基于系统工程法的沉积物分析体系及诊断技术

doi:10.16085/j.issn.1000-6613.2020-1170

摘要/Abstract

摘要：

目前沉积物（污垢）组分分析没有现成的标准分析方法，系统故障诊断和清洗非常困难。为了解决这一问题，本文利用系统工程理论，构建了由基础分析体系和随机分析体系组成的污垢综合分析体系，对垢样组分分析，定性诊断系统的腐蚀、结垢、堵塞等障碍。研究了由X射线荧光光谱（XRF）无标样半定量分析及定性评估确定随机分析体系组成，马弗炉协同ICP-OES准确定量并直接读取基础分析体系和随机分析体系组分含量，污垢综合分析体系测定含量合计在100%±5%（5%为误差合计）为有效，结果归一化；然后根据垢样分析结果及垢样外观，结合工况，通过诊断技术，诊断系统障碍并及时整改。以某煤化工企业水洗水换热器和液氨蒸发器调节阀门污垢为例，XRF测定垢样康普顿线比率在0.967～0.981，说明结果可靠，由此确定随机分析体系组成；ICP-OES测定各组分元素工作曲线相关系数均在0.999以上，线性较好，由此准确定量各组分含量，各元素在垢样中的检出限为0.0004%～0.0010%。垢样中的各种成分的含量均反映某种倾向，通过现场工况和诊断技术，查找故障原因，经整改措施后及时解决了系统故障。研究结果表明：污垢综合分析体系及诊断技术能全面、客观、系统地反映垢样组成；并简便高效、快速准确分析和诊断煤化工换热器、过滤器、塔、管道、阀门等污垢的组分及系统故障。

关键词: 系统工程, 沉积物, 分析体系, XRF无标样分析, ICP-OES定量, 诊断技术, 腐蚀, 结垢

Abstract:

At present, there is no standard analysis method for the analysis of sediment (fouling) components, and it is very difficult to diagnose and clean the system. In order to solve this problem, using the system engineering theory, a comprehensive analysis system of fouling composed of a basic analysis system and a random analysis system was constructed to analyze the scale-like components and qualitatively diagnose the corrosion, scaling, and blockage of the system. The research is composed of XRF standard-free semi-quantitative analysis and qualitative evaluation to determine the random analysis system. The muffle furnace cooperates with ICP-OES to accurately quantify and directly read the content of the components of the basic analysis system and the random analysis system. It is valid at 100%±5% (5% is the total error), and the results are normalized; then according to the analysis results of the scale samples and the appearance of the scale samples, combined with the working conditions, through the diagnosis technology, the system obstacles are diagnosed and rectified in time. Taking the fouling of the control valve of the water washing heat exchanger and liquid ammonia evaporator of a coal chemical enterprise as an example, the ratio of the scale sample Compton line measured by XRF is 0.967—0.981, indicating that the result is reliable, and thus the composition of the random analysis system is determined; ICP-OES The correlation coefficient of the working curve of each component element is above 0.999, and the linearity is good. From this, the content of each component is accurately quantified. The detection limit of each element in the scale sample is 0.0004% to 0.0010%; various components in the scale sample The contents all reflect a certain tendency. Through on-site working conditions and diagnostic techniques, the cause of the fault is found, and the system fault is solved in time after rectification measures. The research results show that: the comprehensive analysis system and diagnostic technology of the scale can comprehensively, objectively and systematically reflect the composition of the scale sample; and it is simple, efficient, fast and accurate to analyze and diagnose the scale group of coal chemical heat exchangers, filters, towers, pipes, valves, etc points and system failures.

Key words: systems engineering, sediments, analysis system, XRF standard-free sample analysis, ICP-OES quantification, diagnostic technology, corrosion, fouling

中图分类号:

TQ016.5⁺5

娄红杰, 张先松, 姜兴剑, 黄起中, 刘威, 何建华, 周苗苗, 胡艳晶. 基于系统工程法的沉积物分析体系及诊断技术[J]. 化工进展, 2020, 39(S2): 97-105.

Hongjie LOU, Xiansong ZHANG, Xingjian JIANG, Qizhong HUANG, Wei LIU, Jianhua HE, Miaomiao ZHOU, Yanjing HU. Sediment analysis system and diagnosis technology based on system engineering method[J]. Chemical Industry and Engineering Progress, 2020, 39(S2): 97-105.

图/表 8

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序号	元素	线性范围/μg·mL^-1	线性方程	相关系数	检出限/%
1	铁	0～20.00	C=0.000002432 I-0.064203838	0.99993	0.0004
2	铝	0～20.00	C=0.000010297 I+0.066971519	0.99993	0.0004
3	钙	0～20.00	C=0.000005408 I-0.015359218	0.99998	0.0006
4	镁	0～20.00	C=0.000018777 I-0.007440642	0.99997	0.0005
5	锌	0～20.00	C=0.009800177 I+0.068958491	0.99995	0.0005
6	铜	0～20.00	C=0.000001403 I+0.107832931	0.99990	0.0004
7	铬	0～20.00	C=0.000004030 I-0.100648503	0.99991	0.0005
8	钾	0～20.00	C=0.000000313 I+0.106970959	0.99978	0.0007
9	磷	0～20.00	C=0.093384396 I-0.124892455	0.99969	0.0010

序号	元素	线性范围/μg·mL^-1	线性方程	相关系数	检出限/%
1	铁	0～20.00	C=0.000002432 I-0.064203838	0.99993	0.0004
2	铝	0～20.00	C=0.000010297 I+0.066971519	0.99993	0.0004
3	钙	0～20.00	C=0.000005408 I-0.015359218	0.99998	0.0006
4	镁	0～20.00	C=0.000018777 I-0.007440642	0.99997	0.0005
5	锌	0～20.00	C=0.009800177 I+0.068958491	0.99995	0.0005
6	铜	0～20.00	C=0.000001403 I+0.107832931	0.99990	0.0004
7	铬	0～20.00	C=0.000004030 I-0.100648503	0.99991	0.0005
8	钾	0～20.00	C=0.000000313 I+0.106970959	0.99978	0.0007
9	磷	0～20.00	C=0.093384396 I-0.124892455	0.99969	0.0010

序号	分子式	质量分数/%	定性评估	康普顿线比率
1	Al₂O₃	53.20		0.981
2	Cr₂O₃	16.3
3	P₂O₅	12.50
4	Si0₂	11.70
5	Fe₂O₃	2.51
6	CaO	1.79
7	MgO	1.70
8	ZnO	0.17
9	CuO	0.10
10	TiO₂	0.07	可忽略不计
11	K₂O	0.03	可忽略不计
12	SrO	0.01	可忽略不计
13	ZrO₂	0.01	可忽略不计

序号	分子式	质量分数/%	定性评估	康普顿线比率
1	Al₂O₃	53.20		0.981
2	Cr₂O₃	16.3
3	P₂O₅	12.50
4	Si0₂	11.70
5	Fe₂O₃	2.51
6	CaO	1.79
7	MgO	1.70
8	ZnO	0.17
9	CuO	0.10
10	TiO₂	0.07	可忽略不计
11	K₂O	0.03	可忽略不计
12	SrO	0.01	可忽略不计
13	ZrO₂	0.01	可忽略不计

序号	分子式	质量分数/%	定性评估	康普顿线比率
1	Fe₂O₃	93.29		0.967
2	SiO₂	3.98
3	AL₂O₃	1.76
4	CaO	0.27
5	MgO	0.14
6	K₂O	0.12
7	Na₂O	0.09	可忽略不计
8	CuO	0.08	可忽略不计
9	Cl	0.08	可忽略不计
10	ZnO	0.06	可忽略不计
11	P₂O₅	0.05	可忽略不计
12	Cr₂O₃	0.02	可忽略不计
13	TiO₂	0.02	可忽略不计
14	BaO	0.02	可忽略不计
15	Ce₂O₃	0.009	可忽略不计
16	SrO	0.007	可忽略不计
17	As₂O₃	0.007	可忽略不计
18	ZrO₂	0.002	可忽略不计