JB/T 6623-1993 Determination of sulfur content in flexible graphite sheets JB/T6623-1993 Standard download decompression password: www.bzxz.net

Mechanical Industry Standard of the People's Republic of China
JB/T 6623--93
Determination method of sulfur content in flexible graphite plate
Published on May 7, 1993
Ministry of Machinery Industry of the People's Republic of China
Implementation on January 1, 1994
Mechanical Industry Standard of the People's Republic of China
Determination method of sulfur content in flexible graphite plate" Subject content and scope of application
This standard specifies the test method for measuring the sulfur content of flexible graphite plate by combustion and heating method. This standard is applicable to the determination of sulfur content in flexible graphite plate. The constant value is 0.05%~1.5%2. Method summary
JB/T 6623-93
The sample is burned in oxygen to oxidize and decompose sulfur in various forms into sulfur-reducing compounds. The solution is dissolved in an emulsified hydrogen sulfide solution to form an acid, and then titrated with a sodium hydroxide standard solution.
3 Reagents and materials
3. Sulfur content: Use a standard sample containing less than 5% sulfur. J.2 Carrier gas, purity greater than 59.5%
3.3 Acid solution (0.05 + 190%)
3.4 ​​Sodium hydroxide standard solution (NeOH> 1 mL). Dissolve 4 mL of sodium hydroxide in 101 mL of water, add 1 mL of the newly prepared barium hydroxide saturated solution, drain, and filter out the precipitate. Put it into a closed material bottle. 3.5 Sodium red-substantially colored indicator
1 part 0.1% nitric acid blue ethanol 2 parts U.S. 1% methyl red ethanol solution. 3.6 Chemical absorption liquid
Add 1mL of material into 100mL of ice, add methyl red and methyl blue mixed indicator; 10 drops, use dilute acetic acid (specified in Section 3.3) until it melts and turns red-purple. 3. Acid (density 1.84g/mL),
3.8 Potassium hydroxide solution (40%).
1 Instruments and devices
fluorescein: length 100mm, inner diameter 1Rm
quartz: length 100mm, width 12mr. height 13m Tibetan burette: sub-scale n. 1 ml.a fixed avoid absorption - female bottle (see Figure 1 www.bzxz.net
tubular high temperature combustion furnace: with adjustment device, thermal power account and value indicating instrument; fixed research and prohibition device (see 2)
Ministry of Machinery Industry 19938507 approved
1994 01 01 implementation
JB/T6623-93
Figure 1 actual pea collection bottle
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Figure 2 fixed flow installation diagram
1--oxygen cylinder, 2-new pressure damage, S maximum design: 440% installed gas, 1-law age shortness of breath: 6, drying tower, to build, 7-high combustion tube, B-high temperature combustion furnace 5-energy rise: 1 quality will control device (with thermocouple) 11-replacement damage: 12-absorption bottle, 17-Test titration 5 Sample and its preparation
5.1 The sample to be tested shall not be less than 20g. The surface of the sample shall be clean, oil-free and dust-free. 5.2 Take square test pieces of the same size from the diagonal of the test plate at equal distances, and the total weight shall not be less than 19g. 5.3 Quartering method: Divide each of the three samples into two parts, one for the test sample and the other for the reserved sample. 5.4 Cut the sample with stainless steel scissors or scissors, and dry it in an oven at 1C5-110℃ for 1 hour. , put it in the blasting device to cool and standby, 6 test steps
6.1, control diagram 2 connect fixed vegetables to replace salt part, 6.2 adjust the temperature control variable, make the furnace rise to 1250 ℃ 720 ℃, oxygen valve, check whether the device is gas-free, note, pass the air bottle to one end with a spring light, open the spring at the carrier gas inlet, if there are no bubbles, it is considered that the device is gas-free. 6.3 add 80~100ml of industrial absorption liquid (according to Article 3) in the absorption bottle, 2730 ~900mL/min flow rate for 5 mil to drive out carbon dioxide in the absorbent and residual gas in the circuit. Then add sodium oxychloride standard solution to make the absorbent bright green.
6.4 Weigh 0.5~7g test solution (depending on the content of sodium oxychloride), accurate to C.003. Pre-lighten the 1250℃ calcined porcelain, push the porcelain boat into the high temperature part of the asset management center with a nickel wire hook, and quickly plug it (pay attention to the seal). After passing 700~ScCmL/mm2
JR/T6623-93
oxygen for 12~15mil, use the standard sodium oxychloride solution to absorb the color from white to bright green as the end point. Stop oxygen flow, record the consumption of hydrogen peroxide, weigh 0.5~1 standard, and reduce it to 0.00U3B. Perform combustion test in steps 6.1~6.4. Use an empty boat that has been burned at 1250℃ in advance, and then perform empty test in steps 6.1~G. 7. Calculate the analysis results. Calculate the hydrogen peroxide consumption according to formula (1). T-
V - V: × 100
The titration of sodium hydroxide standard solution on vegetables/standard test volume g
The total volume of standard sample, 5%;
The volume of sodium hydroxide standard solution consumed by the titration sample, L: The volume of sodium hydroxide standard solution consumed by the empty test. mL 7.2 Calculate the vegetable content in the sample according to formula (2), 4: S
The titration content calculated in the test, %
The volume of sodium hydroxide standard solution consumed by the titration sample m: The sodium hydroxide standard solution consumed by the empty test sample. mL: The titration of sodium hydroxide standard solution on death, al. The result obtained by the test plate
should be expressed as a small percentage, expressed as the arithmetic mean value of the network parallel determination, 8 allowable difference
The cumulative difference of two parallel determinations should not be greater than the difference listed in the following table, change
Test according to the data
2e. 1~u. S0
Indicate the standard number
Material name, brand, specification. Manufacturer
Testing unit name, sample number, number:
Commissioning unit:
Test results, in Ppm form;
Testing unit, test date, tester. e. For
Additional instructions:
.JB/T: 6623-93
This standard is proposed by the Hefei General Machinery Research Institute of the Ministry of Machinery Industry. This standard is developed by the Mechanical Products Research Institute of the Dongxin Electric Carbon Factory of Shanxi Sichuan Baigong. The main drafters of this standard are Xu Pufang and Dai Yingchi.
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