Phosphorus total determination

Total oxidation reactions, in the presence of water, 19 87 Total oxygen demand (TOD) in wastewater treatment, 25 885 Total phosphorus content, determining,... 

This technique has found very limited applications in soil and sediment analysis and is particularly useful when routine automated analyses at the mg L 1 level of large numbers of samples is required. The technique has been applied to the determination of total phosphorus, total organic carbon and total nitrogen in soils, total organic carbon in non-saline sediments and total sulphur in saline sediments. 

Phosphorus was determined in the extracts by the spectrophotometric method of Murphy and Riley [63] and Stickland and Parsons [96]. In Table 12.10 results are shown obtained upon applying the procedure to the determination of total phosphorus in solutions of calcium phosphoglyceric acid. 

Environmental water samples to be analyzed for phosphate are not stored in plastic bottles unless kept frozen, because phosphates can be absorbed onto the walls of plastic bottles. Mercuric chloride, used as a preservative and acid (such as the nitric acid suggested for metals above), should not be used unless total phosphorus is determined. All containers used for water samples to be used for phosphate analysis should be acid rinsed, and commercial detergents containing phosphates should not be used to clean sample containers or laboratory glassware. 

The whole column, apart from a small portion of the sediment, is sam pled in this way. The chemical checks were carried out every 15 days, determining pH, Conductivity, C.O.D., Ammoniacal Nitrogen, Orthophosphate Phosphorus and, furthermore, each month Total phosphorus, Total Kjeldahl Nitrogen, Total Solids and Volatile Solids. The methods utilized are those indicated in the Standard Methods (A.P.H.A., 1980). The amount of matter particles sedimented in the tanks was estimated with the use ol appropriate sampling devices located at the bottom of the tanks and withdrawn after a variable permanence of 40 to 60 days. 

Maher, W. and L. Woo. 1998. Procedures for the storage and digestion of natural waters for the determination of filterable reactive phosphorus, total filterable phosphorus and total phosphorus. Anal. Chim. Acta 375 5 -7. 

Total phosphorus is determined as inorganic phosphate after treatment with hot perchloric acid. Phosphorus in D-glucose-6-phosphate residues is assayed using D-glucose-6-phosphate dehydrogenase. 

The determination of total phosphorus, total nitrogen, and organic carbon was introduced to the chemical monitoring programme of the IfM Warnemunde at selected stations in the 1980s. Since that time, investigations of harmful substances, such as heavy metals as well as chlorinated and petroleum hydrocarbons, started with special experiments and monitoring cruises. The details are shown in the relevant chapters. 

Heavy metals, boron (B(V)), arsenic and total phosphorus were determined in the fraction < 20 pm to improve the comparability of the results. This fraction was separated from the freeze-dried and non-milled samples by ultrasonic sieving (Ackermann 1980). Metals were analysed after microwave-assisted digestion with aqua regia at 180 °C in closed vessels by inductively coupled plasma optical emission spectroscopy, atomic fluorescence spectroscopy (mercury) and hydride atomic absorption spectroscopy (arsenic). 

We noted earlier that mass spectrometry had not been used to any extent in speciation studies of organic phosphorus in natural environments. Here we define phosphorus speciation as the determination of actual molecular formulas and structures of molecules containing phosphorus, and not the more commonly accepted, broad classes of phosphorus such as filterable reactive phosphorus, total filterable phosphorus, filterable organic phosphorus, etc. While a few studies have focused on particular classes of organic phosphorus, such as the inositol phosphates, we are not aware of any attempt to broadly speciate... 

Total phospholipids are quantitated by determination of the phosphorus content of lipid extracts from which non-lipid phosphorus has been removed by purification procedures. For this purpose chloroform-methanol extracts subjected to diffusion purification (Folch et al. 1951, Sperry 1955) are suitable. Lipid phosphorus is determined in aliquots of these extracts after digestion. Most procedures for determination of phosphorus are based on the method of Fiske and Subbarow (1925) which utilizes conversion of phosphate to phosphomolybdate and its subsequent reduction to molybdic blue. Modifications of this method were reviewed by Lindberg andERNSTER (1956). Avery convenient phosphorus assay was described by Bartlett (1959). Total phospholipids are calculated by multiplication of the lipid phosphorus values with 25. These values are only approximations since phosphorus does not represent exactly 4% of each phospholipid molecule. 

This method is used for the determination of total chromium (Cr), cadmium (Cd), arsenic (As), nickel (Ni), manganese (Mn), beiylhum (Be), copper (Cu), zinc (Zn), lead (Pb), selenium (Se), phosphorus (P), thalhum (Tl), silver (Ag), antimony (Sb), barium (Ba), and mer-cuiy (Hg) stack emissions from stationaiy sources. This method may also be used for the determination of particulate emissions fohowing the procedures and precautions described. However, modifications to the sample recoveiy and analysis procedures described in the method for the purpose of determining particulate emissions may potentially impacl the front-half mercury determination. 

The analysis of phosphates and phosphonates is a considerably complex task due to the great variety of possible molecular structures. Phosphorus-containing anionics are nearly always available as mixtures dependent on the kind of synthesis carried out. For analytical separation the total amount of phosphorus in the molecule has to be ascertained. Thus, the organic and inorganic phosphorus is transformed to orthophosphoric acid by oxidation. The fusion of the substance is performed by the addition of 2 ml of concentrated sulfuric acid to — 100 mg of the substance. The black residue is then oxidized by a mixture of nitric acid and perchloric acid. The resulting orthophosphate can be determined at 8000 K by atom emission spectroscopy. The thermally excited phosphorus atoms emit a characteristic line at a wavelength of 178.23 nm. The extensity of the radiation is used for quantitative determination of the phosphorus content. 

An alternative method for the determination of the total amount of phosphorus is the forming of a chinoline-phosphorus-molybdato complex [305]. 

Eberlein and Kattner [194] described an automated method for the determination of orthophosphate and total dissolved phosphorus in the marine environment. Separate aliquots of filtered seawater samples were used for the determination orthophosphate and total dissolved phosphorus in the concentration range 0.01-5 xg/l phosphorus. The digestion mixture for total dissolved phosphorus consisted of sodium hydroxide (1.5 g), potassium peroxidisulfate (5 g) and boric acid (3 g) dissolved in doubly distilled water (100 ml). Seawater samples (50 ml) were mixed with the digestion reagent, heated under pressure at 115-120 °C for 2 h, cooled, and stored before determination in the autoanalyser system. For total phosphorus, extra ascorbic acid was added to the aerosol water of the autoanalyser manifold before the reagents used for the molybdenum blue reaction were added. For measurement of orthophosphate, a phosphate working reagent composed of sulfuric acid, ammonium molyb-... 

Cambella and Antia [385] determined phosphonates in seawater by fractionation of the total phosphorus. The seawater sample was divided into two aliquots. The first was analysed for total phosphorus by the nitrate oxidation method capable of breaking down phosphonates, phosphate esters, nucleotides, and polyphosphates. The second aliquot was added to a suspension of bacterial (Escherichia coli) alkaline phosphatase enzyme, incubated for 2h at 37 °C and subjected to hot acid hydrolysis for 1 h. The resultant hot acid-enzyme sample was assayed for molybdate reactive phosphate which was estimated as the sum of enzyme hydrolysable phosphate and acid hydrolysable... 

Cembella et al. [40] have described a method for the determination of total phosphorus in seawater. The procedure used magnesium nitrate to oxidise organic compounds before standard molybdate colorimetric determination of ortho-phosphate. The method was applied to several pure organic phosphorus compounds and gave 93-100% recovery of phosphorus. 

With the use of the rapid fire detection and water deluge, there was no mass fire and the mix was ckrped into water for continued fire suppression. Any fire with RP results in the formation of white phosphorus (WP). WP must be covered with water since it ignites spontaneously when exposed to air. Processing studies were conducted to determine the best methods for pollution abatement since UP/water mixtures are toxic at 29 pob for blue gill bream and since high levels of phosphorus [reported as total phosphorus may not be durped into the environment. 

Bray RH, Kurtz LT. Determination of total, organic, and available phosphorus in soils. Soil Sci. 1945 59 39 16. 

Blood samples were centrifuged at 1000 x g for 20 min at 0-4°. Ionized calcium levels were immediately determined in serum and urine samples using a calcium ion-selective electrode (Ionetics, Inc., Costa Mesa, CA) urine volumes were recorded. The remaining serum and urine were aliquoted for various analyses and stored at -40°. Serum insulin was analysed by radioimmunoassay (Amersham Corp., Arlington Heights, IL). Serum levels of total calcium, phosphorus and creatinine as well as urine creatinine were determined by colorimetric procedures using an automated analyzer (Centrifichem, Baker Instruments Corp., Pleasantville, NY). Glomerular filtration rates (GFR) were calculated from serum and urine creatinine data GFR = urine creatinine/serum creatinine. 

Suppliers of visible spectrophotometers are reviewed in Table 1.1. Spectroscopic methods are applicable to the determination of phenols, chlorophenols, amines, mixtures of organics, boron, halogens, total nitrogen and total phosphorus in soils, cationic surfactants, carbohydrates, total nitrogen, phosphorus and sulphur in non-saline sediments, boron, total organic carbon, total sulphur and arsenic in saline sediments, cationic surfactants, adenosine triphosphate and total organic carbon in sludges. 

This technique has been applied to the determination of boron, total phosphorus and arsenic in soil, antimony and organosilicon compounds in non-saline sediments, arsenic in saline sediments and silicon and arsenic in sludges. 

Combustion methods have been used to determine total sulphur and total organic carbon and total halides in soil, total and particulate organic carbon, total halide, phosphorus and nitrogen, total and particulate organic carbon in saline sediments and total nitrogen in sludges. 

It is seen by examination of Table 1.11(b) that a wide variety of techniques have been employed including spectrophotometry (four determinants), combustion and wet digestion methods and inductively coupled plasma atomic emission spectrometry (three determinants each), atomic absorption spectrometry, potentiometric methods, molecular absorption spectrometry and gas chromatography (two determinants each), and flow-injection analysis and neutron activation analysis (one determinant each). Between them these techniques are capable of determining boron, halogens, total and particulate carbon, nitrogen, phosphorus, sulphur, silicon, selenium, arsenic antimony and bismuth in soils. 

The Standing Committee of Analysts (UK) have described a method for the determination of total nitrogen and phosphorus in sewage sludges [56]. 

Aspila et al. [60] have described a semi-automated method for the determination of inorganic, organic and total phosphorus in river and lake sediments. Total phosphorus is extracted from sediments with 1M hydrochloric acid after ignition at a high temperature (550°C) (method 1) or by digestion with sulphuric acid-potassium persulphate at 135°C in a sealed PTFE-lined Parr bomb (method 2). 

The automated spectrophotometric procedure [47] for the determination of total nitrogen in soils discussed in section 12.5.1.2 has also been applied to the determination of 0-0.75% phosphorus in soils. The method is based on the formation of the yellow molybdate-vanadate complex which has an absorption maximum at 420nm. 

Olsen et al. [71] have reviewed the determination of inorganic, organic and total phosphorus in soil and sediments. Determination of total phosphorus in aqueous samples commonly involves a hot acid oxidation type digestion procedure, although various other dry-ashing, fusion and UV... 

The coefficient of variation obtained for the determination of total phosphorus in sediment at the 1400ppm level was 2.5%. Some 98-100% recovery of inorganic phosphate was obtained in spiking experiments carried out on sediments. 

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