天然气 用气相色谱法测定组成和计算相关不确定度 第8部分：用微型热导测定氢、氧、氮、一氧化碳、二氧化碳和C1至C5和C6+的烃类 编制说明

《天然气用气相色谱法测定组成和计算相关不确定度第8部分：用微型热导测和C6+的烃类》编制说明一、任务来源及工作简要过程 21、任务来源 22、标准主要起草单位、参加单位 23、工作简要过程 24、工作组成员 二、编制原则 4三、标准技术内容说明 51、背景 2、主要技术内容 四、采标情况 24五、与有关的现行法律、法规和强制性国家标准的关系 24六、重大分歧意见的处理经过和依据 25七、作为强制性国家标准或推荐性国家标准的建议 25八、贯彻标准的要求和措施建议 25九、废止现行国家/行业标准的建议 25十、重要内容的解释和其他应予以说明的事项 252本项国家标准的修订任务来源于国家标准化管理委员会下达计划：国标委发3及研究项目工作会，会上对项目的工作方案、进展情（5）2023年4月~5月：根据工作方案，组织配置不同浓度的天然气组分气体标准4刘明亮：中国石油化工股份有限公司天然气榆济管道分公司郭哲：国家管网集团联合管道有限责任公司5TCD）的原理与传统的热导检测器是一样的，但是由于其采用先进的微机电加工技术（MEMS）制作而成，具有体积小，质量小，功耗低、灵敏度微型热导检测器 微型热导检测器其中的一个流通池只通载气，称之为参比通道；而另一个流通池流过色谱柱的流出物--6控制，微型进样器的进样量是μL级别，配套使用毛细柱或微柱，分为独立的2～3个检和GB/T37124-2018《进入天然气长输管道的气体质量要求》气质仲裁方法，进样系统标法等分析方法。GB/T27894《天然气用气相色谱法测定组成和计算相关不确定度》其中涉及采用毛细柱的色谱仪主要为FID+TCD检测器的实验室色谱仪，并非微型热导色谱。GB/T17281-2016《天然气中丁烷至十六烷烃类的测定气相色谱法》是参考的应用领域也在稳步扩展，天然气管网中，具有微型化特性的色谱仪（AGILENT、而微型色谱仪采用微型阀控结构进行流程控制，分为独立的2～3个检测单元完成气质72、应用微机电加工技术制作的微型色谱具有其具有死体积小、耗气量少、灵敏度3、微型色谱进气量小，流量低，特别对于在线分析应用场景，有必要规范其旁通1Agilent490、990离线2ElsterEncall3000C1~C6+、CO2、N2在线3Daniel370C1~C6+、CO2、N2在线4InficionMicroGCFusion离线5ABBNGC8206C1~C6+、CO2、N2在线6国家管网GW1025-208-ZXSP/BXSP在线/离线7APIXCHROMPIX2/CHROMEX离线/在线及控制方法，选择适宜的分析方法，对微型气相色谱本文件按照GB/T1.1—2020给出的规则及我国气体组分含量测量过程及结果相关8组分和一氧化碳适用浓度参考GB/T13610设定，因为该标准适用范围最广，且与型气质组成浓度访问；氢气浓度范围设置为（已经将氢气最大比例提升至20%）比现有气质组分（如无额外单位标注，则统一为mol%最大值：红色标记，最小值：黄色nC4nC5neoC5N2654482011000000012383099唐山LNG外输06070组分GB/T13610ISO6974-3ISO6974-4ISO6974-5ISO6974-6GB/T17747.2氦气0.01~100.01~0.5--0.002~0.50~0.5氢0.01~100.01~0.5--0.001~0.5氧0.01~20--0.007~5氮0.01~1000.001~150.007~400~200.01~1000.001~100.05~150.001~100~200.01~10040~1000.01~1000.001~100.002~150.01~1000.001~150.001~30.05~100.001~50~3.50.01~100.0001~20.001~10.01~20.0001~10.01~100.0001~20.001~10.01~20.0001~10.01~20.0001~10.001~0.50.005~0.350.0001~0.50~0.50.01~20.0001~10.001~0.50.005~0.350.0001~0.50~0.50.01~20.0001~10.001~0.50.005~0.350.0001~0.50~0.5正己烷0.01~20.0001~0.5--0.0001~0.50~0.1碳六加0.01~1-0.001~0.20.005~0.35--一氧化碳0.01~10~3组分测定范围（摩尔分数/%）氢0.01~30氧0.01~5氮0.01~400.01~300.01~1000.01~350.01~150.01~100.01~100.01~20.01~20.01~20.01~1一氧化碳0.01~1气体标准物质选择。使用单点校准时，标准物质浓度配置应当符合GB/T13610规样品测定中分别规定了离线和在线分析的注意进样要求，特别由于水分子将导致对本文件规定方法的测定范围、线性、精密度根据表4中本文件适用的组分浓度范围，配置11瓶摩尔分数y/%组分123456789氧0.01000.05020.5045.02氮0.01000.05010.5034.9810.0019.9939.60二氧化碳0.01010.04980.5075.0010.0019.9729.7099.8799.3598.7093.4886.7948.6264.9443.7950.0322.7213.820.009970.049800.50035.005.0220.0丙烷0.009960.049780.5005.0214.90异丁烷0.01010.05020.5062.004.999.96正丁烷0.009930.050060.5052.004.989.95新戊烷0.01000.05000.4990.987异戊烷0.009930.050860.5020.9912.00正戊烷0.009960.049570.4982.02正己烷0.009920.050360.4950.20一氧化碳0.010300.050500.5070.980.20氢0.010100.049400.0990.496001.240002.005.0220.0010.40温度5～40）℃,相对湿度20～85）%，仪器周围无强烈机械震动和电磁干AkbN2iC4H10nC4H10neoC5H12iC5H12nC5H12nC6H14BkbN2iC4H10nC4H10neoC5H12iC5H12nC5H12nC6H14CkbN2iC4H10nC4H10neoC5H12iC5H12nC5H12nC6H14DkbN2C2H6C3H8iC4H10nC4H10neoC5H12iC5H12nC5H12nC6H14EkbN2C2H6C3H8iC4H10nC4H10neoC5H12iC5H12nC5H12nC6H14AkbC2H6[0.00997-0.500]、(0iC4H10[0.0101-0.506]、(0.nC4H10[0.00993-0.505]、(0.iC5H12[0.00993-0.502]、(0.nC5H12[0.0100-0.498]、nC6H14[0.0099-0.495]、BkbC2H6[0.00997-0.500]、nC4H10[0.00993-0.505]、(0.iC5H12[0.00993-0.502]、(0.CkbC2H6[0.00997-0.500]、nC4H10[0.00993-0.505]、(0.iC5H12[0.00993-0.502]、(0.DkbC2H6[0.00997-0.500]、nC4H10[0.00993-0.505]、(0.iC5H12[0.00993-0.502]、(0.EkbiC4H10[0.0101-0.506]、(0.50nC4H10[0.00993-0.505]、(0.iC5H12[0.00993-0.502]、(0.50nC5H12[0.0100-0.498]、(0nC6H14[0.0099-0.495]、(0使用表4试验样气，依据GB/T6379.2《测量方法与结果的准确度（正确度与精密测试结果使用分段线性拟合后，按照GB/T6379202122再现性限为0.1271%是由于某实验室测试结果在该分段区间拟合效果＜0.99%，不纳入23摩尔分数重复性再现性绝对摩尔分数/%绝对摩尔分数/%X≤0.10.010.010.1<x≤10.020.10.220.4注：这些值是通过现场试验获得的，验证了方法的可行性。但是不能与GB/T27894其他章节中附录所包含的数据相比。STCD＝AFC／m（2）式中：STCD——热导检测器的灵敏度，mA——正丁烷的峰面积的算术平均值，μV·sFC——校正后的载气流速，mL／minm＝CMV／22.4M——正丁烷的摩尔质量，g／mol；（4）TTj——压力梯度校正因子。（5）p024使用B单位在线色谱仪测试灵敏度，结果见表31，测试结果可见，微热导法气相CMVZmAFc3S2526ABCDInficionMicroGCFusionE表A.1A单位分析仪设备信息气相色谱条件柱Ⅰ柱Ⅱ柱Ⅲ柱Ⅳ色谱柱类型MS5AMS5APoraplotUAl2O3/KCl色谱柱规格10m*0.25mm*30μm20m*0.25mm*30μm10m*0.25mm*810m*0.25mm*4μm柱前压温控程序进样时间4030反吹时间/表A.2B单位分析仪设备信息气相色谱条件柱Ⅰ柱Ⅱ柱Ⅲ色谱柱类型色谱柱规格柱前压(kPa)柱箱温度程序(℃)进样时间(ms)反吹时间(s)7表A.3C单位分析仪设备信息气相色谱条件柱Ⅰ柱Ⅱ柱Ⅲ色谱柱类型MS5APPU5CB色谱柱规格6m柱前压(kPa)200kPa200kPa100kPa柱箱温度程序(℃)恒温80℃恒温60℃恒温55℃进样时间(ms)40ms40ms40ms27反吹时间(s)无反吹表A.4D单位分析仪设备信息气相色谱条件柱Ⅰ柱Ⅱ色谱柱类型RT-Molesieve5ART-Q-Bond色谱柱规格10m×0.25mm×20μm12m×0.25mm×8μm柱前压22psi20psi温控程序60℃保持150s,2.5℃升温至220℃保持6s。60℃保持40s,1℃升温至220℃保持20s。进样时间100ms50ms反吹时间//表A.5E单位分析仪设备信息气相色谱条件柱Ⅰ柱Ⅱ柱Ⅲ柱Ⅳ色谱柱类型MS5A(Ar)MS5A(He)PoraplotUPDMS色谱柱规格15m0.25mmMS5A15m0.25mmMS5A10m0.25mmPoraPlotU10m0.25mmPDMS柱前压(kPa)200200柱箱温度程序(℃)7060进样时间(ms)----反吹时间(s)254028摩尔分数y/%连续10次进样的峰面积平均值SDRSD1234567890.0100.1450.1450.1460.1460.1460.1460.1470.1470.1470.1470.146310.000700.48%0.0500.5180.5200.5200.5200.5200.5200.5200.5200.5210.5210.519840.000620.12%0.1000.9870.9880.9880.9880.9880.9890.9890.9890.9890.9890.988230.000650.07%0.5034.8004.8014.8034.8034.8044.8044.8044.8044.8044.8054.803280.001660.03%1.009.7219.7169.7179.7189.7199.7199.7199.7209.7209.7219.719000.001570.02%4.9847.82647.82947.83047.83047.97747.97747.97748.00048.02948.05647.933120.092900.19%10.090.78790.80690.81490.81690.82990.83590.83690.83790.83890.83990.823810.017260.02%20.0179.900179.915179.935179.939180.087180.219180.248180.365180.573181.094180.227550.377670.21%39.6329.224329.364329.371329.389329.393329.394329.394329.399329.439329.441329.380710.060480.02%摩尔分数y/%连续10次进样的峰面积平均值SDRSD1234567890.01024.725.625.525.024.924.825.025.225.624.825.10050.34431.37%0.05058.057.255.655.754.957.056.055.255.555.956.11110.97861.74%105.397.195.596.797.296.397.495.297.60213.21573.29%0.503397.1397.6397.5397.7395.5395.7396.1397.3396.82090.89510.23%750.2767.1771.0766.4768.3768.7768.6765.73637.00840.92%4.984301.14283.74333.64290.74263.74276.54273.14288.889723.15230.54%298679.78662.58654.38658.08649.08657.28659.88660.07839.65290.11%20.016515.716603.316582.816626.716653.616661.616685.616618.479657.34730.35%39.630921.431055.231104.931110.431201.231205.931232.831236.931133.5874108.77620.35%摩尔分数y/%连续10次进样的峰面积平均值SDRSD1234567890.0104644465246694684470847214731473347494780470744.10710.94%0.050158641588915890159021590515912159151592715930159551590925.33530.16%308473085330854308563085930878308833089230894308963087119.28040.06%0.503151733151847151855151942151961151981152010152094152184152285151989164.59360.11%3023383041853048543055243056603057023057343059743059743060373051981159.18600.38%4.98149094814931091493410149380914943841495995149644014979811498290150072514955092930.27310.20%282767828291942841317284222028435662844437284508728451852845217284560828409516749.92980.24%20.05471646547514254820045483459548836454991685505578550689855095325650114550719152006.57490.94%39.610016142100174141001865710018986100190191002842110029900100302471003101110032021100241826584.17350.07%摩尔分数y/%连续10次进样的峰面积平均值SDRSD1234567890.010823.9825.1825.4831.3833.0833.4833.4833.6835.2835.5830.96524.42520.53%0.0502905.92908.42910.42910.52911.22912.32913.62913.72915.92916.82911.85553.33940.11%5608.85621.65632.85641.15660.45674.75677.15687.95702.45782.65668.915749.99990.88%0.50326709.126761.926776.426783.126788.826798.926803.826809.826825.026856.326791.319039.19000.15%53869.853899.153939.253957.953978.953982.954041.054052.654058.254081.253986.070071.35120.13%304.98266653.7266662.3266767.7266816.1266949.7266958.1266983.0266988.9267129.6267844.4266975.3490341.59460.13%484257.6484373.8484420.1484581.3484605.9484639.6484748.5484808.0485122.7485147.7484670.5160296.55870.06%20.0946163.6946251.7948169.8949077.4951210.3951840.0952252.1952422.2954716.0959666.2951176.90704090.39860.43%39.61676622.41678186.61680812.91682188.21683250.61685389.51686416.51689117.11689792.31691177.41684295.33304948.32940.29%摩尔分数y/%连续10次进样的峰面积平均值SDRSD1234567890.0101.25110.01861.49%0.0503.23.23.23.23.33.33.33.33.33.43.27020.05961.82%4.84.84.84.84.84.84.84.94.95.04.82780.07181.49%0.50325.625.625.725.725.825.826.026.026.226.425.89880.25320.98%47.847.947.948.048.048.048.148.248.448.548.06820.23110.48%4.98233.9234.0234.0234.1234.4234.8234.8234.9235.0235.6234.54200.55750.24%/////////////20.0/////////////39.6249.3249.6249.6249.6249.6249.7249.8249.8249.9249.9249.66970.17270.07%摩尔分数y/%连续10次进样的峰面积平均值SDRSD1234567890.01010.06780.06770.06770.06780.06780.06780.06790.06790.06790.06800.067840.000100.15%0.04980.3680.3680.3680.3680.3680.3680.3680.3680.3680.3680.3680.000130.04%0.7480.7480.7480.7480.7480.7480.7480.7480.7480.7480.7480.000150.02%310.5073.8133.8143.8143.8153.8153.8153.8153.8153.8163.8163.8150.001000.03%7.6147.6157.6157.6177.6177.6177.6187.6197.6197.6207.6170.002090.03%5.0037.69737.69837.70737.71037.71137.72737.73637.74037.74437.74937.7220.019440.05%72.27772.28572.31672.32672.32872.33072.33272.34272.34272.34872.3230.023800.03%20.0140.274140.565140.573140.707140.777140.794140.929140.986140.986141.048140.7640.242110.17%29.7194.019194.039194.069194.202194.208194.223194.4010.111440.06%摩尔分数y/%连续10次进样的峰面积平均值SDRSD1234567890.01018.68.58.68.79.08.78.98.78.88.98.742120.151311.73%0.049842.342.542.742.542.542.342.342.542.542.642.4600.133980.32%84.383.984.583.484.284.383.884.584.584.584.2090.374050.44%0.507426.5424.4424.4426.2427.1427.4426.6425.5427.2425.8426.0931.077400.25%822.5822.9824.7821.2821.3820.9824.7824.6823.8824.3823.0761.536320.19%5.004155.14194.44189.74141.94197.44147.14180.64150.74200.04154.64171.15023.283340.56%8291.28284.08283.98255.78294.48296.98302.48298.58221.88301.98283.07025.509740.31%20.015774.015870.015839.015827.015901.015699.015910.015794.015911.015839.015836.40067.458960.43%29.722633.022635.022575.022558.022646.022646.022531.022641.022642.022651.022615.80043.774170.19%摩尔分数y/%连续10次进样的峰面积平均值SDRSD1234567890.010138543867388138903892390839103921393139433899.728.20.72%0.04981981719842198591988119882198861989320227204272063720035.1290.21.45%324032340355403574039540400404294043940444404524053040412.459.80.15%0.507201747201965201993202057202068202073202111202232202266202316202082.8165.60.08%402076402180402219402265402364402408402556402646402687403146402454.7316.10.08%5.0020016282001902200316120032442003415200341920034792003775200380620072192003504.81500.10.07%39471073947175394728639474623948279394957339496893950011395046439520963948914.21706.80.04%20.078777797886046789672979006977901997790362579037287903958790401979074217898599.99416.20.12%29.71120596411208106112106231121351511215743112172351121888511220353112237951122402411215824.36252.30.06%摩尔分数y/%连续10次进样的峰面积平均值SDRSD1234567890.0101217.4217.9218.6219.6219.7220.1220.8221.7222.1223.9220.182401.999690.91%0.04981154.41155.31156.51157.21158.51158.51158.71159.41159.61162.11158.0382.253180.19%2337.42340.72344.22350.72354.22355.72358.32361.22363.82364.32353.0459.592670.41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