Phosphorus, Reactive HR, 8114

Phosphorus, Reactive
Molybdovanadate Rapid Liquid Method1 HR (0.3 to 45.0 mg/L PO43)
Scope and Application: For treated and natural waters
1

DOC316.53.01114 Method 8114 Pour-Thru Cell

Adapted from Standard Methods for the Examination of Water and Wastewater.

Test preparation

How to use instrument-specific information

The Instrument-specific information table displays requirements that may vary between instruments. To use this table, select an instrument then read across to find the corresponding information required to perform this test.

Table 344 Instrument-specific information

Instrument DR 6000 DR 5000 DR 3900 DR 3800, DR 2800, DR 2700 Pour-Thru Kit LQV175.99.20002 LZV479 LQV157.99.10002 5940400 Pour-Thru Cell Orientation Arrow faces right Align cell flow arrows with arrows on cell compartment 1-inch (round) path aligned with arrow on the adapter Adapter LZV585 (B)

Before starting the test:

See the User Manual for Pour-Thru Module installation instructions. Clean the Pour-Thru cell and all labware as specified in Analysis labware treatment. Protect the Pour-Thru Cell from contamination when not in use by inverting a small beaker over the top of the glass funnel. Make sure the PourThru cell is completely seated in the sample cell compartment. Final samples will contain molybdenum. In addition, final samples will have a pH less than 2 and are considered corrosive (D002) by the Federal RCRA. Refer to the current MSDS for safe handling and disposal information.

Description Molybdovanadate Reagent Water, deionized Cylinder, graduated, 25-mL, poly Dispenser, fixed volume, 1.0-mL, w/bottle Flask, Erlenmeyer, 125-mL, PMP w/cap Instrument-specific information

Quantity 2 mL 25 mL 1 1 2 1

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Description See Consumables and replacement items for reorder information.

Quantity

Molybdovanadate Rapid Liquid method

Stored Programs 489 P React. Mo. HR RL Start

1. Select the test. Insert an adapter if required (see Instrumentspecific information).

2.

3. Rinse a clean plastic 125-mL Erlenmeyer flask and a 25-mL graduated cylinder with deionized water.

4. Blank Preparation: Measure 25 mL of deionized water in the graduated cylinder. Pour the water into the flask.

5. Rinse another clean plastic 125-mL Erlenmeyer flask with deionized water.

6. Prepared Sample: Measure 25 mL of sample in the graduated cylinder. Pour the water into the flask.

7. Add 1.0 mL of Molybdovanadate Reagent to each flask using a Repipet Jr. Dispenser. Swirl to mix. A yellow color will develop in the sample if phosphate is present. A small amount of yellow may be present in the blank due to the reagent.

8. Start the instrument timer. A 7-minute reaction period will begin. If the sample concentration is greater than 30 mg/L PO43, read at exactly seven minutes or make a 1:1 dilution of the sample and begin the test again.

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Phosphorus, Reactive Molybdovanadate Rapid Liquid method (continued)

Zero

Read

9. When the timer expires, pour the blank from the flask into the Pour-Thru Cell.

10. ZERO the instrument. The display will show: 0.0 mg/L PO43

11. Pour the prepared sample from the flask into the Pour-Thru Cell.

12. READ the results in mg/L PO43. Flush the Pour-Thru Cell with 50 mL of deionized water.

Interferences
See the Interfering substances table for a list of substances, interference levels and type of interference. See the Noninterfering substances at low concentrations (less than 1000 mg/L) table for a list of substances that do not interfere in concentrations less than 1000 mg/L.

Table 345 Interfering substances

Interfering substance Arsenate Bismuth Fluoride Iron, Ferrous Molybdate Silica Interference level Negative interference. Positive interference if sample is heated. Negative interference. Negative interference. Blue color is caused by ferrous iron but this does not affect results if the ferrous iron concentration is less than 100 mg/L. Negative interference. Positive interference if sample is heated. Negative interference. Sulfide interference may be removed by oxidation with Bromine Water as follows: 1. Measure 25 mL of sample into a flask. Sulfide 2. 3. Thiocyanate Thiosulfate Thorium Highly buffered samples or extreme sample pH
1

Add Bromine Water1 drop-wise with constant swirling until permanent yellow color develops. Add Phenol Solution1 drop-wise until the yellow color just disappears. Proceed with step 7.

Negative interference. Negative interference. Negative interference. May exceed the buffering capacity of the reagents and require sample pretreatment.

See Optional reagents and apparatus.

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Phosphorus, Reactive Table 346 Noninterfering substances at low concentrations (less than 1000 mg/L)
Pyrophosphate Citrate Oxalate Al3+ Ca2+ Li+ NH4
+

Tetraborate Lactate Tartrate Selenate Ba2+ Na+ Cd2+ NO2 Pb2+ Sn2+ Ag+ AsO3 ClO4 Fe3+

Benzoate Formate Salicylate Mg2+ Sr2+ K+ Mn2+ SO42 Hg+ Cu2+ U Br CN SiO44

NO3 SO32 Hg2+ Ni2+ Zr4+ CO32 IO3

Sample collection, preservation and storage

Collect samples in clean plastic or glass bottles that have been cleaned with 1:1 Hydrochloric Acid Solution* and rinsed with deionized water. Do not use detergents that contain phosphate for cleaning labware. Analyze samples immediately for best results. If prompt analysis is not possible, preserve samples by filtering immediately and storing the sample at 4 C (39 F) or below for up to 48 hours. Warm stored samples to room temperature before analyzing.

Analysis labware treatment

1. Clean containers by normal means (do not use detergents containing phosphorus), then rinse with deionized water. 2. Soak for several minutes in a 1:25 dilution of Molybdovanadate Reagent in deionized water. 3. Rinse well with deionized water. Dedicate these containers for HR PO43 analysis. 4. Fill the Pour-Thru Cell with this same mixture of Molybdovanadate reagent and deionized water and let stand for several minutes. 5. Rinse the Pour-Thru Cell with 50 mL of deionized water.

* See Optional reagents and apparatus.

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Phosphorus, Reactive

How to clean the Pour-Thru Cell

The Pour-Thru Cell may accumulate a buildup of colored products, especially if the reacted solutions are allowed to stand in the cell for long periods after measurement. To clean the PourThru Cell: 1. Remove the color by rinsing with a 1:5 dilution of ammonium hydroxide* 2. Follow with several deionized water rinses. 3. Invert a beaker over the glass funnel of the Pour-Thru Cell when not in use.

Accuracy check
Standard additions method (sample spike) Required for accuracy check: Phosphate Voluette Ampule Standard Solution, 500-mg/L as PO43 Ampule breaker TenSette Pipet and tips Mixing cylinders (3)

1. After reading test results, leave the sample cell (unspiked sample) in the instrument. 2. Select standard additions from the instrument menu: OPTIONS>MORE>STANDARD ADDITIONS. 3. Accept the default values for standard concentration, sample volume and spike volumes. After the values are accepted, the unspiked sample reading will appear in the top row. See the user manual for more information. 4. Open the standard solution ampule. 5. Use the TenSette Pipet to prepare spiked samples: add 0.1 mL, 0.2 mL and 0.3 mL of standard to three 25-mL mixing cylinders and fill to 25 mL with the fresh sample. Mix thoroughly. 6. Follow the Molybdovanadate Rapid Liquid method test procedure for each of the spiked samples, starting with the 0.1 mL sample spike. Measure each of the spiked samples in the instrument. 7. Select GRAPH to view the results. Select IDEAL LINE (or best-fit) to compare the standard addition results to the theoretical 100% recovery.

* Optional reagents and apparatus.

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Phosphorus, Reactive
Standard solution method
Note: Refer to the instrument user manual for specific software navigation instructions.

Required for accuracy check: 10.0-mg/L Phosphate Standard

1. Use the 10.0-mg/L Phosphate Standard solution in place of the sample. Follow the Molybdovanadate Rapid Liquid method test procedure. 2. To adjust the calibration curve using the reading obtained with the standard solution, navigate to Standard Adjust in the software: OPTIONS>MORE>STANDARD ADJUST. 3. Turn on the Standard Adjust feature and accept the displayed concentration. If an alternate concentration is used, enter the concentration and adjust the curve to that value.

Method performance
Program 489 Standard 10.0 mg/L PO43 Precision 95% Confidence Limits of Distribution 9.910.1 mg/L PO43 Sensitivity Concentration change per 0.010 Abs change 0.34 mg/L PO43

Summary of method
In the molybdovanadate method, orthophosphate reacts with molybdate in an acid medium to produce a phosphomolybdate complex. In the presence of vanadium, yellow vanadomolybdophosphoric acid is formed. The intensity of the yellow color is proportional to the phosphate concentration. Test results are measured at 430 nm.

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Consumables and replacement items

Required reagents
Description Molybdovanadate Reagent Water, deionized Quantity/Test 2 mL 25 mL Unit 500 mL 4L Catalog number 2076049 27256

Required apparatus
Description Cylinder, graduated, 25-mL, poly Dispenser, adjustable Flask, Erlenmeyer, 125-mL, PMP w/cap Quantity 1 1 2 Unit each each each Catalog number 108140 2563137 2089843

Recommended standards
Description Phosphate Standard Solution, 10-mg/L as PO4 Phosphate Standard Solution, Voluette
3 3

Unit 946 mL 16/pkg 500 mL

Catalog number 1420416 1424210 2833149

ampule, 10-mL, 500-mg/L as PO4

Wastewater Influent Standard for NH3N, NO3N, PO4, COD, SO4, TOC

Optional reagents and apparatus

Description Ammonium Hydroxide, ACS Bromine Water, 30 g/L Cylinder, graduated mixing, 25 mL Hydrochloric Acid Solution, 6.0 N, 1:1 Phenol Solution, 30 g/L Pipet, TenSette, Pipet, 0.1 - 1.0 mL Pipet Tips, for TenSette Pipet 19700011 Pipet Tips, for TenSette Pipet 19700011 Filter Paper, folded 12.5 cm Filter Funnel, Analytical, 65 mL Thermometer, Non-Mercury, -10 to 225 C Sampling Bottle with cap, low density polyethylene, 250 mL
1

Unit 500 mL 29 mL each 500 mL 29 mL each 50/pkg 1000/pkg 100/pkg each each 12/pkg

Catalog number 10649 221120 189640 88449 211220 1970001 2185696 2185628 69257 108367 2635700 2087076

Other sizes are available

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Optional standards
Description Voluette Ampule breaker, 10 mL Phosphate, Standard Solution, 3 mg/L Phosphate, Standard Solution, 15 mg/L Phosphate, Standard Solution, 30 mg/L Phosphate, Standard Solution, 50 mg/L, 10 mL Voluette Ampules Phosphate, Standard Solution, 100 mg/L Phosphate, Standard Solution, 500 mg/L Unit each 946 mL 100 mL 946 mL 16/pkg 100 mL 100 mL Catalog number 2196800 2059716 1424342 1436716 17110 1436832 1424232

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