Cary Spectrophotometer: User Guide
Manual Information
Author(s) | E. Moortgat | |
Revision | E. MoortgatD. Houpt | |
Reviewer(s) | C. Bennight, M. Bertoli, L. Brandt | |
Management Approval | D. Houpt, Supervisor of Analytical Systems | |
Audience | Laboratory Technicians and Scientists | |
Origination date | 12/12/2011 | |
Current version | Version 1.# (12/17/2015)V3741T | FebJuly 20187 |
Domain | Chemistry (IW) | |
Analysis | Spectrophotometry |
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Introduction
The principles of spectroscopic analysis rely on Beer's law. The principle of Beer's law is that passing light of a known wavelength through a sample of known thickness and measuring how much of the light is absorbed at that wavelength will provide the concentration of the unknown, provided that the unknown is in a complex that absorbs significantly at the chosen wavelength.
Beer's law, expressed for liquids, can be represented as an equation, where A = absorbance, k = an experimentally determined constant, b = path length, and c = concentration:
A = kbc.
Thus, concentration can be determined.
IODP's Agilent Cary 100 double-beam UV-Vis (ultraviolet–visible) spectrophotometer is ideal for shipboard routine and research laboratory work. The system measures analytes in interstitial water obtained from sediment cores using standard colorimetric methodology. Anchor
Hardware and Materials
The Varian Cary 100 is a double-beam, dual-chopper, monochromator UV-Vis spectrophotometer, centrally controlled by a PC. It has a high-performance R928 photomultiplier tube, tungsten halogen visible source with quartz window, and deuterium arc ultraviolet source (Figure 1). More details can be found below.
Name | Agilent Technologies Cary UV-Vis Spectrophotometer |
Model | Cary-100 |
Serial number | UV1110M021 |
Dimensions | 26 × 26 × 13 in (unpacked) |
Weight | 99 lb (unpacked) |
Monochromator | Czerny-Turner 0.28 m |
Grating | 30 × 35 mm, 1200 lines/mm, blaze angle 8.6° at 240 nm |
Beam Splitting System | Chopper (30 Hz) |
Detectors | R928 PMT |
UV-Vis Limiting Resolution (nm) | 0.189 |
Wavelength Range (nm) | 190–900 |
Wavelength Accuracy (nm) | 0.02 at 656.1 nm; 0.04 at 486.0 nm |
Wavelength Reproducibility (nm) | 0.008 |
Signal Averaging (s) | 0.033–999 |
Spectral Bandwidth (nm) | 0.20–4.00 nm, 0.1 nm steps, motor driven |
Spectral Bandwidth Accuracy (nm) | @ 0.2: 0.193; @ 2.0: 2.03 |
Photometric Accuracy (Abs) | @ 0.3 Abs (Double Aperture method): 0.00016 |
Photometric Range (Abs) | 3.7 |
Photometric Display | (Abs) ± 9.9999; (%T) ± 200.00 |
Photometric Reproducibility | (Abs; NIST 930D filters) |
2 s signal averaging time @ 590 nm, 2 nm SBW |
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2 s signal averaging time @ 546.1 nm, 2 nm SBW |
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Photometric Stability (Abs/hr) | 2 h warmup |
Photometric Noise (Abs, RMS) | 2 nm SBW |
Baseline Flatness (Abs) | 0.00022 |
Sample Compartment Beam Separation (mm) | 110 |
Figure 1. Schematic of Cary Spectrophotometer.
Electrical
Power supply (VAC) | 100, 120, 220, or 240 ± 10% |
Frequency (Hz) | 50 or 60 ± 1 with 400 VA power consumption |
Fuses (100–120 VAC) | T5 AH 250 V, IEC 127 sheet 5, 5 × 20 mm ceramic |
COM port (rear) | IEEE 488 |
PC port | USB |
Replacement Parts
Item | Part number |
Instrument fuse, 5 A time lag, ceramic, M205 | 1910009100 |
Peristaltic pump tubing replacement kit | 9910052900 |
Visible source lamp | 5610021700 |
Deuterium lamp | 5610021800 |
Dissolution cell, 715 µL, 10 mm | 6610015200 |
Thumbscrew kit | 9910064100 |
Spares kit: accessory locating pin, accessory fastening screws, instrument feet, instrument cover snap cap washer, snap cap, ACB cover plate, socket covers for ACB | 9910064300 |
Pumps
A double-action peristaltic pump services the feed and waste (Figure 2).
Figure 2. Peristaltic pump. (1) plastic sleeve. (2) metal hook tubing. (3) waste outlet.
Computer Control
An external computer workstation provides control, communication, and data analysis.Anchor
Software
Agilent provides a full suite of applications for various user requirements; for our needs we use the Simple Reads application. Simple Reads is used to perform simple absorbance readings of single samples. There is, however, a built-in programming language, Applications Development Language (ADL), which allows complete customization of Cary WinUV to specific applications.
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Methods
The described methods are based on ODP Technical Note 15, Chemical Methods for Interstitial Water Analysis Aboard the JOIDES Resolution, Aug 1991; J.M. Gieskes, T. Gamo, and H. Brumsack.
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C: Sodium Nitroprusside/Sodium Nitroferricyanide solution (1200 mL) – make fresh daily
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Dissolve 75 mg sodium nitroprusside (Na{~}2{~}\[Fe(CN){~}5{~}NO\]) in 100 mL nanopure water. *Note:* do not mix sodium nitroprusside with acid, as HCN fumes can will be liberated.! |
D: Alkaline solution (500 mL) – make fresh monthly
D: Alkaline solution (500 mL) – make fresh monthly
Dissolve 7.5 g trisodium citrate (Na3C6H5O7) and 0.4 g sodium hydroxide (NaOH) Dissolve 7.5 g trisodium citrate (Na3C6H5O7) and 0.4 g sodium hydroxide (NaOH) in 500 mL nanopure water.
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F: Ammonium standard: 0.10 M Ammonium (1000 mL) – make fresh monthly
a. | Dry ammonium chloride (NH4Cl) in oven overnight, then dissolve 5.345 g dried NH4Cl in nanopure water; bring to 1000 mL in a volumetric flask. |
b. | Alternatively, use non-dried NH4Cl and determine the chloride content of the standard solution by means of chloride titration. For reasonable accuracy, use a 500 µL aliquot (Cl = 0.1 NM) to obtain almost the same concentration of Cl as in IAPSO reference standard seawater. |
Standards
50 mL batches are stable for 1 month. (Note that the 50 µM solution is prepared from the 1000 µM standard, and the rest of the standards are made from the 100 mM primary stock standard.)
concentration | volume of nanopure water | volume of standard | note |
|---|---|---|---|
0 | 50.00 | 0 |
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50 | 47.50 | 2.50 | (dilute from 1000 µM std) |
100 | 49.95 | 0.05 | (dilute from 100 mM std) |
200 | 49.90 | 0.10 | (dilute from 100 mM std) |
400 | 49.80 | 0.20 | (dilute from 100 mM std) |
600 | 49.70 | 0.30 | (dilute from 100 mM std) |
800 | 49.60 | 0.40 | (dilute from 100 mM std) |
1000 | 49.50 | 0.50 | (dilute from 100 mM std) |
1500 | 49.25 | 0.75 | (dilute from 100 mM std) |
2000 | 49.00 | 1.00 | (dilute from 100 mM std) |
3000 | 48.50 | 1.50 | (dilute from 100 mM std) |
Procedure
Concentrations of ammonium may differ occur at different sites. Typically in areas with strong evidence of organic carbon diagenesis (e.g., organic carbon–rich sediments), high concentrations of NH4+ can be expected. In that case, sample aliquots must be made appropriately small or sample dilution may be required. The range can be established by using a sample near the alkalinity maximum. Once the range has been determined, prepare standards that cover this range. In this manner, samples and standards are treated in a similar way.
The high range of the instrument is 3.0 Absorbance units (Abs). The results are linear up to this point. If the readings are expected to be higher than 3.0 Abs, use a sample volume of 30 µL instead of 100 µL and divide measured concentrations by 0.3 to arrive at the final sample concentration.
Care should be taken to use clean vials, preferably not those used for Si and PO4 determinations, in which ammonium molybdate is used as a reagent. Note: The order of dilution matters, so do not change this order. Shake samples after EACH addition.
1. | Transfer 200 µL of sample to an 8 mL glass vial. |
2. | Add 2 mL of nanopure water to each vial and shake. |
3. | Add 1 mL phenol-alcohol solution to each vial and shake. |
4. | Add 1 mL sodium nitroprusside to each vial and shake. |
5. | Add 2 mL of oxidizing solution to each vial and shake. |
6. | Let the color develop (in a dark place) for 6.5 hr* and then determine the absorbance at 640 nm wavelength. |
*(from a series of measurements over 8 h, it was found that results stabilized after 6.5 hr.)
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B. Antimony Potassium Tartrate solution (1000 mL) – make fresh every two months; store in amber glass @ 4°C
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C. Ammonium Molybdate solution (1000 mL) – stable indefinitely; store in polyethylene @ 4°C
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In a 1000 mL volumetric flask, dissolve 2 g of ammonium molybdate tetrahydrate (\[NH{~}4{~}\]{~}6{~}Mo{~}7{~}O{~}24{~}- 4H{~}2{~}24·4H2O) in ~600 mL of nanopure water. Dilute to 1000 mL with reagent water.
D. Ascorbic Acid solution (1000 mL) – make fresh every week; store in amber glass @ 4°C
In a 1000 mL volumetric flask, dissolve 3.5 g of ascorbic acid (C6H8O6) in ~600 mL nanopure water. Dilute to 1000 mL with nanopure water. Note: If the reagent is discolored upon creation, the dry ascorbic acid is probably oxidized and must be replaced.
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Add the following solutions to an appropriate container. Do not add the ascorbic acid reagent until immediately before use. Mix well after each addition to prevent the solution from darkening.
solution | volume (mL) |
Ammonium molybdate | 50 |
Sulfuric acid | 125 |
Antimony potassium tartrate | 25 |
Ascorbic acid (immediately before use) | 50 |
Antimony potassium tartrate
F. Primary standard: 0.01 M Phosphorus (1000 mL) – make fresh every 4 weeks; store @ 4°C
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Dry monobasic potassium phosphate monobasic (KH2PO4) in oven at 100°C for two hours; keep in a desiccator while it cools before weighing.
In a 1000 mL volumetric flask, dissolve 1.361 g oven-dried KH2PO4 in ~600 mL nanopure water, then dilute this solution to 1000 mL with nanopure water.
Standards
concentration (µM) | volume of primary standard (mL) | volume of reagent water |
|---|---|---|
0 | 0 | 100 |
5.0 | 0.050 | 99.95 |
10.0 | 0.100 | 99.90 |
15.0 | 0.150 | 99.85 |
20.0 | 0.100 | 49.90 |
40.0 | 0.200 | 49.80 |
60.0 | 0.300 | 49.70 |
80.0 | 0.400 | 49.60 |
100 | 0.500 | 49.50 |
200 | 1.000 | 49.00 |
300 | 1.500 | 48.50 |
Procedure
1. | Add 2 mL nanopure water to an 8 mL glass vial. |
2. | Add 600 µL sample or standard. |
3. | Add 4 mL mixed reagent. |
4. | Shake well. |
5. | After a few minutes a blue color develops, which remains stable for a few hours. It is best to make the readings at 885 nm ~30 min after addition of the mixed reagent. |
Note: | Use a smaller aliquot of sample if the result exceeds the linear range of the spectrophotometer, making up the volume with nanopure water. (For example, for a 300 µL aliquot of a sample, add 300 µL nanopure water.) |
Silica
Note: Silica Silicon Silicon is routinely measured on the ICP, so measurement by spectroscopic analysis is can be considered an alternate method.
Dissolved silica determinations are of great importance in interstitial waters. Often they represent the lithology of the sediments, and the concentrations can vary substantially, especially if highly dissolvable phases such as biogenic opal-A, volcanic ash, or smectite are present. Thus, a wide range of concentrations can be expected, typically from 50 to 1200 µM or higher (especially in hydrothermally affected sediments). The method below usually covers the range, although greater dilutions may be appropriate if sediments or sample sizes necessitate this.
This method is based on the production of a yellow silicomolybdate complex. The complex is reduced by ascorbic acid to form molybdenum blue, measured at 812 nm. The blue complex is very stable, which will enable delayed reading of the samples.
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C: Metol Sulfite solution (500 mL) – make fresh every month; store in amber glass, tightly sealed @ 4°C
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Dissolve 6.0 g anhydrous sodium sulfite, Na{~}2{~}SO{~}3{~}, in a 500 mL volumetric flask. Add 10 g Metol (p-methylaminophenol sulfate \ [(C{~}7{~}H{~}10{~}NO){~}2{~}SO{~}4{~}\]) and then nanopure water to make the volume to 500 mL. When the Metol has dissolved, filter the solution through a Whatman No. 1 filter paper. *Note:* This solution may deteriorate quite rapidly and erratically.
D: Oxalic Acid solution (500 mL) – make fresh every month; store in glass
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E: Reducing solution (150 mL) – make fresh daily
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Note: When sodium silicofluoride (Na2SiF6) is dissolved in water, it hydrolyzes to form reactive dissolved silica. Place 1 g of Na2SiF6~ in an open vial and place in a vacuum desiccator overnight to remove excess water. Do not heat.
In a 1000 mL polyethylene volumetric flask, dissolve 0.5642 g dried sodium silicofluoride in ~800 mL nanopure water. Dissolution is slow; allow at least 3 minutes. Dilute the solution to 1000 mL with nanopure water.
Standards
Using a 50 mL volumetric flask, add the following amounts of primary standard to approximately 30 mL of nanopure water and then bring to a total of 50 mL. Store in polyethylene containers.
concentration(µM) | volume of primary standard (mL) | volume of nanopure water (mL) |
30 | 0.5 | 49.5 |
60 | 1.0 | 49.0 |
120 | 2 | 48.0 |
240 | 4 | 46.0 |
360 | 6 | 44.0 |
480 | 8 | 42.0 |
600 | 10 | 40.0 |
900 | 15 | 35.0 |
1200 | 20 | 30.0 |
Procedure
Make sure that all reagents are prepared ahead of time. The method has a time factor built in, and therefore it is of great importance to have all necessary reagents ready to go.
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12.
Measure 48 mL of nanopure water into the vials (7.63.8 mL for standards and blanks). |
2. | For standards and blanks (nanopure), pipette 2400 µL of synthetic seawater into the vials. |
3. | Pipette 4200 µL of sample/standard/blank into the vials. |
4. | Record time. |
5. | Add 24 mL of molybdate solution (reagent B) to the vials. A yellow color will develop; allow to mature for exactly 15 minutes (± 15 s). |
6. | Add 36 mL of the reducing solution (reagent E). |
7. | Cap the vials and let stand for at least 3 hours. |
8. | Read absorbances on the spectrophotometer at 812 nm. |
Procedure notes
– | Do not handle more than about thirty samples at a time in order to ensure that the 15 min time limit can be adhered to. Make sure that there are no large fluctuations in room temperature. |
– | Do not use synthetic seawater in dilutions of the primary standard. This could cause the decrease in reactive silica in a few hours as a result of polymerization reactions. |
– | The reason for adding 400 µL of synthetic seawater to the standards is to maintain a reasonably uniform salt content in relation to the samples, this suppressing a potential salt effect on the method. |
– | It is important to wait at least three hours for the blue color to develop; the higher the concentration, the longer the time. The color remains stable for many hours, and reading after 4–5 hours may, in fact, be a good idea. Again, consistency in time limits is advisable. |
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The sulfide method is based off a method developed by Cline in 1969. This method called for very large volumes of water (50mL). This method was modified on the BONUS Baltic Gas expedition in 2011 to work with sample volumes in the 1-5mL range.
The method is a bit tricky in that the reagent concentrations change depending on what concentration range your samples fall in:
- High range: 6-80 uM
- Low range: 1-10 uM.
All samples need to be preserved during splitting with a 1% Zinc Acetate Solution. It can require a relatively large amount of sample in order to do this analysis.
The high range method uses less sample (~500 µL), but if the sulfide level is below 6 µM, it won't be enough. It may still be worth screening samples with the high-range method in order to conserve interstitial water (IW) sample volume. The low-range method requires 4 mL (8x the amount of sample) but is sensitive down to 1 µM. The scientist will have to determine if consumption of 4 mL, possibly 4.5 mL, of sample is worth obtaining the sulfide concentration.
Reagent Solutions
A: 1% zinc acetate (w/v)
For Standard: Prepare 1 L of 1% zinc acetate by dissolving 10 g zinc acetate dehydrate into about 600 mL DI water in a 1 L volumetric flask. Add 1 mL of concentrated acetic acid, bring up to volume, and mix well.
For Splits: Prepare 100 mL of 1% zinc acetate by dissolving 1.0 g zinc acetate dehydrate into about 60 mL DI water in a 100 mL volumetric flask. Add 100 µL of concentrated acetic acid, bring up to volume, and mix well. Set aside for use on the splits.
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B: 1 mM zinc-sulfide standard suspension
Before weighing the sodium sulfide nonahydrate, wash the crystals off with DI water and dry with a clean Kim Wipe to remove the oxidation products from the crystal before weighing. Try to select very small crystals (or break them up) to facilitate accurate weighing. Dissolve 0.20 g of Na2S·9H2O in 1 L of 1% zinc acetate solution (Reagent A). Store in plastic and cool. Shake vigorously each time before using.
Note: It is very difficult to weigh 0.20 g of this reagent accurately because of the size of the crystals. Weigh 0.20 g within 5 mg and then record the mass used on the bottle. The Baltic Gas methods paper (Ferdelman et al., 2011) describes the use of sodium thiosulfate to standardize the Zn-S suspension, but this has not been the standard practice.
C: 100 µM zinc-sulfide standard
Dilute 10 mL of 1 mM zinc-sulfide standard suspension (Reagent B) up to 100 mL with DI water. This is the stock standard for the dilution of the standard curve.
D: High-Range Sulfide Diamine Reagent
For the high-range (6-80 µM) method, add 500 mL of concentrated HCl to 500 mL of DI water. Mix thoroughly and allow to cool to room temperature. Add 4.0 g of N,N-dimethyl-p-phenylenediamine sulfate and 6.0 g iron chloride hexahydrate (FeCl3·6H2O), mix well, and refrigerate in an amber Nalgene bottle.
E: Low-Range Sulfide Diamine Reagent
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Make dilutions of the 100 µM zinc-sulfide standard (Reagent C) for the standards to create 0.5 mL of standard at each level. Add the specified volume of Reagent C and DI water as shown in the table below to create the standards.
| µL 100 µM |
| Concentration (µM) |
Blank | 0 | 500 | 0.0 |
6 | 30 | 470 | 6.0 |
20 | 100 | 400 | 20 |
40 | 200 | 300 | 40 |
60 | 300 | 200 | 60 |
80 | 400 | 100 | 80 |
Shake the zinc acetate-preserved sample well before pipetting into it. For this method, the sample volume should be 0.5 mL. Add 40 µL of the high-range diamine reagent (Reagent D) to the sample, blank, and standards, and shake each vial. Place the samples, blank, and standards, into the dark for 30 minutes; the standards should turn blue. If the visual appearance of any of the samples is darker blue than the highest standard, dilute the sample in the dilution reagent (Reagent F) until it is within the color range of the standards.
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Make dilutions of the 100 µM zinc-sulfide standard (Reagent C) for the standards to create 4 mL of standard at each level. Add the specified volume of Reagent C and DI water as shown in the table below to create the standards.
| µL 100 µM |
| Concentration (µM) |
Blank | 0 | 4000 | 0.0 |
1 | 40 | 3960 | 1.0 |
2.5 | 100 | 3900 | 2.5 |
5 | 200 | 3800 | 5.0 |
7.5 | 300 | 3700 | 7.5 |
10 | 400 | 3600 | 10 |
Shake the zinc acetate-preserved sample well before pipetting into it. For this method, the sample volume should be 4 mL. Add 320 µL of the low-range diamine reagent (Reagent E) to the sample, blank, and standards, and shake each vial. Place the samples, blank, and standards into the dark for 30 minutes; the standards should turn blue. If the visual appearance of any of the samples is darker blue than the highest standard, dilute the sample in the dilution reagent (Reagent F) until it is within the color range of the standards.
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Analyzing Samples
Preparing the Instrument
1. | Engage the tubing on the peristaltic pump. Make sure that the waste line goes into a receptacle. |
2. | Turn on the unit and let it warm up for at least three hours. |
3. | Confirm that the instrument Beam Mode is correctly configured. This shouldn't change, but to confirm, in Varian > Cary WinUV start the Advanced Read application. Click the Setup button and select the Options tab. Confirm in the Beam Mode area that Double Beam is selected and Normal is also selected. (Figure 3) |
4. | To start the measuring computer application, select Varian > Cary WinUV > Simple Reads. |
5. | Clean the 'fill' tubing with a Kimwipe and aspirate nanopure water about six times, without returning. This is done by depressing the fill button on the front of the Cary unit. (Figure 4) |
Note: The Simple Reads application must be running to be able to operate the fill/return features on the Cary unit.
Figure 3. Setup Screen.
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Figure 4. Peristaltic Pump.
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Running Samples
Preparing Samples
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Setting up Instrument Parameters
1. | Click the Setup button to display the Setup dialog box (Figure 5). |
2. | Select Read at Wavelength and enter the wavelength for the analysis along with 1 s measurement time. |
2. | Click OK. The new wavelength is shown in the Abscissa status display at the top right of the application window. |
3. | To zero the current ordinate value, click the Zero button at the left side of the screen. This is best done after aspirating with nanopure water a few times. Do not re-zero the instrument during a measurement batch run. |
4. | In the Y Mode group, select the ordinate mode required (Abs). |
5. | To clear the contents (text) of the Report area, click on the Clear report button. |
Figure 5. Setup Dialog Box.
Measuring the Samples
1. | Insert the aspiration tube completely into the sample vial. |
2. | Depress the fill button on the front of the Cary. Make sure that the peristaltic pump aspirates the liquid. Do this a second time. |
3. | Monitor the absorbance value in the top left (above the Setup button) of the application window. When the value stabilizes, or wait at least 5 to 8 seconds, CONSISTENTLY, click the Read button to measure the sample at the specified wavelength. |
4. | The result of the sample read appears in the Report area and includes the ordinate reading obtained and the wavelength at which the reading was measured (Figure 6). |
5. | Depress the return button on the front of the unit to return the aspirated sample to the sample container for further analysis if required. |
6. | Remove the aspiration tubing from the sample vial and wipe clean with a Kimwipe. |
7. | Aspirate nanopure water in between samples to flush out the line. |
8. | Continue sample readings. Once all samples have been read, the data can be saved and/or printed. |
10. | Click on the Print… button to display the Windows Print dialog box to choose the printer and pages to print of the current displayed report (Figure 7). |
11. | To save data, select Save Data As… from the top File menu option. Save the data in an RTF format. |
12. | This file may be opened in Excel, using space-delimited option, and formatted per the requirements of the |
READ button 
Figure 6. Measuring Samples.
Figure 7. Print/Save Samples.
Data Analysis
Using the results from the reads of the standards, create a calibration curve from the plot of the concentration vs. absorbance values. Use this equation to extrapolate the sample concentrations from their corresponding absorbance value. This can be done in the same spreadsheet as created above in the Simple Reads application. This sheet can be loaded into the LIMS Spreadsheet Loader application as outlined in the LIMS Integration section.
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Aspirate approximately eight cycles of nanopure water, release the tubing on the peristaltic pump, turn off power to the unit and exit from the software. Clean any spills that may have occurred.
Empty the waste container and rinse with tap Anchor
QAQC
QA/QC for analysis consists of calibration verification using check standards, blanks and replicate samples.
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If the control limits are exceeded (generally 3 standard deviations from the mean), the instrument system is considered out of control and all samples in the current analytical batch are invalid and must be rerun after the system is proved to be in control.
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LIMS Integration
Results are stored in the LIMS database associated with an analysis code and an analysis component.
Analysis | Component Name | Component value | Unit |
SPEC | analyte | ammonium | — |
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| phosphate |
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| silica |
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| concentration | concentration of analyte | µM |
Data collected is transferred to the LIMS database using IODP's Spreadsheet Loader application. This is best done by entering the results into an Excel spreadsheet in a format similar to the pattern below, keeping the appropriate number of columns blank, and omitting the column headers. Then run the Spreadsheet Loader application. Go to File > Load and it should import something like below. To upload into the database, go to Lims > Upload and status messages will appear in the blank window (Figure 8).
Figure 8. Spreadsheet uploader.
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Maintenance and Troubleshooting
Cleaning
Any spills in the sample compartment should be immediately wiped up and any deposits on the sample compartment windows should also be removed.
The exterior surfaces should be cleaned with a soft cloth and, if necessary, this cloth can be dampened with water or a mild detergent.
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To replace a fuse, disconnect the unit from the power supply, and replace the blown fuse with one of the type and rating as outlined in the hardware specifications section.
1. | Disconnect the instrument from the power supply. |
2. | Undo the fuse cap by pressing the cap and turning it counter-clockwise. |
3. | Carefully pull out the cap. The fuse should be held in the fuse cap. |
4. | Check that the fuse is the correct type and is not damaged. If necessary, replace it. |
5. | Place the fuse into the cap, push the cap in and then turn the cap clockwise. |
6. | Reconnect the instrument to the power supply. |
Cary Win UV Help
Varian provides extensive help resources, available from the software CD. After installing the help utilities, go to START > All Programs > Varian > Cary WinUV > Cary Help.
Cary Help offers troubleshooting information, maintenance information like how to replace lamps, aligning lamps and mirrors, and replacing fuses and cleaning the flowcells.
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Contact Information
Sales and ServiceVarian Instruments2700 Mitchell Dr.Walnut Creek, CA 94598 Phone:1 800 926 3000 E-mail: customer.service@varianinc.com
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Health & Safety
Ultraviolet Radiation
The deuterium in the instrument emits hazardous ultraviolet radiation that can cause serious damage to eyes. NEVER look directly at the lamp.
Ozone can be generated by radiation from the source lamp. Exposure to ozone can result in irritation to exposed severe radiation damage to the skin, eyes, and upper respiratory system. The maximum permissible exposure level is 0.1 ppm. Be sure to work with the deuterium lamp using adequate ventilation.
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Ammonium Chloride
Health effects
Inhalation: | irritant |
Ingestion | irritant |
Contact: | irritant |
Incompatible materials
Concentrated acids, strong bases, silver salts, potassium chlorate, ammonium nitrate, hydrogen cyanide
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Ammonium Molybdate Tetrahydrate
Health effects
Inhalation: | irritant |
Ingestion: | irritant |
Contact: | irritant |
Incompatible materials
Alkali metals
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Hazards
Poison
Health effects
Inhalation: | irritant |
Ingestion: | toxic |
Contact: | irritant |
Incompatible materials
Alkali metals and their carbonates, perchloric acid, reducing agents
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Ascorbic Acid
Health effects
Inhalation: | mild irritant |
Ingestion: | mild irritant |
Contact: | mild irritant |
Incompatible materials
Strong oxidizers, alkalis and alkali hydroxides, iron, copper
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Bleach (Sodium Hypochlorite)
Health effects
Inhalation: | irritant |
Ingestion: | irritant |
Contact: | irritant |
Stability
Decomposes in air and sunlight
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Hazards
Flammable
Health effects
Inhalation: | irritant |
Ingestion: | irritant |
Contact: | irritant |
Incompatible materials
Oxidizing agents, acids, alkali metals, ammonia, peroxides, silver nitrate
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Poison, corrosive
Health effects
Inhalation: | corrosive, may be fatal |
Ingestion: | corrosive, may be fatal |
Contact: | corrosive, may cause permanent damage |
Incompatible materials
Strong bases, metals, metal oxides, hydroxides, amines, carbonates, alkaline materials and strong nitric acid.
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Magnesium Sulfate heptahydrate
Health effects
Inhalation: | minor irritant |
Ingestion: | minor irritant |
Contact: | minor irritant |
Stability
Stable but loses some moisture on exposure to dry air at room temperatures
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Combustable, toxic, possible sensitizer
Health effects
Inhalation: | harmful |
Ingestion: | harmful |
Contact: | harmful |
Incompatible materials
Strong oxidizing agents, acids, acid halides
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Poison, corrosive
Health effects
Inhalation: | may cause severe burns |
Ingestion: | toxic, may be fatal |
Contact: | may cause severe burns |
Stability
May become unstable under heat
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Hazards
Carcinogen
Health effects
Inhalation: | slightly hazardous, non-corrosive for lungs |
Ingestion: | VERY hazardous |
Contact: | VERY hazardous |
Skin contact: | corrosive, sensitizer, permeator |
Eye contact: | corrosive |
Stability
Stable but air and light sensitive
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Potassium Phosphate, Monobasic
Health effects
Inhalation: | irritant |
Ingestion: | irritant |
Contact: | irritant |
Sodium Chloride
Health effects
Inhalation: | mild irritant |
Ingestion: | mild irritant in large doses |
Contact: | irritant with eye contact |
Incompatible materials
Lithium, bromine trifluoride
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Sodium Sulfite
Health effects
Inhalation: | mild, cough, sore throat |
Ingestion: | mild |
Contact: | mild |
Stability
Stable
Incompatible materials
...
Hazards
Toxic
Health effects
Inhalation: | toxic |
Ingestion: | toxic, may be lethal |
Contact: | irritant |
Stability
Hygroscopic
Incompatible materials
...
Hazards
Toxic
Health effects
Inhalation: | toxic |
Ingestion: | toxic |
Contact: | irritant |
Incompatible materials
Metals
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Poison, danger, corrosive
Health effects
Inhalation: | strong irritant |
Ingestion: | corrosive, may be fatal |
Contact: | corrosive, may cause severe burns |
Stability
Reacts violently with water
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Trisodium Citrate
Health effects
Inhalation: | irritant |
Ingestion: | irritant |
Contact: | irritant |
Incompatible materials
Strong oxidizers
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Guidelines for Handling Chemicals
– | Wear gloves to protect from specific hazards. |
– | Wash hands immediately after removing gloves, after handling chemical agents, and before leaving the laboratory area. |
– | Wear laboratory coats and gloves only in the laboratory area. |
– | Confine long hair and loose clothing. |
– | Wear close-toed shoes. |
– | Do not store or prepare food, eat, drink, chew gum, apply lip balm or cosmetics, or handle contact lenses in areas where chemicals are handled. |
– | Label all chemical containers and reagent solution bottles. |
– | Keep laboratory work areas clean and uncluttered. |
– | Consult the MSDS before using any chemical. |
– | Know the emergency procedures for handling chemicals used. |
– | Vent into local exhaust devices vapors, fumes, mists, dusts, or gases. |
Waste Management
Waste management includes proper handling or reaction byproducts, surplus and waste chemicals, and contaminated materials. Each worker is responsible for ensuring wastes are handled in a manner that minimizes personal exposure and the potential for environmental contamination.
Dispose of cleaning solutions properly.
Dispose of surplus and expended reagents properly.
Select the least hazardous chemical for the job and use only in quantities needed. Minimize waste whenever possible by reducing both the volume and physical hazard or toxicity of the material.
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Gieskes, J.M., Gamo, T., and Brumsack, H., 1991. Chemical methods for interstitial water analysis aboard JOIDES Resolution, ODP Tech. Note, 15. doi:10.2973/odp.tn.15.1991.
Kastner, M., Elderfield, H., Martin, J.B., Suess, E., Kvenvolden, K.A., and Garrison, R.E., 1990. Diagenesis and interstitial water chemistry at the Peruvian margin—major constituents and strontium isotopes. In Suess, E., von Huene, R., et al., Proc. ODP, Sci. Results, 112: College Station, TX (Ocean Drilling Program), 413–440. doi:10.2973/odp.proc.sr.112.144.1990
Noriki, S. 1983. Silicate correction in the colorimetric determination of phosphate in seawater. J. Oceanograph. Soc. Japan, 39(6):324–326. doi:10.1007/BF02071829
Presley, B.J., 1971. Techniques for analyzing interstitial water samples: Appendix Part 1: determination of selected minor and major inorganic constituents. In Winterer, E.L., et al., Init. Repts. DSDP, 7(2): Washington, DC (U.S. Govt. Printing Office), 1749–1755. doi:10.2973/dsdp.proc.7.app1.1971
Solorzano, L., 1969. Determination of ammonia in natural waters by phenol-hypochlorite method. Limno. Oceanogr., 14:799–801.
Strickland, J.D.H., and Parsons, T.R., 1968. A manual for sea water analysis. Bull. Fish. Res. Board Can., 167.
Appendix
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Reagent Cheat Sheet
Ammonium |
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reagent | total volume (mL) | solute | amountadded | solvent | when |
A | 100 | 95% ethanol | 100 mL | NA | daily |
B | 101 | phenol | 1 mL | reagent A | daily |
C | 100 | sodium nitroprusside | 75 mg | nanopure | daily |
D | 500 | trisodium citrate / | 7.5 g /0.4 g | nanopure | monthly |
E | 50 | Sodium hypochlorite (bleach) | 1 mL | reagent D | daily |
F | 1000 | ammonium chloride (dried) | 5.345 g | nanopure | monthly |
Phosphate |
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Reagent | Total volume (mL) | Solute(s) | Amountadded | Solvent | When |
A | 1000 | sulfuric acid | 10 mL | nanopure | anytime |
B | 1000 | antimony potassium tartrate trihydrate | 0.102 g | nanopure | every two months |
C | 1000 | ammonium molybdate tetrahydrate | 2 g | nanopure | anytime |
D | 1000 | ascorbic acid | 3.5 g | nanopure | weekly |
E | 250 | reagent Creagent Areagent Dreagent B | 50 mL125 mL50 mL25 mL |
| 6 hours |
F | 1000 | potassium phosphate monobasic (dried) | 1.361 g | nanopure | monthly |
Silica |
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Reagent | Total volume (mL) | Solute(s) | Amountadded | Solvent | When |
A | 500 | sulfuric acid | 250 mL | nanopure | monthly |
B | 500 | ammonium molybdate tetrahydrate | 4 g | nanopure | monthly |
C | 500 | anhydrous sodium sulfite Metol | 6.0 g10 g | nanopure | monthly |
D | 500 | oxalic acid dihydrate | 50 g | nanopure | monthly |
E | 150 | reagent Creagent D | 50 mL30 mL | nanopure | daily |
F | 1000 | sodium chloridemagnesium sulfate heptahydrate | 25 g8 g | nanopure | monthly |
G | 1000 | sodium silicofluoride (dried) | 0.564 g | nanopure | bi-monthly |