Journal of Analysis and Testing

, Volume 1, Issue 4, pp 267–273 | Cite as

Recent Development of Gas–Solid Phase Chemiluminescence

  • Dingkun Zhang
  • Jin-Ming Lin


Serving as a classic and interesting strategy, gas–solid phase chemiluminescence (CL) has recently been a rapidly growing area where CL is emitted through chemical reactions between gas and solid reactants occurred on the surface of solid matter. This CL system provided a sensitive and simple spectral method for investigating gas–solid phase reactions while information on the rate constants, intermediate productions, surface states and reaction mechanisms of interaction could be acquired. Recent progresses mainly concentrate on development of new gas–solid phase CL systems and their practical applications. This review paper summarized main classifications, mechanisms and applications of gas–solid phase CL. The future prospects for gas–solid phase CL are discussed.


Gas–solid phase chemiluminescence Recent development Main classifications Mechanisms Applications 

1 Introduction

Chemiluminescence (CL) is the light emitted during chemical reactions where unstable products are evolved in the reaction process. These intermediates transformed from electronically excited to ground state with CL emission as energy release (> 45 cal/mol) [1]. Since the fireflies and other luminescent organisms in the environment have been found, CL has aroused considerable interest for deeper research and application [2]. Definitely, CL analysis has excellent advantages including high sensitivity, low background interference, highly responsive signals, safe operation process and portable equipment [3], which has been applied to detection towards the concentration of catalyst, reactant, CL inhibitor and enhancer [4]. A great many articles have reported the applications of CL in environmental analysis [5], medical diagnosis [6], health management [7], food safety [8] and pharmaceuticals [9], etc.

Among numerous branches of CL systems, acting as a classic and interesting strategy, gas–solid phase CL has recently been a rapidly growing area. Such CL evolves in infrared, visible, and even in ultraviolet regions through chemical reactions between gas and solid reactants on the surface of solid matter. It acts as an indicator and monitor of gas–solid phase reactions to provide information during the process of reaction [10]. Moreover, this strategy also enables investigations of gas–solid phase reactions through sensitive and simple spectral method [11]. In addition, application of gas–solid phase CL has extended to gas-phase and solid-phase diagnose and detection due to its strong intensity of signals and unique property. Over decades of years of investigation and development, gas–solid phase CL has become an effective detection method in analytical chemistry. Recent progress mainly focuses on development of new gas–solid phase CL systems and their practical applications, while many interesting results have been reported. Obviously, the excellent sensitivity and intensity of gas–solid phase CL has made it a good candidate as a novel CL technology, which has revealed great potential for future analysis and test.

Considering the aforementioned properties, gas–solid phase CL have received considerable attentions in different areas of CL analysis. The present paper introduces the main classifications including O3-solid, O2-solid, “S-based”-solid, H2-solid and CO-solid CL systems. Besides, specific mechanisms, applications and future prospects of gas–solid phase CL are also covered.

2 Main Classifications of Gas–Solid Phase CL

2.1 O3-Solid System

2.1.1 O3–Ba System

Serving as a critical oxidant for decades of researches and applications, O3 specializes in strong oxidizability, high speed, efficient sterilization and disinfection, no secondary pollution and cheap source. It is not surprising that many studies have been accomplished on investigating reactions between O3 and other molecules through CL strategy. Definitely, most researches concentrate on traditional gas–gas and gas–liquid phase based on O3 oxidation, while gas–solid phase CL analysis has received little attention owing to its incomplete transformation. However, previous articles also reported some interesting results with obvious CL signals. Since Ar matric with Ba atoms has displayed special aberration comparing with traditional CL performance, while the CL intensity increases with raised temperature, which has aroused interest of many researchers. Pimentel et al. [12] investigated CL performance between O3 and Ba in solid Ar at temperatures below 15 K where obvious CL signal was detected in the spectral region of 5500–7300 Å. It was found that Ba was oxidized by O3 to evolve BaO* (Eq. 1) [13] in the ã 3Σ+\( \tilde{X} \) 1Σ+ transition. Subsequently, some Ba atoms would be excited by BaO* via near resonant energy transfer process with 6s6p 1P → 6 s2 1S transition (Eq. 2) [14].
$$ {\text{Ba}} + {\text{O}}_{3} = {\text{BaO}}^{*} + {\text{O}}_{2} $$
$$ {\text{BaO}}^{*} + {\text{Ba}} = {\text{BaO}} + {\text{Ba}}^{*} $$

2.1.2 O3–Ca System

It is reported that CL effect of CaO has shown wide emission bands including green, orange and red region when reacting with oxidants, which is different from the ways of traditional transitions, where upper electronic states and lower states lead to long-time emission. Lee et al. [15] studied CL performance in the 4300–6600 Å region with reactions between O3 and Ca in solid Ar. It was observed that d 3∆ → a 3∏ and D 1∆ → A1∏ transitions occurred in CaO through oxidation by O3 (Eq. 3) [16]. Similarly, energy transfer from CaO* to Ca also existed through 1P(4s4p) → 1S(4 s2) and 3P(4s4p) → 1S(4 s2) transitions (Eq. 4) [17].
$$ {\text{Ca}} + {\text{O}}_{3} = {\text{CaO}}^{*} + {\text{O}}_{2} $$
$$ {\text{CaO}}^{*} + {\text{Ca}} = {\text{CaO}} + {\text{Ca}}^{*} $$

2.1.3 O3-Alcohols, Phenols and Saccharides System

As is widely known that alcohols, phenols and saccharides have always been used as ideal antioxidants or reductants, It is of great importance to investigate the redox reactions between these species and oxidants performed with gas–solid phase interaction. Lin et al. [18] reported gas–solid phase CL effect between O3 and solid alcohols, phenols and saccharides. Obvious CL was obtained with interactions occurring at the surface of solid powder. Definitely, evolution of ROOOH intermediate through oxidation of O3 and subsequent release of emissive 1O2 molecule resulted in such strong CL intensity (Fig. 1).
Fig. 1

CL spectra and mechanism of reactions between O3 and solid alcohols, phenols and saccharides powders [18]

2.2 O2-Solid System

2.2.1 O2–Na System

O2 has always played as an effective oxidant towards all kinds of solid reactants for so many years. Researchers found that freshly cut Na would emit faint green light, which opens a new area of luminescence by Na metal. In 1931, Bowie [19] has investigated the color and intensity of CL emitted by solid Na existed in the air. He found that relevant intensity ranged from 3.5 to 10.5 × 10−7 lumens per square inch of the surface of Na and the CL spectrum was composed of a band of 5000–5300 Å. The CL intensity was too much low and corresponding color was green. He also investigated the mechanism within this process and believed that the CL has close relationship with formation of hydroxide from the moisture in the air where the breaking of H–O bond within a vaporous and polar molecule played as the main role [20].

2.2.2 O2-Fuel System

Investigation towards reactions of fuel will definitely acquire the information on ballistic property, which in return guides further modification and development. Campbell and Hulsizer [21] obtained the CL spectra of ammonium perchlorate composite solid propellant burned in the combustion zone. They found that A 2Σ+ electronic state of OH· was evolved in the flame, while these short-lived OH· also exist in the place very far from the surface of propellant. This system facilitated investigating the internal energy levels of ground and excited state during the process of combustion occurred at the surface of solid propellant.

Researches towards combustion in hybrid rocket motors in real condition is challenging due to complicated process and many interference factors. The introduction of CL strategy has offered an excellent solution. Jens et al. [22] studied combustion of solid hydrocarbon fuel in a turbulent boundary layer by CL imaging strategy, which is a typical combustor within hybrid rocket motors. O2 stream flew through solid fuel grain in the combustor and CL was generated simultaneously. The data also revealed that CL intensity was roughly proportional to the burn rate of fuel (Fig. 2).
Fig. 2

Facility and image of CL analysis. a Facility for investigating combustion of solid hydrocarbon fuel through CL imaging technology; b detailed structure within combustor and c CL image of combustion of fuel. Boundary layer edge (blue line), lame location (magenta dots) and initial fuel grain shape (orange line) were drawn on original grey image [22]

2.2.3 O2-Polymer System

Research towards oxidation of polymer via CL strategy has enabled evaluation of oxidation mechanism, rate constant and further application of such process. Zlatkevich [23] utilized CL method for discussing heterogeneous oxidation of polypropylene. This work pointed out the erroneous evaluation of the activation energies and interpretation by previous articles. He also believed that experimental support is inadequate while the evolution of volatiles in the induction process also lacked sufficient consideration.

2.3 “S-Based” Solid System

2.3.1 S2-Solid Ar System

Since S atom was observed to have the tendency to recombine in solid Ar to generate obvious CL in the spectrum ranging from 365 to 555 nm [24], the unique luminescence property of S-based gas–solid phase CL system has been widely studied. Pimentel [25] explored the CL effect of S2 in solid Ar and found that reaction between two ground state S atoms would produce excited S2 (Eq. 5) [26]. Subsequently, two kinds of transitions of S2 also occurred as c 1Σ u  → a 1 g and A3 u  → X 3Σ g with emission in 6680–8750 and 5580–6890 Å, respectively.
$$ 2{\text{S}}({}^{3}{\text{P}}_{2} ) \to {\text{S}}_{2}^{*} $$

Kiljunen et al. [27] also investigated electronic structure and short-range recombination dynamics of S2 in solid Ar by classical molecular dynamics simulations. Result showed that S atom separated by closest distance of the lattice would recombine immediately even at 1 K with excitation energies of 2 eV or more to give excited S2.

2.3.2 SO-Solid Ar System

Due to the excitation of S2 has been revealed to evolve excited electronic state, it is natural to pay attention to its analogous species SO, which will also produce similar state and provide the information of reaction process. Pimentel et al. [28] reported the first observation of transition of SO in solid Ar through CL strategy. He claimed that reactions between ground state O and S atoms would give electronic excited SO (Eq. 6) [29] where transition of \( \tilde{c} \) 1Σã 1∆ of SO existed. Besides, combination of two S atoms would also produce excited S2 (Eq. 5). It was also notable that excited S atom was generated through energy transfer mechanism (Eq. 7) [30].
$$ {\text{O}} + {\text{S}} = {\text{SO}}^{*} $$
$$ {\text{S}}_{2}^{*} + {\text{O}}_{2} = {\text{SO}}_{2} + {\text{S}}^{*} $$
Smardzewski et al. [31] also concentrated on the CL of SO in solid Ar and he found that the red (490–870 nm) and blue (385–600 nm) SO emissions were attributed to c 1Σ → a 1∆ and A3∆ → X 3Σ transitions, respectively. This work also pointed out existence of SO2 CL from reactions between O atom and SO (Eq. 8) [32].
$$ {\text{O}} + {\text{SO}} = {\text{SO}}_{2}^{*} $$

2.3.3 SO2-Solid Y2O2S–Eu System

Serving as a classic atmosphere of heteronuclear molecules, reaction of SO oxidation on the solid surface have attracted considerable attentions owing to its unique property and high CL intensity. Khoruzhii et al. [10] focused on heterogeneous SO + O CL effect via oxidation occurring on the surface of solid Y2O2S–Eu crystal upon adsorption, oxidation and desorption process (Fig. 3). He revealed that atom–molecule exchange reactions also took place between O atom and SO2 molecules (Eq. 9) [33].
$$ {\text{O}} + {\text{SO}}_{2} - {\text{crystal}} = {\text{SO}} - {\text{crystal}} + {\text{O}}_{2} $$
Fig. 3

CL spectra of SO + O occurred on the surface of Y2O2S–Eu with: free of SO2 on the surface (curve 1), following SO2 absorption for 16 h (curve 2) and result of theoretical calculations (curve 3) [10]

2.4 H2-Solid System

2.4.1 H2-Solid Zn2SiO4–Mn System

Researches towards gas–solid phase CL based on H2 always occurs with dissociation of H2 molecule to produce H atoms. Subsequent recombination of these H atoms would generate CL through interaction with solid reactant on the surface. Tyurin et al. [34] studied recombination of H atoms on the surface of Zn2SiO4–Mn composition using CL technique. The data indicated that the total rate and CL intensity of this reaction acted as a function of H atom flux and sample temperature. He also found that this process obeyed both Rideal–Eley (Eq. 10) [35] and Langmuir–Hinshelwood (Eq. 11) [36] mechanisms.
$$ \begin{aligned} & {\text{H}} + {\text{HL}} + {\text{Mn}}^{2 + } \to {\text{H}}_{2}^{\text{V}} {\text{L}} + {\text{Mn}}^{2 + } \to \\ & {\text{H}}_{2}^{{}} {\text{L}} + ({\text{Mn}}^{2 + } )^{*} \to {\text{H}}_{2}^{{}} {\text{L}} + {\text{Mn}}^{2 + } + {\text{hv}} \\ & \quad \quad ({\text{L}} = {\text{an}}\;{\text{active}}\;{\text{site}}) \\ \end{aligned} $$
$$ \begin{aligned} & 2{\text{HL}} + {\text{Mn}}^{2 + } \to {\text{H}}_{2}^{\text{V}} {\text{L}} + {\text{L}} + {\text{Mn}}^{2 + } \to \\ & {\text{H}}_{2}^{{}} {\text{L}} + {\text{L}} + ({\text{Mn}}^{2 + } )^{*} \to {\text{H}}_{2}^{{}} {\text{L}} + {\text{L}} + {\text{Mn}}^{2 + } + {\text{hv}} \\ & \quad \quad ({\text{L}} = {\text{an}}\;{\text{active}}\;{\text{site}}) \\ \end{aligned} $$

2.4.2 H2-Solid ZnSCdS-Cu System

The energy and H2 molecule absorbed on the solid surface will result in high-frequency oscillation and dissociation of molecular H2 to atomic H, which will emit light through subsequent recombination process of free atoms. Styrov et al. [37] paid attention to heterogeneous CL evolved from interactions between H atoms and solid ZnSCdS-Cu with different quantities of CdS (0–40%) where he believed that the relationship between CL intensity and concentration of CdS was attributed to electron–hole pairs multiquantum generation mechanism. Besides, the results also indicated that the established models (Eqs. 1214) [38] could be applied to evaluate the influence of CdS within ZnSCdS-Cu on CL performance:
$$ \begin{aligned} & \varGamma_{\text{ev}} = \frac{{4m_{2} \theta^{2} f(m_{\text{r}} h\omega_{0} )^{1/2} }}{{h\omega_{0} Mm_{\text{e}} E_{\text{g}} }}\left[ {\frac{{\mu (r_{0} )e(\varepsilon + 2)}}{{3a^{3/2} \varepsilon }}} \right]^{2} \hfill \\ & \quad \quad \phi (q/E_{\text{g}} )\exp \left( { - \frac{{E_{\text{g}} }}{{h\omega_{0} }}P} \right) \hfill \\ \end{aligned} $$
$$ p = z\ln z/(z - 1) $$
$$ z = (4q + h\omega_{0} )/(E_{\text{g}} + h\omega_{0} ) $$
where m e is mass of electron, e is elementary charge, ω 0 is oscillator cyclic frequency, µ is dipole moment of binding, f is oscillatory force, e is permittivity at the transmission frequency, q is adsorption potential depth, E g is width of forbidden zone, m r is equivalent effective mass of an electron–hole pair, a is minimal distance of energy transportation.

2.4.3 H2-Solid SiC System

SiC polytypes have been widely used in diodes and detectors where researches towards its surface properties and reactions with gas molecules are of great importance. Styrov et al. [39] also investigated CL effect of chemical reactions between H atoms at SiC surface and revealed the process of adsorption and recombination of H atoms (Fig. 4). He also claimed the binding energy between H atom and SiC was ranged from 2 to 3 eV, which facilitated the subsequent generation of gas–solid phase CL. Moreover, such CL performance also provided information on reaction process so that relevant surface situation can be better understood.
Fig. 4

The CL spectra of reactions between H atoms and SiC-polytypes at 130 K [39]

2.5 CO-Solid System

Acting as a classic model of heterogeneous reaction, oxidation of CO with heterogeneous catalysis has significant meaning of development of catalytic filters and elimination of organic compounds. Shigalugov et al. [11] reported heterogeneous CL analysis towards reactions between CO + O mixture and solid crystallophosphors (CaO–Bi and Zn2SiO4–Mn). Such process has followed Rideal–Eley mechanism with CO-attachment (Eq. 15) [40] or O-attachment (Eq. 16) [41] routes. He also thought that the CL obtained could also be an indicator for further discussing elementary act, rate constant and cross-section of CO-based heterogeneous CL.
$$ {\text{O}} + {\text{CO}} - {\text{lattice}} = {\text{CO}}_{2} - {\text{lattice}} + {\text{hv}} $$
$$ {\text{CO}} + {\text{O}} - {\text{lattice}} = {\text{CO}}_{2} - {\text{lattice}} + {\text{hv}} $$

3 Mechanisms of gas–solid phase CL

Based on above main classifications, relevant mechanisms of gas–solid phase CL can be regarded as excitation of the radical-recombination process where adsorption, ionization and heterogeneous recombination of atoms have ensured effective electronic excitation of the solid. Results showed that the mechanisms of gas–solid phase CL act as a function of (1) the component and concentration of gas atoms and molecules and (2) the solid temperature, which plays an important role in determination of reaction route. Generally, the mechanisms could be divided into four basic steps: adsorption and desorption of gas atoms and molecules at the lattice of the solid (Eq. 17) [42], recombination of gas atoms on the surface of solid (Eqs. 1819) [43], ionization of traps (Eqs. 2024) [44] and generation of electron–hole pairs through gas–solid interaction with subsequent emission (Eqs. 2527) [45]. Corresponding chemical equations are shown as follows:
$$ {\text{R}} + {\text{L}} = {\text{RL}} $$
$$ {\text{R}} + {\text{RL}} = {\text{R}}_{2}^{\text{v}} {\text{L}} $$
$$ {\text{R}}_{2} + {\text{L}} = {\text{R}}_{2}^{{}} {\text{L}} $$
$$ {\text{R}}_{2}^{\text{v}} {\text{L}} = {\text{R}}_{2}^{{}} {\text{L}} + {\text{ph}} $$
$$ {\text{R}}_{2}^{\text{v}} {\text{L}} = {\text{R}}_{2}^{{}} {\text{L}} + {\text{eL}} + {\text{pL}} $$
$$ {\text{R}}_{2}^{\text{v}} {\text{L}} + {\text{TeL}} = {\text{R}}_{2}^{{}} {\text{L}} + {\text{TL}} + {\text{eL}} $$
$$ {\text{AL}} + {\text{pL}} = {\text{ApL}} $$
$$ {\text{TL}} + {\text{eL}} = {\text{TeL}} $$
$$ {\text{hv}} = {\text{eL}} + {\text{pL}} $$
$$ {\text{ApL}} + {\text{eL}} = {\text{A}}^{*} {\text{L}} $$
$$ {\text{A}}^{*} {\text{L}} = {\text{AL}} + {\text{hv}} $$
where R is gas atom, R2 is gas molecule, L is solid lattice, AL is luminescence center, TL is an electron trap, e is a free electron, p is a free hole. Definitely, these steps cooperate with each other to assure the process of gas–solid phase reactions while obvious CL could be obtained. In addition, the investigations towards these mechanisms could also facilitate further improvement and optimization of gas–solid phase CL systems with higher CL intensity.

4 Applications of Gas–Solid Phase CL

A variety of equipment has been realized for detection and analysis of specific atoms or radicals based on gas–solid phase CL occurred at the surface of solid reactant, which laid foundation for obtaining information about rate constant, intermediate production, surface state and reaction mechanism of a CL system. What is more, this strategy could also be utilized in realistic determination to acquire real-time results of samples.

4.1 Chemical Sensor

A novel gas–solid phase chemical sensor based on CL strategy was devised by Karpov et al. [46]. Serving as an effective complementary facility for traditional analytical techniques, this sensor has been applied to measurement towards the concentration of H, O and other gaseous chemical radicals. With the CL induced by Eley–Rideal recombination process took place, relevant property of such sensor has reached the sensitivity of 105 cm−3 with test time about 1 s.

4.2 CL Imaging

Stenberg et al. [47] presented an CL imaging equipment towards oxidation of polymers (nylon and polybutadiene) by O2. This equipment was composed of an imaging photon counting system installed on a oven where stable thermal environment was maintained in specific atmosphere (Fig. 5). The data revealed availability of this facility in investigating controlled gas–solid phase reaction and evaluating the surface of solid before and after oxidation.
Fig. 5

Structure of CL imaging equipment [47]

4.3 CL Spectrometer

Pronko and Chapman [48] have developed a microcomputer-controlled CL spectrometer with effective response and low cost, which could be utilized to study CL effect on the surface of materials in certain atmosphere. In addition, the CL spectra as a function of time and temperature could be recorded completely automatically. With the control of microcomputer, CL spectra in different regions could also be obtained.

5 Conclusions and Future Prospects

In this review article, we mainly concentrated on recent development of gas–solid phase CL. The main classifications including O3-solid, O2-solid, “S-based”-solid, H2-solid and CO-solid CL systems are summarized. In addition, specific mechanisms and applications of gas–solid phase CL in chemical sensor, imaging and spectrometer are also concluded. Results demonstrate that gas–solid phase CL system acts as a novel and effective platform for detection and analysis.

The investigation on gas–solid phase CL will create a new area by analyzing chemical reactions through gas–solid phase CL performance thus the information on rate constants, intermediate productions, surface states and reaction mechanisms could be acquired.

Moreover, gas–solid phase CL has provided a novel alternative in determining the concentration of gaseous atoms or radicals (H, O, S, etc.) which is complicated through traditional analytical methods. The unique characteristics of gas–solid phase CL like high sensitivity and strong CL intensity have made it an excellent tool in probing the emissive property of solid reactant in certain atmosphere.

Notably, gas–solid phase CL also eliminated the interference from solution where impurity and other reactants would inevitably influence the detection procedure and later deduction of mechanism. Serving as a simple CL process, gas–solid phase interaction facilitates fast identification and verification in real samples.

Although gas–solid phase CL also suffers from incomplete transformation due to surface reaction where most reactants in the bulk stay unreacted, the endeavor of establishment of new CL system and application in sample analysis will be invaluable to make contribution to further development of gas–solid phase CL system. With new achievement and challenges appearing continuously, research towards gas–solid phase CL remains a hot theme.



This work was supported by the National Natural Science Foundation of China (Nos. 21227006, 21435002, 81373373, 21621003). The authors declare no competing financial interests. All authors have given approval to the final version of the manuscript.


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Copyright information

© The Nonferrous Metals Society of China and Springer Nature Singapore Pte Ltd. 2017

Authors and Affiliations

  1. 1.Department of Chemistry, Beijing Key Laboratory of Microanalytical Methods and Instrumentation, The Key Laboratory of Bioorganic Phosphorus Chemistry & Chemical BiologyTsinghua UniversityBeijingChina

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