How Lignosulfonate Is Tested: Key Lab Methods

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How Lignosulfonate Is Tested: Key Lab Methods

Lignosulfonate is tested for identity, composition and performance. Routine quality checks cover dry matter, lignosulfonate content, pH, water-insoluble matter, ash, sulphate, reducing sugars and the cation (calcium, sodium, magnesium). Identity is confirmed by UV absorption at about 280 nm and by infrared spectrum; food-grade material is also tested for molecular weight, degree of sulfonation and heavy metals.

Routine Quality Tests

TestWhat it tells youTypical principle
Dry matter / moistureWater content; powder grades are usually ≤5–8% moistureOven drying to constant weight (JECFA loss on drying: 105 °C, 24 h)
Lignosulphonate contentHow much of the solids is active polymerUV absorbance of a diluted solution against a reference, or gravimetric methods
pHAcidity of a defined solution (often 10%)pH meter
Water-insoluble matterUndissolved residue such as fibre or saltsFiltration and drying of residue
AshInorganic content including the cationIgnition in a furnace
SulphateInorganic sulfate from pulping chemicalsGravimetric (barium sulfate) or ion chromatography
Reducing sugarsResidual wood sugars; affects setting and feed limitsCopper-reduction method or chromatography
Calcium, magnesium, sodiumConfirms the cation and hardnessTitration (EDTA), AAS or ICP

Identity Tests

TestJECFA criterion for calcium lignosulfonate (40-65)
UV spectrumAbsorption maximum at 280 nm in a diluted solution adjusted to pH 2.0–2.2
IR spectrumCharacteristic absorptions at 1210–1220, 1037 and 655 cm-1
SolubilitySoluble in water, practically insoluble in organic solvents
pH2.7–3.3 (10% solution)
Weight-average molecular weight40,000–65,000 by SEC with light scattering
Degree of sulfonation0.3–0.7 (organic sulfur to methoxyl)
Source: JECFA specification, 2008. Industrial grades are not required to meet these values.

Purity Tests for Food and Feed

ParameterJECFA calcium lignosulfonate (40-65)Typical feed-grade data sheet
Reducing sugars≤5.0% (dry basis)EU 1g565: ≤20% (dry matter)
Total ash≤14.0% (dry basis)Stated on TDS
Lead≤2 mg/kgFor example ≤0.5 mg/kg (GAC-CaLS-Feed TDS)
Arsenic≤1 mg/kgFor example inorganic As ≤0.1 mg/kg (GAC-CaLS-Feed TDS)
Sulfite≤0.5% (dry basis)—

Performance Tests by Application

ApplicationCommon performance test
ConcreteWater reduction and setting time against a reference mix; mortar or concrete flow
Dye and pigment dispersionDispersion and filter tests, heat stability (for disperse dyes, e.g. GB/T 5541 double-filter-paper test)
AgrochemicalsSuspensibility and dispersibility (CIPAC MT 184, MT 174)
Feed pelletsPellet durability index (ASAE S269 tumbling box, or Holmen tester)
Drilling fluidsRheology (yield point, gel strength) and filtrate loss of a test mud
BindersGreen and dry strength of test pellets or briquettes

Reading Results Correctly

  • Check the basis: “dry basis” and “as is” values differ by the moisture content.
  • Compare methods: lignosulfonate content and sugars depend strongly on the method used.
  • A TDS gives typical values; the COA gives batch results. Agree which values are the contract specification.

Frequently Asked Questions

How is lignosulfonate content measured?

Most often by UV absorbance of a diluted solution at around 280 nm against a reference material. Because the result depends on the reference, values from different methods should not be compared directly.

What tests confirm that a product is lignosulfonate?

A UV maximum near 280 nm, characteristic infrared absorptions (JECFA lists 1210–1220, 1037 and 655 cm-1), water solubility and insolubility in organic solvents.

Which tests matter for concrete use?

Reducing sugars, water reduction and setting time in a trial mix, because sugars and low-molecular-weight fractions retard cement.

References

Questions about a specification, a test method or a trial: contact us or email info@greenagrochem.com.