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High-frequency infrared carbon and sulfur analyzer dosage study with porcelain crucible reuse and flux


Simple high-frequency infrared carbon and sulfur analyzer operation, accurate results rapidly, is widely used in pig iron sulfur, sulfur in silicomanganese alloy analysis. Since pure co-solvent consumption, high cost analysis, the paper porcelain crucible reuse and reducing the amount of flux added to test a lot of work, proved by analysis of pig iron or steel samples for analysis of sulfur porcelain crucible can be reused, saving co-solvent improves the quality of the analysis also reduces the cost of analysis.

      Test Part 1

      1.1 Instruments and reagents

      On Haide Kai HCS-140-type high-frequency infrared carbon and sulfur analyzer; special porcelain crucible (at about 1000 ℃ high temperature furnace burning 4h to blank the lowest value); flux: metal grains, 425 mm (40 mesh); metallic tin grain; crumb-like iron.

      1.2 Analysis conditions

      Pig Iron S: shortest analysis time 25s, the longest analysis time 50s; sulfur cutoff level 7; sample weight is about 0.200g; silicomanganese, ferromanganese S: ??shortest analysis time 35s, the longest analysis time 50s; sulfur cut-off level of 7; sample weight is about 0.200g; oxygen input pressure are about 0.3Mpa.

      1.3 Experimental Methods

      1.3 .1 iron sulfur analysis:

      Weigh about 0.200g of the sample in the high temperature-treated has a new (or used once, twice) crucible, was added about 1.4 g of (crucible used only about 0.9g) of metallic tungsten particle flux, press Determination analysis conditions [2].

      1.3.2 silicomanganese, ferromanganese sulfur analysis:

      First Weigh about 0.200g (crucible used only about 0.150g) metallic tin particles at high temperature has been a new (or used once, twice) in the bottom of the crucible, the balance to zero, weigh about 0.200g sample cover thereon, said after the sample volume entered into the computer, then add approximately 0.250g of pure iron flux of about 1.4g (crucible used only about 0.9g) of tungsten metal particle flux overlying sample press analysis condition analysis.

      2 Results and discussion

      2.1 Comparison of blank value

      The blank value is the key to affect the results of the blank value of the new porcelain crucible and reusable porcelain crucible after pretreatment temperature, see Table 1. Table 1 New crucible reuse of the crucible sulfur blank values ??(n = 6) of the crucible using the conditions of the new crucible blank average crucible sulfur crucible third use second use (%) 0.000170.000150.00012 standard deviation S (% ) 0.0000760.0000780.000068

      2.2 Test sample weight

      Infrared carbon and sulfur analyzer analysis iron sulfur, test the sample weight 0.100g-0.600g of the plurality of data from said measured sample volume found in 0.200g-0.500g did not affect the results, in order to improve efficiency, and more good re-use and conservation of the crucible amount of flux, the choice of analysis of pig iron, ferro-manganese and silico-manganese sulfur, said sample is about 0.200g.

      2.3 crucible Reused test

      It was found that the analysis of pig iron (or steel-like)) when sulfur sample more likely to burn completely, less flux type, amount less, to ensure the results are stable and suitable for reuse. However, when using the crucible 3 times and then carry out the 4th analysis, slag crucible easily spill, burner fouling more difficult to maintain, after analysis of the crucible melt more, high temperatures, strong liquidity, taking under unsafe. Experimental results show that the choice analyzed pig iron (or steel-like) crucible be reused three times better.

      2.4 flux amount

      Test during the test found that the crucible be reused, since the metal oxide slag in the crucible improved combustion environment, and the more metal oxide slag, combustion also increases the flow plate, used as a porcelain crucible blank analysis when flow is about 300mA, used twice a porcelain crucible flow analysis reaches a blank around 350mA, oxide slag sample analysis will help melt after effects, it may be appropriate to reduce the amount of flux. When the crucible reusable analysis iron sulfur again, test the amount of tungsten flux from 0.50g ~ 1.20g, we found that when tungsten flux added is less than 0.800g, the combustion plate flow is low, about 310mA, the crucible the melt flow weakened, analytical data fluctuate, when the amount is more than 0.800g burning flow is 380mA or more complete combustion sample analysis results are stable. In order to facilitate the operation and to ensure that the result is stable, tungsten flux added volume is selected as about 0.900g, and specially prepared a volume of approximately 0.900g special spoon. Crucible reusable analysis of silicomanganese, ferromanganese sulfur, tin tablets tested, iron, tungsten particle measurement results of different proportions, found that when the amount of tin particles added 0.150g, iron 0.250g, tungsten particles 0.900g when the measurement results are stable.

      2.5 Accuracy and precision test

      Selection of pig iron, SiMn standard sample and a sample for analysis has been determined by the analytical conditions were measured with a sulfur content of the new crucible and crucible reuse analysis results are shown in Table 2 and Table 3.

      2.6 re-use storage time test crucible

      According to the continuity of the laboratory work, and just burn the high temperature of the crucible, the crucible is generally used directly stored in steel containers within the opening, since the moisture in the air, dust will be absorbed by the crucible, it affects the results, so the repeated crucibles used may be stored for test results shown in Table 4.

      Results Table 4 shows that: the longer the crucible stored reusable sulfur analysis blank value is greater, and the relative standard deviation is also growing, until it does not meet the analytical requirements. Therefore, when stored in open containers, the longest not more than two days; when stored in a dryer, for no longer than four days.

      3 Conclusion

      3.1 Test results show that the crucible reuse, blank value of sulfur is low, it does not affect the results of the analysis, and the analysis again sample crucible melt fluidity, analysis better, so porcelain crucible reuse is feasible.

      Crucible metal oxide slag 3.2 reusable help melt effects, so again for the analysis of a sample may be appropriate to reduce the amount of flux added; repeated use porcelain crucible, can save a lot of porcelain crucible, but also saving two-thirds of the new crucible pretreatment required electricity and other costs, reduce the cost of analysis, according to our laboratory using a crucible and a flux month average calculation, cost savings of about 1,600 yuan / month, the annual cost savings 20,000 yuan, and to a certain extent, but also improve the quality of the analysis.

      3.3 In order to maintain a consistent base and analytical conditions, thereby reducing the error results when the analysis of the sample with a new crucible and standard samples must also use new crucible analysis, a correction factor; crucible Similarly use reusable analysis, the correction coefficient should also be used by the same number of crucibles analysis results.

      3.4 specimen must be complete primary combustion, slag crucible bottom should be flat and smooth. So we chose to analyze iron (or steel-like) crucible reuse, analysis of finished iron alloy crucible no longer used. But analysis ferroalloys, pig iron or better analyzed using a kind of crucible steel analysis results, we recommend using the analysis crucible reusable analysis.

      3.5 The test results found that: Crucible reusable storage time should not be too long, so as not to absorb moisture from the air, dust, impact analysis results: best used when stored in an open container or on duty in the next class, for no longer than two day; extended stored in the dryer to about 4 days.


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