Green analytical chemistry metrics
Principles of green analytical metrics. National environment method index. Application of GAC metrics. Complementary green analytical procedure index. Additive color model to analytical method evaluation. Examples of analytical eco-scale calculation.
| Рубрика | Экология и охрана природы |
| Вид | дипломная работа |
| Язык | английский |
| Дата добавления | 27.11.2022 |
| Размер файла | 2,0 M |
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Step 8. Read the algorithm's outcomes: the final quantitative measure of the method's adequacy, i.e., the method brilliance (MB), its qualitative evaluation - the final color, and the CS values for each primary attribute (in the template worksheet they are also calculated automatically) Figure 13.
Figure 13 Evaluation of the volumetric titration method aimed at determination of acetic acid in vinegar (RSD, relative standard deviation; RE, relative error)
2.6 Examples of analytical Eco-Scale calculation
In this sub-section, we evaluate examples of analytical procedures for greenness using the analytical Eco-Scale. Example - determination the amount of Cu in brass sample:
Table 10
The penalty points (PPs) for Cu determination by titration in a brass sample
|
Reagents |
|||
|
Penalty points |
|||
|
HNO3: 10 mL |
8 |
||
|
NH3(aq.): 2 mL |
6 |
||
|
CH3COOH: 10 mL |
2 |
||
|
KI: 2 g |
0 |
||
|
Na2S2O3 |
0 |
||
|
Starch |
0 |
||
|
KSCN: 2 g |
1 |
||
|
?17 |
|||
|
Instruments |
|||
|
Penalty points |
|||
|
Heater |
2 |
||
|
Occupational hazard |
3 |
||
|
Waste |
8 |
||
|
?13 |
|||
|
Total penalty points: 30 |
|||
|
Analytical Eco-Scale total score: 70 |
3. Problems and solutions
3.1 Qualitative problems
Ш Assess the greenness of procedure using NEMI tool:
For RP-HPLC method for olanzapine and metformin [27] ethanol and water were used as a mobile phase. The used mobile phase had a pH approximately 6.5. The generated waste was 14 g/run.
Solution
Ethanol and water are not estimated as PBT or hazardous waste in reference to EPA's Toxic Release Inventory and hazardous waste list. Mobile phase has pH = 6.5 and so it is not estimated as corrosive. The amount of waste is less than 50 g. As a result, NEMI pictogram would look like this:
Figure 14 NEMI pictogram for olanzapine and metformin
Ш Assess the greenness of procedure using NEMI tool:
For micellar HPLC method for chlorpheniramine maleate [28] EtOH, 50 mM sodium dihydrogen phosphate and 30 mM sodium dodecyl sulfate were used as a mobile phase. The used mobile phase had a pH approximately 5. The generated waste was 1-10 g/run.
Solution
Ethanol, sodium dodecyl sulfate and sodium dihydrogen phosphate are not estimated as PBT or hazardous waste in reference to EPA's Toxic Release Inventory and hazardous waste list. Mobile phase has pH = 5 and so it is not estimated as corrosive. The amount of waste is less than 50 g. As a result, NEMI pictogram would look like this:
Figure 15 NEMI pictogram for chlorpheniramine maleate
Ш Assess the greenness of procedure using NEMI:
Analyses of neurotransmitters was performed using LC-MS method [29]. Chromatography technique: LC that coupled with electrospray tandem MS. No. of analytes: 2 analytes including (dopamine and tetrahydrobiopterin). Stationary phase: Sepax Polar-Imidazole (2.1x100 mm, i.d., 3 µm) column. Mobile phase: Isocratic, 10 mM NH4HCO2 in CH3CN/H2O (75:25, х/х, 300 µL/min). Flow rate: 0.3 mL min-1. Time of analysis: 5 min vii. Biological sample: mouse brain tissue.
Figure 16 NEMI pictogram for neurotransmitters
Ш Assess the greenness of procedure using GAPI:
Analyses of ibuprofen was performed using HPLC method [30]. All needed characteristics of procedure are listed in the Table 11:
Table 11
Analyses of ibuprofen
|
Category |
Analyses of ibuprofen |
|
|
Collection (1) |
At-line |
|
|
Preservation (2) |
None |
|
|
Transport (3) |
Required |
|
|
Storage (4) |
Under special conditions |
|
|
Type of method: Direct or indirect (5) |
Extraction required |
|
|
Scale of extraction (6) |
Microextraction |
|
|
Solvents/reagents used (7) |
Solvent-free methods |
|
|
Additional treatments (8) |
Advanced treatment |
|
|
Amount (9) |
10-100 mL |
|
|
Health Hazard (10) |
1) Acetonitrile - 2 2) Water - 0 3) Ortho-phosphoric acid - 3 |
|
|
Safety hazard (11) |
1) Acetonitrile - 3 2) Water 3) Ortho-phosphoric acid - 0 |
|
|
Energy (12) |
HPLC consumes ? 1.5 kWh per sample |
|
|
Occupational hazard (13) |
HPLC analysis will be done in a closed environment, so the chance of occupational hazards is less |
|
|
Waste (14) |
1-10 mL |
|
|
Waste treatment (15) |
No treatment |
Solution:
Figure17 GAPI pictogram for ibuprofen
Ш Assess the greenness of procedure using GAPI:
Analyses of neurotransmitters was performed using LC-MS method [29]. All needed characteristics of procedure are listed in the Table 12:
Table 12
Analyses of neurotransmitters
|
Category |
Analyses of neurotransmitters |
|
|
Collection (1) |
Offline (red) |
|
|
Preservation (2) |
None (green) |
|
|
Transport (3) |
None (green) |
|
|
Storage (4) |
None (green) |
|
|
Type of method: |
||
|
Direct or indirect (5) |
Extraction required (red) |
|
|
Scale of extraction (6) |
Nano-extraction (green) |
|
|
Solvents/reagents used (7) |
Non-green solvents and reagents (red) |
|
|
Additional treatments (8) |
Simple treatment (yellow) |
|
|
Amount (9) |
10< mL (green) |
|
|
Health Hazard (10) |
NFPA = 2, moderate toxicity (yellow) |
|
|
Safety hazard (11) |
NFPA = 3, high flammability (yellow) |
|
|
Energy (12) |
>1.5 Kwh per sample (red |
|
|
Occupational hazard (13) |
Hermetic sealing of analytical process (green) |
|
|
Waste (14) |
1-10 mL (yellow) |
|
|
Waste treatment (15) |
Recycling possible (green) |
Solution:
Figure 18 GAPI pictogram for neurotransmitters
3.3 Quantitative problems
Ш Assess the greenness using AGREE:
For the determination of Flibanserin [30] LC was used. In this method external sample preparation with reduced number of steps was used. Amount of sample is equal to 25 mg. Analytical device was located in-line. Sample preparation include 3 or fewer main stages (filtration, sonification). Method is not automated, but with miniaturized sample preparation, as well as derivatization agent is not used. There is no waste in the method and number of analytes determined in single run is equal to 4, the time needed for one run 3 minutes. In this method all reagents from biobased resources and they are not toxic, but one reagent is highly flammable.
Solution:
Principle 1. The procedure involves external sample treatment with reduced number of steps. > 0.3
Principle 2. 0.025 g of soil sample is needed. > -0.142 ln (0,025) + 0,65 = 1
Principle 3. The measurement is in-line. > 1
Principle 4 the procedure involves 3 distinct steps. > 1
Principle 5. The procedure is not automated but miniaturized. > 0.5
Principle 6. No derivatization agents are involved in the analysis. > 1
Principle 7. No waste > 0
Principle 8. Four analytes are determined in a single run and the sample throughput is ? 20 samples h?1. · > 1
Principle 9. LC is the most energy demanding analytical technique. > 0.5
Principle 10. All reagents can be from bio-based sources. > 1
Principle 11. Toxic solvents are not used > 1
Principle 12. Acetone is considered highly flammable. > 0.8
Figure 19 AGREE pictogram for Flibanserin
Ш Assess the greenness using AGREE:
For the determination of Glibenclamide [31] LC was used. In this method at-line was used. Amount of sample is equal to 0.010 ml. Analytical device was located on-line. Sample preparation include 3 or fewer main stages. Method is semi-automated with miniaturized sample preparation, as well as derivatization agent is not used. Number of wastes is equal to 5 ml and number of analytes determined in single run is equal to 1, the time needed for one run 5 minutes. In this method all reagents from biobased resources and they are not toxic, but one reagent is highly flammable.
Solution:
Principle 1. At-line sample preparation. > 0.3
Principle 2. 0.010 ml of sample sample is needed. > -0.142 ln (0,010) + 0,65 = 1
Principle 3. The measurement is on-line. > 0.66
Principle 4 The procedure involves 3 distinct steps. > 1
Principle 5. The procedure is semi-automated and miniaturized. > 0.75
Principle 6. No derivatization agents are involved in the analysis. > 1
Principle 7. 5 ml of wastes. > -0,134 · ln (5) +0,6965 = 0.48
Principle 8. One analyte is determined in a single run and the sample throughput is ? 12 samples h?1. · > 0.55
Principle 9. LC is the most energy demanding analytical technique. > 0.5
Principle 10. Some reagents are from bio-based sources. > 0.5
Principle 11. The procedure includes 5 ml of toxic solvents > 0.5
Principle 12. Methanol is considered highly flammable. > 0.8
Figure 20 AGREE pictogram for Glibenclamide
Ш Assess the greenness of procedure using Eco-scale (electrogravimetric Cu determination in a brass sample) [5]:
Weighing 1 mg of brass sample. Addition of 25 mL of HNO3 (1:1); heating until the sample dissolves. Addition of: distilled water, NH3(aq), 2 mL of H2SO4, 2 g of NH4NO3. Electrolysis at a temperature of 80oC; amperage: 1-2 A; voltage: 2 V; time: 2 hours; Pt electrodes Table 13:
Table 13
The penalty points (PPs) for electrogravimetric Cu determination in a brass sample
|
Reagents |
|||
|
Penalty points |
|||
|
HNO3: 10 mL |
8 |
||
|
NH3(aq.) |
6 |
||
|
H2SO4: 2 mL |
2 |
||
|
NH4NO3:2g |
1 |
||
|
?17 |
|||
|
Instruments |
|||
|
Penalty points |
|||
|
Heater |
2 |
||
|
Occupational hazard |
3 |
||
|
Waste |
5 |
||
|
?15 |
|||
|
Total penalty points: 27 |
|||
|
Analytical Eco-Scale total score: 73 |
Ш Assess the greenness of procedure using Eco-scale (for PCB determination in sewage sludge by GC-MS) [5]:
Sampling. Sample lyophilization (temperature: -50oC, pressure: 0,025 mbar). Mixing of 2 g of sample with 1,5 g of activated Cu and 4,5 g of anhydrous Na2SO4; shaking; spiking with internal standard (13C). Addition of activated basic Al2O3; accelerated solvent extraction (pressure: 1500 psi, temperature: 125oC, solvent: n-hexane-acetone 1:1, preheating time: 1 min, heating time: 6 min, static time: 5 min). Addition of 1 mL of isooctane to the extract; evaporation to approx, 1 mL with a rotary evaporator; SPE column with acidic silica (40% w/w) and a 0,5 cm thick layer of anhydrous Na2SO4; solvent: n-hexane (20 mL for washing the bed and 25 mL for elution); addition of 1 mL of isooctane; evaporation to approx. 1 mL with a rotary evaporator, evaporation to approx 0,5 mL under N2 stream. Analysis by GC-MS; Injector type: PTV - splitless, 85oC (0,1 min), 4oC/min to 270oC (3 min), 2oC/min to 350oC (15 min); injected volume: 2 µL, injector temperature: 65oC, carrier gas type and linear velocity: He, 1,5 mL/min; column: fused silica, 60 m, 0,25 mm i.d., stationary phase: 50% phenyl-methylpolysiloxane; film thickness: 0,25 µm (J&W, Db17); temperature program: from 60oC (2 min), 20oC/min to 200oC (1 min), 4oC/min to 280oC (15 min), MSD conditions: GC-MS interface: direct with temperature 250oC, MS source: electron impact with temperature 180oC; MS acquiring in SIM mode; m/z 256, 258, 268, 270, 290, 292, 302, 304, 326, 328, 340, 360, 362, 372, 374, 394, 396, 406, 408; qualitative analysis: MS peak area, average response factor of different PCBs relative to icotopically labelled PCBs Table 14.
Table 14
The penalty points (PPs) for PCB determination in sewage sludge by GC-MS
|
Reagents |
|||
|
Penalty points |
|||
|
Cu powder: 1.5 g |
1 |
||
|
HCl: 2 mL |
3 |
||
|
Na2SO4 (drying agent): 4.5 g + 1 g |
0 |
||
|
Isotopically labeled PCBs standard mixture |
4 |
||
|
Activated Al2O3:1g |
0 |
||
|
n-Hexane: 15 mL + 45 mL |
16 |
||
|
Acetone: 15 mL |
8 |
||
|
Isooctane: 2 mL |
8 |
||
|
Acidic silica (98% of H2SO4: 20 mL) |
4 |
||
|
PCBs standard solution |
4 |
||
|
?48 |
|||
|
Instruments |
|||
|
Penalty points |
|||
|
Sampler |
1 |
||
|
Transport |
1 |
||
|
Freeze-drying instrument (50oC, 0.025 mbar) |
2 |
||
|
ASE extractor (1500 hPa, 125oC) |
2 |
||
|
Rotary evaporator |
2 |
||
|
Oven (for acidic silica preparation) |
2 |
||
|
GC-MS |
3 |
||
|
Occupational hazard |
0 |
||
|
Waste |
4 |
||
|
?17 |
|||
|
Total penalty points: 65 |
|||
|
Analytical Eco-Scale total score: 35 |
Ш Assess the greenness of procedure using Eco-scale (e for a determination of mercury in an animal tissue by cold-vapor atomic absorption spectrometry) [5]:
Sampling. Lyophilization, weighing of sample directly in ceramic boat. Additions of additives M and B. Inserting a ceramic boat into MA-2000 instrument and performance of the measurement Parameters set: concentration level: mode LOW or HIGH; temperature program: MODE2. Calculation of Hg concentration. Table 15.
Table 15
The penalty points (PPs) for Hg determination by CVAAS in an animal tissue
|
Reagents |
|||
|
Penalty points |
|||
|
Additives M and B |
0 |
||
|
Hg standard solutions |
2 |
||
|
?2 |
|||
|
Instruments |
|||
|
Penalty points |
|||
|
Freeze-drying instrument |
2 |
||
|
Hot-plate |
2 |
||
|
Spectrometer |
2 |
||
|
Occupational hazard |
0 |
||
|
Waste |
2 |
||
|
?8 |
|||
|
Total penalty points: 10 |
|||
|
Analytical Eco-Scale total score: 90 |
Conclusion
Each metrics has its own merits and demerits, which were well defined in Table 8. While each evaluation tool provides its unique conclusions about adopting the green metrics, these conclusions may vary, causing the analyst's decision-making process challenging. NEMI is a classical and simple evaluation tool for greenness assessment in analytical methods. However, despite its simplicity, NEMI does not cover all the green analytical principles, which is the main drawback in the adoption as an evaluation tool; apart from that, NEMI helps to select solvents that do not cover under the PBT list and makes the steps towards greenness. GAPI is the best available qualitative assessment tool that covers all the green analytical principles with three color coding, makes the assessment simple but due to its representation of 15 quadrants which makes it a little complex. Analytical Eco-Scale is a quantitative tool; The scores obtained with Analytical Eco-Scale are quantitative, but their calculation is based on qualitative pictograms. Further, biobased solvents such as ethanol have few penalty points, restricting the analysts to select ethanol as mobile phases in LC methods. Instead, Analytical Eco-Scale can help the analyst select the chemicals that have a less toxic effect (fewer pictograms) on the environment rather than having more pictograms. The subsequent flaw is in the amount of reagent used, which was approximate rather than accurate. AGREE metrics a practical, user-friendly software that covers GAC principles, and it works on the mode of Graphical User Interface (GUI). The outcomes do not often provide details around the structure of hazards, or including too general data about the evaluated analytical method may not be a more significant drawback than other metrics. Among all the other metrics available for green analytical evaluation tools, AGREE is among the top to cover all the nooks of GAC principles ultimately and provides weightage for the principles on which the users focus specifically.
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