活性炭的检测方法之CALGON炭素公司TM-3活性炭糖蜜值的测定(局部)

发布日期:2015-1-29 11:34:34 浏览次数:作者:Admin

CALGON炭素公司检测方法(199510月发布) TM-3  活性炭糖蜜值的测定
1
、适用范围
   本方法专用于测定活性炭的脱色能力。
2
、限定因素
   检测所用糖蜜溶液的浓度依标准炭样而定。当待检活性炭产品糖蜜值的预估值低于350时,须采用250号标准炭样;当糖蜜值的预估值高于350时,则须选用400号标准炭样。不推荐采用分光光度计来替代本方法指定的电子光度计作为检测仪器,只有当建立起两种检测仪器的等量关系数据对比关系之后,才允许采用分光光度计来检测。糖蜜溶液不允许进行稀释。必须采用固定径长2.5mm的比色皿。
3
、检测原理
   用脱色能力未知的炭,及具有250400糖蜜值的标准炭分别处理赤糖糊(blackstrap molasses)的溶液,400号标准炭样用来检测脱色性能曲线扁平区域的数值(见图1)。用一台附带专用颜色过滤器的电子光度计来检测滤液的吸光率,然后用试样与标准炭样的吸光率的比值来计算获得试样的糖蜜值。
4
、安全预防措施
   在操作实验仪器过程中,应保持细心,操作规范,并应具备良好的实验基本技能。与本检测方法有关的所有工作人员均应知悉在检测程序中所用仪器的潜在安全危害性。
5
、仪器
 5.1 烘干炉。能维持150±5稳定温度的电热型强制鼓风烘干炉。
 5.2
平板加热器(可带搅拌器)。能在3.5分钟或更短时间内使50毫升去离子水或蒸馏水达到沸腾状态。康宁公司(Corning)产PC-320型或相似设备。
 5.3
费舍尔电子光度计型双光束色度计(Fisher Electrophotometer Double-Beam Colorimeter)。配备一个最高波长为447nm的专用蓝光糖蜜过滤器工作单元,和一个可容纳一只2.5mm固定径长的Klett-Summerson比色皿(cell)的适配器。适配器和专用蓝光过滤器产自R&D公司。
   Klett-Summerson
比色皿:2。5mm固定径长,光学玻璃材质,产自Hellma公司,该公司联系方式为118-21Queens Blvd, Forest Hills, NY11375, 718-544-9534,地区编号为700.011
 5.4
烧杯。Griffin型,Kimax牌号或Pyres牌号,400毫升容量。仔细检查以确认所使用的所有烧杯的底面玻璃都是平坦的。凹面形或凸面形底面会引起错误结果。烧杯的可供选择的使用标准列于附录B”中,标准化可以提高实验的精密度,但是供应商也许不能做到在所有时间都能供应质量稳定的烧杯。
 5.5
量筒。刻度型,50毫升和1000毫升规格。
 5.6
移液管。50毫升容量。
 5.7
布氏漏斗(Buchner Funnels)。D型,公称尺寸71毫米。
 5.8
烧瓶。250毫升容量,带支管的过滤用烧瓶(Filtering flasks)。
 5.9
滤纸。7厘米的怀特曼(Whatman3号滤纸,或同型号的其它牌号滤纸。
 5.10
真空泵。任意牌号均可,只要能用其获得27#汞的真空度(a vaccum of 27# of mercury)。
 5.11
天平。精确度0.1毫克。
 5.12
数显式热电偶或温度计。在10120范围内具有0.1的检出精度,可每秒钟记录一次温度。
 5.13
秒表。
6
、试剂
 6.1 去离子水或蒸馏水。要求电阻率大于16MΩ·cm(megohms×cm),或电导率小于1微西(μmhos/cm。
 6.2
滤纸悬浮液。将16张圆的怀特曼3号滤纸与1升水加入混合器中,高速混合30秒,然后转移到一个适当的容器中。
 6.3
光谱标定液。用于检定电子光度计的分度值。将约1克铬酸钾(K2CrO4)于105烘干3个小时,称取0。4000克干燥后的K2CrO43.3KOH,放入洁净的,容量为1升的烧瓶中,加入足量的去离子水或蒸馏水使上述试剂溶解,加水至刻度线并充分混合。用去离子水或蒸馏水对仪器进行零位校准,然后将上述光谱标定液注入2.5mm固定径长的比色皿中读取光谱标定液的吸光率,该吸光率数值应在0.0700.090单位范围内,如果上述光谱标定液吸光率不在此限定范围,就必须停用电子光度计并送到制造商那里进行维修或重新校准。
  6.4
糖蜜标准炭样。250400号标准炭样由R&D公司专供。糖蜜值预估数据低于350的所有活性炭产品均采用250号标准炭样,而预估数值高于350的活性炭则选择400号标准炭样。
  6.5
内部使用的标准炭样。取足够数量的糖蜜值在200300范围的炭,并将其制成小于325目的质量比例达95%以上的粉炭,经电炉烘干后,检测获得十组成对的糖蜜值数据。采用这些数据描绘获得SPC图,选用标准的SPC指示线来预测炭的糖蜜值是否超出或低于控制范围。一旦确定了控制范围,就可以在分析炭样之前先分析内部使用的标准炭样,若分析数据在内控区则可进而进行试样分析;若内部标准炭样的分析结果不在控制区,则须重复进行上述一系列步骤操作以确认原因,当内部标准炭样的复测结果仍在控制区内时可继续进行试样分析,当确认内部炭样的复测数据确实超出控制区时则需要标绘复测结果并与标准SPC指示线进行比较以确认偏离方向。

 6.7
糖蜜溶液。用1升去离子水或蒸馏水稀释足够数量的赤糖糊(约50/升),获得的全部糖蜜溶液用250号标准炭处理之后,制成的滤液其吸光率为0.6100.670;当用400号标准炭处理后滤液吸光率为0.3900。410附录A”给出了适用两种标准炭样的糖蜜溶液的制备和标定方法。

1.  APPARATUS
   
1Drying Oven----electrically heated forcedconvertion drying oven capable of maintaining a constant temperature of 150±5.
  2Hotplate/Stirrer----Capable of boiling 50mL of deionized/distilled waterin 3.5minutes or less; Corning Model PC-320 or similar.
 
3Fisher Electrophotometer Double-Beam Colorimeter----Unit equippedwith a special blue molasses filter having a peak wavelength of 447nm and anadapter to accommodate a 2.5mm fixed path length Klett Summerson cell. Adapterand special blue filters are available from R&D.
 
4Klett Summerson Cell----2.5mm fixed pathlength, optical glass; available from Hellma, 118-21Queens Blvd, Forest Hills.NY 11375,718-544-9534;Part No.700.011.
 
5Beaker----Griffin type, Kimax or Pyrex brand400mL. Inspect all beakers to insure the bottom of the glass is flat. Concaveor Convex shaped bottoms will give erratic results. Optional Standardizationfor Beakers included in Appendix B. Standardization will improveintralaboratory precision, however suppliers may not be able to supplyconsistent beakers over time.
 
6Cylinders----Graduated, 50mL and 1000mL.
 
7Pipette----50mL Volumetric.
 
8Buchner Funnels----Size D,71mm ID.
 
9Flasks----Filtering flasks with sidearm,250mL.
 
10Filter paper----Whatman No.3,  175pxor similar.
 
11Vacuum Pump----Any unit capable of pulling avacuum of 27#of mercury.
 
12Balance----Capable of weighing to thenearest 0.1mg.
 
13Digital Thermocouple/Thermometer----Capableof measuring to the nearest tenth of a degree between 10 and 120, updating the reading at least every second.
 
14Stopwatch

2。  REAGENT
 
1Deionized/Distilled Water----Resistivitygreater than 16 megohms×cm or conductivity less than 1 μmhos/cm is recommended.
 
2Filter Paper Suspension----Add 16 circles ofWhatman No.3 filter paper and one liter of water to a blender. Mix on high for30 seconds. Transfer to a suitable container.
 
3Spectral Standard----This solution is usedto check the calibration of the Electrophotometer. Dry approximately 1 gram ofPotassium Chromate, K2CrO4, at 105 for three hours. Weigh 0.4000 grams of the driedPotassium Chromate and 3.3 grams of Potassium Hydroxide, KOH, and transfer to aclean 1 liter volumetric flask. Add enough deionized/distilled water todissolve the reagents. Dilute to the mark with deionized/distilled water andmix thoroughly. Zero the instrument on deionized/distilled water. Read theabsorbance of the Spectral Standard in the 2.5 mm fixed path length cell. Theabsorbance should fall between 0.070 and 0.090. units. If the absorbance of theSpectral Standard falls outside these limits, the Electrophotometer must beremoved from service and sent to the manufacturer for repair and recalibration.
 
4Molasses Standard Carbons----The 250 and 400Standard Carbons are available exclusively from R&D. The 250 StandardCarbon is to be used for all activated carbon products having a predictedmolasses number less than 350. For activated carbons having a molasses numbergreater than 350, a 400 Standard Carbon is to be used.
 
5Internal Carbon Standard----Obtain asufficient quantity of carbon having a molasses number etween 200 to 300 andpulverize to 95%, 325 mesh. Oven dry the carbon and determine ten replicate molassesnumber analyses of the carbon. Using the data obtained from the ten replicates,establish an SPC chart. Use standard SPC guidelines to calculate upper andlower control limits for the carbon. Once the limits are established, analyzethe Internal Carbon Standard before analyzing samples. If the result is foundto be in-control, proceed with sample analysis. If the result isout-of-control, steps must be taken to determine the cause for theout-of-control result. Once a result is obtained for the Internal CarbonStandard that is in-control, proceed with sample analysis. Continue to plotresults and follow standard SPC guidelines for determining out-of-controltrends for the Internal Carbon Standard.

 
7Molasses Solution----Dilute a sufficientquantity (approximately 50 grams/liter) of blackstrap molasses with one literof deionized/distilled water total volume to produce a filtrate with anabsorbance of 0。610 to 0。670 when treated with Molasses 250 Standard Carbon,and an absorbance of 0。390 to 0。410 when treated with Molasses 400 StandardCarbon。 See Appendix A for Preparation and Standardization of the MolassesSolution for both Standard Carbons。

木质粉状活性炭的质量只能根据不同的用途提出不同的质量指标。通常我们主要从木质粉状活性炭的含水率、挥发分率、灰分率及固定碳含量、发热量来衡量木质粉状活性炭的质量。http://www。gyjylc。com/content/?140。html

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