GB/T 5686.6-1988 锰硅合金化学分析方法气体容量法测定碳量 GB/T5686.6-1988 标准下载解压密码：www.bzxz.net

中华人民共和国国家标
锰硅合金化学分析方法
气体容量法测定碳量
Methods for chemical analysis of silicomanganese allayFhe gastmetric method for the detcrminationol carbon content
本标准适用于锰硅合金中碳量的测定。测定范围：0.100%～4.000%，UDC 669. 74' 782
GB 5686. 6 ---88
本标准遵守GB1467-…78冶金产品化学分析方法标准的总则及-般规定》。1方法提要
试样置于管式然烧炉中加热并通氧燃烧，生成的：氧化碳等混合气体经除硫后收集于量气管中，然后以却氧化钾溶液吸收其中的二氧化嵌，吸收前后体积之差即为一氧化碳体，再换算为碳量。2试剂及材料
助熔剂：锅粒(0.4~0. 8 mm)、铜、铁粉、五化二等，助熔剂中含碳不人于 0. 002%。2.2石棉纤维。
2.3碱石灰或氢氧化伪，
2.4氧化铝：活性、粒状。
二氧化锰：活性、粒状。
硫酸( p 1. 84 g/mL)。
硫酸（0.1±100):滴加甲基红溶液呈红色2.8铬酸饱和的硫酸溶液：宁蔬酸（2.6）中加重饹酸钾或铬酸酐至饱和使用其上涩清溶液。2.9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（11）至酸性、氧气：纯度大于99.5%。
3仪器及设备
3.1气体容法定碳装骨如下图。
3.1.1洗气瓶（5):内盛铬酸饱和的硫酸溶液（2.8)。3.1.2洗气瓶(6)：内装破石火或氢氧化3.1.3干燥塔（7.8)：内装氧化铅（2.4)。高温燃烧管（9)：Φ×T，，mn;23～24×600。3. 1. 4
管式燃烧炉（10);可调节电流以保证燃烧诚样所需温度。3.1.6石棉纤维（11):灼烧至无碳。3.1.7棕硫管（12)：内装一氢化锰（2.5）中华人民共和国治金工业部1958-02-02批准1989-03.01实施
1氧气瓶：2一氧气表18一缇冲瓶：4-微型转于流计，、6洗气瓶：「、·十燥饼;9高温境管;10管或燃烧炉，1一石糖红维，12一除硫管，15—密取定碳位(包括;冷凝管a、气管b、水准瓶c、吸收器d、小话案 c、三通活塞f、激度计g),14一高温控制墨，15一磨砂恶璃案，16-瓷归
3.1.8瓷舟（16）：长88mm或97mm，应预先十:1200℃管式燃烧炉中通氧灼烧至无碳，也可干1000℃高温炉中均烧4h以上，冷却后旺于盛有碱石棉（或城石炭）和无水愈化钙的未涂油脂的干燥器中。
3.1.9量气笋（b）内盛氯化钠溶液（2.10）或硫酸溶液（2.7）。每一格刻度为0.05mL，它是在16℃101.32kPa（760mmHg)标准状况下刻制的。3.1.10吸收器据（d):内盛氢氧化钾溶液（2.9)。3.1.71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战。3.3水银气压计：气压值应按公式（1）校止：P -P/ (1—0. 000 163 t -0. 002 6 c8s240. 000 000 2 11)戏中，P
-校正后的气床值,kPa,
一水银气压计测得的气压,kPa，t-水银气压计所在处温度，℃;
中·水银气压计所在处纬度.；下载标准就来标准下载网
4试样
水银气压计所在处游拨高度，m。锈硅试样府全部通过0.125mm筛批。5分析步骤
5. 1试样量
按表1称取试样和熔剂。
0. 400~1. 200
>1.200-2, 50
>2.50~4.00
5.2空白试验
试样域
随同试样做空白试验。
5.3分析前的准备
GB 5686.6-88
赵化铜
汇氧化
0. 5--1, 0
鼠化+五氧
铁粉+氢化钢
花二钒
(1: 1)
0. b~1, 0
0. 5-~1. 0
+铁粉
0, 5 --1, c
将炉温升至1200～1350℃，检查管路及活塞是节漏气、装置是否正带，燃烧标准试样，检查仪器及燥作。
5. 4测定
将试样5.1）置于瓷盘（3.1.8）中，按表1覆盖助焙剂，将瓷舟推入高温燃烧温度最商处立即塞紧磨砂离塞（15)，将载气表上的三通活寒（f）打开，--近谢节氧气流速至120140 mL/min。边通氧约3 min，使高溢然烧管的温度恒定。按容虽定碳仪操作规程，将混会气体导入量气管，定窄、吸收后，测量其读数，并确认残留的气体体积效有变化后，启开磨砂玻璃寒,用长钩将瓷舟拉，检查器块，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(%)-- :A=4)-Y4×IX100
式中：A
16℃气压101.32kPa，用酸性水作封闭液时，封闭滤面上每毫升二氧化碳含碳量A值为0.00050008：用氛化钠酸性溶液作封闭液时A值为0.001522g：混合气体的体积，L；
W，残留气体的体积，n!.;
一空自试验的气体体积,mL：
m二一试样电，B：
广—-溢度、气压校正系数，见附录A表A1或表A2。7允许差
实验室之间分析结果的差值应不大下表2 所列允许差。表2
400~1.205
>1.200~2.503
>2. 54--4. 06
Gk 5686.6—88
气体容量法测定碳的温度
气压补正系数表
（本表用1：1000
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的硫酸溶液作封闭液）
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10541,001.04610411037l1032,102B/121091.141,0091005100009909910609810.91,057/10521.0481.0431,0391.0341030.1.0251,0211.0161011/1.0071.0020,9970,9930,s880,9830,978100990
1063105a,t.054i1.0491045/1.0401036.103/1.0271.0221018|1.01310081.0030.909/0.9940.989.0.98d1,0651.060/1.0561.9511.017;1.042.1.0381.0331.0291.0241.0201.0151,0101.0051.001/0.9960,991i0,9881067162105b10541.049/10441040103510311.0261022.10171121.00710030.9980.0030.98
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