GB/T 30044-2013Coal direct liquefaction—Determination of constituents of heavy products—Solvent extract (English PDF)
煤炭直接液化 液化重质产物组分分析 溶剂萃取法
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Issued by
SAMR; SAC
Level / Type
National · Recommended
Issue date
December 17, 2013
Implementation date
May 1, 2014
Scope
GB/T 30044-2013 is the English-translated version of 煤炭直接液化 液化重质产物组分分析 溶剂萃取法.
GB/T 30044-2013 lays down a solvent extraction method for determining the constituents of the heavy products of coal direct liquefaction.
Clause 1 states that it specifies the terms and definitions, the reagents and materials, the equipment, the measuring steps, the calculation of results, the precision of the method and the test report for the component analysis of direct coal liquefaction heavy products, and that it applies to that analysis; no exclusion is stated.
Clause 2 cites GB/T 23251 alone, and clause 3 takes over part of its terms and definitions while adding five of its own: direct coal liquefaction, quoted from GB/T 23251-2009 definition 3.8 as the process in which coal reacts with hydrogen at high pressure and high temperature over a catalyst and is turned directly into liquid fuel; heavy product; liquefied oil, the n-hexane-soluble part of the product; asphaltene, the n-hexane-insoluble but toluene-soluble part; and preasphaltene, the toluene-insoluble but tetrahydrofuran-soluble part.
Clause 4, Method summary, describes placing a sample ground below 0.2 mm in a filter cartridge, extracting it with n-hexane, drying the n-hexane insoluble matter to constant mass and calculating its mass fraction, then extracting that residue with toluene in the same way and a further portion of sample with tetrahydrofuran.
The later clauses printed on the page are 7 analytical sample preparation, where the heavy product sample is crushed below 3 mm, reduced to about 50 g and ground below 0.2 mm, 8 measuring step with 8.1 Determination of n-hexane insolubles, 8.2 Determination of toluene insolubles and 8.3 Determination of THF insolubles, weighing 1 g plus or minus 0.1 g of sample to the nearest 0.0002 g in 8.1 and in 8.3, pre-dispersing it in an ultrasonic oscillator at 55 degrees C for at least 30 min and extracting it in a Soxhlet extractor over a thermostatted oil bath for not less than 48 h with n-hexane, about 24 h with toluene and 4 h to 8 h with tetrahydrofuran, then drying at 100 to 105 degrees C until two successive weighings differ by no more than 0.0020 g, 9 result of the calculation, which gives the six formulas for the n-hexane insolubles content HI, the liquefied oil mass fraction X0, the toluene insolubles content TI, the asphaltene content Xasp, the tetrahydrofuran insolubles content THFI and the preasphaltene content Xpreasp, and 10 precision of the method, with 10.1 Repeatability limit and 10.2 Reproducibility limit, both set at the 95 per cent confidence level against Table 1.
The draft jumps from clause 4 to the apparatus items 6.7.1 to 6.7.3, a Soxhlet extractor of 45 mm to 55 mm diameter, a 500 mL flat-bottomed flask of 28 mm to 30 mm bottle diameter and a condenser with a water jacket at least 300 mm long, so the titles of clauses 5 and 6 and the test report clause named in the scope are not shown.
It was proposed by the China Coal Industry Association and is kept by the National Coal Standardization Technical Committee (SAC/TC42), under ICS 73.040 and Chinese classification D21, with about 9,950 words estimated.
It was issued on 17 December 2013 and has applied since 1 May 2014; the page does not say which edition it replaces.
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Document preview — GB/T 30044-2013
National Standard of the People's Republic of China
- ICS
- 73.040
- Classification
- D 21
Issued by: State Administration for Market Regulation; Standardization Administration of the PRC
Contents
- Foreword
- 1 Scope
- 2 Normative references
- 3 Terms and Definitions GB/T 23251 define the
- 4 Method summary
- 7 Analytical sample preparation
- 8 Measuring step
- 9 Result of the calculation
- 10 Precision of the method
Foreword
This standard was drafted in accordance with GB/T 1.1-2009 given rules. The standard proposed by China Coal Industry Association.
This standard coal by the National Standardization Technical Committee (SAC/TC42) centralized.
1 Scope
This standard specifies the terms and definitions of direct coal liquefaction heavy product component analysis method feeds, reagents and materials, equipment, measuring Set step, the results of the calculation, method precision and test reports.
This standard applies to direct coal liquefaction heavy product components analysis.
2 Normative references
The following documents for the application of this document is essential. For dated references, only the dated version suitable for use herein Member. For undated references, the latest edition (including any amendments) applies to this document.
GB/T 23251 coal chemical coal Technical Guidelines
3 Terms and Definitions
GB/T 23251 define the terms and definitions section and the following terms and definitions apply to this document.
3.1 Direct coal liquefaction
Coal under the action of high pressure, high temperature and the hydrogenation reaction catalyst with hydrogen, whereby liquid fuel directly into the process. [GB/T 23251-2009, the definition 3.8]
3.2 Heavy product
For other liquefied under the direct coal liquefaction of solid residues generated or at room temperature.
3.3 Liquefied oil
Direct coal liquefaction product n-hexane-soluble components.
3.4 Asphaltene
Direct coal liquefaction products of n-hexane-insoluble and soluble components of toluene.
3.5 Before asphaltene
Direct coal liquefaction product in a toluene-insoluble and soluble components of tetrahydrofuran.
4 Method summary
The sample size of less than 0.2mm is placed in the filter cartridge using hexane extraction, n-hexane insoluble matter was dried to a constant mass-based dry Quality insolubles after drying to calculate the mass fraction of n-hexane insolubles. In the same way, the n-hexane insoluble matter was extracted with toluene Take, measuring the mass fraction of a toluene-insoluble matter. Similarly, the particle size of less than 0.2mm specimen was placed a filter paper tube and extracted with tetrahydrofuran, the
6.7.1 Soxhlet extractor
Diameter 45mm ~ 55mm. […]
6.7.2 Flat-bottomed flask
500mL, bottle diameter 28mm ~ 30mm.
6.7.3 Condenser
Spherical end mill with port and extractor, and with two symmetrical holes, water jacket length of at least 300mm.
7 Analytical sample preparation
The heavy coal liquefaction product samples crushed to less than 3mm, reduced separation of about 50g, ground to less than 0.2mm as a sample for analysis, spare.
8 Measuring step
8.1 Determination of n-hexane insolubles
8.1.1 Weighed sample
0.5g of cotton, divided into two approximately equal parts, put in filter cartridge made funnel-shaped, the other part is placed a filter paper The upper portion of the cylinder, and then the filter cartridge into the weighing bottle, in a blast in the oven at 100 °C ~ 105 °C drying to constant mass (for two consecutive Poor quality of the drying times of no more than 0.0020g), record the mass (m1). Weigh a sample for analysis (1 ± 0.1) g (m), accurate to 0.0002g, from Remove the upper part of the filter cartridge cotton, the sample was placed in the filter cartridge, and then placed on top cotton filter cartridge.
8.1.2 Pre-dispersed sample
The sample is weighed into a paper cylinder containing n-hexane lidded jar, bottle hexane height above the filter drum samples Height, capped the jar into an ultrasonic oscillator, shaking at 55 °C at least 30min.
8.1.3 Sample extraction
The filter cartridge moved Soxhlet extractor, a jar of n-hexane solvent into the flat-bottomed flask, added in the flask solvent amount of solvent 2/3 of the volume of the flask, and the extract is placed in a preheated oil bath at a constant temperature, according to Figure 1 shown installed Soxhlet extraction apparatus. Open cooling water control Oil bath temperature to about reflux hexane solvent 6min average time until the filter cartridge leaking nearly colorless solvent, extraction time is not usually Less than 48h.
8.1.4 Drying constant weight
After extraction stop oil bath was heated until the oil bath was removed after cooling extractor, remove the filter paper tube, placed in a beaker, in a fume hood to be positive After the hexane solvent play to make, weighing bottle into the weighing bottle placed in a vacuum oven at 100 °C ~ 105 °C dried for at least 3h, remove the weighing Bottles and cover caps, placed in a desiccator to cool to room temperature and weighed. Then check Sjogren, every 1h, until the last two weighing result If the difference does not exceed 0.0020g, quality as the basis for the final weighing (m2) result of the calculation.
8.2 Determination of toluene insolubles
8.2.1 Pre-dispersed sample
The hexane insolubles were placed in cylindrical filter paper containing toluene lidded jar, to be higher than the height of the bottle toluene high sample cartridge filter Degrees, capped the jar into an ultrasonic oscillator, shaking at 55 °C at least 30min.
8.2.2 Toluene extraction
The filters were transferred to soxhlet tube, the toluene solvent was poured into the jar Florence flask, the flask was added the amount of solvent is the solvent 2/3 of the volume of the flask, and the extract is placed in a preheated oil bath at a constant temperature, as shown in Figure 1 installed good Soxhlet extraction apparatus. Open cooling water control Oil bath temperature solvent such as toluene reflux average 6min around again until the filter cartridge leaking solvent nearly colorless, usually extracted a lot of time In 24h.
8.2.3 Drying constant weight
After extraction stop oil bath was heated until the oil bath was removed after cooling extractor, remove the filter paper tube, placed in a beaker, in a fume hood to be A Benzene play to make, weighing bottle into the weighing bottle placed in a vacuum oven at 100 °C ~ 105 °C dried for at least 3h, dried or placed blast Box, at 110 °C ~ 115 °C dried for at least 2h, remove the weighing bottle and cover caps, placed in a desiccator to cool to room temperature and weighed. then Sjogren check every 30min, until the difference between the results of the last two weighing not more than 0.0020g, in order to quality for the last weighing Basis (m3) as a result of the calculation.
8.3 Determination of THF insolubles
8.3.1 Sample Weighing
0.5g of cotton, divided into two approximately equal parts, put in filter cartridge made funnel-shaped, the other part is placed a filter paper The upper portion of the cylinder, and then the filter cartridge into the weighing bottle, in a blast in the oven at 100 °C ~ 105 °C drying to constant mass (for two consecutive Poor quality of the drying times of no more than 0.0020g), the recording quality (m4). Weigh a sample for analysis (1 ± 0.1) g (m5), accurate to 0.0002g, from Remove the upper part of the filter cartridge cotton, the sample was placed in the filter cartridge, and then placed on top cotton filter cartridge.
8.3.2 Pre-dispersed sample
The paper said that a good sample tube containing tetrahydrofuran into the jar lid, to be more than the height of the bottle tetrahydrofuran filter cartridge like Height goods, capped the jar into an ultrasonic oscillator, shaking at 55 °C at least 30min.
8.3.3 Extraction
The filter cartridge soxhlet moved, the tetrahydrofuran solvent was poured into the jar Florence flask, the flask was added the solvent and the solvent An amount of 2/3 volume flask, the extractor is placed in a constant temperature oil bath preheated, according to Figure 1 shown installed Soxhlet extraction apparatus. Open cooling water, Controlled oil bath temperature to about reflux tetrahydrofuran solvent 6min average time until the filter cartridge leaking solvent nearly colorless, usually extracted when Room is 4h ~ 8h.
8.3.4 Drying constant weight
After stopping the extraction of oil bath was heated until the oil bath was removed after cooling extractor, remove the filter paper tube, beaker, in a fume hood, to be After the tetrahydrofuran solvent play to make, into a weighing bottle. The weighing bottle is placed in a vacuum oven at 100 °C ~ 105 °C dried for at least 3h, remove Weighing bottle and cover caps, placed in a desiccator to cool to room temperature and weighed. Then check Sjogren, every 1h, until the last two, said The amount does not exceed the difference between the results of 0.0020g, quality as the basis for the final weighing (m6) result of the calculation.
9 Result of the calculation
9.1 Calculation of heavy oil in the liquefied product
9.1.1 N-hexane insolubles content HI according to formula (1)
HI = (m2-m1) / m x 100% (1)
Where.
HI --- sample of n-hexane insolubles content (%); m2 --- weighing bottle, the quality of the filter cartridge, cotton and n-hexane insolubles and units of grams (g); m1 --- weighing bottle, the quality of the filter cartridge and cotton and, in grams (g); M --- the quality of the sample, in grams (g).
9.1.2 Calculate the mass fraction of heavy products X0 liquefied oil by the formula
X0 = 100-HI (2)
Where.
X0 --- heavy products in mass fraction (%) of liquefied oil.
9.2 Asphaltenes heavy products Calculation
9.2.1 Toluene insolubles content of TI according to equation (3) Calculated
TI = (m3-m1) / m x 100% (3)
Where. TI --- sample mass fraction of toluene insolubles (%);
Quality of m3 --- weighing bottle, filter cartridges, cotton and toluene insolubles and units of grams (g).
9.2.2 Heavy products in asphaltene content Xasp according to formula (4) Calculated
Xasp = HI-TI (4)
Where. Xasp --- heavy products in asphaltene content (%).
9.3 Product before heavy asphaltenes computing
9.3.1 THF insolubles content of THFI according to formula (5) Calculated
THFI = (m6-m4) / m5 x 100% (5)
Where.
--- THFI sample tetrahydrofuran-insoluble fraction of the mass (%);
Quality of m6 --- weighing bottle, paper tubes, cotton wool and tetrahydrofuran-insoluble and, in grams (g); m4 --- weighing bottle, the quality of the filter cartridge and cotton and, in grams (g); m5 --- sample mass, in grams (g).
9.3.2 Heavy product before asphaltene content Xpreasp according to equation (6) Calculated
Xpreasp = TI-THFI (6)
Where. Xpreasp --- heavy products in mass fraction (%) before asphaltenes.
10 Precision of the method
10.1 Repeatability limit
The absolute difference between two independent test results obtained under repeatability conditions at the 95% confidence level should not exceed specified in Table 1.
10.2 Reproducibility limit
The absolute difference between two independent test results obtained under reproducibility conditions at 95% confidence level should not exceed specified in Table 1.
......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 15 pages — is available in the English PDF.
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