【国家标准(GB)】 磷铁化学分析方法气体容量法测定碳量

中华人民共和国国家标准
磷铁化学分析方法
气体容量法测定碳量
Methods for chemical analysis of ferrophosphorusThe gasometric method for the determinationof carbon content
本标准适用于磷铁中碳量的测定。测定范围：0.400%～1.200%。UDC 669. 15'779
GB 8705.2-88
本标准遵守GB1467—78《治金产品化学分析方法标准的总则及一般规定》。1方法提要
试样置于管式燃烧炉中加热并通氧燃烧，生成的二氧化碳等混合气体经除硫后收集于量气管中，然后以氢氧化钾溶液吸收其中的二氧化碳，吸收前后体积之差即为二氧化碳体积，再换算为碳量。2试剂及材料
2.1助熔剂：锡粒（0.4~~0.8mm）、铜、铁粉、五氧化二钒等。助熔剂中含碳量不大于0.002%。石棉纤维。
碱石灰或氢氧化钠。
氧化铝：活性、粒状。
二氧化锰：活性、粒状。
硫酸(p1.84g/mL)。
硫酸0.1+100）：滴加甲基红溶液呈红色。铬酸饱和的硫酸溶液：于硫酸(2.6)中加重铬酸钾或铬酸酐至饱和，使用其上部澄清溶液。氢氧化钾溶液（40%）。
氯化钠溶液（26%）：以甲基红溶液作指示剂，滴加硫酸（1+1)至酸性。氧气：纯度大于99.5%。
3仪器及设备
3.1气体容量法定碳装置如下图。中华人民共和国治金工业部1988-02-02批准372
1989-03-01实施
GB 8705.2~-8 8
1一氧气瓶，2一氧气表，3一缓冲瓶：4一微型转于流量计;5.6一洗气瓶，7、8一干燥塔：9-~高温然烧管：10--管式燃烧炉：11—石摘纤维：12—除硫管，13—容量定碳仪(包括：冷凝管 a、量气管 b、水推瓶 c、吸收器 d.小活塞 e、三通活塞f、游度计 g), 14一高温控制器:15—磨砂玻璃塞；16—瓷盘
3.1.1洗气瓶(5)：内装铬酸饱和硫酸溶液(2.8)。3.1.2洗气瓶(6)：内装碱石灰或氢氧化钠。3.1.3干燥塔（7、8)：内装氧化铝（2.4）。3.1.4高温燃烧管（9)：±×L，mm：23~24×600。3.1.5管式燃烧炉(10)：可调节电流以保证燃烧试样所需温度。3.1.6石棉纤维（11)：灼烧至无碳。3.1.7除硫管（12)；内装二氧化锰(2、5）。3.1.8瓷舟（16）：长88mm或97mm，应预先于1200℃管式燃烧炉中通氧灼烧至无碳，也可于1000C高温炉中灼烧4h以上，冷却后于盛有碱石棉（或碱石灰）和无水氟化钙的未涂油脂的干爆器中。下载标准就来标准下载网
3.1.9量气管（b）：内链鼠化钠溶液（2.10）或硫酸溶液（2.7）。每格刻度为0.05mL，它是在16C、101.32kPa(760mmHg）标准状况下刻制的。3.1.10吸收器(d)：内盛氢氧化钾溶液(2.9)。3.1.11小活塞(e)：有--方可通大气。3.2长钩：用低碳镍铬丝或耐热合金丝制成。3.3水银气压计：气压值应按公式（1)校正：p= p* (1 -- 0. 000 163t - 0. 002 6cos2@— 0. 000 000 2H)式中：P~--校正后的气压值，kPa;pr
一水银气压计测得的气压值，kPa;t水银气压计所在处温度，℃
一水银气压计所在处纬度，，
H --水银气压计所在处海拨高度,m。573
4试样
GB 8705.2—88
磷铁试样应全部通过0.088mm筛孔。5分析步骤
试样量
按表1称取试样和助熔剂。
助熔剂量(任选其一)，8
0.400~1.200
5.2空白试验
试样量
随同试样做空白试验。
5.3分析前的准备
铜或氧化铜
0. 5 ~~1. 0
五氧化二钒
0. 5 ~~ 1. 0
氧化铜+
五氧化二钒
0. 5~~1. 0
铁粉+
氧化铜
0. 5~1, 0
五氧化-·钒
+铁粉
(1--1)
0. 5～1. 0
将炉温升至1200～1350℃，检查管路及活塞是否漏气、装置是否正常，燃烧标准试样，检查仪器及操作。
5.4测定
将试样（5.1）置于瓷舟（3.1.8）中，按表1覆盖助熔剂，将瓷舟推入高温燃烧管温度最高处，立即塞紧磨砂玻璃塞（15），将氧气表上的三通活塞（f)打开，一边调节氧气流速至120～140mL/min，一边通氧约3min，使高温燃烧管中的温度恒定。按容量定碳仪操作规程，将混合气体导入量气管，定容、吸收后，测量其读数，并确认残留的气体体积没有变化后，启开磨砂玻璃塞，用长钩将瓷舟拉出，检查熔块，确认燃烧完全后，将残留气体放空。6计算
按公式（2)计算碳的百分含量：C(%) (VIA-V.A)-VeA× f× 100m
式中：A
温度16℃，气压101.32kPa，用酸性作封闭液时，封闭液面上每毫升二氧化碳中含碳量A值为0.0005000g：用氯化钠酸性溶液作封闭液时A值为0.0005022g；V.——混合气体的体积，mL;
V，—一残留气体的体积，mL；
V。—-空白试验的气体体积，mL；m试样量，g;
温度、气压校正系数，见附录A中表A1或表A2。371
允许差
GB8705.2-88
实验室之间分析结果的差值应不大于表2所列允许差。表2
≥0.400~1.200
允许差
GB8705.2—88
气体容量法测定碳的温度、气压补正系数表附
（本表用1：1000
lo.7740.771j0.7680.764i0.7610.7570.7540.750l0.7460.7430.739/0.735.732/0.7280.7240.7200.7160.7120.7770.773:0.7700.7660.763/0.7590.756|0.752/0.7480.7450.741j0.7370.7340.730|0.726|0.7220.718|0.714o.779/0.7750.7720.768/0.7650.7610.7580.7540.7510.7470.7430.7400.736o.7320.7280.7240.720/0.716o.7810.777/0.7740.7700.7670.7630.7600.7560.753j0.7490.7450.7420.7380.7340.7300.7260.7220.718j0.7830.7790.7760.772l0.7690.7650.7620.7580.755l0.751j0.7470.74410.7400.736.0.7320.7280.7240.720jo.78510.7810.778j0.7740.7710o.767j0.764/0.7600.7570.7530.749/0.746i0.7420.738j0.7340.730l0.72610.7220.7870.7840.780:0.7770.7730.7690.7660.7620.7590.7550.7510.748.0.744.0.7400.7360.7320.7280.724lo.7890.786o.7820.779.0.7750.7710.7680.7640.7610.7570.7530.7500.7460.7420.7380.7340.730/0.726j0.7910.788o.7840.7810.77707740.770o.7660.7630.7590.7550.752/0.7480.7440.7400.7360.7320.728l0.793/0.7900.786j0.783'0.7790.77610.7720.768j0.7650.761/0.757/0.754/0.750l0.746l0.742/0.7380.7340.7300.7950.792.0.7880.785l0.781j0.778.0.774j0.7700.7670.7630.759/0.756j0.752/0.7480.744.0.740j0.7360.7320.797.0.794.0.790.0.7870.7830.780:0.776l0.7720.769j0.765jo.761j0.758.0.7540.7500.7460.7420.7380.7340.8000.96j0.7920.7890.7850.782j0.7780.7740.7710.67o.763o.600.7560.7520.748o.7440.7400.36o.802j0.7980.795io.7910.7870.7840.780.0.7760.773j0.769/0.765o.7620.7580.7540.750j0.7460.742j0.7380.8040.8000.7970.7930.7890.7860.7820.7780.7750.7710.767l0.764/0.7600.7560.7520.7480.74j0.7400.8060.8020.9907950920.788.840810.7770.7730690.766j620580.7540.750.460.742j0.8080.804j0.801j0.7970.794/0.7900.786j0.7830.779/0.775/0.7710.7680.764j0.760.0.756j0.7520.7480.744lo.8100.8060.B03o.7990.7960.7920.7880.7850.7810.7770.773j0.7700.7660.7620.758j0.754o.7500.7460.8120.8090.8050.8010.798j0.7940.7900.787l0.7830.779i0.7750.7720.7680.7640.7600.7560.7520.7480.8140.8110.8070.803/0.8000.7960.7920.789o.785,0.7810.7770.7740.7700.766j0.7620.7580.754/0.7500.8160.813:0.8090.8050.8020.7980.7940.7910.7870.783/0.7790.7760.77210.768/0.7640.7600.7560.7520.8180.8150.8110.808j0.8040.8000.7960.7930.789/0.7850.782i0.7780.7740.770i0.766j0.7620.7580.754.0.8200.817io.8130.8100.806o.8020.7990.7950o.791o.787l0.783/0.7800.7760.7720.768/0.764fo.7600.7560.8230.819:0.8150.8120.808/0.8040.8010.7970.7930.789:0.785j0.7820.7780.7740.770/0.766j0.7620.75810.8250.8210.817:0.8140.8100.806:0.8030.7990.7950.791.0.7880.7840.7800.7760.7720.7680.7640.7600.827'0.8230.8190.8160.8120.8080.8050.8010.797/0.793:0.7900.7860.7820.7780.774:0.7700.7660.7620.8290.8250.8220.8180.8140.8100.807/0.8030.7990.7950.7920.7880.7840.780.7760.7720.768jc.764（补
充件；
的硫酸溶液作封闭液）
GB.8705.2--88
1mbar=0.750mmHg
(1bar10’Pa)
o.7080.7040.7000.696jo.692/0.687o.6830.6780.6740.6690.6640.659o.6540.6490.64410.6390.6330.6280.622i0.6160.7100.706l0.7020.698/0.6940.689o.6850.6800.6760.6710.666l0.6610.6560.651o.6460.6400.6350.629/0.624l0.6180.7120.7080.7040.700/0.695o.6910.6870.682/0.6770.6730.6680.6630.658j0.6530.6480.6420.637.0.6310.6260.6200.7140.710/0.7060.702/0.6970.6930.6890.684/0.6790.675/0.6700.665l0.660/0.6550.650:0.6440.639/0.633/0.627/0.622lo.7160.7120.7080.7040.6990.695/0.6910.6860.681/0.6770.6720.667/0.6620.657/0.651/0.6460.6410.635/0.629/0.623lo.718/0.140.7100.760.7010.97o.6930.6880.68306780.674o.669/0.6640.59/0.6530.6480.6420.6370.6310.62o.7200.7160.712lo.708/0.7030.6990.6940.6900.6850.6800.6760.671o.666/0.6600.6550.650.0.6440.639/0.6330.627o.7220.718/0.7140.7100.7050.7010.696/0.692/0.6870.6820.677/0.6720.667/0.662/0.657/0.6520.6460.6410.6350.629jo.724/0.720jo.716o.711o.707/o.703j0.6980.694/0.689/0.6840.679i0.674o.669/0.664/0.6590.6540.6480.642i0.6370.631o.7260.722o.7180.7130.709/0.7050.700/0.6960.6910.6860.6810.676o.6710.6660.661o.6550.6500.6440.6380.6330.728/0.7240.720/0.715/0.7110.707/0.7020.697l0.693/0.6880.6830.678/0.673/0.6680.6630.6570.6520.646l0.6400.6340.7300.726/0.722/0.717lo.713/0.708/0.7040.6990.695/0.690/0.685.0.680/0.675/0.6700.665/0.6590.6540.648:0.6420.636jo.7320.7280.724/0.719o.7150.710j0.7060.7010.697/0.6920.687:0.6820.677/0.6720.666/0.6610.6550.6500.6440.638(o.7340.7300.725o.7210.717o.7120.7080.7030.698/0.6940.6890.684/0.679o.6740.668/0.6630.6570.6520.6460.6400.736j0.732/0.727lo.723/0.719/0.7140.7100.7050.700.0.696/0.6910.686lo.681o.676/0.670/0.6650.6590.654/0.6480.6420.738/o.7340.729/0.725/0.721/0.716/0.712:0.7070.702/0.698/0.6930.6880.683j0.678/0.6720.6670.6610.6550.650/0.644o.740/0.7350.7310.727/0.722/0.718/0.714/0.709i0.704/0.6990.695/0.690j0.684/0.679j0.6740.668/0.6630.657/0.6510.645o.7420o.738o.733j0.729o.725jo.720j0.716lo.711jo.706j0.701l0.6960.691o.686jo.6810.676.0.670lo.665j0.659i0.6530.6470.744/0.7390.735/0.7310.7260.722/0.717/0.7130.7080.7030.6980.6930.6880.683/0.6780.6720.6670.6610.655/0.6490.7460.7410.737/0.7330.7280.7240.7190.7150o.710.0.705/0.700i0.6950.690.0.685.0.6800.6740.6690.6630.657/0.651o.7480.743/0.7390.7350.730jo.7260.7210.717/0.7120.707/0.7020.697/0.69210.6870.6810.6760.6700.6650.6590.6530.7500.745(0.7410.737/0.732/0.7280.7230.7190.7140.7090.704:0.699/0.6940.6890.6830.6780.6720.6670.6610.6550.7520.747/0.743/0.739/0.734/0.730l0.7250.7200.716/0.7110.706,0.7010.696/0.6910.6850.6800.6740.6680.6630.6570.754/0.7490.745o.741o.736o.732j0.727lo.7220.718.0.713j0o.7080.7030.698j0.692i0.6870.6820.6760.6700.6640.658j0.7550.751/0.747l0.7430.7380.7340.7290.7240.72010.715i0.710.0.7050.700/0.6940.6890.6830.6780.672.0.6660.6600.7570.753j0.749j0.744/0.740o.735/0.7310.7260.7210.717/0.7120.707i0.7010.6960.6910.6850.6800.674:0.6680.6620.7590.7550.7510.746j0.7420.737/0.733/0.7280.7230.718:0.7140.708/0.7030.6980.693:0.6870.6820.6760.6700.664577
GB8705.2--88
0.8310.827/0.8249
0.8200.816
0.8090.8050
07970794
0.7900.7860.7820.7780.7740.77010.7660,8330.829/0.826/0.8220.818l0.815/0.8110.807/0.803/0.7990.7960.792/0.788/0.784i10.780/0.776j0.7720.7680.8350.8310.828|0.824j0.820/0.817/0.8130.809/0.805/0.802/0.7980.7940.790l0.78610.782/0.7780.7740.7700.8370.8330.830|0.826/0.8220.8190.8150.8110.8070.804/0.800/0.796/0.7920.788:0.7840.780/0.776j0.771o.839/0.8360.832/0.828/0.8240.8210.817o.8130.8090.806/0802/0.798/o.7940.790:0.786jo.7820.7780.7730.8410.838o.834/0.830o.826/0.8230.819/0.8150.8110.8080.804/0.00/0.7960.7920.7880.7840.780/0.775o.8430.8400.836/0.832/0.829/0.8250.821017/0.8130.100.8060.8020.7980.7940.7900.786/0.782/0.7770.8450.842o.8380834o.8310.8270.8230.819/0.8160.8120.808/0.040.8000.7960.792/o.788j0.7840.779(0.848/0.8440o.8400.836/0.8330.829/0.8250.8210.818/0.14/0.8100.806/0.802o.7980.794/0.790/0.7860.7810.8500.846/0.842/0.838/0.835/0.831/0.827/0.8230.82010.816/0.812/0.8080.8040.800/0.796j0.792/0.788l0.7830.8520.848/0.844j0.8410.8370.8330.8290.825j0.822/0.8180.814/0.100.8060.802j0.798/o.7940.7890.7850.854/0.8500.846|0.843/0.839/0.8350.8310.827/0.824:0.8200.816/0.812/0.808/0.8040.800/0.796/0.7910.7870.856/0.8520.848/0.845/0.841o.837/0.8330.8300.826/0.8220.818/0.8140.8100.806/0.8020.7980.7930.79o858/0.8540.850/08470.8430.839/0.8350.8320.828/0.824/0.82008160.8120.88/0.8040.8000.7950.7910.8600.8560.8530.8490.8450.8410.8370.8340.8300.826/0.8220.818/0.8140.8100.8060.8020.797/0.7930.8620.8580.855/0.85.8470.8430.390.8360.8320.8280.8240820/0.16/0.81208080.8040.799/0.7950.8640.8600.8570.8530.8490450.8420.380.834/0.300.826j0.822/0.818o.8140.8100.80608010.7970.866/0.863/0.859/0.855/0.8510.8470.844:0.840/0.836i0.8320.8280.824/0.8200.816/0.8120.8080.8030.7990.8680865/.8610857/0.853/049/0460.8420380.834/0.8300.826/0.822/0.818/0.140100805080jo.8710.8670.863/0.859/o.855/0.852o.8480.8440.8400.836/0.8320.8280.824/0820j08160.8110.807/o.8030.8730.8690.8650.8610.570.85408500.8460.8420.838/0.8340.830082608220.818/081308090.8050.875io.871jo.867:0.863j0.859/0.856.0.852/0.848/0.8440.840/0.836/0.8320.8280.824l0.820.0.815/0.811j0.8070.877/0.873j0.869/0.865j0.862/0.8580.854.0.8500.846'0.8420.838/0.834l0.8300.826l0.8220.817l0.813/0,8090.879/0.875l0.871/0.867/0.8640.860j0.856/0.8520.848j0.8440.8400.8360.8320.828jo.8240.8190.815/0o.8110.8810.877/0.8730.870/0.866/0.862/0.858/0.8540.8500.846/0.8420.8380.834/0.830/0.826/0.8210.817/0.813jo.8830.879/0.8750.8720.868/0.864/0.860/0.560.8520.848/0844/0.8400.836j0.320828/0.8230.19/0.150.8850.881/0.878/0.874i0.870/0.866|0.862/0.8580.854j0.850j0.846/0.8420.838/0.834/0.8300.8250.8210.8170.887/0.883j0.880/0.8760.8720.868/0.864i0.860.0.856j0.852/0.848/0.8440.840i0.836lo.832/0.827b.8230.819j0.889/0.886l0.882/0.878/0.8740.8700.866i0.862:0.8580.854/0.850l0.8460.8420.83810.834/0.829/0.8250.821表A1
GB 8705.2 ---88
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GB 8705.2
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GB8705.2-88
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GB 8705.2-88
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GB8705.288
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