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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.
The following main changes have been made with respect to GB/T 4649-2008:
——Description of ethylene glycol production process is deleted (see Clause 1; Clause 1 of Edition 2008);
——Technical requirements for acceptable products are deleted (see Table 1; Table 1 of Edition 2008);
——"superior products" are modified to "polyester grade", and "first-class products" to "industrial grade" (see Table 1; Table 1 of Edition 2008);
——The appearance requirements of polyester grade and industrial grade products are changed from "colorless, transparent and free of mechanical impurities" to "transparent liquid and free of mechanical impurities" (see Table 1; Table 1 of Edition 2008);
——The content index of polyester grade ethylene glycol is changed from “≥99.8%” to “≥99.9%” and that of diethylene glycol is changed from “≤0.10%” to “≤0.050%”; the content of diethylene glycol in industrial grade ethylene glycol is changed from “≤0.80%” to “≤0.600%”; the water content index is changed from “≤0.10%” to “≤0.08%” (see Table 1; Table 1 of Edition 2008);
——Items including 1,2-butanediol, 1,4-butanediol, 1,2-hexanediol and ethylene carbonate are added, with the index of "report" (see Table 1; Table 1 of Edition 2008);
——Polyester grade UV transmittance is increased by 250nm, with the index of "report" (see Table 1; Table 1 of Edition 2008);
——Chloride ion item and its test methods are added under the polyester grade, with the index of "≤0.5mg/kg" (see Table 1 and 4.14; 5.7 of Edition 2008);
——The measurement unit for content of acidity, iron, ash, aldehyde and other items is changed from "%"to "mg/kg" (see Table 1; Table 1 of Edition 2008);
——The requirement of test by gravimetric method is modified in case of any dispute in the visual appearance test results (see 4.3, 4.1 of Edition 2008);
——The determination method of ethylene glycol content is modified; the original equation 1 is deleted; and the determination methods for contents of 1,2-butanediol, 1,4-butanediol, 1,2-hexanediol and ethylene carbonate are added (see 4.4; 4.2 and 4.10 of Edition 2008);
——GB/T 6324.6 is added for determination of chroma and GB/T 3143 is adopted as the arbitration method; relevant contents are moved to Annex A (see 4.5 and Annex A; 4.3 of Edition 2008);
——The U-shaped vibrating tube method given in GB/T 2013-2010 is added for density determination; the content of temperature correction in the test by density bottle method is deleted, the density bottle method given in GB/T 4472 is taken as the arbitration method, and the relevant contents are moved to Annex B (see 4.6 and Annex B; 4.4 of Edition 2008);
——104C-75 thermometer conforming to GB/T 7534-2008 is added for determination of boiling range (see 4.7);
——SH/T 1055 is added for determination of water, and the method is taken as arbitration method (see 4.8; 4.6 of Edition 2008);
——"Manual method is taken as the arbitration method" is added for determination of acidity (see 4.9; 4.7 of Edition 2008);
——The sampling amount for determination of iron content is modified from "80g" to "70g" (see 4.10; 4.8 of Edition 2008);
——The analytical balance and constant weight requirements for determination of ash are modified from "sensitivity 0.1mg" to "sensitivity 0.01mg", the "porcelain crucible” is changed to "platinum crucible", and the relevant contents are moved to Annex C (see 4.11 and Annex C; 4.9 of Edition 2008);
——The starting condition of type inspection is modified (see 5.1; 5.1 of Edition 2008);
——The determination method for inspection results is changed from "full value comparison method" to "rounded-off-value comparison method" (see 5.3);
——The clause "Safety” is deleted and the relevant contents are included in the informative annex (see Annex E; Clause 7 of Edition 2008).
This standard was proposed by China Petrochemical Corporation.
This standard is under the jurisdiction of Subcommittee on Petrochemistry of National Technical Committee on Chemical of Standardization Administration of China (SAC/TC 63/SC 4).
The previous editions of this standard are as follows:
——GB 4649-1993, GB/T 4649-2008.
Ethylene glycol for industrial use
Warning——This standard does not purport to address all the safety problems, if any, associated with its use. Producers must explain to users the hazards of the product, the safety and protective measures in use, and the user of this standard is obliged to take appropriate safety and health measures which are guaranteed conforming to the conditions specified in the relevant national law and regulations.
1 Scope
This standard specifies the technical requirements, test methods, inspection rules, marking, labeling and accompanying documents as well as packaging, transportation and storage of ethylene glycol for industrial use.
It is applicable to ethylene glycol used as the monomer for producing polyester and alkyd resin, as well as the electrolyte, antifreeze, plasticizer and solvent for electrolytic capacitors.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.
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
GB/T 6283 Chemical products - Determination of water - Karl·Fischer method (general method)
GB/T 6324.6 Test method of organic chemical products - Part 6: Determination of color for liquids - Tristimulus colorimetry
GB/T 6678 General principles for sampling chemical products
GB/T 6680 General rules for sampling liquid chemical products
GB/T 6682 Water for analytical laboratory use - Specification and test methods
GB/T 7531 Determination of ignition residue for organic chemical products
GB/T 7534-2004 Volatile organic liquids for industrial use - Determination of boiling range
GB/T 8170-2008 Rules of rounding off for numerical values & expression and judgment of limiting values
GB/T 10479 Aluminum rail tank cars
GB/T 14571.1 Test method of monoethylene glycol for industrial use - Part 1: Determination of acidity - Titration method
GB/T 14571.2 Test method of ethylene glycol for industrial use - Part 2: Determination of purity and impurities - Gas chromatography
GB/T 14571.3 Ethylene glycol for industrial use - Determination of content of total aldehydes present - Spectrophotometric method
GB/T 14571.4 Ethylene glycol for industrial use - Determination of ultraviolet transmittance - Ultraviolet spectrophotometric method
GB/T 14571.5 Test method of monoethylene glycol for industrial use - Part 5: Determination of chloride ion - Ion chromatography
SH/T 1053 Determination for boiling range of industrial diethylene glycol
SH/T 1055 Determination of water content in industrial diethylene glycol by microcoulometric titration
3 Technical requirements
See Table 1 for the technical requirements of ethylene glycol for industrial use.
Table 1 Technical requirements of ethylene glycol for industrial use
S.N. Item Index
Polyester grade Industrial grade
1 Appearance Transparent liquid and free of mechanical impurities
2 Ethylene glycol, ω/% ≥ 99.9 99.0
3 Diethylene glycol, ω/% ≤ 0.050 0.600
4 1,4-butanediol a, ω/% Report b
5 1,2-butanediol a, ω/% Report b
6 1,2-hexanediol a, ω/% Report b
7 Ethylene carbonate a, ω/% Report b
8 Chroma (platinum-cobalt) / scale
Before heating ≤
After heating with hydrochloric acid ≤
5
20
10
—
9 Density (20℃)/(g/cm3) 1.112 8~1.113 8 1.112 5~1.114 0
10 Boiling range (at 0℃, 0.101 33MPa)
Initial boiling point / ℃ ≥
Final boiling point / ℃ ≤
196.0
199.0
195.0
200.0
11 Water content, ω/% ≤ 0.08 0.20
12 Acidity (by acetic acid) /(mg/kg) ≤ 10 30
13 Iron content / (mg/kg) ≤ 0.10 5.0
14 Ash / (mg/kg) ≤ 10 20
15 Aldehyde content (by formaldehyde) / (mg/kg) ≤ 8.0 —
16 Ultraviolet transmittance/%
220nm ≥
250nm
275nm ≥
350nm ≥
75
Report b
92
99
—
17 Chloride ion /(mg/kg)≤ 0.5 —
a This item is not required for ethylene oxidation/ethylene oxide hydration process.
b "report" refers to the item shall be determined and the measured data shall be provided.
4 Test methods
4.1 Sampling
The sampling shall be carried out in accordance with GB/T 3723, GB/T 6678 and GB/T 6680. Mix the samples uniformly and put into two clean, dry and sealable glass bottles, attach labels on each bottle to indicate the manufacturer’s name, product name, batch No., sampling date and sampling place; keep one bottle for analysis and inspection and the other for future reference.
4.2 General requirements
Unless otherwise specified, only recognized analytical reagents and Grade 3 water complying with GB/T 6682 may be used during analysis.
4.3 Appearance determination
Take 50mL~60mL of industrial ethylene glycol sample, place it in a clean and dry 100mL-colorimetric tube, and perform direct visual observation under the transmission of daylight or daylight lamp.
In case of any dispute, take 100g±0.5g of sample and subject it to suction filtration with a No.4 glass filter crucible of constant weight at the suction filtration speed of making the filtrate drop-like, and then wash the glass filter crucible with distilled water for 4~5 times, with an amount of about 20mL each time. Next, move the glass filter crucible into an oven, dry it at 105℃±2℃ for at least 45min, take it out, cool it in a dryer for 30min, and weigh it to the nearest 0.000 1g. Dry the glass filter crucible for another 30min, take it out, cool in a dryer for 30min, and weigh it; repeat this process until the difference between two consecutive weighing does not exceed 0.000 4g. Compare with the glass filter crucible before filtration, when the increment is not more than 0.001g, it is regarded as free of mechanical impurities.
4.4 Determination of the content of ethylene glycol, diethylene glycol, 1,4-butanediol, 1,2-butanediol, 1,2-hexanediol and ethylene carbonate
It shall be in accordance with GB/T 14571.2.
4.5 Determination of chroma
It shall be in accordance with Annex A.
4.6 Determination of density
It shall be in accordance with Annex B.
4.7 Determination of boiling range
It shall be in accordance with GB/T 7534-2004. The heat source is a 500W electric furnace or gas lamp. The main thermometer is a rod-shaped glass thermometer marked with scales of 150℃ ~ 220℃ at the division of 0.1℃. The distance from the top of the bulb to the first scale line is at least 100mm. It is also allowed to use the 104C-75 thermometer recommended in Table 1 of GB/T 7534-2004. The difference between the results of the two repeated determinations shall be no more than 0.5℃ at the initial boiling point and no more than 0.4℃ at the final boiling point. It is also allowed to use the device specified in SH/T 1053 for determination. In case of any dispute on the result, it shall be subject to the arbitration of GB/T 7534-2004.
4.8 Determination of water content
It shall be in accordance with SH/T 1055 or GB/T 6283. In case of any dispute on the result, it shall be subject to the arbitration of SH/T 1055.
Where GB/T 6283 is adopted, the arithmetic average obtained from two repeated determinations is taken as the analysis result. When the water content is in the range of 0.02%~0.10%, the difference between the results of two repeated determinations shall not exceed 15% of the average; when the water content is more than 0.10%, the difference between the results of two repeated determinations shall not exceed 10% of the average.
4.9 Determination of acidity
It shall be in accordance with GB/T 14571.1. In case of any dispute on the result, manual titration method shall be adopted as the arbitration method.
4.10 Determination of iron content
It shall be in accordance with GB/T 3049. Adopt 100mL volumetric flask or 100mL colorimetric tube and 3cm (or 5cm) cuvette when plotting the standard curves and performing sample determination. The sampling mass is 70g±0.5g. The arithmetic average of the results of two parallel determinations is taken as the analysis result. When the iron content is less than or equal to 0.5mg/kg, the difference between the results of two repeated determinations shall not exceed 15% of the average; when the iron content exceeds 0.5mg/kg, the difference between the results of two repeated determinations shall not exceed 10% of the average.
4.11 Determination of ash
It shall be in accordance with Annex C.
4.12 Determination of aldehyde content
It shall be in accordance with GB/T 14571.3.
4.13 Determination of ultraviolet transmittance
It shall be in accordance with GB/T 14571.4.
4.14 Determination of chloride ion
It shall be in accordance with GB/T 14571.5 or Annex D. In case of any dispute on the result, it shall be subject to the arbitration of GB/T 14571.5.
Foreword i
1 Scope
2 Normative references
3 Technical requirements
4 Test methods
5 Inspection rules
6 Marking, labeling and accompanying documents
7 Packaging, transportation and storage
Annex A (Normative) Determination of chroma
Annex B (Normative) Determination of density
Annex C (Normative) Determination of ash
Annex D (Normative) Determination of chlorine ion content
Annex E (Informative) Safety
