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RSIL Home > Isotope Fractionation Project > Instructions for Collecting Samples

Instructions for Collecting Samples

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Lab Code Description Bottle
489
1142
1172
1574		 O-18/O-16 and/or H-2/H-1 of water 2 oz (60 mL) glass bottle with Polyseal cap available free from RSIL (or order Q411FLD at One-Stop Shopping)

For small samples, 11 mL glass vials with Polyseal caps are available for purchase from RSIL in boxes of 144 units.
Treatment, Preservation, and Sample Amount
Do not field rinse bottle. Do not add chemical treatment. Fill bottle two-thirds full with either raw or filtered water so that if sample expands or freezes during shipping, bottle will not break. Cap bottle with Polyseal cap. Store at ambient temperature until shipped to laboratory.

For sample amounts as small as 0.5 mL, please contact RSIL.
  • Lab code 489 Only O-18/O-16 isotope-ratio analysis of water
  • Lab code 1142 Both H-2/H-1 and O-18/O-16 isotope-ratio analysis of water
  • Lab code 1172 Both H-2/H-1 and O-18/O-16 isotope-ratio analysis of water (quantity of 40 or more)
  • Lab code 1574 Only H-2/H-1 isotope-ratio analysis of water

Lab Code Description Bottle
N/A H-2/H-1 and O-18/O-16 of pore water in sediments or biological material such as branches and plants (toluene extraction method) Container that prevents evaporation of water.
Treatment, Preservation, and Sample Amount
Ship sediments so that they do not freeze. Freeze biological material after collection and ship frozen.

Sufficient sample should be shipped to provide at least 5 g water.

Lab Code Description Bottle
1135
1137		 C-13/C-12 and O-18/O-16 of calcite HDPE 20-mL scintillation vial with Polyseal cap, Wheaton 986706.
Treatment, Preservation, and Sample Amount
Sample should be dried and powdered to between 100 and 200 micrometer to ensure isotopic homogeneity.

Maximum sample amount of calcite is 0.5 g. For sample amounts as small as 0.02 g, contact RSIL.
  • Lab Code 1135 Both C-13/C-12 and O-18/O-16 of powdered calcite
  • Lab Code 1137 Only O-18/O-16 of powdered calcite

Lab Code Description Bottle
1710 C-13/C-12 of dissolved inorganic carbon in water precipitated as strontium carbonate 250 mL glass bottle with Polyseal cap or if concentration is low, 1-L bottle with Polyseal cap.
Treatment, Preservation, and Sample Amount
Do not field rinse bottle. Fill bottle to overflowing. Decant about 20 mL of sample. With a 5 or 10-mL plastic syringe having a 15-cm Tygon tube on its end, withdraw a syringe full of ammoniacal strontium chloride (see below) and discard to clean out any carbonate in the syringe. Transfer 5 to 20 mL ammoniacal strontium chloride to sample bottle and cap immediately.

Ammoniacal strontium chloride preparation: Dissolve 500 g of SrCl2 6H2O reagent in a standard 4–pound NH4OH reagent bottle (or 4 to 1 ratio of NH4OH to SrCl2). Let stand for 2 days. Decant the clear reagent into clean glass field reagent bottle. Always use the clear reagent in the upper part of the field reagent bottle. Minimize head space in reagent bottles because air contains carbon dioxide, which can precipitate as solid strontium carbonate in field reagent bottle.

Lab Code Description Bottle
1832
2893		 N-15/N-14 and/or C-13/C-12, and N and C conc. in of invertebrates, plants, or sediments HDPE 20-mL scintillation vial with Polyseal cap, Wheaton 986706.
Treatment, Preservation, and Sample Amount
Sample should be dried and powdered to 100 to 200 micrometer to ensure isotopic homogeneity. No treatment, preservation, or special shipping requirements.

Concentration of N in sample must be at least 1 mg/g; concentration of C in sample must be at least 1 mg/g. Total amount of N in sample must be at least 0.15 mg; total amount of C in sample must be at least 0.15 mg. Maximum sample amount is 1 g.
  • Lab Code 1832 C-13/C-12, N-15/N-14, C conc, & N conc in invertebrates, plants & sediments
  • Lab Code 2893 N-15/N-14 & N conc in invertebrates, plants & sediments

Lab Code Description Bottle
1851 C-13/C-12 of dissolved inorganic carbon in water 40-mL clear EPA VOC vials with open-top septa-lined caps (teflon-lined silicone septa should be REPLACED with hand-punched black butyl-rubber septa). Bottles with septa provided by RSIL at no cost to sample submitter.
Treatment, Preservation, and Sample Collection
1. Collect 2 to 3 bottles of sample water.
2. Needed:
   a. 60-mL syringe and syringe filters (or filter disks in Swinnex holder). Recommended type: Whatman Polysulfone GD/X Syringe Filters or equivalent (Whatman catalog #: 6876-2502; VWR catalog #: 28138-166), Low protein binding filter for aqueous samples. Filtering assembly includes two prefilters [graded density Multigrade GMF 150 (10:1 µm) and Grade GF/F (0.7 µm)] and a 0.2 µm polysulfone final filter. Prefilters allow filtration of even the most difficult samples with minimal hand force. Choose the 25-mm (0.98 inch) size for sample volumes greater than 10 mL.

Sample Collection:

1. Pull sample water into a 60-mL syringe and empty 2 to 3 times to rinse the syringe with fresh sample.
2. SLOWLY pull sample for collection into the syringe (try to avoid entraining excess sediment and air bubbles).
3. Remove bubbles/headspace from syringe by tilting syringe upwards and expelling excess air.
4. Attach syringe filter. Flush filter with approximately 10 mL of water (to rinse filter).
5. SLOWLY push sample water into the vial. Vials need to be COMPLETELY FULL—fill until a positive (convex upward) meniscus forms over the vial opening.
6. Screw the cap onto the vial firmly (some spillage will occur) until the septa slightly pops up into the cap opening, but DO NOT OVERTIGHTEN CAP. If the septa appears to be creased or if it is off-center, the vial may leak and the sample will be compromised.
7. Keep the vials chilled until analysis. DO NOT FREEZE VIALS. Freezing will cause the water to expand and crack the vials.
8. No preservative is needed.

Lab Code Description Bottle
1852 C-13/C-12 of dissolved organic carbon in water 40-mL amber EPA VOC vials with open-top septa-lined caps (septa are made of teflon-lined silicone). Bottles with septa provided by RSIL at no cost to sample submitter.
Treatment, Preservation, and Sample Collection
1. Collect 2 to 3 bottles of sample water.
2. Needed:
   a. 60-mL syringe and syringe filters (or filter disks in Swinnex holder). Recommended type: Whatman Polysulfone GD/X Syringe Filters or equivalent (Whatman catalog #: 6876-2502; VWR catalog #: 28138-166), Low protein binding filter for aqueous samples. Filtering assembly includes two prefilters [graded density Multigrade GMF 150 (10:1 µm) and Grade GF/F (0.7 µm)] and a 0.2 µm polysulfone final filter. Prefilters allow filtration of even the most difficult samples with minimal hand force. Choose the 25-mm (0.98 inch) size for samples greater than 10 mL.
   b. ASC grade 85-percent phosphoric acid (H3PO4).

Sample Collection:

1. Add a small drop (20 uL) of 85-percent phosphoric acid to the vial prior to filling to preserve the sample.
2. Pull sample water into a 60-mL syringe and empty 2 to 3 times to rinse the syringe with fresh sample.
3. SLOWLY pull sample for collection into the syringe (try to avoid entraining excess sediment).
4. Remove bubbles/headspace from syringe by tilting syringe upwards and expelling excess air.
5. Attach syringe filter. Flush filter with approximately 10 mL of sample water (to rinse filter).
6. SLOWLY push sample water into the amber vial. Vials need not be completely full—a small headspace is acceptable.
7. Screw the cap onto the vial firmly, but DO NOT OVERTIGHTEN CAP. If the septa appears to be creased or if it is off-center, the vial may leak.
8. Keep the vials chilled until analysis. DO NOT FREEZE VIALS. Freezing will cause the water to expand and crack the vials.

Lab Code Description Bottle
1947 S-34/S-32 of total sulfide in rock Contact RSIL
Treatment, Preservation, and Sample Amount
Contact RSIL

Lab Code Description Bottle
1948 S-34/S-32 of dissolved sulfide, pure Ag2S Contact RSIL
Treatment, Preservation, and Sample Amount
Contact RSIL

Lab Code Description Bottle
1949 S-34/S-32 (with or without
O-18/O-16) of dissolved SO4 < 20 mg/L		 Collected on anion exchange resin (Amberlite IRA-400 (RN(CH3)3 + Cl-) ordered from RSIL ($35 each). Rinse with 50 mL DI water before use.
Treatment, Preservation, and Sample Amount
Sulfate and sulfide concentration should be determined in the field before sample collection. Each sample that contains < 20 mg/L sulfate should be collected on anion exchange resin, chilled, and maintained at 4 deg C until shipped. Fill a 10-L bucket with sample and acidify with 1M HCl to pH of 3 to 4. With a rate of 0.4 liter/minute, pump with a peristaltic pump sufficient sample through resin to collect 20 to 40 mg of sulfate. Resin capacity is such that it can easily accommodate 4 L water having a sulfate concentration of 10 mg/L, or 8 L of 5 mg/L, or 20 L of 1 mg/L. If the water contains sulfide, the collection should be fast to avoid possible oxidation by oxygen in air of the sulfide to sulfate.

1M HCl can be prepared by adding 40.4 mL of 38% commercial HCl solution to 500 mL of DI water.

Lab Code Description Bottle
1950 S-34/S-32 of sulfate in rock or sediment Contact RSIL
Treatment, Preservation, and Sample Amount
Contact RSIL

Lab Code Description Bottle
1951 S-34/S-32 (with or without
O-18/O-16) of dissolved SO4 > 20 mg/L		 32 oz (1 L) polyethylene bottle (Q35FLD at One-Stop Shopping)
Treatment, Preservation, and Sample Amount
Sulfate and sulfide concentration should be determined in the field. Each sample should be filtered by a 0.4 µm polycarbonate membrane filter. Sample should be collected in a maximum of 1-L glass or plastic bottle. For sulfate concentration less than 20 mg/L, use 1949. A sample that contains > 0.01 mg/L sulfide or has a sulfate/sulfide ratio < 40 should be stripped of its sulfide in the field (please see USGS Open File Report 97-234).

Lab Code Description Bottle
1800 S-34/S-32 of biological material, sediment, and other solids Contact RSIL
Treatment, Preservation, and Sample Amount
Contact RSIL

Lab Code Description Bottle
2894
2897		 N-15/N-14 (with or without
O-18/O-16) of nitrate in soil		 HDPE 20-mL scintillation vial with Polyseal cap, Wheaton 986706.
Treatment, Preservation, and Sample Amount
Sample should be dried (or frozen) to prevent biological reaction of nitrogen-bearing species during storage or transport to laboratory. No special shipping is required.

Concentration of nitrate in sample must be at least 1 mg/kg as N. Total amount of nitrate in sample must be at least 0.02 mg as N. Maximum sample amount is 30 g. For samples containing atmospheric nitrate, the bacterial method may overestimate the delta N-15 values by as much as 1 to 2 per mill. For samples that may contain more than about 20 percent atmospheric nitrate, users should collect samples with a minimum of 0.4 mg of N and contact RSIL about methods to avoid this problem.

For samples containing nitrite, the bacterial method will determine the N isotopic composition of the nitrate + nitrite, but the O isotopic composition may be incorrect. If nitrite concentrations are known to be significant, they should be provided to RSIL.

If nitrate concentration is too low or insufficient nitrate is provided, the RSIL will attempt an isotopic analysis, but may not be successful. The sample submitter will be charged for the full cost of the analysis. Sample submitters with laboratory capabilities may want to dissolve nitrate from sediments themselves and confirm that the nitrate concentration is sufficient prior to submitting the dissolved nitrate sample for isotopic analysis. The following procedure is suggested. Approximately 30 mg of solid sample is placed in a 150-mL beaker and 80 mL of DIW (deionized water) is added; the sample and water are stirred well and allowed to sit overnight covered. The sample is then filtered and rinsed several times with 10-mL aliquots of DIW, not to exceed more than 300 mL of water in total. An aliquot is submitted for determination of nitrate concentration--LC 1979 is recommended. The remaining sample is frozen. If LC 1979 indicates that the concentration is greater than 0.03 mg/L as N, the frozen sample is submitted on ice to the RSIL for isotopic analysis.
  • Lab Code 2894 N-15/N-14 of nitrate in soil
  • Lab Code 2897 N-15/N-14 and O-18/O-16 of nitrate in soil

Lab Code Description Bottle
2895 N-15/N-14 of ammonium in soil 16 oz (500 mL) polypropylene bottle, 89 mm cap, Q413FLD (bottle) and Q422FLD (cap) at One-Stop Shopping
Treatment, Preservation, and Sample Amount
Sample should be dried (or frozen) to prevent biological reaction of nitrogen-bearing species during storage or transport to laboratory. No special shipping is required.

Concentration of ammonium in sample must be at least 0.2 mg/kg as N. Total amount ammonium in sample must be at least 0.2 mg as N. Maximum sample amount is 1 kg.

Lab Code Description Bottle
2898 N-15/N-14 of ammonium dissolved in water 32 oz (1 L) polyethylene bottle (Q35FLD at One-Stop Shopping)
Treatment, Preservation, and Sample Amount
Field rinse bottle. Filter sample thru 0.45 micron filter. Collect filtered water in polyethylene bottle with a Polyseal cap, leaving enough headspace to add preservative. Preserve the sample by adding concentrated (1:1 or 18N) H2SO4 to achieve a pH between 1.8 and 2.2. Usually 1 mL of 18N acid or 4 mL of 4.7N acid will be sufficient. Label the bottles to indicate how much H2SO4 has been added. Samples can be stored and shipped chilled or at room temperature. Submitter must provide concentration of ammonium in sample before sample can be analyzed. LC 3116 is satisfactory for this determination. Sample should be held until the ammonium concentration is available.

Concentration of ammonium in sample must be at least 0.2 mg/kg as N. Total amount of ammonium in sample must be at least 0.2 mg as N. Maximum sample amount is 1 L.

Lab Code Description Bottle
2899
2900		 N-15/N-14 (with or without
O-18/O-16) of nitrate dissolved in water		 4 oz (125 mL) amber polyethylene bottle, untreated (Q33FLD or Q405FLD in One-Stop Shopping). It is recommended that conical insert Polyseal caps be used with these bottles. Secure the caps with Parafilm or electrical tape to prevent leakage.
Treatment, Preservation, and Sample Amount
Field rinse bottle. Normally, there are two steps needed to filter the samples. The first filtration step is performed in the field with a 0.45 μM filter. The second filtration step is carried out with a 60 mL syringe and a 0.2 μM syringe filter either on site or in the laboratory. If the sample submitter is unable to perform the second filtration step, please contact RSIL.

Fill the bottle only ¾ full. Secure the caps with electrical tape to prevent leakage. Freeze sample to prevent biological reaction of nitrogen-bearing species during storage or transport to laboratory. Alternatively, samples can be preserved by adding reagent-grade NaOH or KOH to achieve a pH greater than 10, but not higher than 11.95 (typically 1 “pellet” per 125-mL bottle). Label the bottles to indicate if hydroxide has been added. Submitter must provide concentration of nitrate in sample with an accuracy of ± 10 percent or better before sample can be analyzed. A “‹” value is not acceptable. LC 1975 can be used for samples with concentrations above 0.06 mg/L as N. LC 1979 can be used for samples with concentrations less than 0.06 mg/L. If concentration provided is not accurate to within ±10 percent, the normal accuracy of the technique cannot be achieved and the submitter will be charged for any additional isotopic measurements needed. Samples should be held until nitrate concentration is available. Ship on ice or at 4 deg C if not preserved.

Concentration of nitrate in sample must be at least 0.03 mg/kg as N. The minimum sample amount is 30 mL. M
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