification
All index items in Table 1 are type inspection items and are exit-factory
inspection items except for boiling range, density, iron content, ash content, and
chloride ion. When one of the following conditions is encountered, it shall carry
out the type inspection:
a) Every 3 months during normal production;
b) Key production process updates and major equipment changes;
c) The main raw materials change and affect the product quality;
d) Production resumes after suspension;
e) The exit-factory inspection result is quite different from the previous type
inspection.
5.2 Lot grouping rules
The same-quality and uniform products are one lot. According to the production
cycle, production shift, or product storage tank, lot grouping may be carried out.
5.3 Judgement rules
It shall be carried out according to the rounded-off value comparison method of
GB/T 8170-2008. If the inspection results all meet the technical requirements
of Table 1 of this Standard, this lot of products is judged as qualified. If any of
the indexes of the inspection results does not meet the requirements of this
Standard, according to 4.1, double quantity of samples shall be re-taken for
inspection. If the re-inspection result still does not meet the requirements of the
product of corresponding grades specified in this Standard, this lot of products
shall be judged as unqualified.
6 Marks, labels, and accompanying documents
6.1 Packaging containers of ethylene glycol products for industrial use shall
have a strong mark, indicating manufacturer name, product name, this
Standard number, lot number or production date, net content.
Appendix B
(Normative)
Determination of density
B.1 Density bottle method
According to the provisions of 4.3.1 of GB/T 4472-2011, USE a 50 cm3 density
bottle.
The density ρ of ethylene glycol product, expressed in g/cm3, is calculated
according to formula (B.1):
Where:
m1 - Mass of density bottle, in grams (g);
m2 - Mass of density bottle plus sample, in grams (g);
m3 - Mass of density bottle plus water, in grams (g);
0.0012 - The value of air density at 20 °C, in grams per cubic centimeter (g/cm3);
ρwater - The value of water density at 20 °C, in grams per cubic centimeter
(g/cm3).
The arithmetic mean of two repeated determination results is taken as the
analysis result. The difference between the two repeated determination results
shall be no more than 0.0002 g/cm3.
B.2 U-shaped vibrograph method
It shall be determined according to Clause 6 of GB/T 2013-2010.
When the result is controversial, the density bottle method is used as the
arbitration method.
water
Appendix D
(Normative)
Determination of chloride ion
D.1 Method principle
The chloride ion in the sample reacts with silver nitrate to form a white silver
chloride precipitate. Then, compared with the standard solution, perform
turbidimetry.
D.2 Reagents
D.2.1 Sodium chloride: Primary reagent.
D.2.2 Ammonia aqueous solution: 1+1.
D.2.3 Nitric acid: Analytically pure.
D.2.4 Silver nitrate, 5% (mass fraction) aqueous solution: WEIGH 5 g of silver
nitrate dissolved in water; DILUTE to 100 mL. STORE in a brown bottle.
D.2.5 Chlorine standard solution:
D.2.5.1 Chlorine standard solution A: WEIGH 0.1649 g of sodium chloride
(D.2.1) ignited at 500 °C~600 °C to a constant weight dissolved in water;
TRANSFER to a 1000 mL volumetric flask; DILUTE to the mark and shake well.
This solution contains 0.1 mg of chlorine per milliliter.
D.2.5.2 Chlorine standard solution B: USE a pipette to pipette 5 mL of chlorine
standard solution A into a 100 mL volumetric flask; ADD water to dilute to the
mark and shake well. This solution contains 0.005 mg of chlorine per milliliter.
D.3 Instruments and equipment
D.3.1 Thermostatic water-bath.
D.3.2 Ground colorimetric tube: 25 mL.
D.4 Determination procedures
D.4.1 TAKE 2 ground colorimetric tubes (D.3.2). One of which is added with 4.5
mL of ethylene glycol sample and the other with 0.5 mL of chlorine standard
solution B.
......
 
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.