| Literature DB >> 35498251 |
Matheus C Carvalho1, William Eickhoff2, Michael Drexl3.
Abstract
Elemental and isotopic analyses are performed using elemental analyzers, and are widely employed for diverse scientific fields. An elemental analyzer is typically equipped with an autosampler. Here we present an open-source autosampler for elemental and isotopic analysis of solid samples. The autosampler consists of 1) a sampling table, on which a carousel pushes samples inside an orifice, and 2) a purging pipe, placed directly beneath the orifice, where the sample is purged off surrounding air, and then delivered to the reaction tube. The action of the purging pipe ensured that air contamination, an issue for the analysis of some elements like nitrogen and oxygen, was negligible, and results for elemental and isotopic composition of nitrogen and carbon were inside specs. Compared to commercial alternatives, the autosampler presented here has the advantages of lower cost to build and maintain, universal compatibility with instruments from different manufacturers, capacity do deal with bulky samples, capacity for a larger number of samples in a single run, and no necessity for time-consuming purging in-between sample loading. The autosampler could potentially also be employed for the analyses of other elements (e.g. oxygen, hydrogen and sulfur) because they are performed using similar equipment.Entities:
Keywords: 3D printing; Arduino; AutoIt; Autosampler; Carbon; Elemental analysis; Laboratory automation; Nitrogen; OpenSCAD; Sampling; Stable isotopes
Year: 2020 PMID: 35498251 PMCID: PMC9041227 DOI: 10.1016/j.ohx.2020.e00123
Source DB: PubMed Journal: HardwareX ISSN: 2468-0672
Fig. 1EA autosampler mounted on top of an elemental analyzer. The sample table is the four-legged acrylic sheet supporting the carousel. The purging pipe is the pipe beneath the sampling table and connected to the elemental analyzer.
Fig. 2EA autosampler. A table made of aluminum extrusion profiles holds an acrylic sheet, on top of which a carousel spins delivering samples through a hole on the sheet. The hole is placed directly above the purging pipe, where three ball valves, actuated by servo motors, ensure that minimal air contamination occurs when the sample is delivered to the elemental analyzer.
Fig. 3Scheme of the operation of the purging pipe. Arrows indicate helium flow. Full description in the text, Section 2.
Fig. 4Carousel made of clear PLA, allowing writing of the sample positions with a pen.
Fig. 5Wheels fixed to the one of the acrylic supports.
Fig. 6Stepper motor fixed to one of the acrylic supports. Here only 3 screws are holding the motor.
Fig. 7Bracket fixed to acrylic support.
Fig. 8Acrylic support placed on a 22 cm aluminum extrusion profile. The support should move smoothly with the wheels inside the groove.
Fig. 9Timing belt around stepper motor pulley, and fixed on aluminum extrusion profile.
Fig. 10Bracket (2028) connecting extrusion profiles. Notice M5 screws and washers. Hammer nuts are inside the extrusion profile grooves.
Fig. 11Acrylic sheet connected to extrusion profile using hammer-head screw and wingnut.
Fig. 12Stepper motor fixed to extrusion profile using stepper motor mount (Section 3).
Fig. 13Carousel connected to stepper motor by shaft.
Fig. 14Valve with lever replaced by a custom-made one. This lever is made from a steel striping (middle of the figure), being cut and drilled according to the necessary dimensions. Here, the existing holes on the stripping were used as a starting point, and matching holes with enough diameter (here, 3 mm) were also drilled at the servo arm (right of the figure). The rotation center of the lever and the arm must also match when assembled (Fig. 15).
Fig. 15Valve lever connected to servo arm. Notice screws connected at opposing orientations.
Fig. 16Servo motor fully connected to ball valve.
Fig. 17Purging pipe fully assembled.
Fig. 18Sieve to be placed inside the T piece to avoid samples to settle at the perpendicular connection.
Fig. 19Control board fixed to the autosampler, positioned on reach of servo wires.
Fig. 20Stepper motor wires connected to the control board.
Fig. 21Servos connected to positions 0, 2 and 3. These positions are arbitrary and match the code in Supplementary Information 2. Different positions can be chosen, as long as the code is modified accordingly.
Comparison between the autosampler presented here and two commercial models.
| Parameter | This autosampler | Costech Zero Blank Autosampler | Thermo-Fisher MAS200r |
|---|---|---|---|
| Number of samples per tray | 95; can be expanded without modifying sample size if a larger tray is designed; or a larger tray can be built, along a larger table, so that a larger number of large samples can be accommodated | 49 for 6 mm samples | 32; more samples can be added if extra trays are pilled upon each other, but these need to be purchased separately |
| Maximum sample size | Sphere with 10 mm in diameter | Sphere with 6 mm in diameter when using a tray for 49 samples; it can take larger samples but then the tray needs to be swapped with one for less samples at once | Sphere with 10 mm in diameter, but only if purging flow is largely increased |
| Sample adding procedure | Samples need to be placed inside their respective holes in the carousel | Samples need to be placed inside carousel, and then a flushing procedure lasting about 10 min is needed. If more samples need to be added, the flushing needs to be repeated again. | Samples need to be placed inside their respective holes in carousel and a lid needs to be placed over the tray. If the lid is forgotten, large air blanks are introduced in the measurement. |
| Cost | AU$540 plus extras | AU$20,000 | AU$10,000 |
| Replacement parts | 3D-printed or readily available from hardware stores | Proprietary | Proprietary |
| Compatibility | Universal via AutoIt | Proprietary, only for designed partner companies | Proprietary, only for designed partner companies |
Fig. 22Comparison between chromatograms generated by elemental analyzer when only the elemental analyzer is used, and when the elemental analyzer is used together with the autosampler. Both chromatograms are shown with very large augmentation, and perturbations on the base line are very small in both cases.
Fig. 23Comparison of chromatograms when the autosampler delivers no sample, and when samples with small and larger amounts of material are delivered. The first and last two peaks (the four rectangles) are reference gas peaks, the first two for N2, and the last two for CO2. The gaussian peaks are for the analyzed samples, the first one for N2, and the second one for CO2.
| Hardware name | Oseas |
| Subject area | Chemistry and Biochemistry Environmental, Planetary and Agricultural Sciences Medicine, Forensics |
| Hardware type | Solid sample handling |
| Open Source License | GNU General Public License (GPL) 3.0 |
| Cost of Hardware | AU$ 542 plus extras |
| Source File Repository | https://osf.io/utzse/ or |
| Design file name | File type | Open source license | Location of the file |
|---|---|---|---|
| Carousel | OpenSCAD | GNU General Public License (GPL) 3.0 | |
| Gantry support | Libre Office Draw | GNU General Public License (GPL) 3.0 | |
| Table top | Libre Office Draw | GNU General Public License (GPL) 3.0 | |
| NEMA 17 stepper motor mount | OpenSCAD | GNU General Public License (GPL) 3.0 | |
| Servo to ball-valve connector | OpenSCAD | GNU General Public License (GPL) 3.0 | |
| Spacer for 4 mm screws | OpenSCAD | GNU General Public License (GPL) 3.0 | |
| Spacer for 3 mm screws | OpenSCAD | GNU General Public License (GPL) 3.0 | |
| Sieve for half inch pipe | OpenSCAD | GNU General Public License (GPL) 3.0 |
| Figure or reference | Component | Number | Cost per unit –AU$ | Total cost –AU$ | Source of materials | Material type |
|---|---|---|---|---|---|---|
| T slot 20x20mm, 35 cm | 4 | $3.85 | $14.00 | Aluminum | ||
| T slot 20x20mm, 22 cm | 7 | $2.42 | $16.94 | Aluminum | ||
| T slot 20x20mm, 10 cm | 3 | $1.10 | $3.30 | Aluminum | ||
| T slot 20x20mm, 25 cm | 1 | $2.75 | $2.75 | Aluminum | ||
| 2028 bracket, pack with 20 | 1 | $10.15 | $10.15 | Aluminum | ||
| Long 90°bracket | 2 | $1.06 | $2.12 | Steel | ||
| NEMA 17 stepper motor | 2 | $13.66 | $27.32 | Metal, plastic | ||
| Shaft coupler, 5 mm to 8 mm | 1 | $5.56 | $5.56 | Metal | ||
| Acrylic sheet, A4 size | 2 | $9.50 | $19.00 | Plastic | ||
| M3 screws, 10 mm length, pack with 10 | 2 | $7.20 | $14.40 | Metal | ||
| M3 screws (16 mm length), pack with 10 | 1 | $7.20 | $7.20 | Metal | ||
| M3 nuts, pack with 10 | 1 | $5.50 | $5.50 | Metal | ||
| M3 hammer nuts, pack with 10 | 1 | $6.50 | $6.50 | Metal | ||
| M4 screws, 40 mm length, fully threaded, pack with 10 | 1 | $1.87 | $1.87 | Metal | ||
| M4 hammer nuts, pack with 10 | 1 | $6.00 | $6.00 | Metal | ||
| M4 nuts, pack with 10 | 1 | $5.50 | $5.50 | Metal | ||
| M5 screws, 10 mm length, pack with 100 | 1 | $21.00 | $21.00 | Metal | ||
| Washer for M5 screw, pack with 100 | 1 | $9.80 | $9.80 | Metal | ||
| Hammer nut for M5 screw, pack with 100 | 2 | $9.69 | $19.38 | Metal | ||
| M5 screws with hammer-head, 16 mm length, pack with 10 | 1 | $3.18 | $3.18 | Metal | ||
| Wingnut for M5 screw, pack with 5 | 1 | $8.90 | $8.90 | Metal | ||
| M5 screws, 35 mm length, fully threaded pack with 10 | 1 | $3.36 | $3.36 | Metal | ||
| Spacer for M5 screws, 10 mm length, set with 25 | 1 | $2.47 | $2.47 | Nylon | ||
| GT2 Timing belt, 1 m | 1 | $1.83 | $1.83 | Rubber | ||
| 20 teeth Pulley for GT2 timing belt, 20 teeth | 1 | $4.50 | $4.50 | Metal | ||
| Wheels 625ZZ, 21.5 cm in outer diameter, pack with 9 | 1 | $7.91 | $7.91 | Metal, plastic | ||
| 3D-printed carousel | 1 | <$0.10 | <$0.10 | PLA | ||
| 3D-printed servo to ball valve connector | 3 | <$0.10 | <$0.30 | PLA | ||
| 3D-printed spacer for M4 screws | 6 | <$0.05 | <$0.30 | PLA | ||
| 3D-printed NEMA 17 motor mount | 1 | <$0.10 | <$0.10 | PLA | ||
| 3D-printed sieve for half inch pipe | 1 | <$0.10 | <$0.10 | PLA | ||
| MKS Gen L control board with stepper motor drivers (A4988) | 1 | $32.01 | $32.01 | Metal, plastic | ||
| Cables with adapters to connect stepper motors to control board (1 m), set with 4 | 1 | $3.75 | $3.75 | Metal, plastic | ||
| Cable wrapper 2 m | 1 | $8.89 | $8.89 | Plastic | ||
| USB cable, 5 m long | 1 | $6.50 | $6.50 | Metal, plastic | ||
| Not shown | 24 V, 5.62A power supply | 1 | $29.00 | $29.00 | Metal, plastic | |
| Not shown | Adapter for power supply to the control board (2.1 mm illuminated polarity sensing DC socket) | 1 | $8 | $8 | Metal, plastic | |
| Hitec HS-805BB servo motor | 3 | $60.00 | $180.00 | Metal, plastic | ||
| ½ inch ball valve | 3 | $7.70 | $22.10 | Brass | ||
| ½ inch female-female-female T tube | 1 | $4.50 | $4.50 | Plastic | ||
| ½ inch male-male connector | 4 | $1.15 | $4.60 | Brass or plastic | ||
| ½ inch unthreaded to threaded connector | 1 | $0.95 | $0.95 | PVC | ||
| Thread tape (roll) | 1 | $3.00 | $3.00 | Teflon | ||
| Not shown | O-ring set | 1 | $3.85 | $3.85 | Rubber | |
| Perforated steel stripping (20 × 2 × 0.2 cm) | 2 | $1.72 | $3.44 | Steel |